Keywords: Synchrotron, Tomography, 3D integration, 3D imaging, Slice and View, Plasma FIB, Diraction, Copper pillars, Hybrid bonding, Failure analysis

i Remerciements t9imeris ii en tout premier lieu remerier ten glude oyer et xiols vherE metD les deux direteurs suessifs du ervie de grtéristion des wtériux et gomposnts @gwgA u sein duquel s9est déroulée m thèseF weri de m9voir E ueillie dns e servieD où j9i énormément grndi et déouvert un domine qui me pssionneF te tiens à exprimer toute m grtitude ux memres de mon juryF weri à wro gntoni et à prnçoise eyrin d9voir epté de relire mon mnusrit et d9y voir pporté leurs ommentiresF weri églement à toeri he os et à vu lvo d9voir prtiipé à e juryD et tout prtiulièrement à vu d9voir epté d9en être le présidentF in(nD meri à innio gpri d9voir epté notre invittion à rejoindre e juryF v disussion menée durnt l soutenne été très stimulnteD et enrihie de vos ontriutions venues de milieux ien di'érentsF gette thèse n9urit ps été l même sns mon direteur de thèse et endrntD ierre fleuetD insi que prédéri vorutD qui oEendré e trvilF te tiens ii à les remerier hleureusement pour leur soutien u ours de es trois nnéesF ous vez su me lisser lire de poursuivre m thèse dns l diretion qui me pssionnit sns pour utnt que je me sente perdueF ous m9vez permis d9en fire réellement m thèseF ierreD meri pour tes explitionsD t ptienteD et ien sûr ton sens de l9humour et de l réprtie 3 te tiens ii enore une fois à remerier innioD pour s qulité de soutien ip F u nous s énormément idésD et s toujours été là pour me rendre l vie plus fileF ge trvil s9est déroulé u sein du gieD ve une ollortion forte ve l9ip et wiroeletronisF feuoup de personnes ont epté de jouer le jeuD de roire u projetD que e soit du ôté mtériu ou rtéristionF te les en remerie vivementF weri ux équipes de shHID shITeD et shIW pour leur ide et onseilsD et meri tout prtiulièrement à tulio h ilvD eter gloetensD wxime ruertD et wrie sngrid ihrd pour voir répondu à mille questions 3 n grnd meri pour votre disponiilité et votre ptieneF weri églement ux équipes intégrtion Qh du gie et de D et tout prtiulièrement à ndrine vhostis et téphne woreu pour leurs explitions et leur intérêt pour mon trvilF weri à emndine touveD prnk pournelD hierry wourier et xiols fresson d9voir répondu présents ux ppels ux dons d9éhntillons 3 weri églement à hvid fouhu pour toutes les disussions pssionnntes que l9on eues u oin du psfF it puisque l9on prle du psfD un grnd meri à quillume eudoit pour m9voir formée sur ette mhine et voir répondu à toutes mes questionsF weri u psf luiEmêmeD ve qui on prtgé des moments forts etGou prtiulièrement frustrnts 3 t9i ussi eu l9opportunité durnt e trvil d9endrer un exellent stgiireD ierre ylivier eutrnD que je remerie hleureusement ii pour son trvil et ette expériene enrihissnteF t9i eu l hne de fire m thèse dns un grnd lortoireD et i insi pu ôtoyer un grnd nomre de personnes d9horizons di'érentsF te tiens don ii à remerier toute l9équipe de l pxgD tous ronymes rres onfondusF weri pour les disussions en slle fé ou dns les ouloirsF weri tout prtiulièrement u groupe de thésrds et postEdosD insi qu9à he y0e of inD es trois nnées n9urient ps été les mêmes sns vous X eurèleD emndineD vyndD ristnD idourdD eudreyD wximeD vszloD vuisD itorD endreD tulienD voïD wrtinD onyD et émy @mis nous y reviendronsAF ineD meri pour les lundiD 9étit un moment fort de m semine 3 gonstntinD pour les petites disussions qui font du ienF sselleD un immense meri pour t préseneD ton soutienD et les puses fés virtuelles ou nonD ien méritées ou seulement néessiresF in(nD à tousD à très ientôt 3 n grnd meri à tout mon entourge d9voir été làD dns les moments funs et moins funsF weri à l rue ghenoiseD wnonD wrieD hilippeD et ernudD pour le onneuD le hr hD et le gp inexpliqué entre minuit et Sh du mtF wilieD meri d9être toiD meri d9être venue et meri d9être toujours làF n gigntesque meri à mes prentsD enn et qeorgesD qui me guident et me soutiennent de mnière exeptionnelleD et qui osent mintenir que 9est normlF weri à rugolndF e wthieuD mon frèreD pour les disussions toujours sns (nD mis prfois ve un sensF e uzyD pour t gentillesse et ton indulgene envers les jeux de motsF it à rugoD qui nous pporte à tous tnt de joieF in(nD meri à émyD qui su roire en moi u point de me onvinreF Introduction générale 5

1 Characterization for 3D integration 11

IFI owrds Qh integrtion F F F F F F F F F F F F F F F F F F F F F F F F F IP IFP yjets of interest F F F F F F F F F F F F F F F F F F F F F F F F F F F F IS IFPFI hrough ilion i @A F F F F F F F F F F F F F F F F F F F IT IFPFP ferEtoEwfer @PA onding F F F F F F F F F F F F F F F F F IT IFPFQ gopper pillr @guA F F F F F F F F F F F F F F F F F F F F F F F IV IFQ ghrteriztion methods F F F F F F F F F F F F F F F F F F F F F F F F PH IFQFI ghrteriztion needs F F F F F F F F F F F F F F F F F F F F F F PH IFQFP trin mesurement method F F F F F F F F F F F F F F F F F F F PH IFQFQ smging methods F F F F F F F F F F F F F F F F F F F F F F F F F PH
F F F F F F F F F F F F F F F F F PR PFP oures of eletrons nd ions F F F F F F F F F F F F F F F F F F F F F F PT PFPFI iletron guns F F F F F F F F F F F F F F F F F F F F F F F F F F F PT PFPFP son guns F F F F F F F F F F F F F F F F F F F F F F F F F F F F F F PV PFQ yjetsGmtter intertions nd pplitions F F F F F F F F F F F F F QH PFQFI willing F F F F F F F F F F F F F F F F F F F F F F F F F F F F F F F QP PFQFP wtter deposition F F F F F F F F F F F F F F F F F F F F F F F F QS PFQFQ smging F F F F F F F F F F F F F F F F F F F F F F F F F F F F F F QS PFR epplitions of poused son fem mirosopes F F F F F F F F F F F F QU PFRFI lie nd iew proedure F F F F F F F F F F F F F F F F F F F F QU PFRFP mple preprtionX liftEout proedures F F F F F F F F F F F F RH 3 X-ray imaging methods 45 QFI ilements of xEry physis F F F F F F F F F F F F F F F F F F F F F F F F RT QFIFI ytining n xEry em F F F F F F F F F F F F F F F F F F F F RT QFIFP EryGmtter intertions F F F F F F F F F F F F F F F F F F F F SQ QFP ixperimentl setups F F F F F F F F F F F F F F F F F F F F F F F F F F F SU QFPFI shITeX nnoEtomogrphy emline F F F F F F F F F F F F F F SV QFPFP shIWX verstile tool for oherent imging nd di'rtion F F TH QFPFQ shHIX vol strin mesurement F F F F F F F F F F F F F F F F TI QFQ Ery trnsmission Qh imging F F F F F F F F F F F F F F F F F F F F F TP QFQFI Ph imge formtion F F F F F F F F F F F F F F F F F F F F F F F TP QFQFP ytining Qh reonstrution F F F F F F F F F F F F F F F F F UH QFQFQ mple reprtion F F F F F F F F F F F F F F F F F F F F F F F UR QFR trin mesures y frgg di'rtion F F F F F F F F F F F F F F F F F F UT QFRFI wonohromti frgg hi'rtion F F F F F F F F F F F F F F F F UT QFRFP he shHI work)ow F F F F F F F F F F F F F F F F F F F F F F F F UV QFRFQ mple reprtion F F F F F F F F F F F F F F F F F F F F F F F VP 4 Development of 3D imaging in a single column PFIB 85 RFI eutomtion of the dt quisition F F F F F F F F F F F F F F F F F F F VT RFIFI he ipst softwre F F F F F F F F F F F F F F F F F F F F F F F F VT RFIFP ht quisition work)ow F F F F F F F F F F F F F F F F F F F F VV RFP ht postEproessing F F F F F F F F F F F F F F F F F F F F F F F F F F F WR RFPFI glultion of the tul sliing step F F F F F F F F F F F F F F WT RFPFP lies registrtion F F F F F F F F F F F F F F F F F F F F F F F F F WT RFPFQ olume reEsmpling F F F F F F F F F F F F F F F F F F F F F F F WV RFQ esults F F F F F F F F F F F F F F F F F F F F F F F F F F F F F F F F F F F WW RFR vimits of the tehnique nd possile improvements F F F F F F F F F F IHR RFS gonlusion F F F F F F F F F F F F F F F F F F F F F F F F F F F F F F F F F IHU 5 Contribution to the ID16A workow for 3D integration 111 SFI yriginl shITe work)ow F F F F F F F F F F F F F F F F F F F F F F F F F IIP SFP xew smple preprtion sheme F F F F F F F F F F F F F F F F F F F F F IIR SFPFI xew smple supports F F F F F F F F F F F F F F F F F F F F F F F IIS
SFPFP wking the most of the smple preprtion nd instlltion F IIS SFQ edution of the numer of projetions F F F F F F F F F F F F F F F F F IPQ SFR eutomtion of the postEproessing F F F F F F F F F F F F F F F F F F F IPT SFS ime gin nd disussion F F F F F F F F F F F F F F F F F F F F F F F F IPV SFT epplition to Qh integrtion imging F F F F F F F F F F F F F F F F F IQH SFTFI smging of lrge numer of postEeletromigrtion smples F IQH SFTFP worphology study on opper pillrs F F F F F F F F F F F F F F F IQQ SFTFQ owrds lrger (eld of view F F F F F F F F F F F F F F F F F F IQU SFU gonlusion F F F F F F F F F F F F F F F F F F F F F F F F F F F F F F F F F IQW 6 Local strain measurements in stacks 143 TFI ryrid onding stk strin mesure in silion F F F F F F F F F F F F IRR TFIFI imultneous oservtion of two silion lyers F F F F F F F F F IRR TFIFP trin mps nd morphology orreltion F F F F F F F F F F F F IRT TFP hiret onding inEsitu strin mesure in opper

F F F F F F F F F F F F IRV TFQ gonlusion F F F F F F F F F F F F F F F F F F F F F F F F F F F F F F F F F ISI

General introduction

sn the miroeletronis industryD one of the min res of interest for development hs eenD in the lst SH yersD to redue the size of the deviesD t every sleF o frD the min strtegy to do so hs een to redue the size of the trnsistorsD whih triggered the redution of the onnetions sizeF his llows to inrese the trnsistors densityD redue the devie footprintD nd therefore to inrese the glol performnes of the devieF ody howeverD we fe the limits of this miniturE iztionD oth euse the trnsistors size rehes physis limits nd euse the orresponding onnetions length inreses the toule heting too muhD inresing the signl propgtion timeF o overome this issueD nother geometry for miroeletroni devies hs een developedD sine the IWVHsF st relies on stking the dies in the vertil diretionD insted of setting them next to one notherF his tehnologyD lled Qh integrtion @QhiAD llows oth for the redution of onnetion length nd the glol devie footprintD without reduing the trnsistors sizeF es suhD it hs een of growing interest in the lst ten yersD oth in the demil nd industril ommunities IF pigure I on(rms this trendX the numer of rtiles nswering to the keywords 4Qh integrtion4 nd the typil ojets it fetures hs een onstntly inresing sine the IWVHsF pigure IX xumer of rtiles per yer nswering to the keyword 4Qh integrtion4 or keywords onneted to Qh integrtionD suh s 4ryrid onding4D 4hiret onding4D 4opper pillrs4D 4opper umps4D 4opper pillrs4D nd 4through silion vis4D s found in the opus dtse @https: //www.scopus.comA his new diretion of development rises new di0ultiesF he geometry eing di'erent from previous tehnologiesD new onnetions hd to e designedF emong themD hrough ilion is @sA llow for onnetions etween two sides of given wfer or dieD nd hve een widely investigtedF heir frition proess is tody mostly msteredD nd the mehnisms tht govern it re wellEknownF o onnet dies nd wfers togetherD other ojetsD suh s opper pillrs or hyrid ondingD re usedF hey re still under developmentD nd their hrteriztionD e it eletrilD mehnilD of morphologilD is of high vlue for the proess nd filure nlysis ommunitiesF e here fous on those spei( ojetsD nd more preisely on severl miron wide opper pds nd severl tens of miron wide opper pillrsF iletril or mehnil filure tests llow to otin informtion out the glol funtioning of the devieD ut do not provide informtion out the origin of filureF smgingD on the ontrryD provides informtion out the morphology of the devieD tht n e linked to its further ehviorF sn prtieD the oservtion of defets @voids for exmpleA t the interfe of wfer to wfer onding is ruil for the monitoring of the onding proess nd redue the risk of filureF uh studies neessitte routine imging proessD whih llow to otin esy to proess sttistil informtionF glssillyD in the (eld of miroeletronisD suh morphologil hrteriztions n e performed on iws @nning iletron wirosopesA or iws @rnsmisE sion iletron wirosopesAF roweverD s the geometry of the oserved ojets is not the smeD lssil imging methods must e dptedF sn ftD the imging of Qhi devies is quite demndingD due to severl resonsF @iA he ojets to hrE terize re in three dimensionsF elthough they o'er high reoslution informtion @up to the nnometer for iw nd the ngstrom for iwAD eletron mirosopes only provide informtion on very thin lyer @less thn IHH nmA of the smpleF Qh imging method therefore hve to e set in pleF @iiA Qh imging methods exist nd re pplile to the industryF st is the se for exmple of l xEry tomoE grphsF roweverD their resolution is often limited to the mirometerD minly euse of their soure sizeF sn the se of Qh integrtion ojetsD the serhed defets n e s smll s severl nnometersD nd most of them re severl tens of nnometers lrge PF he imging tehnique must therefore provide resolution tht is omE ptile with those dimensionsF @iiiA es mentioned eforeD the investigted ojets re quite igD up to severl tens of mirometersF righ resolution lol tehniquesD suh s eletron tomogrphyD require SH nm wide smplesD nd therefore nnot e ppliedF psfGiw @poused son fem G nning iletron wirosopeA lie nd iew tehniquesD re often limited to smples of IH µm in widthD nd therefore reh their limits in the se of Qh integrtion ojetsF @ivA hue to the industril ontext of the studyD the hosen tehnique should e le to provide sttistil informtionF his implies either n even lrger (eld of viewD or n utomted imging proessF wore generllyD the hosen tehnique should e s utomti nd fst s possileD nd provide esyEtoEproess dtF he gol of the work presented here is to develop new hrteriztion tehE niquesD wellEsuited for Qh integrtion imgingF he fous is set on the morphology nd di'rtion imging of oth to opper pillrs nd pdsF e here im t deE veloping those Qh tehniquesD for them to eome routine tools for Qh integrtion hrteriztionF o do soD lrge (eld of view @IHH µmA hs to e omined with high resolution @`IHH nmAD nd the omplete work)owD from the smple prepE rtion to the postEproessingD must e mde s utomti s possileF his work is losely linked to industryD nd the onduted experiments were dpted to the smples under onstnt developmentF st is however quite explortoryD s it ene(ts from very reent tehniquesD whih were often not originlly ment for utomtion nd industril pplitionF he min tehniques investigted here hve een developed in the lst few yersF hey inlude the shITe nd the shHI emlines from the ip @the iuropen ynE hrotron dition pilityAF foth were uilt during the (rst phse of the ip upgrdeD tht lst from PHHW to PHISD nd ene(t from stteEofEtheErt tehnologies from vrious (eldsD inluding xEry optisD detetorsD lrge dt proessing lustersD nd engineeringF he shHI emline o'ers the possiility for nnoEdi'rtion imgE ing of lrge smples @IHH µm in widthAD providing lol strin informtionD sine the em o'ered on this emline n e foused down to PHH nmF ixperiments hve een onduted on this emlineD showing it possiilities for lrge re lol strin mesurementsF he shITe emline is the (rst hrd xEry emline dediE ted to nnoEtomogrphyF st ims t Qh resolutions down to SH nmD for smples elow IHH µm in widthF he min work presented here hs een onduted on this emlineD with the gol to dpt it to industry sttistil imging needsF e third ip emlineD lredy wellEestlished for industril needsD hs lso een investigtedX on the shIW emlineD tomogrphy nd lminogrphy were rried outF he preprtion of the smples ws mde possile y psf @lsm poused son femAF uh mhines hve een ommerilly ville only for the lst few yersF huring this workD Qh imging tehniques hs lso een developed on the sme mhineD originlly only designed for smple preprtionF his hh thesis widely ene(ts from rnd new smples nd hrteriztion tehniquesF he ess to suh equipments ws mde possile y the spei( ontext of this workF st ws in ft relized in the frme of the s 1 xnoeleD nd more spei(lly inside the Grands instruments progrmF his progrm ims t ringing lrge instruments suh s synhrotrons @nd more preisely here the ipA loser to industril needsF sn prtiulrD three tors took prt in this workX the gie visD the ipD nd wiroeletronisD ll loted ner qrenoleD s presented in pigure PF he results presented here were otined in the frme of n iv @innovtionEled vong erm rojetA funded y ollortion etween those three torsF his iv ensured synhrotron em time on three emlines @shITe for UI7D shIW for IU7D nd shHI for IP7A during the time of the hh thesisF his very vlule essD together with rnd new smples nd the equipments of the pxg 2 D mde this work nd the results it led to possileF he (rst three hpters re dedited to the ontext of this workF sn (rst hpterD generl priniples of Qh integrtion re presentedD together with the ojets of interest minly studiedF he fous is set on the hrteriztion needs of suh pigure PX sndustril nd demil tors involved in this workX the ipD gie visD nd wiroeletronisF ojets nd the possile nswersF e seond hpter is dedited to eletron nd ion sed mirosopesF heir ommon nd spei( working priniples re presentedD together with two of their pplitionsD used during this hhF sn hpter QD the xEry hrteriztion methods used in the frme of this work re desriedF v nd synhrotron soures nd experimentl setups re depitedD oth for imging nd strin mesurementsF he next three hpters im t presenting the min results otined during this hhF sn hpter RD the development of the psfGpsf lie nd iew imging is detiledD presenting oth the utomtion of the dt quisition nd the postE proessingF e disussion out the possiilitiesD limitsD nd possile improvements of suh setup is providedF ghpter S is dedited to the shITe emlineD on whih most of the experiments nd developments were ondutedF he originl work)ow of the emline is presentedD together with strtegies iming t mking this emline routine tomogrphy tool for the industryF e glol disussion is led on the time sved using the proposed work)owD followed y seleted pplitions relized on the shITe emlineF ghpter T presents two studies relized on the shHI emlineD respetively otined on two silion lyers of stkD nd on fullEsheet opper lyerD performed oth t room temperture nd t RHH • gF pinllyD summry of the work done in the frme of this hh is providedD together with glol ssessment of the tehniques developed or usedF erspetives for routine hrteriztion of Qh integrtion devies re proposed for further workF hns l9industrie de l miroEéletroniqueD l9ugmenttion des performnes des omE posnts s9est fiteD durnt les SH dernières nnéesD pr l diminution de leur tilleF in prtiulierD el psse pr l diminution de l tille des trnsistorsD e qui enE trine l rédution de l tille de toutes les onnetionsF he ette mnièreD l densité de trnsistors ugmenteD réduisnt l tille glole du omposnt et l longueur de hque onnetionD ugmentnt lors les pités de l9ppreilF eujourd9hui epenE dntD ette ourse à l minituristion tteint ses limitesF in e'etD l tille des trnsistors tteint les limites de l physiqueD et l longueur glole des onnetions est telle que l9e'et toule dns le omposnt devient trop importnt et limite le temps de propgtion de l9informtionF e(n de répondre à es di0ultésD une nouvelle géométrie pour les omposnts miroEéletronique se développe depuis les nnées IWVHF sl s9gitD non plus de pler les éléments d9une même pue les uns à ôté des utresD mis de les empilerF gette tehnique est ppelée intégrtion Qh @QhiAF ille réduit à l fois l longueur des onE netions et l9empreinte u sol du omposnt (nlD sns réduire l tille du trnsistorF eu ours des IH dernières nnéesD ette tehnique ggné en intérêt et populritéD à l fois dns les mondes industriel et démique IF v pigure Q souligne ette tendneD puisqu9elle montre que le nomre d9rtiles puliés omportnt le mot lé 4Qh integrtion4 ou un motElé ssoié est en onstnte ugmenttion depuis IWVSF pigure QX xomre d9rtiles pr n omportnt le mot lé 4Qh integrE tion4 ou des mots lés ssimilés @4gopper pillrs4D 4hyrid onding4D 4diret onding4D 4hrough ilion is4AD selon l se de données opus @https: //www.scopus.comA fien qu9pportnt des réponses tehnologiques intéressntesD ette nouvelle diE retion de développement pporte ussi de nouvelles di0ultésF in e'etD l géométrie utilisée en intégrtion Qh étnt nouvelleD de nouveux types de onnetions ont du être développésF ves @hrough ilion isAD qui onnetent deux fes d9un même wfer ou d9une même pueD ont notmment fit l9ojet de nomre d9étudesF eujourd9huiD leur proédés de frition insi que les ménismes les ommndnt sont pour l pluprt onnus et mîtrisésF h9utres ojetsD tels les piliers de uivre @ou guA et les pds de uivreD sont utilisés pour onneter életriquement et méniqueE ment les wfers et puesF ges ojets sont ujourd9hui en ours de développementD et leur rtéristion est don d9un grnd intérêtD qu9elle soit életriqueD méniqueD ou morphologiqueD à l fois pour mieux omprendre les ménismes qui se produisent pendnt leur fritionD et pour limiter l défillne du produit (niF hns ette étudeD nous nous intéressons en détils à es ojetsD et plus prtiulièrement ux pds de uivre de quelques miromètres de lrgeD insi qu9ux opper pillrs de quelques dizines de miromètres de dimètreF our rtériser de tels ojetsD des tests életriques et méniques peuvent être rélisésF 9ils permettent d9otenir une informtion sur l (ilité du omposntD ils ne fournissent que peu d9informtions sur l9origine d9une éventuelle défillneF v9imgerie qunt à elle permet d9otenir une informtion sur l morphologie de hque ojetD elleEi pouvnt être orrélée à son fontionnementF in prtiqueD l9oservtion de trous à l9interfe de ollge entre deux pds de uivreD ou u sein de piliers de uivre est ruile pour le suivi du proédé de ollgeF our être pertinentes sur le long termeD de telles études doivent fournir une informtion sttistique et don être rélisles de mnière routinièreF in miroEéletroniqueD l rtéristion morphologique est ommunément rélE isée pr mirosopie életroniqueD sur un mirosope életronique à lyge @wifA ou à trnsmission @wiAF gependntD l tehnique de rtéristion doit s9dpter à l géométrie de es nouveux ojetsF in e'etD l9imgerie de omposnts utilisés dns l9intégrtion Qh est ssez ontrignnteD et e pour plusieurs risonsF @iA ves tehniques telles que le wif et le wiD ien qu9tteignnt de hutes résolutions @quelques nnomètres et quelques ngstromsD respetivementA ne fournissent qu9une informtion onernnt une file épisseur de l9éhntillonD typiquement moins de IHH nmF ves ojets onsidérés sont ependnt tridimensionnelsD et l tehnique de rtéristion doit don l9être églementF @iiA hes méthodes d9imgerie QhD telles que les tomogrphes de lortoireD existent et peuvent être ppliquées à l9industrieF gependntD leur résolution est ujourd9hui souvent limitée u miromètreF hns le s de l9intégrtion QhD les défuts reherhés mesurent typiquement quelques dizines de nnomètresD les plus petits fisnt jusqu9à quelques nnomètres PF v tehnique d9imgerie doit permettre d9otenir de telles résolutionsF @iiiA gomme mentionné préédemmentD les ojets oservés sont reltivement grnds X ils peuE vent mesurer quelques dizines de miromètresF hes tehniques d9imgerie Qh à hute résolutionD telles que l tomogrphie életronique pr exempleD imposent des éhntillons de moins de SH nm de dimètreD et ne s9ppliquent don ps iiF hes tehniques destrutives de type lie nd iewD implémentées dns un psfGiwD sont qunt à elles souvent limitées à des régions d9intérêt de IH µm de ôtéF illes tteignent don églement leurs limites iiF @ivA hu fit du ontext industriel de ette étudeD l tehnique d9imgerie hoisie devr fournir des informtions sttisE tiquesD soit à trvers un hmp de vue lrgeD soit grâe à un proédé utomtiséF lus générlementD il est ruil que l9informtion otenue le soit de mnière ussi utomtique que possileD et soit filement exploitleF ve ut de e trvil de thèse est de développer de nouvelles méthodes d9imgerie QhD dptées à l9intégrtion QhF ves prinipux ojets étudiés sont les piliers et les pds de uivreD et le développement ser orienté vers une utilistion routinière et utomtique des tehniques de rtéristionF gomme expliqué préédemmentD ei requiert une tehnique d9imgerie Qh ssoint un lrge hmp de vue @IHH µmA à une hute résolution @`IHH nmAD et dont le proédé d9nlyse ompletD llnt de l préprtion d9éhntillon u résultt (nlD peut être utomtiséF ge trvil été rélisé à des (ns industriellesD et les expérienes rélisées ont été dptées à des éhntillons en onstnte évolutionF sl s9git de e point de vue d9un trvil ssez explortoireD d9utnt plus qu9il est sé sur des tehniques très réentesD qui n9ont souvent ps pour ut originel une utilistion routinièreF ves priniples tehniques étudiées dns e trvil dtent de seulement quelques nnéesF rmi ellesD les lignes de lumière shITe et shHI de l9ip @iuropen ynhrotron dition pilityAD ont été onstruites durnt l première phse du progrmme 4pgrde4 de e synhrotronD qui eu lieu entre PHHW et PHISF illes éné(ient don des dernières vnées fites dns de nomreux dominesD qui ont fourni pr exemple de nouvelles optiques pour les ryons D des déteteurs rpiE desD une puissne de lul pouvnt gérer de grndes quntités de donnéesD ou des moteurs ultrEpréis pour le positionnement des éhntillonsF qrâe à un fiseu pouvnt être folisé jusqu9à PHH nmD l ligne shHI o're l possiilité de mesurer lolement les déformtions dns de grnds éhntillons @des zones d9intérêt de IHH x IHH µm 2 peuvent être oservéesAF hurnt ette thèseD il été possile de réliser des expérienes sur ette ligneF v ligne shITe est l première ligne de ryons durs dédiée à l nnoEtomogrphieF ille vise une résolution Qh de moins de SH nmD pour des éhntillons pouvnt ller jusqu9à IHH µm de dimètreF v pluE prt des expérienes rélisées durnt ette thèse ont été fites sur ette ligneD ve pour ut de l9dpter ux esoins de l9industrieF hes mesures ont églement été rélisées sur une troisième ligne de lumière de l9ipD shIWD plus nienne et orienE tée vers l9industrieF ille o're l possiilité d9quérir des données de tomogrphie et de lminogrphieF v préprtion des éhntillons été rélisée u sein d9un psf @lsm poused son femAD qui est une mhine ommerilisée depuis seulement quelques nnéesF ne tehnique d9imgerie lie nd iew ussi été développée dns e psfD originellement prévu pour l préprtion d9éhntillonsF gomme on peut le voirD des éhntillons et des tehniques de rtéristion de dernière génértion ont été essiles durnt ette thèseD grâe à un ontexte prE tiulierF ille en e'et été rélisée dns le dre du progrmme Grands Instruments de l9s @snstitut de eherhe ehnologiqueA xnoeleD qui vise à rpproher les grnd instruments tels que les synhrotrons @et en prtiulier l9ipA du monde de l9industrieF hns e dreD un iv @innovtionEled vong erm rojetA été monté pr trois teurs X l9ipD le gieD et wiroeletronisD tous situés dns les environs de qrenole @voir rte en pigure RAF ge iv grntit un temps d9ès ux trois lignes de lumières présentées préédemment X UI7 du temps été lloué à shITeD IU7 à shIWD et IP7 à shHIF get ès privilégié à l9ipD insi que l9utilistion des équipements de l pxg @lteporme de xnogrtéristion du gieAD ont permis d9otenir les résultts présentés dns e mnusritF pigure RX ves teurs @démiques et industrielsA impliqués dns e trvil X le gieD l9ipD et miroéletroniqueF ves trois premiers hpitres de e mnusrit présentent le ontexte de e trvilF n premier hpitre introduit les prinipes de l9intégrtion QhD et les prinipux ojets étudiésF veurs esoins en termes de rtéristion et les réponses possiles sont déritsF hns un seond hpitreD les mirosopes életroniques et ioniques sont présentésF veurs prinipes de fontionnement ommuns et spéi(ques sont déritsD insi que deux pplitions possilesD utilisées durnt ette thèseF in(nD les tehniques de rtéristion pr ryons utilisées dns le dre de e trvil sont présentées dns le hpitre QF ves soures de ryons de lortoire et synhrotron sont détilléesD de même que les dispositifs expérimentux permettnt l9imgerie et les mesures de déformtionsF ves trois hpitres suivnts présentent les prinipux résultts otenus pendnt e trvil de thèseF ve hpitre R est dédié u développement de l9imgerie Qh pr lie nd iew u sein d9un psfF v9utomtistion de l9quisition elleEmêmeD insi que le postEtritement des donnéesD sont déritsF ves possiilitésD limitesD et éventuelles méliortions futures d9un tel dispositif sont détillésF ve trvil mené sur shITe est présenté u hpitre SF ve proédé omplet originl y est détilléD insi que les di'érentes strtégies mises en ple pour fire de ette tehnique une méthode d9imgerie routinière pour l9industrieF ne disussion est menée sur le temps ggné pr l9utilistion de es strtégiesF uelques exemples d9pplitions sont donnésD supportés pr des résultts otenus pr d9utres moyens d9imgerieD à des (ns de omprisonF ve hpitre T illustre les possiilités de l ligne shHI pour l9intégrtion Qh u moyen de deux étudesD visnt respetivement à oserver les déformtions dns les ouhes de siliium d9un empilement fontionnelD et à mesurer les déformtions dns une ouhe de uivre pleine plqueD prévue pour du ollge diretF in(nD une onlusion reviendr sur tous les résultts otenus u ours de e trvilD ve pour ut l9évlution des di'érentes tehniques utiliséesF uelques perE spetives onernnt l rtéristion ppliquée à l9intégrtion Qh seront présentées et disutéesF eny miroeletronis devie is sedD on the smllest sleD on trnsistorsD tht n e s smll severl tens of nnometersF prom this sle to the mrosopi one we re le to mnipulteD severl intermedite ojets ply roleD suh s diesD hipsD nd pkged integrted iruits @sgAF he ltter usully ontins dieD pled inside plsti pkgingF he die itself is piee of silion wfer on whih network of trnsistorsD resistorsD pitorsD is fritedF he network itself is mde of gold or opper nd is usully edited on the hip itselfF rnsistorsD whih re the very se of miroeletronisD re omponents tht regulte the urrent or voltge )ow in the iruitD nd n therefore tD when omined togetherD s logil gtesF e omplex network of onnetionsD with lrge vriety of sptil slesD onnets the trnsistorsD tht n e s smll s severl tens of nmD to the (nl pkgeD whih is severl entimeters lrgeF o limit the size of the whole hipD the min strtegy sine the IWUHs hs een to derese the size of the trnsistors themselvesD together with their onnetionsF sn IWUID the (rst miroproessor ontined PQHH trnsistorsD while in PHIH the numer of trnsistors on miroproessor ws out 10 9 F fetween those two dtesD the expnsion ws exponentilD s the numer of trnsistors per miroproessor hs douled every P yers E this is the soElled woore9s lwF his ws mde possile minly y the improvement of preision in iruit editingF roweverD this strtegy rehes its limitsD nd woore9s lw is sid to e impossile to follow y PHPHF here re severl resons for thtF pirstD s the (nl trnsistors eme smllerD the onnetions eme thinner nd more numerousF his rose issues regrding toule hetingD inresing the resistivity of the onnetions nd thus the signl propgtion timeF his is tody nswered y new mterilsD suh s opper onnetions insted of luminum onesD nd lowEk mterils repling the Si0 2 insultorF woreoverD the minituriztion of trnsistors itself rehes its limitsF sn ftD lthough trnsistors of W nm hve een shown to work QD some of the mnufturing steps re impossile to hieve in n industril ontextF woreoverD from quntum physis point of viewD the minituriztion is ssessed to reh its limits y PHQT RF 1.1 Towards 3D integration yne pth for further development of miroproessors is therefore to inrese the density of trnsistorsD while limiting the onnetions lengthD whih will llow for redution of the power onsumptionF he glol footprint of the iruit is to e tken into ount s wellF es the diret diminution of trnsistors size is not solution nymoreD new geometry of the glol iruit is to e developedF o some extentD ystems on ghips @ogA nswer the prolem of the onnetion lengthD s they onentrte severl types of elements on single hipX the onnetions re therefore shorter @see left hnd side of pigure IFIAF roweverD the issue of onnetions etween dies still reminsD so does the footprint nd power onsumptionF pigure IFIX riniple of Qh integrtionF sn ogD heterogeneous strutures re present on single hipF his llows to redue the length of onnexionsF o further redue the onnetionsD nd limit the footprint s wellD Qh integrtion is eing developedF Image source: http: //www.athenis3d.eu/technology.php he kge on kge @oA is good strtegy to nswer those needs @see right hnd side of pigure IFIAF st relies on vertil onnetions etween dies inside the sme pkge or hipF hey llow for gin of footprintD while llowing for the stking of heterogeneous units inside pkgeF wo onding systems re used tody inside suh deviesX the wire onding nd the )ipEhipD oth illustrted in pigure IFPF he wire onding simply uses wires @usully mde of opper or goldA to onnet one prt of the upper die to nother prt of the lower die inside the pkgeD while the )ipEhip tehnique relies of the rottion of the upper hipD in order for its tive lyer to fe the tive lyer of the lower hipF he onnetion is mde using solder umps or llsD whih n e mde of n lloy of n or negF hose two tehniques n e ominedD s illustrted in pigure IFPD nd n redue the interonnetion length y RH7 in R tive lyer stk SF pigure IFPX smges of two onding tehnologies used in the ystem in kge A wire onding @imge soureX TA A )ipEhip @imge soureX httpX GGwwwFtreskyFomA F A hemti of the two tehnologies used together @imge soureX eletronisFstkexhngeFomAF his (rst Qh geometryD lled Qh sg pkgingD pves the wy for tul Qh inteE grtionF he pssge ws mde possile y the development of hrough ilion is @A TF hose ojetsD (rst imgined in IWSTD re tody of high interestF hey re severl tens of miron lrge ylindersD (lled with opper or tungstenD nd going through n entire thinned wfer in the vertil diretion @up to IHH µmAF es suhD they llow for n eletri signl to ross the wferD mking vertil ommunition possileF Qh integrtion n e seprted into Qh sg integrtionD where dies re stked togetherD using oth s nd solder umpsD nd Qh i integrtionD where wfers re onded together using onlyF pigure IFQ o'ers n overview of Qh pkging nd integrtion tehnologiesD with their use of s nd their mturity in PHIRF Qh pkging is tody ommerilizedD espeilly for moile pplitions suh s smrtphones nd tletsD while Qh integrtion is tody still in development phse UF everl miroeletronis industry tors re urrently working on Qh sg integrE pigure IFQX A Qh integrtion tehnologies nd their mturity regrding industry in PHIRF Image source: [6]F A gross setion view of the ony imging sensor ontining sF sn this stkD s ensure the onnetion etween the top nd ottom lyersF @smge soureX VAF A gross setion of msung hhR hewD with s onneting opposite sides of dies nd pillrs onneting dies together @ smge soureX WAF tion ID nd some ommerilized devies lredy ontin s IHF ony relesed in PHIQ n imging sensor sed on sD where the onding itself ws mde y diret SiO 2 /SiO 2 diret ondingD s n e seen in pigure IFQ VF uh senE sor llows for the signl proessing unit to e loser to the pixelsD nd therefore to otin etter imgesF st is tody used in ony peri s smrtphones for exE mpleF sn this devie howeverD s onnet eletrilly two lyers of the stkD nd not two fes of the sme wferF purther development of Qh integrtion leds to eletril onnetions t the interfe itselfD using hyrid onding for exmpleD s will e desried in setion IFPF Qh integrtion hs lso een implemented for other pplitionsD suh s high performne omputing unitsD in whih digitl nd nlog funtions of produt re mnuftured seprtely nd onneted with opE per pillrs nd s IIF hynmi ndom eess wemories @hewA were lso investigted IPD nd re lredy ommerilized y msungD in the TR q hhR modelD illustrted in pigure IFQ WF hen ompred to Qh pkgingD it is ler tht Qh integrtion o'ers higher eletril performnesD lower power onsumption due to shorter onnetionsD higher density nd lighter weightF he two tehnologies re however omplemenE try nd n e pplied together UF rere we fous on Qh sg integrtionD s it rises most hllenges todyF xext setion is dedited to the desription of sevE erl ojets of interest used in Qh sg integrtion nd thoroughly nlyzed during this hhF he issues they feD together with their hrteriztion needsD will lso e disussed IQF sn seond setionD onventionl hrteriztion methods will e ssessed in the se of Qh integrtionF ghrteriztion methods proposed nd developed during this hh thesis will e introdued nd their use justi(edF 1.2 Objects of interest es mentioned previouslyD Qh integrtion relies on the stking of dies or wfers in the vertil diretionF he onnetions etween two fes of die or wfer re mde y sF he onding is lled fer to fer nd noted PF st n e performed y using n dditionl mteril etween the surfesF his indiret onding n e performed using polymerD or euteti lloyF st n lso e mde with no intermedite lyer etween metlsD oxidesD or dieletrisF st is then lled diret onding IRF ryrid onding will our when diret onding is performed on surfe ontining two types of mterilsD for exmple metl nd dieletri PF sn the se of Qh sg integrtionD the onnetions etween dies re performed t di'erent slesD depending on the level of the onnetionF older lls re pled lose to the sustrteD while smller solder umps re situted further wyF o improve oth the density nd the qulity of onnetionsD opper pillrsD lter noted gups hve een developed for upper levelsF sn this setionD insight will e given into some spei( ojets of interest used in Qh integrtionF will e rie)y desriedD s they ply huge role in Qh integrtionD lthough they were of little onern during this hhF qolsD frition proessesD nd hrteriztion needs will e provided for diret nd hyrid ondingD s well s for opper pillrsF his setion voluntrily ontins very generi informE tion out proesses nd fetures of interest inside the ojetsF hen neededD more spei( informtion will e provided long the mnusript out the mnufturing proess of given smples nd their hrteriztion needsF e word will e given out how the smples n e hndled fter the mnuftureD s this will hve n impt on possile hrteriztion nd on smple preprtionF 1.2.1 Through Silicon Via (TSV) hrough ilion is @sA re high form ftor @or depth to dimeter rtioA strutures inside silion wferF fsillyD they re severl µm wide ylindril holes in the wferD (lled with ondutive mteril suh s opper or tungstenF hepending on their role inside the iruitD their shpe nd (lling mteril di'erF heir dimeter rnges from Q to VH µmD while their form ftor rnges from I @for lrge A to up to IH @for smller onesAF heir mnufturing proess is tody wellEunderstoodD nd they were not studied in this workF 1.2.2 Wafer-to-wafer (W2W) bonding hiret nd hyrid onding re wfer to wfer onding tehniques with no use of dditionl onding lyerF o hieve good qulity ondingD the surfe my e polished using gw @ghemil wehnil olishingA efore ondingD nd the ondE ing n e ssisted y thermoEompressionF snside iruitD diret onding n link opper pds togetherD s illustrted in pigure IFRF huring this hhD widely studied onding type is the hyrid ondingD whih onds metl pds nd dieletri mteril @Si0 2 A res togetherD s illustrted in pigE ure IFRF wore spei(llyD disyEhin strutures were studiedF hey re eletril test struturesD tht rete k nd forth onnetions etween two levels of the stkD using S µm wide opper pds nd vi mtriesD s illustrted in pigure IFRF yne possile mnufture proess for hyrid onding pds is presented in pigure IFSF everl hllenges our during this proessF e (rst onsidertion is tht for ptterned struturesD pds must e wellEligned to mximize the urrent )owF his lignment must therefore e ontrolled ITD IUF purthermoreD voids n pper t the onding interfeD for two min resonsF pirstD the opper n ontin vnies in its strutureF huring the re)owD those vnies migrte nd ggregteD reting voidsF e seond origin is in the proess itselfF e smll lyer of oxide n pper on the wfers surfesD efore the ondingF his will lso generte voids IVD IWF uh voids re illustrted in the se of fullEsheet guEgu onding nd opper pd in pigures IFT nd IFTD respetivelyF heir size rnges from severl nnometersD up to severl tens of nnometers PF gontrry to notEonded res of wfersD in the se of smll voids the onding still exists nd provides n eletril nd mehnil onnetionF es the smllest onnetions t this level re QSH nm wide visD voids pigure IFTX A iw imge of voids t the interfe of fullEsheet guEgu ondingD otined with iw PHY A iw imge of voids @in lkA t the interfe etween two opper pds PIF A nning eousti wirosope @ewA imge from whole QHH mm wferF he white res re illEonded smller thn SH nm re unlikely to e n issueF st is however of gret importne to monitor their sizeD in order to ssess new frition proessesF hen they exit the mnufturing proessD smples re still QHH mm lrge wfers stked togetherF wost of the timeD the upper wfer is thinned down to thikness of Q to IH µmF he ottom wfer is USH µm thikF he wfers n e swn nd leved quite esilyD nd n undergo psf @lsm poused son femA smple preprtionF 1.2.3 Copper pillar (CuP) gonnetions etween hips re mde y solder umpsD llsD or opper pillrs @gusA PPF imilrly to sD their shpe nd size vries ording to their posiE tion in the stk nd their purposeF sn this studyD the fous hs een set on opper pillrsD whih re opper ylinders of typilly IH to SH µm in dimeterD surmounted y n lloy usully mde of opperD silverD nd tin @lled eg for negguAD s illustrted in pigure IFUF ine their mterils ehvior still rises questionsD espeE illy in the se of smller gus @IH µmAD their morphologil hrteriztion is tody of high importneF pigure IFUX iw ro(le view of PH µm wide opper pillrF everl frition proesses oexist when it omes to opper pillrs PQD PRD nd one of them is illustrted in pigure IFVF gopper nd neggu lloys re usully deposited y eletrodeposition in regions delimited y resinD reting ylinders @the neggu lloy eing deposited on top of the opperAF he resin is then removed hemillyD nd re)ow gives the (nl opper pillr shpeF his re)ow retes intermetlli lloys nd voids t the interfe etween opper nd negguD s well s eg preipittes in the umpF his is ll the more signi(nt sine the lyers re stked one fter the otherD whih mens pillrs situted t the ottom of the stk will undergo multiple re)owsF hose fetures re likely to in)uene the eletril nd mehnil ehviors of the pillr PSD PTD PUD PQF es suhD we here fous on the morphologil oservtion of opper pillrsD minly regrding the possiility to oserve voids nd intermetlli lloys et the interfe etween the opper ylinder nd the umpF pigure IFVX sllustrtion of the frition steps of opper pillrsF efter the growthD opper pillrs re situted on the top of QHH mm lrge nd USH µm thik wfers nd re orgnized into mtries on the wfer surfeF hey re therefore quite sensitiveD nd the smple preprtion must not require ny ontt with the top prt of the wferF he wfer levge nd swing is possileD while psf or psf preprtion requires protetive depositF 1.3 Characterization methods 1.3.1 Characterization needs rere we summrize the hrteriztion demnds for opper pillrs nd wfer to wfer ondingD together with the hrteriztion tools suseptile to nswer themF es presented in the previous setionD voids nd intermetllis n hve n impt on the eletril nd mehnil ehvior of P onding nd opper pillrsF e (rst hrteriztion n e mde y hrterizing the ondutivity of the feturesD nd their mehnil resistne PVD PQF hose tehniques o'er sttistil informE tionD nd re quite fst to setF roweverD they o'er very glol informtionD with little informtion out the uses of the prolemF 1.3.2 Strain measurement method e study of strin inside the smples n lso e performedD in order to isolte the res sujet to filureF es the res to explore re severl µm 2 wideD iw hrteriztion is not well dptedD while l xEry di'rtion o'ers resolution of severl tens of mironsD whih often does not llow to disriminte res within given dieF e lol strin informtion n e otined with foused synhrotron xEry emF hi'rtion ptterns re reorded for every point of snned region of inE terest @ysAD nd strin n e deduted in this ysF hi'rtion n e performed in trnsmission geometry @vue di'rtionA or re)etive one @frgg di'rtionAF he limit of resolution is therefore set y the fous size @whih n e few hundred of nm in modern emlinesAD nd the (eld of view is determined y the time vilE le for the snF sn the se of monohromti frgg di'rtionD fst snning quisition system hs een implemented in the shHI emline t ipF qiven the possiility to quire dt from IHH x IHH µm 2 res within n hourD nd the ft tht silion used in wfers is monorystl @thus does not require polyhromti em to e nlyzedAD strin mesures were performed on shHI during this hhF e more detiled presenttion of this emline is provided in hpter QD while results of the experiments re displyed in hpter TF 1.3.3 Imaging methods es explined in the previous setionD the oservtion of di'erent fetures is interE esting is the se of opper pillrs nd pdsF por the formerD the oservtion of voidsD for monitoring purposesD is of vlueF por the ltterD oth voids nd interE metlli lloys will e oservedD for etter understnding of the ehvior of gusD from mteril siene point of viewF o otin those informtionD imging is suitle solutionF st lso o'ers informtion out possile mislignment of pds in the se of hyrid ondingF sn the se of P ondingD nning eousti wirosopy @ewA is n pproprite imging tehniqueD in whih ousti wves re projeted on the smpleD nd re re)eted y interfesF oids therefore pper in whiteD s n e seen on the ew lihé from pigure IFTF sllEonded res re lerly visileD nd whole wfer n e imged within minutesF his tehnique however lks resolutionD whih is limited to severl tens of µm PHF righ resolution tools n e pplied to the imging of oth gus nd onding interfesD suh s nning iletron wirosopy @iwA nd rnsmission iletron wirosopy @iwAF hose tehniques re wellEestlished nd widely pplied in the miroeletronis (eldF hey o'er good oservtion of voidsD s hs lredy een shown in pigures IFT nd IFTF roweverD they o'er quite nrrow (eld of viewD whih redues the sttistil informtion one n get from n nlysisF fesidesD those imging tehnique only o'er Ph informtionD while the ojets re threeE dimensionlF Qh imging tools re lso villeF v tomogrphs imed for industry o'er the possiility to imge in three dimensions ojets up to severl entimeters in widthF he omplete nlysis is relized in few hoursD whih is omptile with the industry requirementsF heir resolution is however often limited to out I µm in ommeril equipments PWF omogrphy performed in iw o'ers high Qh resolution utD s in the Ph seD hs very limited (eld of view @SH nmAF sn this workD xEry tomogrphy performed in synhrotron ws investigted for Qh integrtionD in two di'erent imging emlinesD tht re shITe nd shIWF hey re dedited to nnoE nd miroEtomogrphy respetivelyD with resolutions rehing SHH nd UHH nmF heir spei(ities will e given in hpter QD while results otined on those emlines will e presented in hpter SF sn order to hieve high resolutionD lie nd iew tehniques n e performed in psfGiw instrumentF hey o'er resolutions of severl nnometersD ut require long dt quisition timesD whih limit the nlyzed volume to out IH µm 3 QHF huring this hhD lie nd iew method hs een implemented inside lsmE psf @poused son femAD in order to redue the dt quisition time nd inrese the imged volumeF e more detiled desription of the lie nd iew tehniques will e given in setion PFRD while the development of this tehnique inside lsmE psf will e presented in hpter RF Caractérisation pour l'intégration 3D

Résumé du chapitre ge premier hpitre introduit les prinipes de l9intégrtion Qh en miroEéletroniqueF v9ugmenttion des performnes des omposnts de miroEélétronique psse jusqu9à ujourd9hui pr l diminution de l tille des trnsistorsF gette pprohe tteignnt ses limites physiques et tehniquesD une nouvelle géométrieD ppelée intégrtion QhD est en ours de développementF ille onsiste en l9empilement des di'érents éléE ments des iruits intégrésF gei peut être rélisé u niveu du pkging ou des pues ellesEmêmesF hns ette étudeD nous nous intéressons à e seond sD qui est tuellement en ours de développementF our elD di'érents ojets tels que les @hrough ilion isAD les piliers de uivre @opper pillrsAD et les pds de uivre @opper pdsAD sont développés dns l9industrieF v rtéristion des deux derniersD dont les ménismes ne sont ps enore prfitement onnusD font l9ojet du présent trvilF veurs esoins en termes de rtéristion sont dé(nisF h9une prtD le suivi du proédé de frition de es ojet néessite une informtion morphologique sur les trous à l9interfe entre deux pdsD insi que sur les trousD les lliges intermétlliquesD et les préipités d9rgent u sein des piliers de uivreF v9imgerie de es ojets néessite une tehnique perE mettnt un lrge hmp de vue @quelques dizines de miromètresA et une hute résolution @quelques dizines de nnomètresAF h9utre prtD l mesure des déforE mtions u sein de telles strutures permet de omprendre et prévenir d9éventuelles défillnesF si ussiD l méthode de rtéristion doit pouvoir ouvrir de lrges zones d9un éhntillon @typiquement IHH x IHH µm 2 A et fournir une informtion lole @SHH nmAF hns les deux sD pour stisfire les esoins de l9industrieD l rtéristion doit pouvoir être fite de mnière utomtique et routinièreD (n d9otenir des données sttistiquesF uelques méthodes lssiquement utilisées pour de telles nlyses sont évoquéesD et les solutions proposées et développées u ours de e trvil sont introduitesF sl s9gitD pour les mesures de déformtionD de l ligne shHI de l9ipD etD pour l9imgerie QhD des lignes shITe et shIW de l9ipD insi que d9une proédure lie nd iew implementée dns un psf @lsm poused son femAF nning iletron wirosopes @iwA re tody widely used in vriety of (eldsD s they represent fst solutions for surfe imging nd provide lrge pnel of informtionD inluding topologyD hemistryD nd rystlline orienttionF ht is usully lled psf @for poused son femA is snning ion mirosopeF son soures hve een developed in the SHsD together with the eletron gunsD ut their pplition ws restrited for time to rod emsD iming t glol ethingF poused son fem souresD whih llow for snning mirosopy nd therefore lol ethning nd imgingD re more reentX psf mirosopes hve minly een developed sine the IWVHsF heir minstrem re of pplition is tody the smple preprtion for rnsmission iletron wirosopy @iwAD prtiulrly for the miroeletronis industryF foth types of mirosopes rely on the sme si priniples nd physi phenomE enD lthough their prtil hrteristis vryF sn oth sesD hrged em is foused nd elerted towrds the surfe of smpleF he intertions etween the em nd the smple emits new hrged prtilesD tht n e ptured y detetors nd nlyzedX they will provide pnel of informtionD e it topologilD hemilD or rystllineF woreoverD for hevy nd energeti ojets suh s ionsD the smple itself is lteredX mtter n e removed from the surfeD mking the ion gun milling tool s muh s n imging toolF sn this hpterD generl overview of suh mirosopes is presentedD with strong fous set on three versionsX the iwD the gllium psfD nd the xenon psf @lter noted psfAD iming t lyout of their similrities nd di'erenesF he psf ws extensively used in this workD while the psf nd iw me s side toolsF es they ful(ll di'erent yet lose purposesD we here hoose to present the three mhinesF sn (rst setionD the min prts onstituting suh mirosopes re presentedF e detiled desription of the existing soures is given in setion PFPD while the smpleE ojets intertionsD with fous set on their properties nd the onsequenes on the mirosopes9 pplitionsD re exmined in setion PFQF pinllyD two pplitions of ion mirosopes re introduedX lie nd iew proedures nd smple preprtionF 2.1 General overview and relevant values rere we present the generl priniple nd instrumenttion for n eletron or ion sed mirosopeF ht provided for eletron mirosopes re minly tken from QID while the physis of ion mirosopes were investigted with the support of QP nd QQF eferenes for spei( informtion nd vlues re given long the textF he eletron nd ion mirosopes re mde of three min omponentsD shown in pigure PFIF es their designs my di'erD the sis omponents or the di'erent mirosopes re quite similrF pirstD eletrons or ions re extrted from soure thode nd elerted using n nodeF sn the se of n eletron soureD the thode n e hirpin or (eld emission gunY ions n e extrted using viquid wetl son @vwsA or plsm souresF he em then enters the olumnD in whih it is foused nd its energy seletedF eording to the originl em nd the olumn settingsD wide pnel of spot sizes nd energies n e otinedF he em is elerted towrds the smpleD whih is pled down the olumn nd mounted on stge with S degrees of liertyX D D D tilt nd rottionF por eh mhineD omputer is onneted to the system nd softwre llows the user to ontrol the mhineF es we will seeD the di'erent setups do not nswer the sme needsD they hve their own ssets nd drwks when it omes to resolutionD sputtering rteD smple dmge etF st is therefore relevnt to omine the tools togetherF hul em mirosopes re ommerilized todyD llowing for simultneous psf nd iw pplitions on given smpleD in order to omine their dvntgesF pigure PFIX sllustrtions of olumns for A iw @soureX eiss qeminiA A psf with Ga + viquid wetl son oure @qA A psf with Xe + plsm soure @soureX yrsy hysisAF 2.2 Sources of electrons and ions rere we desrie the si priniples of the extrtion of eletrons nd ions from metlli mterilF por the emission of eletronsD the thermioni e'et nd the (eld e'et will e desriedD followed y their respetive pplitionsF es ion gun n rely on either viquid wetl son oures @vwsA or lsm sndued son ouresD these two phenomen will e desriedD together with the soures designs they led toF iletron nd ion mirosopes n e desried y mny quntittive feturesF ome relevnt fetures re presented in tle PFID oth for eletron nd ion gunsF o hrterize ion nd eletron soures loneD one of the most often used is the redued rightness β r QRF st reltes to the mount of ojets @eletrons or ionA tht exit the soureD per solid ngleD per thode surfe unitD nd per energy unitX it determines the mximum urrent in sptilly nd temporlly oherent emF es suhD it summrizes severl soure hrteristis suh s the soure sizeD the totl intensity exiting the thodeD the ngulr intensityD the urrent density of the thodeD nd the energy spred of the soureF 2.2.1 Electron guns sn metlli mterilD eletrons hve high energy ut re on(ned to the mterilF heir energy levels (t in rngeD nd the highest rehed energy level is lled the permi level E F F o espe the mterilD n eletron needs n energy ED de(ned y E = E W -E F D with E W the work funtion of the mterilF o otin eletronsD one hs to provide enough energy to the mteril for some eletrons to reh the energy level EF his n e done y providing therml energy to the mteril @the thermioni e'etA or through n eletri (eld @the hottky e'etAF he thermioni e'et ours when metlli mteril is heted to the point were some eletrons n overome the work funtion energy rrierF he thode urrent density J C is given y the ihrdson9s equtionX

Value

Electron Guns Ion Guns LaB 6 Schottky FE Ga

+ LMIS Xe + ICP Reduced brightness (A • m -2 • sr -1 • V -1 )
J c = A C • T 2 • e -( E W k.T )
@PFIA here A C is the onstnt for thermioni emittersD with vlue of IPH A • nA -2 F T @uA is the emission tempertureD while k is the foltzmnn9s onstnt @8.6•10 -5 eV • k -1 A nd E W @eA the work funtion of the mterilF o mximize the eletron emission of the gunD one either hs to lower the work funtionD or to inrese the tempertureF roweverD higher temperture n led to mteril evportion nd therefore shortens the lifetime of the soureF he emitter mteril therefore hs to feture low work funtion omined with high melting tempertureF e good ompromise n e found y using tungstenD s its work funtion vlue is RFSS e for melting temperture of QTUH uF his mteril ws used in the (rst eletron souresD lled tungsten hirpin eletron gunsF es shown in pigure PFPD thin @IHH µmA tungsten (lment @the thodeA is urved in Eshpe nd heted to out PUHH uF he temperture is hosen t plteu of eletron emissionD where smll hnge in temperture does not hnge the urrent muhF he eletron emission ours t the highest urvture pointD nd n node extrts them using voltge rnging from HFI to QHH kF he soure thus reted mesures from 30 to IHH µm nd hs typil urrent density of 3.4 A • nA -2 D with n energy spred of Q eF pigure PFPX sllustrtions nd tul pitures of A (lment eletron soure @soureX nnosieneFomAD A (eld emission gun @piqA @nnosieneFomAD A the vws @soureX yrsy hysisAD nd dA the sndutively goupled lsm @sgA soure @soureX elementlnlysisFomAF o inrese oth the urrent density nd lifetime of the soureD other mterils n e used s n thodeF e populr mteril is the vnthnum hexoride @LaB 6 AF st presents lower work funtion thn tungsten @PFS eAD whih llows for similr or even higher density with lower tempertureF por exmpleD to otin the urrent density provided y thode t PUHHuD LaB 6 thode only needs to e heted to ITHH uF sts typil working temperture is however IVHH uD for whih it provides urrent density of 40A • nA -2 F he typil soure size is S µm nd the energy spred lose to IFS eF yther mterils suh s the gerium rexoride @CeB 6 A hve lso een used s eletron gun thodesF enother mnner to llow the espe of eletrons from the mteril is to set the thodeD in tht se wire with shrp point @out IHH nm in dimeterD s presented in pigure PFPA to negtive potentil of Q to S k nd to use the (eld e'et thus retedF he eletri (eld t the top is strong nd nrrows the potentil rrier for the surfe eletronsX tht is the hottky e'etF he eletrons n tunnel through the rrierD with no supplementry energyF he gold pield imission @gpiA gun ws the (rst used nd fetures urrent density of 10 5 A • nA -2 with smll soure of S nm in widthF st however presents high emission ngle @PH¦AF everl improvements hve een mde on the piq @pield imission qunAD y inresing the working temperture or hnging the thode mterilF he most dvned gun tody is the hottky pield imission @piA gun QSF st omines the (eld emission phenomenonD together with thermioni emissionF e `IHHb oriented tungsten tip is overed with ry lyer tht lowers the work funtion of from RFS e to PFV e QTD QUF hese llow for high urrent density @SQHH A • nA -2 AF st is moreover omined with reltively smll soure @IS nmAD whih ltogether leds to high redued rightness of 10 8 A • m-2 • sr -1 • V -1 QVD QRF elthough this type of soures hs een developed sine IWTRD severl phenomen ourring during the emission proess re still unexplined nd there is still ongoing reserh QWF 2.2.2 Ion guns sn n ion gunD voltge is pplied to thodeD whih will eome the ion providerF es soon s the proess provides n energy higher thn the (rst ioniztion potentil of the mtterD ions re retedF woreoverD the mtter is put in stte @liquid or gsA tht enles the ions to espeF e (rst nd most lssi model of ion soures is the viquid wetl son soure @vwsAF sn this type of souresD needle @usully mde of tungstenA with dimeter of P to S µm is pled under reservoir (lled with nother metl @usully glliumAF he reservoir is heted nd the metl wets the needle surfeF en eletri (eld is pplied to the top of the needleX the lne etween the surfe tension fores nd the eletrostti fores is hngedD foring the gllium one on top of the needle to hnge its shpeF st forms ylor oneF yne it rehes the equiliriumD the tip of the one is smll enough for the (eld to extrt q ions from the needleF everl resons mke the gllium good ndidte for these souresF pirstD it fetures low melting point @QH¦AD whih mens it is esy to design nd operte t room tempertureF hue to its superEooling propertiesD gllium sty molten weeks fter it hs een meltedF sts low vpor pressure ensures low evportion rteD whih inreses the lifetime of the soureF he wetting of gllium on tungsten is quite goodD nd the low operting temperture ensures no retion ours etween the two metlsF e typil Ga + vws soure is tody out SH nm wideD with (nl spot size of S to RHH nm @respF t I pe nd PH neAF heir energy spred is quite low @S eA nd they o'er n overll redued rightness of 10 6 A • m -2 • sr -1 • V -1 F uh soure however presents some limittions @RHAF he sputtering yield it n o'er is of severl µm 3 • s -1 @RHD QQAD whih llows for typil removed volumes elow 10 4 µm 3 F por some psf pplitions howeverD inluding miroeletronisD muh lrge volumes hve to e milledF imply inresing the em urrent is not solutionD s the spot size inreses drstilly for urrents ove S neD s presented in pigure PFQF his is due to the reltively low ngulr density of vws soures @IH µA • sr -1 A together with their lrge emission ngle @20¦AF sn ftD the repulsion fore etween the positively hrged prtiles widens the emD whih mkes it di0ult for the optis to fous the emF pigure PFQX roe size vs proe urrent for three di'erent types of ion souresX the @Ga + A vwsD the @Xe + A lsm psfD nd the @Ar + A duoplsmtronF yther solutionsD suh s plsm soures nd the di'erent ion speies they llowD hve een onsidered over the lst RH yersD iming t inresing the urrent with little inrese of the spot sizeF p to the PHHH9sD the most populr ommerilly ville plsm soure ws the duoplsmtronF st is mde of thode (lment whih emits eletrons when hetedD s in n eletron soureF e gs @often rgonA is introdued into the hmer with very low pressureF es this gs is ionized y the free eletrons of the thodeD it eomes plsmF st n therefore e elerted y hrged eletrodeD reting n ion emF elthough their spot size remined quite stle with the inrese of urrent @see pigure PFQAD those soures presented low redued rightnesses @IIQH A • m -2 • sr -1 • V -1 )D low ngulr densities nd too lrge spot sizes for snning tehniqueF fesidesD their lifetime ws very low @out PSHESHHh RHAF huoplsmtrons were therefore minly used for surfe leningD depth pro(ling in ei nd D nd s primry ion soures for sw pplitionsD using Ar + ions RIF sn PHHSD ueller et lF ptented new type of plsm ion soureD lled sg @sndutively goupled plsmA souresD where the urrent ws indutively set into plsm RPD RHD QQF sts generl priniple is presented in pigure PFPdF e similr soureD sed on eletron ylotron resonne @igAD ws lso introduedD with simE ilr (nl hrteristisF rere we fous on the sg souresF e reservoir ontining low pressure gs is surrounded y oil ntennF e rdio frequeny power supE ply provides n lternting urrent in this ntennD whih indues time vrying mgneti (eld in the gsF fy the prdy9s lw of indutionD this genertes time vrying eletri (eld in the gsD nd therefore time vrying urrentF he frequeny is hosen to e ove the eletrons resonnt frequeny nd elow the ion resonnt frequenyD whih results in high density plsm @10 13 cm -3 for xenon souresA sine the eletrons re given high therml energy while ion therml energy remins lowF hose soures were (rst used with O + ions to reple the Ar + duoplsmtron for sw pplitionsD s they o'ered n inresed urrent densityD higher depth resolution nd smller spot sizeF es summrized in tle PFID Xe + sg soures o'er muh higher emission urrent thn Ga + vws ones with similr energy spredF hey su'er from lrge virtul soure @IQ µm ompred to SH nmAD whih they ompenste for with their quite prllel emX their ngulr density is muh higher thn the one otined with vws @10 mA • sr -1 ompred to IS µA • sr -1 D with respetive emission ngles of I¦nd PH¦AF hose fetures llow the Xe + sg soures to reh typil redued rightness of 10 4 A • m -2 • sr -1 • V -1 )F es we will see lterD this leds to muh higher sputtering rtes thn those otined with vwsF huring the work presented hereD smple preprtion ws minly performed on sg psfD s the onsidered smples were quite lrge @out IHH µm in dimeterAF he mhine used ws ion single em Xe + psf from pisF por puntul requirementsD trt dul em Ga + psf from pis ws lso usedF 2.3 Objects/matter interactions and applications efter the eletron or ion em exits its olumnD it is foused nd ims t the smple surfeF he em itself is hrterized y four min feturesX its spot size @d p AD its onvergene ngle @α p AD its urrent @eFgF how mny ojet re projeted on the surfeD i p AD nd its elerting voltge @eFgF how fst the ojets re going towrds the surfeD V p AF sts intertion with the smple will depend on those feturesD s well s the type of ojets it rriesD the nture of the smpleD nd the inidene ngleF yne the em rehes the smpleD severl phenomen n ourF ell phenomen ome from the intertions etween the rriving eletrons ndGor ions nd the trget eletrons ndGor ionsF hose intertions n e elstiD with lmost no energy loss in the emD or inelstiD where the eletrons or ions from the inoming em lose energyF rtiles resulting from those intertionsD together with their mirosopyE relted pplitionsD re illustrted in pigure PFRF sn the se of n eletron iming t trget tomD the negtive hrge of the tom eletrons n repulse the inident eletronF st will therefore e de)etedD with little loss of energyF efter eing de)eted severl timesD the eletron n (nd its wy k to the surfe nd leve the smpleF st n therefore e ptured y detetorD whih detets its high energy nd lels it s ksttered eletronF sf pigure PFRX hi'erent phenomen of interest ourring etween n ion or eletron em nd the smple surfeF the kineti energy of the inident eletron is high enoughD it n remove low energy eletron from n tom oritD reting seondry eletronF he otined eletron hs low energyD nd is therefore used for topology imging if it n exit the surfe of the smple nd e ptured y detetorF he distintion etween ksttered nd seondry eletrons is mde using n energy (lterD with limit ritrrily set to SH e QIF ith eletrons with even higher energiesD inner eletrons of toms n e removedD triggering either the emission of photon or n euger eletronF he former provides the user with generl hemil informtion nd leds to ih nlysisD while the ltter provides the hemistry of the very surfe of the smple @severl nmAD through euger spetrometryF elthough mny imging tehniques re ville inside psf mirosopeD only seondry eletron imging will e detiled in this study @see setion PFQFQAF wost of these intertions produts @euger eletronsD seondry eletronsD nd xEryA re oservle oth in the se of snning eletron mirosopy nd snning ion mirosopyD s they ome from the diret intertions etween the eletrons from the em nd the eletrons from the smpleF sn the se of n ion em howeverD other mehnisms n dd upD given the reltively high mss of the ions ompred to the eletrons @the eletrons re 10 5 times lighter thn gllium ions nd 2 • 10 5 times lighter thn xenon ionsAF ypillyD for n QH k elertion voltgeD gllium ion9s momentum is QTH higher thn n eletron9s oneF his energy mkes it possile for ions to ejet surfe toms from the smpleD resulting in sputtering of the mtterF eondry ions n therefore e reted nd used for imgingF roweverD the pility of ion ems to sputter mtter mkes it ove ll well suited tool for smple preprtionF rmeters must e dpted to mximize the milling while limiting the redeposition of mtter lose to the milling reD s will e explined in setion PFQFIF he (nl smple n su'er from other severl side e'ets ourring during this proessF he mteril is heted y the ion emD nd morphiztion n ourF woreoverD ions n remin in the smple nd eome implnted ionsD nd stress n e generted y the smple preprtion proessF hether those side e'ets re ritil or not on the smple will depend on the further nlysis to e performed on itF pinllyD the ion or eletron em energy nd its ility to rek some juntions n e exploited for mtter depositionD y iletronGson fem sndued heposition @ifsh or sfshAD s will e presented in setion PFQFPF 2.3.1 Milling he pility of given ion to ejet n tom from the smple is linked to whetherD during the ollisionD it trnsfers enough momentum to the tom for it to overome the surfe inding energy @fiA of the mterilF hether the sputtering hppens or not will therefore depend on the smple mterilD the ions ntureD their veloity nd diretionF st n e desried y the sputtering yield D whih is de(ned s the men numer of sputtered trget toms per inident ionF e si intuitive model is tht the sputtering yieldD for given trgetD t norml inident nd for given elertion voltgeD would e proportionl to the momentum M ion of the inident ionF vet9s ompre the vlues of moment for gllium nd xenon ionsD elerted t the sme voltgeF sn oth sesD the ions kineti energy is equl to e • ∆V D whih leds toX

Ec Ga + = Ec Xe + @PFPA 1 2 • m Ga + • v 2 Ga + = 1 2 • m Xe + • v 2 Xe + @PFQA v Xe + v 2 Ga + = m Ga + m Xe + @PFRA
he omprison of moment risesX

M Xe + M Ga + = m Xe + • v Xe + m Ga + • v Ga + @PFSA = Ec Xe + Ec Ga + • v Ga + v Xe + @PFTA = m Ga + m Xe + @PFUA
es the vlues of gllium ions nd xenon ions re known nd worth 1.2 • 10 -25 kg nd 2.2 • 10 -25 kg respetivelyD we otin M Xe + = 1.35 • M Ga + F sing this simple modelD one otins Y Xe + = 1.35 • Y Ga + F igmund et lF presented in IWUU the viner gollision gsde theory to explin onditions for sputtering hppening RQF he theory relies on the suessive intertions etween primry ions nd smple tomsD the intertion series possily ending in providing energy nd momentum to n tom lose to the surfeD whih n then espe from the smpleF hen ompring the vlues provided y this theory for gllium nd xenon on silion trget with n elertion voltge of QH kD one otins Y Xe + = 5.2 nd Y Ga + = 4D whih rises rtio of IFQF husD the hoie of xenon ions for lrge volume milling is motivted y the intrinE si sputtering yield of xenon ionsD IFQ times igger thn the gllium oneF gomined with this fetureD xenon ions n e extrted from plsm soureD s explined previouslyD whih llows for P µA urrent rehing the trget @ompred with PH ne with Ga + vwsAF his mens the sputtering hppening during given durtion is IHH times higher with sg thn with vwsF his leds to higher sputtering rtes tE tinle y Xe + sg ion em @more thn IHH µm 3 • s -1 ompred to SFR µm 3 • s -1 A F efter leving the smple surfeD sputtered toms hve quite low energy @Q to S eAF hey n e ionized ndD s hrged prtilesD they n e ttrted y grid nd hit detetorF hey n therefore e used for imging @seondry ions imgingAD lthough they re muh less numerous thn seondry eletrons @IH to IHHH times less QPAF wost of ejeted toms remin in the re of the milling zoneD s their low energy prevents them from levingF hey will likely redeposit on the surfeF edeposited mtter is minly spotted on the side wllsD where it n hve width of IUH nm for Ga + milling on i RRF he redeposition phenomenon is to e tken into ount when millingD sine it dds mtter in the re supposed to e milledF inough spe must therefore e llowed for redeposition to hppen fr enough for the milled reD nd urrents must e dpted for milling to previl on redepositionF edeposited mtter hs een shown to ontin up to IP7 tF of qD nd to hnge ondutivity of the surfeF his will hve n impt not only on the milling nd the imging of the smpleD ut lso on the ondutivity of the (nl smpleF hue to inner repulsive intertions etween positively hrged ionsD it is hrd to fous the whole ion emD whih will hve one shpeF iven if the top of the one is highly foused s quite smllD the til of the em will e muh lrgerF hereforeD in the se where deep milling ours @severl mirons in the se of psfD severl tens of mirons for psfAD s the em sns the smple disretelyD vertil line n pper on the rossEsetionD s illustrted in pigure PFSF his is ll the more true when the smple is mde of severl mterils with di'erent sputtering yieldsF his side e'et is ritil for imgingD s the vertil lines mke imge interprettion di0ultF everl strtegies hve een developed to overome this issueF hey n rely on the ddition of n morphous protetive lyer on top of the surfeD whih will rndomize the diretion of ions nd redue the urtining RSD RTF roesses sed on roking urve round the horizontl diretion re lso studiedF he smple is tilted during the millingD in plne oplnr with the inident ionsD so pigure PFSX sllustrtion of urtining rtiftsX surfe imging of opper stk inside n oxide mtrixD ut nd imged with Xe + psfF Image: Ion-induced secondary electron image acquired in a PFIB. tht the ions do not ome from the sme diretion during the whole proess RUD RVF gurtining is minly n issue for further imging of the milled rossEsetionD for exmple in the se of lie nd iew proedures or for very thin lmelle mde for iw oservtionsF purthermoreD the psf preprtion dmges the smple round the milling or imging reF yn the ottom wll of the milled reD heting ours in the mterilF por gllium psfD the inrese in temperture is less thn IH¦u for gllium psf RWF everl de(nitions of psf dmges n e found in the litertureF st n e de(ned s hnge in the smple morphology outside of the milling reD or the derese of the eletril properties of the smple SHF wo min prolems of psf preprtionD espeilly in the se of thin smples imed for iw oservtionD re morphiztion nd implnttionF emorphiztion ours euse of the sustrte toms reoilD oming from the intertion etween toms nd ionsF he lttie order is then destruted nd prt of the rystlline sustrte eomes morphousF woreoverD s inident ions lose energy with every ollision inside the lttieD they my remin in the mterilD s implnted ionsF ghrged sustrte ions n lso e implnted in the mteril @selfEimplnttionAF por silion sustrte nd gllium ions elerted t QH kD the thikness of morphous mteril next to the side wlls is QH nmD while it is ST nm next to the ottom wllF he implnttion of Ga + ion ours on IQ nm next to the side wlls @QT nm for the ottom wllAD while the self implnttion is present on PT nm ner side wlls @SV nm for the ottom wllA RRF he use of xenon ions seems to redue the morphiztion of the sustrteD s its thikness ner side wlls hs een evluted to onlyIQ nm with Xe + elerted t QH k QHF hose two phenomen must e tken into ount when setting prmeters for millingD s for low doses of ionsD they previl upon millingD nd indue swelling of the smple SHF hen de(ning the dmged zone s the eletrilly modi(ed oneD the thikE ness of the 'eted res is however muh higher nd n reh up to severl miE rons SHD SIF his n e explined y em rodening nd di'usionF sn xEry tomogrphy experiments presented hereD the smples were severl tens of mirons wideF herefore the regions of interest did not su'er from dmges used y the psf during smple preprtionF 2.3.2 Matter deposition he seondry eletrons nd ions reted y the intertions of the em with the smple hve lower energy thn the primry emF es suhD they hve higher rossEsetion nd re more likely to intert with ny prtile present in the smple environmentF his phenomenD together with the het the intertions generteD is used for mtter depositionF por thisD preursor moleulr gs ontining the wnted mteril toms is introdued in the hmer through qs snjetion ystem @qsAD ner the smpleF st is dsored on its surfeF he ion or eletron em is then direted towrds the surfeD drwing ptternF he seondry eletrons nd ions reh the gz moleules lose to the intertion pointD nd seprte their two prtsX the gs itself leves the reD while the mteril to e deposited stys on the surfe of the smple nd uilds lyersF hepending on the used emD this proess is lled ifsh @iletron fem sndued hepositionA or sfsh @son fem sndue hepositionAF everl proesses re therefore ompeting during the proeduresF en equilirium hs to e found in order to provide the right mount of gs for the dsorption to hppen lyer fter lyer nd the right urrent to seprte the gs moleules without milling the smpleF ifsh nd sfsh re used for severl purposesF pirstD for ny extrting proeE dureD s will e presented in setion PFRFPD metl joints @typilly tA re reted etween the seleted region of interest nd miromnipultorD llowing for the displement of the future smpleF snsultor n e deposited to seprte two onE dutive zonesD while ondutive ptterns or gridsD or even iruitsD n e designed nd relized using metl lol depositionF he deposition of thik @severl mirons in the se of psfA lyer of n dpted mteril n lso serve s protetion of the smple surfeD either to redue its dmgeD either to ounter the urtining rtiftsF 2.3.3 Imaging rereD only seondry eletron imging is onsideredD s it is the most ommonly usedF eondry eletrons re emitted fter n eletron from the inident em hs ejeted n eletron from one smple tomF yne it exits the smple surfeD it is ttrted y thode nd detetedD typilly using iverhrtEhornley detetorF es the seondry eletrons ome from n inelsti intertionD they hve low energyF he informtion they provide therefore omes from the region lose to the surfe @typilly few nnometersAD with little sensitivity to the hemistryX they provide topologil informtionF he eletron re (rst ttrted y positive potentil grid @t out RHH AD nd elerted towrds sintilltor @using P k voltgeAD whih onverts the eletroni signl into lightF his signl genertes the (nl imgeX for every snned pointD the more eletrons reh the sintilltorD the rightest the equivlent imge pointF he i yield is de(ned s the numer of i deteted per inident ojet nd highly depends on the inidene ngle SPX the topology is therefore esily visile in the otined imgesF sn this proessD the spot size d p will determine the lterl resolution of the (nl imgeD while the voltge V p will ply role on the penetrtion of ions or eletrons in the smpleF he signl to noise rtio will e linked to the urrent i p together with the exposure timeF he depth of fous will ome from the vlue of the onvergene ngle α p F hue to the reltive vlues of eletron nd ion soures sizeD emission nglesD nd emitted intensitiesD the rehle spot sizes vry in lrge rngeF qenerllyD the smllest proe sizes re otined for iwD with spot sizes smller thn I nm SQF Ga + vws soures llow for spots s smll s S nmD while Xe + sg soures reh PS nm lrge spot sizesF his indues higher imging resolutions for iw thn for vws psfsD nd ever higher thn for sg psfsF es mentioned erlierD topologil ontrst in i imges omes from the di'erE ene in i yield depending on the orienttion of the surfeF hen it omes to polyristlline mterilsD this e'et llows the visuliztion of grins using iX the i yield will depend on the orienttion of oth the surfe nd the ristlline plnesF his e'et is lled hnneling SRF es ions hve smller penetrtion depth in the mteril thn eletrons QP nd thus higher sensitivity to orienttionD they o'er higher sensitivity to the hnneling e'et SSF his high orienttion ontrst hs een shown to llow for quntittive nlysisD giving results lose to the ones oE tined y ifh @iletron fktter hi'rtionA imgingD provided the dequte postEproessing STF

en importnt e'et to e tken into ount when imging surfeD nd esE peilly n insultorD is lso the hrging e'etF hen imging the smple with eletronsD if the eletron nnot )ow through the mteril towrds the groundD they remin trpped t its surfeD lose to the impt lotionF fy their negtive hrgesD they will devite ny supplementry eletron rriving t the surfeD resulting in rE tifts @minly extremely right regionsA on the (nl imgeF his e'et lso ours for positive ion imgingX s they nnot )ow through the smpleD positive hrges will umulte on the surfeF sn ddition to the devition of inoming ionsD if i re retedD they re ttrted k to the surfeD resulting in drk res in the (nl imgeF everl solutions re deployle when deling with hrging e'etF pirstD the ondution of hrges n e ssured y ondutive oting or onttD together with good groundingF hen performing the oservtion in psf olumnD seE ondry ion imging n e usedD s ions will not e ttrted k to the smE pleF purthermoreD neutrlizing eletron )ood n suppress the remining positive hrges nd llow the imging @for timeAF pinllyD one hs to keep in mind tht when imging with ionsD ll the proE lems enountered when milling re presentF husD imging whith ions n led to ion implnttionD swelling of the surfeD nd sputtering when it ome to frgile mterilsF 2.4 Applications of Focused Ion Beam microscopes psf mirosopes o'er lrge set of tools tht llow to sputter nd deposit mtterD s well s to imge given smpleF hey re tody used in vrious (eldsD rnging from iology to the semiEondutor industry SUF rereD two pplitions of interest re reviewedD s they hve een extensively used during this hhF mple preprtion using the liftEout tehnique llows to selet region of interest @ysA from piee of wferD nd to instll it on top of support for further oservtions suh s tomogrphyF lie nd view proedures re used to diretly imge volume inside dul em or single em foused ion em mirosopeF 2.4.1 Slice and View procedure lie nd view @A is destrutive Qh imging method whih relies on the sequenE til sliing of the smple with regulr stepD nd the imging of the newly reted surfe t eh stepF efter quiring lrge numer of suh rossEsetionsD one n otin Qh rendering of the nlyzed region of interestD ssuming n interpoltion etween slies leds to n urte enough estimtion of the ojetF he sliing n e done using mirotomy SVD foused ion em @psfA SWD or polishing THD while imging n e performed with ll ville Ph tehniquesD using lightD eletronsD ionsD or xEry for exmple TID TPD TQF yservle volumes nd hievle resolutions oviously depend on the hosen sliing nd imging toolsF sn Qh integrtionD oserved volumes n mesure up to 100 3 µm 3 F he resolution should e elow IHH nmF qiven these onstrintsD ion sliingD together with ion nd eletron imgingD re prtiulrly relevntF sn this setionD generl work)ow of lie nd iew proedures is presentedD together with four sliingGimging tools ouplesD hosen mong eletronsD Ga + ionsD nd Xe + ionsF 2.4.1.1 Slice and View workow elthough the sliing nd imging tools used for lie nd iew proedures n di'erD the work)ow itself remins similrF st is illustrted in pigure PFTF hen performed inside foused ion em hmerD ll proedures demnd preprtion stepD during whih deep trenhes @typilly IH to IHH µm deepA re milled round the region of interest @ysAF his step is neessry in order to redue future redepositionF he dt quisition simply relies on the suessive sliing of rossEsetion nd its imgingF hepending on the type of implementtion @whether the sliing tool is the sme s the imging one or notAD hnge of urrent vlues nd of smple position n our etween those two stepsD s will e presented in setion PFRFIFPF yne ll the slies hve een quiredD they re ligned with one nother nd volume is otined y stking them togetherF sn ion nd eletron imgingD the Ph rossEsetions pixel size is usully muh smller thn the sliing step @up to Q times smller for psfGiw or psfGiwAF sn order to otin isotropi voxelsD the postEproessing step my inlude resmpling stepF pigure PFTX sllustrtion of the lie nd iew @A proedure work)owF Images:

Ion-induced secondary electron images acquired in a PFIB.

Dierent implementations

rere we present most ommon implementtions of the lie nd iew tehnique for resolutions nd volumes omptile with Qh integrtion smplesF pigure PFU presents typil voxels sizes nd nlyzed volumes s found in the literture for those tehniquesF pigure PFUX gomprison of rehle volumes nd pixel sizes for lie nd iew proeduresF he most ommon implementtion of proedures is performed in psfGiw dul em mirosopeF st ws introdued in PHHR SW nd hs een used in mny (elds sine TRD TSF he sliing of the smple is performed using Ga + ionsD while the imging is mde with the eletron olumnF xo movement of the smple is neessry etween the sliing nd imging stepsD s the two olumn form n ngle of SP • F he imge pixels however re not squreEshped nd resmpling step is usully neessryF es the seondry eletron imging o'ers high resolutionD the slies pixel size re typilly S nm wideD while the sliing step n e s smll s IH nmF sing this tehniqueD volumes of 10 3 µm 3 n e imged in out QH hoursF es presented in setion PFQFQD ions re more sensitive to hnneling thn eletronsF fetter orienttion di'erentition n therefore e otined y induing seondry eletrons with ionsF por given pplitionsD psfGpsf proedure si therefore releE vnt TTD TUF st pplies perfetly to the distintion of intermetlli ompound inside opper pillrsD for exmpleF he dt quisition is performed using only the ion emX thereforeD the smple must e rotted nd the urrent vlue hnged etween sliing nd imgingF elthough psf sliing llows for smll voxel sizesD it lso limits the oservle volumes to out 10 3 µm 3 F o hieve lrger volumesD proedures in dul em psf hve reently een developedF hile the imging is still performed using eletronsD the sliing step is mde using Xe + ionsD whih redues the time needed for this stepF olumes of IHH µm 3 hve een oserved TVD QHF he time needed for the nlysis rnges from few hours to TS hoursD depending minly on the sliing stepF huring this hhD n implementtion of psfGpsf lie nd iew proedure hs een designed nd set on single olumn psfF he detils of these hrdwre nd softwre developments re presented in setion RF

Sample preparation: lift-out procedures

Ga + poused son fem mirosopes o'er the possiility to mill nd mnipulte ojets smller thn IH µm 3 D nd to extrt them from piees of wfersF hey re extremely well dpted for smple preprtion for iwD whih require lmell whose thikness is elow IHH nmF o perform this smple preprtionD psf liftEout tehniques TWD UH hve een developed nd re urrently extensively usedD espeilly in the (eld of miroeletronis UIF he method ws further dpted for eletron tomogrphy UPD UQD tom proe tomogrphy URD USD nd xEry tomogrphy UTD UUF o overome the limit in time nd volume (xed y the psf millingD the tehnique hs lso een implemented in psf RVD UVF es will e presented in setion QFQD the smples needed for xEry tomogrphy @in the se of the shITe nd shIW emlinesA hve typil width of severl tens of mirometersF he psfD omined with liftEout tehniqueD is therefore relevnt for their preprtionD nd is illustrted in pigure PFVF he liftEout tehnique forms into severl stepsX A pirstD the region of interest is oted with protetive lyer of t nd the region round it is milled t high em urrent @2µAAF A yne side of the ylindril smple is prtly ut using the ion emF he smple is then rotted y IVH¦in order to ess the other sideF A e miromnipultor @isyviftA is pprohed to the region of interest together with qs snjetion ystem @qsAF e t join is deposited etween the ys nd the miromnipultor using the sfsh method presented in setion PFQFPF dA he smple is relesed from the wfer using seond utD performed t high urrent @typilly 2µAAF he miromnipultor is lifted together with the smpleF eA he miromnipultorD on top of whih the smple is tthedD is pled lose to the smple supportF fA e t deposition solders the smple to the supportF gA en ion rsion releses the miromnipultor from the smpleF pigure PFVX sllustrtion of the liftEout proedure performed in psf mirosopeF Images: Ion-induced SE images acquired in a PFIB.

hA en optionl nnulr milling gives the (nl smpleF he ion urrent is set to lower vlue @typilly SW neA in order to otin ylindril shpe while limiting the dmged re round the smpleF he (rst irulr milling ws originlly performed using onentri irleEshped ptternsD s shown in pigures PFW nd PFWF he suessive ptterns were triggered using the ipst pis softwreF e typil milling of SH µm wide smple took out R hoursF huring the time of this hhD new nd more e0ient milling method ws developed in the lortoryD nd hs een routinely used sineF st is desried in detils in UV nd illustrted in pigure PFWF st relies on n ellipseEshped pttern nd new dwell time mngement throughout the ptternD iming t more e0ient millingF his new milling method tkes out I hour nd llows for the extrtion of the smple with only one ut @insted of twoAF he remining steps sty the sme s in the originl methodF pigure PFWX sllustrtion of the originlly used irulr milling method @with A tiltaH¦ nd A tiltaRS¦A nd the improved ellipseEshped milling method @with A tiltaH¦nd dA tiltaTH¦AF Images: Ion-induced SE images acquired in a PFIB.

Microscopes électroniques et ioniques

Résumé du chapitre hns e hpitreD les mirosopes életroniques et ioniques sont présentés et déritsF ves di'érentes soures d9életrons et d9ions sont présentéesD ve leurs rtérisE tiquesF v9utilistion de soures plsm d9ions xénon est justi(ée pr leur fort tux d9rsion de l mtièreD ien supérieur à elui des soures gllium lssiquesF ve psf @lsm poused son femA est don hoisi omme outil pour l préprtion de grnds éhntillons @IHH µm de dimètreA omme eux utilisés dns e trvilF ves di'érentes intertions possiles entre les fiseux de prtiules hrgées @életrons ou ionsA et l mtière sont pssées en revueF ves di'érentes tions possiles u sein d9un tel mirosopeD provennt de es intertionsD sont déritesF sl s9git de l9rsion de mtièreD du dépôt de mtière sur l9éhntillonD et de l9imgerie @ii uniquement pr életrons seondiresAF in(nD deux pplitions spéi(ques de mirosopes à fiseu d9ionsD utilisées pendnt e trvil de thèseD sont introduitesF out d9ordD les proédures dites lie nd iewD tehniques d9imgerie Qh destrutivesD sont détilléesF sl s9git de méthodes onsistnt à déouper des trnhes suessives de l9éhntillon onsidéréD et d9imger à hque étpe l surfe nouvellement rééeF rois implémenttions déjà utilisées sont présentées X le psfGiwD le psfGpsfD et le psfGiwF v tehnique de préprtion d9éhntillons nommée liftEout est églement présentéeD puisqu9elle été utilisée sur on nomre d9éhntillons u ours de e trvilF sl s9git d9une tehnique onsistnt à détourer une zone d9intérêt grâe à un fiseu d9ionsD puis de (xer ette zone à un miromnipulteurF v9éhntillon insi formé est lors (xé à un supportD que l9on pourr mnipuler pour une nlyse futureF es seen in the previous hpterD eletrons o'er gret fetures for imgingD s they n e foused nd prtiipte in high resolution snning imging tehniquesF hey n lso e used for di'rtion mesuresD lthough their penetrtion depth remins elow the mirometerF yn the ontrryD xEry o'er high penetrtion depthD nd wvelength omptile with the size of rystlline ltties in mtterF sn ftD their energy is omprised etween IPR e nd IPR keD for wvelengths omprised etween HFHI nm to IH nmF Ery hve onsequently widely een used for di'rtion mesuresF ith the improvement of fousing Ery optis nd souresD it is lso possile to perform ondensed mtter imging using EryD s will e shown in this hpterF woreoverD hrd xEry @de(ned s hving n energy ove SEIH keA n penetrte into severl millimeters or even entimeters of ondensed mtterD o'ering the possiility to nlyze the inside of quite lrge smplesF o exploit those dvntgesD mny experimentl setups hve een designedD depending on the wnted informtion nd the nlyzed mterilF hey n e implemented in l instrument or in synhrotronF elthough some tehniques rely on similr physis prinipleD the hrteristis of the em they use will hve ritil impt on the type nd preision of informtion they llow forF he em hrteristisD suh s its energyD its monohromtiity nd shpe for exmpleD n e tuned ording to the given experimentF his is ll the more true in synhrotronD s will e presented lter onF uh em interts with the smpleD e it y sorptionD stteringD or refrtionD nd exits itF e detetor then llows to reord the exiting signlD nd postEproessing step hopefully provides the wnted informtionF his hpter provides n introdution to the xEry hrteriztion methods used in this workF e (rst setion provides the min elements of xEry physis exploited hereD inluding the genertion of xEry nd their intertion with mtterF he fous is set on the verstility of xEry souresD nd more spei(lly of synhrotron onesF e setion is dedited to the presenttion of the hrteristis of the emlines used hereF pinllyD mode detiled desription of xEry imging nd strin mesurement is providedF 3.1 Elements of x-ray physics sn this setionD lrgely sed on UWD the min steps of the experimentl prt re depitedF pirstD we will present the di'erent wys to otin n xEryD in l instrument or in synhrotronD nd the di'erent fetures it n e givenF he min intertions of xEry with mtter will then e desriedD s they will give the reder n insight on the hrteriztions xEry n provideF 3.1.1 Obtaining an x-ray beam everl proesses llow for the retion of n xEry emF wo types of xEry soures re depited hereX lortory soures nd synhrotron onesF he ommon priniple is tht xEry re emitted when hrged prtilesD suh s n eletron emD is elerted or deelertedF sn l souresD the em is deelerted when pprohing trget thodeD while in synhrotron souresD the devition of trjetory of the eletrons y mgnets produes the xEry emF sn this setionD more detiled presenttion of those soures is providedD toE gether with some relevnt hrteristis of n xEry em @see tle QFIAF st is notiele tht the notion of soure is miguous in the se of synhrotronF es will e presented in setion QFIFIFQD severl types of devies @ending mgnets or insertion deviesA llow for the genertion of photonsF woreoverD for synhrotron emD mny (lters nd optis our etween the soure nd the smpleD hnging its hrteristisF sn the se of n experimentD relevnt vlues re the one onerning the em tht interts with the smpleF hereforeD in tle QFID only vlues of the (nl em re givenD for three ip @iuropen ynhrotron dition pilityA emlines where experiments were rried outX shITeD shIWD nd shHIF sn the se of l soureD the generl priniples pply to ny soureD ut vlues given in this hpter pply more prtiulrly to the rdi tomogrphD whih ws used in this workF he hrteristis given here for xEry soures n e linked to the vlues provided in tle PFI @see hpter PA out hrteristis of eletron nd ion souresF le QFIX ome relevnt fetures of xEry souresD for one l soure @the rdi tomogrphA nd three ip emlinesX shITeD shIWD nd shHIF he given vlues re the ones otined ner the smpleD during this experiments presented in this workF 3.1.1.1 Relevant features of an x-ray beam hen ompring xEry ems from di'erent instrumentsD the minly used prmeter is the rilline BF st is somewht equivlent to the redued rightness presented for eletron nd ion ems @see hpter PAF frilline is de(ned sX

B = photons second • mrad 2 • (mm 2 sourcearea) • 0.1%BW @QFIA
st represents the numer of photons of given wvelength produed y the soure per seondD in surfe unit re nd for n ngle unit divergeneF he higher the rillineD the more photons of similr energy will reh the smple per seondF elthough rilline summrizes the min fetures of n xEry emD it n e roken down into simpler hrteristisD lso relevnt for the omprison of xE ry emsF heir desriptions re given hereD nd their vlues for lssi soures re provided in tle QFIF he )ux of the emD expressed in photonsGseond @ph./sec.AD is ritil pE rmeter for the speed of n experimentF e high )ux will llow for sttistil or even inEsitu experimentsF woreoverD high )ux will llow the (ltering of the em in energy while keeping enough photons for the tul experimentF sn the sme order of idesD the glol divergene of the em mkes the (ltering possile or notX if the em is too wideD fousing optis9 ngulr eptne will e too smll to pture nd fous the whole emD nd lrge frtion will e lostF ine the mnufturing of lrge xEry optis remins hllengeD otining low divergene em is very importnt for further (ltering nd fousingF he energy spred ∆E E nd the soure size de(ne the em ohereneF goherene of the em reltes to the ility of interferenes to our in the emD nd is useful for phseEontrst imging nd oherent di'rtionF he oherene of soure is deE (ned y the longitudinl nd trnsverse oherene lengthsD s well explined in UWF sn simple models of propgting wvesD the soure is often onsidered puntul nd monohromtiD whih is never the seF o illustrte the notion of ohereneD rel soure n e modeled s two soure points @the soure is not puntulA whih emit two wves with di'erent wvelengths @the soure is not monohromtiAF his leds to the two situtions illustrted in pigures QFI nd QFIF sn the (rst oneD two wves re emitted in sme diretion with slightly di'erent wvelengthF heir pigure QFIX vongitudinl nd trnsverse oherene lengthsF @A wo plne wves with di'erent wvelengths re emitted in the sme diretionF por lrity we hve shown the wves displed from eh other in the vertil diretionF @A wo wves with the sme wvelength re emitted from the puntul ends of (nite sized soure of height hF Image source: [79]F wvefront oinide t the origin @AD nd the longitudinl oherene is de(ned s the distne needed for the wvefronts to oinide ginF st is lso given y the expression QFPF

L L = λ 2 ∆λ = λ E ∆E @QFPA
where ∆λ @respF ∆EA is the di'erene etween the two wvelengths @respF energiesA nd λ the entrl wvelength @respF energyAF he longitudinl oherene refers to how monohromti the soure isF sn the seond situtionD two monohromti nd puntul souresD seprted y distne hD emit wves t wvelength λF he wves re oserved from the point F prom its point of viewD the two wves rrive from two slightly di'erent diretionsD seprted y ngle ∆θF he trnsverse oherene length is de(ned y the distne from the soure where the wvefronts will oinide @where the soure will pper puntulAF sts expression is given y eqution QFQF

L T = λ R D @QFQA
with nd h de(ned in pigure QFI nd λ the wvelength of the emF he trnsverse oherene refers to the size of the soureD s seen from the trget point of viewF he longer those two hrteristi distnesD the more oherent the soureF prom those equtionsD we n see tht to improve the oherene of the soureD one n redue its wvelength mplitudeD redue its ngulr divergeneD ndGor set the oservtion further wyF gonsequenes of this remrk will e disussed in setion QFPF 3.1.1.2 Laboratory sources pirst lortory xEry souresD lled goolidge tues nd (rst ommerilized in IWIPD were simply mde of metlli nodeD typilly tungstenD towrds whih n eletron em ws elertedF he em otined this wy is omposed of two prtsD s n e seen in pigure QFP @in lueAF pirstD the deelertion of eletrons retes remsstrhlung rditionD whih presents ontinuous spetrum whose mximum energy is the kineti energy of the inident emF sn dditionD muh more intense shrp peks pper on the spetrumF hey re )uoresene peksX when n energeti enough photon rehes the trget mteril tomsD it n ejet n inner eletronD reting holeF en externl eletron (lls the gpD nd this desexittion releses photonD with n energy spei( to the mterilF es the intertion etween the eletron em nd the node genertes hetD the thode must e wterEooledF ine the IWTHsD in order to dissipte het more e0ientlyD rotting node soures hve een ommerilly villeF he priniple of suh soures is illustrted in pigE ure QFQF he typil rightness otined with suh soures is fa10 8 ph./s/mrad 2 /mm 2 /0.1%BW D with )ux of 10 6 ph./sec. nd soure size of severl mironsF es the soure size is de(ned y the sphere of intertion etween the eletrons nd the thodeD furE ther studies im tody t fousing the eletron em on nnowiresF he soure size otined this wy is suEmironi VHF ell those soures however lk )ux when it omes to seleting spei( enerE gies for monohromti experiments for exmpleD nd generlly led to low sigE nl to noise rtiosF hey imply long quisition time @TH se for rdiogrphAD whih prevents ny timeEresolved experiment or sttistil studyF es presented in pigure QFRD synhrotrons soures o'er muh higher rillines @typilly 10 20 ph./s/mrad 2 /mm 2 /0.1%BW AD whih implies they re muh more verstile toolF 3.1.1.3 Synchrotron sources he priniples presented in this setion re vlid for ny third genertion synE hrotronD s they re sed on the sme rhitetureF heir preise fetures re however not extly the smeF ih synhrotron is est suited for set of ppliE tionsF sn this setionD exmples whih re provided illustrte the ipF ipD s ny third genertion synhrotronD is omposed of severl prtsD illusE trted in pigure QFSF pirstD IHH k triode pield imission qun provides n eletron em whih is injeted nd elerted inside liner setion @lled vsxegA thnks to series of rdioEfrequeny vitiesD until it quires n energy of PHH weF he eletron em is then trnsferred to irulr oosterD where it is elerted until it gets n energy of TFHR qeF yne this energy is rehedD the eletron em is trnsferred into the storge ringD whih hs irumferene of VRR m nd is under ultr high vum @`10 -8 mrD in order to void ollisionsAF he eletrons will trvel inside the ring severl hoursF he storge ringD despite its nmeD is tully polygonD with suessive liner setionsF et eh sumit of the polygonD ending mgnet @fwA ensures oth the devition of the eletronsD in order to keep them pigure QFPX ypil spetrum otined with di'erent types of xEry souresX rotting node @in lueAD ending mgnet @in purpleAD wiggler @in greenAD nd n undultor @in redAF pigure QFQX hemtis of A rotting node soureY A ending mgnet (source: http: //uspas.fnal.gov)Y A n undultor (source: http: //uspas.fnal.gov)F pigure QFRX ypil rilline of l nd synhrotron xEry souresF inside the loopD nd the retion of xEryD due to the sid devitionF sn the liner setionsD devies tht n produe xEry without hnging the eletrons9 glol diE retion n e insertedF hey re lled insertion devies @shAD nd n either e undultors or wigglersF pigure QFSX hemti view of typil third genertion synhrotronF Image source: wikipedia.org fending mgnets re used for two purposesF pirstD they mintin the eletron em inside the storge ringF fy doing so howeverD they modify the eletrons veloity nd therefore generte xEryF e ending mgnet is illustrted in pigure QFQ nd its typil spetrum is presented in pigure QFPF he energy spetrum of the xEry it produes is ontinuous nd overs rod spetrl rngeF he ritil wvelength λ c is de(ned s the wvelength tht seprtes the emitted power in two equl prtsF por the rdition emitted y ending mgnetsD it is de(ned @in nmA y eqution QFR VIX

λ c = 0.599 R E 3 = 1.865 B E e 2 @QFRA
E e is the eletrons energy in qeD the urvture in metersD nd f the mgneti indution of the ending mgnet in eslF λ c is representtive of the xEry energies rehle with given synhrotronD nd therefore the nlyses tht n e rried insideF et the ipD the eletrons hve n energy of TFHR qeD nd the ending mgnets produe HFV mgneti (eldF his leds to ritil wvelength of HFHT nm @or n energy of PI keAX the ip is optimized for hrd xEryF snsertion devies re pled in the stright regions of the storge ring nd re mde of numer x of mgnetsF sn undultors @see pigure QFQAD eletron re devited periodilly in the horizontl plne y wek mgneti (eldsF he emitted spetrum is mde of severl hrmoni peksD sine the ontriution of xEry from every period dd oherentlyF igglers on the ontrry ontins periodi strong mgnetsF he trjetory of eletrons inside the wiggler is not perfetly sinusoidlD nd the ontriutions dd inoherentlyX the emission is ontinuousD similrD lthough more intenseD to the one in ending mgnetsF ypil spetr from those three devies re presented together in pigure QFPF he shpe of the emitted em lso vries from one devie to notherF vet us de(ne γ s the rtio etween the eletrons energy nd the rest mss energyX

γ = E e -
Er D with the rest mss energy E r a m e -c 2 a 0.511 weF he one of emission for ending mgnet hs hlfEngle of θ = 1 γ D while the one oming from wiggler is muh lrgerF pinllyD the one for n undultor is muh shrperD nd depends on the numer of mgnets x it is mde ofF st is de(ned y θ = 1 γ• √ N F vet9s now fous more spei(lly on the intertions ourring etween the xEry em nd the mtterD nd wht informtion n e retrieved from themF 3.1.2 X-ray/matter interactions hen n xEry em enounters mtterD mny intertions n ourF wuh inE formtion n e otined from the result of these intertionsF his setion does not im t n exhustive desription of the intertions ourring etween xEry nd mtterD it is fr eyond the sope of this workF e here present generlly the possile intertionsD nd fous on those leding to trnsmission imging nd strin mesureD s they re the tehniques used hereF e lrger pnel of intertions is deE pited in UWD while mny pplitions of synhrotron rdition re well presented in VIF X-ray based strain measurement vet9s imgine sitution where monohromti photon em propgtes long diretion zD nd enounters smpleF sn ddition to eing group of photons trvE eling in the sme diretionD n xEry em n e desried s n eletromgneti plnr wve of wvelength λF es suhD the xEry em n e di'rted y fetures of the sme size s its wvelengthD typilly severl tens of ngstroms in the se of xEryF wore spei(llyD it will e di'rted y rystlline strutures in mtterD nd for em oherent enough interferenes will our fter the em leves the smpleF hose will rete di'rtion ptternsD tht n e reorded on detetorF hether the interferenes re onstrutive or destrutive depends on the inident ngleD s illustrted in pigure QFTF por every rystlline struture nd mterilD the inident ngles using onstrutive interferene re given y the frgg lw @see eqF QFSAF sf θ is the inident ngle of the em @etween the surfe nd the inident emAD the di'rted em will form n ngle of 2θ with the originl diretion of the emF

2d • sin θ = m • λ
@QFSA where θ is the ngle etween the smple surfe nd the inident emD λ the wvelength of the emD d the interplnr spingD nd m positive integerF he pprition of the di'rtion pttern is highly dependent on the inident ngle nd the interplnr sping dX ompression or dilttion of the lttie n e seen on pigure QFTX sllustrtion of the onstrutive nd destrutive interferene ourring fter rystlline strutureD depending on the inident ngle of the emD on whih the vlue of the phse shift reliesF Image source: WikipediaF the di'rtion ptternF ine λ is lose to dD xEry di'rtion is wellEdpted tool for strin mesurement inside rystlline strutures nd hs given rise to vriety of tehniquesD inluding vue di'rtionD mde in trnsmissionD nd frgg di'rtionD performed in re)etionF sn this studyD only frgg di'rtion with monohromti em will e studiedF he experimentl setupD together with the nlysis priniplesD will e presented in setion QFRF X-ray based imaging Ery ttenution in mtter n e desried y four min e'etsX the photoeletri e'etD the yleigh stteringD the gompton e'et nd pir produtionF eording to the tomi numer of the smple nd the photons energyD one or nother will e predominntD nd some n e negletedF por energies nd mterils onsidered in this workD the photoeletri e'et is predominntD s presented in pigure QFUF he photoeletri e'et ours when photon is fully sored y n tomD nd ejets n inner eletronD whih is lled photoeletronD ioninzing the tom @see pigure QFVAF sn order for the tom to eome stleD n eletron from n outer lyer will reple the ejeted eletronF he energy relesed y suh n opertion will e ejeted in the form of photonD whih energy will e equl to the energy gp etween the two lyersF his is lled )uoresent emission nd is illustrted in pigure QFVF he xEry em eing plnr wveD if trveling in vuumD it n e desried y its wvenumer kD linked to its wvelength y k = 2π λ F sn mediumD for wve propgting long diretion zD the front wve eomesX φ(x, y, z) = exp(ikn(x, y, z)z), @QFTA where n is the omplex refrtive index of the mediumD de(ned for eh @xDyDzA pigure QFUX egions of reltive predominne of the three min forms of photon intertion with mtterF he purple region represents the energies used for imging in this study @IU ke nd QQFT keAD nd the onsidered mterilsX i @aIRAD gu @aPWAD eg @aRUAD nd n @aSHA VPF pigure QFVX sllustrtionD t the tomi sleD of the sorption nd )uoresene phenomenF point of the medium y eqution QFUF n forms into rel prtD 1 -δD with δ the refrtive index derementD nd n imginry prt βD the sorption indexF δ is usully very lose to zero @10 -5 in solids nd 10 -8 in irA nd positiveD whih mkes the rel prt of the refrtive index inferior to I for xEryF δ reltes to the phse shift tht the wve undergoes inside mediumF β desries the derese of mplitude of the em while going through the mediumF hose two e'etsD in the se of the em going through smpleD re illustrted in pigure QFWF n(x, y, z) = 1 -δ(x, y, z) + iβ(x, y, z) @QFUA pigure QFWX sllustrtion of the sorption nd the phse shift phenomen when n xEry em goes through smpleF es the em trvels inside the mterilD its totl phse shift nd the ttenution of its mplitude re proportionl to the length it hs overed in the sid mterilF vet9s ssume the em is monohromtiD of energy E 0 F por the mplitudeD if we de(ne N 0 (E 0 ) the numer of photons rriving t the smpleD nd N t (E 0 ) the numer of photons present fter length t long the propgtion diretion zD the feerEvmert lw providesX

N t (E 0 ) = N 0 (E 0 ) • exp(- path µ(z, E 0 )dz)
@QFVA with µ eing de(ned s the liner ttenution oe0ientD linked to β y eqF QFWF

µ(x, y, z) = 4π λ β(x, y, z)
@QFWA he feerEvmert lw desries the frtion of photons whih re neither E sored or sttered y the smple per length unitD nd is hrteristi of the mE terilD s it is proportionl to its tomi numer F hereforeD mesuring the rtio etween inident photons nd exiting ones provide informtion out the smpleF esorption imging tehniques use this property to imge the inside of ojetsF st is widely used in the medil setorD where it provides high ontrst etween ones nd surrounding mterilsF wost of l tomogrphs imed for industril imging lso use sorption imgingF δ is lso hrteristi of the mterilD nd n even e linked to the lol eletroni density ρ e y eqF QFIH @where r c is the lssil eletron rdiusAF

δ = r c λ 2 2π ρ e
@QFIHA he vlue of δ would therefore provide informtion out the omposition of the smpleF he mesurement of the phse is however not diretD s detetor is only ple of mesuring the intensityF por oherent enough em howeverD interferenes n our fter the em exits the smpleF snterferene fringes tht n e ptured y detetorX they will e oservle on the rw rdiogrphsF everl experimentl setups exist to mke those interferenes hppenD ndD in mny sesD provide muh etter ontrst thn sorption imgingD s will e presented in setion QFQFIFPF es presented in this setionD mny intertions our etween the xEry em nd ondensed mtterF hepending on the informtion one wnts to otin @morphologyD strinD etFAD onstrints on the em fetures will e di'erentF xext setion presents the em otined inside typil l tomogrphD followed y the desription of three ip emlinesD together with the demnds they re designed to meetF 3.2 Experimental setups: tuning the x-ray path and the detection system hepending on the (nl experimentl setupD the requirements for the xEry em rehing the smple will not e the smeF e l soure suh s the rdi tomoE grph o'ers ontinuous lrge spetrum propgting in every diretion of spe @inluding towrds the smpleAF he relevnt prt of the em is oneEshpedD nd the soure size depends on the intertion sphere etween the originl eletron em nd mtterF sullyD the detetion of photons is mde using sintilltorD followed y visile light optis tht llow for further mgni(tionD efore the em rehes ggh @ghrge goupled hevieA detetorF es mentioned previouslyD synhrotron soures o'er more ltitude for em dE justments to given useD due to their high )ux omined with reltively low diverE geneF sn the next setionsD three ip emlines re presentedD with their originl spei(tionsD the min optis hosen to ful(ll those requirementsD nd the detetors used to perform the experimentsF shIW nd shITe re two long emlinesD imed for high resolution imgingD respetively t pixels sizes elow the miron nd elow SH nmF shIW ims t fst dt quisition nd postEproessing for industril ppliE tionsF shITe9s experiment setup implies longer quisition nd postEproessingD s it ims for higher resolutionF shHI is lso long emlineD designed for di'rtion nlysisF st is quite verstileD nd only its pity to lolly mesure strin with oherent frgg di'rtion ws used during this workF emong those three emlinesD shHI nd shITe were uilt during the (rst phse of the ip upgrdeD tht hs run from PHHW to PHISF ell three re long emlinesD tht exploit the oherene of the emF hey ene(t from stteEofEtheErt developE ments in vrious (elds linked to xEryF sn ftD the soure itself is third genertion synhrotronD optimized for hrd xEryD s explined in QFIFIFQF Ery optis inlude monohromtors nd presnel pltes tht use ltests tehnologies developed origiE nlly for the miroeletronis industryD in prtiulr for surfe preprtionF tges re preisely ontrolled vi piezoeletri motorsD while detetors hve een improved in order to inrese the resolution nd the redEout timeD to mke the most out of the inoming emF pinllyD s will e presented in the next prtD lgorithms hve een written to quire nd exploit the dt from those emlineD mking the exE periments s e0ient s possileF hose emlinesD mong other newlyEonstruted onesD re the outome of mny yers of engineering nd physisD performed in vrious (eldsF 3.2.1 ID16A: a nano-tomography beamline shITe is newlyEuilt emlineD s (rst experiments were onduted t the end of PHIRF sts gol is high resolution Ph nd Qh imging for iologyD mediineD nd nnoE tehnologyF o hieve thisD smll soureD together with high )ux nd ohereneD re neessryF prom eqF QFP nd eqF QFQD it hs een deduted tht improving the oherene of the em implies either improving the monohromtiityD or setting the oservtion point fr wy from the xEry soure @or oth3AF o hieve its oherene golD shITe is long emlineX IVS m seprte the originl xEry soure from the smpleF pigure QFIH provides very simpli(ed view of the optil pth etween the originl xEry soure nd the em interting with the smpleF his optil pth is desried herefterF pigure QFIHX impli(ed view of the optil pth in the shITe emlineF he em9s trjetory goes from left to rightF pper sheme shows the top view of the emD where only the uf @uirkptrikEfezA mirror is presentF he lower shemeD showing the pro(le view of the emD fetures the monohromtorD the slitsD nd the uf @uirkptrikEfezA mirrorF he smple is pled fter the (nl fousF wo inEir revolverEtype undultors set in series produe the xEryF hepending on the hosen mgnet periodD they provide either xEry with n energy of IU ke @with period of IVFQ mmA or QQFT ke @with period of PPFR mmAF he emission rilline t this point is 8.2 • 10 19 ph./s/mrad 2 /mm 2 /0.1%BW t IU ke nd 2.5 • 10 19 ph./s/mrad 2 /mm 2 /0.1%BW t QQFT ke VQF efter the xEry genertionD the generl ide is to limit s muh s possile the numer of optis present on the optil pthD in order to preserve the oherene of the emF he originl xEry soure mesures PP µm in the vertil diretion @with divergene of UFR µradAD nd WRH µm in the horizontl one @with divergene of PS µradAF st is therefore possile to let the em propgte freely in the vertil diretionD ut the soure must e demgni(ed in the horizontl diretionD otherwise most of the em will e lost in the fousing proess to omeF woreoverD the em hs to e monohromtized efore it rehes the experimentl huthF et PV m from the soureD the em therefore enounters mutliElyer monohromtorF sts gol is twofoldF pirstD the di'erent lyers overing the spheril mirror it is mde of im t seletingD using frgg onditionD one hrmoni of the emD improving its monohromtiityF sn dditionD its spheril shpe fouses the em in the horizontl diretionF hisD omined with slitsD retes SH µm wide horizontl seondry soureD t RH m from the originl oneF he em is then monohromti with ∆E E = 10 -2 D whih is rther modest for synhrotronD ut the use of suh monohromtor @insted of rystl monohromtor for exmpleA is justi(ed y the will to sve the )ux of the originl emF efter propgting long IVS m from the xEry soureD the em rehes the experimentl huthF hereD it is foused in oth horizontl nd vertil diretionsD using pir of uirkptrikEfez @ufA mirrors VRD s illustrted in pigure QFIIF hey re urved sustrteD oted with multilyer depositD nd pir of those mirrors @one in eh diretionA hs een designed for eh energy @IU ke nd QQFT keAF uh setup llows to fous the em down to IQ nm VSD VTF his fous size is minly used for snning pplitionsD suh s ptyhogrphy nd )uoreseneY during the experiments performed in this workD the fous ws mesured to e QV x PU @horizontl x vertilA t IUFS ke @in perury PHISA nd PU nm x PI nm @horizontl x vertilA t QQFT ke @in tuly PHISAF he uf mirrors re pled inside vessel under vuumD where the smple stge is lso lotedF efter interting with the smpleD the em n e ptured y severl types of detetorsF por the quisition of holoEtomogrphy projetionsD the detetor uses semiEtrnsprent sintilltor llowing the em to propgte towrds pevox ggh @pst edout vow xoiseA imge sensorF st mesures PHRV pixels x PHRV pixels with n e'etive pixel size of IFI µmF es the em is folisedD it is oneEshped while interting with the smpleD nd the reorded imges re mgni(ed when rehing the detetorF his llows for n improvement of the resolutionX y setting the soureEtoEsmple nd smpleEtoE detetor distnesD one n hoose mgni(tion of the ojetF et the shITe emlineD it lso possile to perform )uoresene snning imgE ingF he smple is then pled in fousD nd the exiting em is ptured y two pigure QFIIX sllustrtion of the xEry em fousing using pir of uf mirrorsF Image source: http: //www.spring8.or.jp six elements silion drift diode detetorsF huring this workD one experiment t the shITe emline ws performed t IU keF he other S were performed t QQFT keF goherene lengths n e lulted for the emlineD using eqF QFP nd eqF QFQF qiven the fetures of the emD one otins longitudinl oherene length of UFQ nm t IU ke nd QFT nm t QQFT ke Fhe trverse oherene length is @horizontl x vertilA IRFR µm x TII µm t IU keD nd UFQ µm x QIH µm t QQFT keF 3.2.2 ID19: a versatile tool for coherent imaging and diraction shIW is lso sed on oherent imging nd is therefore long emlineX the exE perimentl huth is pled IRS m wy for the xEry soureF roweverD it is imed t eing more verstile thn the shITe emlineF st llows for fst tomogrphyD lminogrphyD nd di'rtion mesuresF R undultors nd I wiggler re ville on shIWF yne of them is hosen ording to the experimentl needsD nd typilly leds to soure size of @horizontl x vertilA IPH µm x QH µmF hey provide lrge spetrum emD rnging from T to PSH keF foth multilyer nd rystl monohromtor re villeD leding respetively to monohromtiity of 10 -2 nd 10 -4 F lits llow the seletion of the inner nd oherent prt of the emD whih leds to prllel em rehing the smpleF huring the experiments presented hereD xEry were provided y IQ shortE period permnentEmgnet undultorD with period of IQ mmD whih o'ered n energy of PTFS ke @with ∆E E = 10 -4 AF elong the optil pthD n PFV mm el (lter ws usedD nd the em ws ollimted using IH fe lensesF es for the shITe emlineD the detetion of photon is indiretD sintilltor (rst onverts photons to visile lightF sn this se howeverD de)etion mirror is pled fter the sintilltor nd direts the em towrds the ggh merF woreoverD ojetive lenses re pled etween the sintilltor nd the mirrorD in order to dd mgni(tion to the otined projetionsF et PTFS keD the longitudinl oherene length t shIW is out RU nm @using rystl monohromtorAD while the trnsverse oherene length is out @horizontl x vertilA IHWµm x RP µmF 3.2.3 ID01: Local strain measurement shHI is ment for oherent di'rtionF st hs een upgrded in PHIR nd is now long emlineD s IIV meters seprte the xEry soure from the experimentl huthF wny experiments n e performed on this emlineD inluding smllEngle xEry sttering @eAD grzingEinidene di'rtion @qshA nd grzingEinidente smll ngle xEry sttering @qseAF e here fous on the optil pth leding to frgg oherent di'rtion experimentsF o generte xEryD eletrons pss through three undultors set in seriesF his llows the emline to tune its energy from S ke to TH keD y hnging the gp eE tween the mgnets of the undultorsF he horizontl divergene of the em is then redued y white em mirrorD whih lso direts it towrds the monohromtorD whih is i@IIIA frgg monohromtorF his elements provides monohromti emD with ∆E E = 10 -4 F purther wy from the soureD trnsfotor using SV fe lenses fouses the em vertillyD while inresing the )ux densityF et tht pointD the size of the xEry em is igger thn its oherene lengthF o perform the experE imentsD only the oherent prt of the em must e seletedX moile horizontl nd vertil slits re usully pled right efore the smpleD nd the open re etween them is elow the theoretil trnsverse oherene lengths @severl tens or hundred of µmAF sn order oth to hve lol informtion nd to inrese the )ux foused on the smpleD fousing optis re then usedF sn this seD presnel one ltes re usedD s they o'er the smllest fous sizeF he urrent fousing optis re optimized for n energy of V keD nd then llow for fous size of out @horizontl x vertilA QHH nm x PHH nmF he )ux (nlly rehing the smple is out 10 9 ph.s -1 VUF he Ph detetionD whih is the only one performed during this workD is mde with Ph wess VVF st is photonEounting systemD with SIT pixels x SIT pixelsD the pixel size eing SS µmF sn this workD two experiments were rried on the shHI emlineF yne ws performed t n energy of V keD nd the seond t n energy of W keF qiven the fetures of the emline @size of the xEry soureD length of the emlineD together with the energy ndwidthAD equtions QFP nd QFQ provide vlue of IFR µm @respF IFSS µmA for the longitudinl oherene length t W ke @respF V keAF he trnsverse oherene length is @horizontl x vertilA IPS µm x VIP µm t W ke @respF IRH µm x WIP µm t V keAF sntertions etween xEry nd mtter generte muh informtion tht n e used to hrterize smplesF woreoverD xEry soures n e highly dptle to the experimentl needsD s illustrted with Q ip emlinesF sn the two next setionsD we will fous on the experimentl setups nd postEproessing leding to xEry Qh imging nd strin mesurementD respetivelyF 3.3 X-ray transmission 3D imaging fsed on the intertions of xEry with mtterD severl imging tehniques hve een developedF rere we present the experimentl setups used in this study nd the imging tehniques they led toF hey n e sed on the illumintion of the whole smpleD s in sorption nd phse ontrst imgingD or e performed y snning the smple pled inside the fousF his lst setup is used in )uoresene imgingD to otin lol informtion on the smple hemistryF hose Ph imging tehniques re presented in the (rst setion @QFQFIAF es will e shownD the Ph imges otined re projetions of the smple hrE teristis long the xEry em propgtion diretionF es suhD severl imges tken from di'erent ngles n e omined nd form Qh digitl reonstrution of the ojetF he spei( setups to do soD together with severl reonstrution lgorithmsD re presented in setion QFQFPF ih experimentl setup hs its limits nd onstrintsF sn prtiulrD the requireE ments for the smple shpes nd size will di'er from one to notherF e summry of these requirementsD together with the smple preprtion methods used to nswers themD is provided in setion QFQFQF everl experimentl setupsD with di'erent tehniques nd prmetersD were used in this workF por lerer further redingD tle QFP summrizes those feturesF es presented in setion QFIFPD when n xEry em trvels through smpleD long diretion zD its mplitude is reduedD nd its phse shiftedF hen detetor ptures the exiting emD the reorded intensity on the detetor is proportionl to the squre of the wve modulusF he intertion etween the wve nd the smpleD for rottion ngle θD n e desried y trnsmittne funtion T θ D de(ned sX

T θ = exp(-B θ (x) + iφ θ (x))
@QFIPA where x is the projetion plne @xDyAD nd B θ nd φ θ the projetions long the smple of the sorption index nd the refrtive index derementD respetivelyF hey n e written sX

B θ = 2π λ β(x, z)dz @QFIQA φ θ = -2π λ δ n (x, z)dz @QFIRA
vet9s now imgine the projetion plne is situted right fter the smple @haH in pigure QFIPAF henD if the inident wve front is u inc D the wve front rehing the detetor isX

u 0,θ = T θ (x)u inc (x)
@QFISA hereforeD the intensity mesured y the detetor isX

I 0,θ = |u 0,θ (x)| 2 @QFITA = |T θ (x)u inc (x)| 2 @QFIUA = |e -B θ (x) | 2 • |e iφ θ (x) | 2 • |u inc (x)| 2 @QFIVA es φ θ is rel numerD |e iφ θ (x) | = 1F woreoverD y de(nition |u inc (x)| 2 = I 0 F reneX I 0,θ = I 0 |e -B θ (x) | 2 @QFIWA = I 0 • e -2B θ (x)
@QFPHA he lst line orresponds to the feerEvmert lw for sorption imgingD stted in eqF QFVF ytining the projeted vlue of β is however not diretD sine the detetor often presents drk urrentF wterils n still e distinguished y the grey levels of the imgeD s n e seen in pigure QFIQX the opper the smple is mde of n e distinguished from the silion it stnds onF his tehnique is lrgely used in l tomogrphy setups nd medil imgingD ut enounters limits for mterils with lose tomi numers or wekly soring mterilsF his tehnique is lrgely used in l tomogrphy setupsD for exmple in the eiss rdi tomogrph used in this studyF 3.3.1.2 Phase contrast imaging es presented in the previous setionD imging ontrst n e otined y mesuring the sorption underwent y the em when rossing the smpleF roweverD this method rehes its limit for lose tomi numers or low soring mterilsF hseE ontrst imging is sed on the em phseEshift ourring in the smple nd the sttering of the emF st is diretly linked to the vlue of δF pigure QFIR represents the rtio δ β in funtion of the energy for opper nd silionF por hrd xEryD δ is severl orders of mgnitude higher thn βF ytining phse mp @representing δA rther thn n sorption mp @representing βA would therefore provide high sensitivity imgesF nfortuntelyD the vlue of the phse shift is not diretly essile on the E quired projetionsF hse ontrst tehniques must e implemented in order to enE ode enough informtion on the rdiogrphsD on whih phse retrievl lgorithm must then e ppliedF everl experimentl setups llow to pture phseEontrst on detetorD suh s rystl interferometry WHD nlyzerEsed phse imging WID grtingEsed phse imging WPD or the edgeEillumintion tehnique WQF he simplest method pigure QFIQX diogrphs of SH µm wide opper pillrD otined with two di'erent tehniquesF A esorption ontrst imging otined on the rdi l tomogrphF A phse ontrst imging on shITeF A zoomedEin view of imge F dA zoomedEin view of imge D where interferene fringes re lerly visileF pigure QFIRX δ/β rtio of opper @in lueA nd silion @in red dshed lineAD s funtion of the energyF ht soureX op softwre VW to otin suh ontrst is propgtionEsed phse ontrst imgingD or free spe propgtion phse ontrst imgingF st relies on the propgtion of sptilly oherE ent em in the spe etween the smple nd the detetorF o otin higher phse ontrstD the distne etween the smple nd the detetor is simply inresedF sn prtieD on the shITe emline it is done y hnging the fousEtoEsmple distne @while the fousEtoEdetetor distne remins the smeAD while in shIW the smple remins t the sme position nd the detetor is movedF sn the se where further free propgtion is llowed fter the smple @hbHAD presnel trnsform must e dded to the otined wve frontF st requires the use of propgtor noted P D D whih form is given in eqF QFPI @where λ is the monohromti em wvelength nd h the propgtion distneA WRF

P D (x) = 1 iλD exp(i π λD |x| 2 )
@QFPIA essuming u inc (x) a ID the wve front on the projetion plne x is the onvolution of the trnsmission funtion inside the smple nd the propgtor long distne h fter the smpleX

u θ,D (x)(T θ * P D )(x)
@QFPPA his leds to the expression of the intensity on the detetorD expressed here in the pourier domin WSX

ĨD (f) = T θ (x - λDf 2 )T * θ (x + λDf 2 ) exp(-2ix.f)dx @QFPQA
he olleted intensity is linked quntittively to the phse shift of the wveF sn prtieD interferene fringes pper on the rdiogrphsD s n e seen in pigE ure QFIQ nd dF he propgtion is diret proessD nd retrieving the phse shift from the rdiogrphs is the orresponding inverse prolemF es it is quite omplexD severl pproximtions nd lineriztions of the prolem hve een deE veloped WTD WUF he gontrst rnsfer puntion @gpA is wellEdpted to slowly vrying phse nd wekly ttenuting ojets nd hs een minly used hereF sn this pproximtionD the trnsmission funtion is developed to the (rst orderD rising T θ (x) = 1 -B(x) + iφ(x)F his ledsD when sustituting this expression in eqF QFPQD to new expression of the intensity @still in the pourier dominAX

ĨD (f) = δ(f) -2cos(πλD|f| 2 ) B(f) + 2sin(πλD|f| 2 ) φ(f)
@QFPRA where δ is the impulse funtionD B(f) nd φ(f) re the pourier trnsforms of the sorption nd the phseD respetivelyF his expression n e solved oth for the sorption f nd the phse φD ut present the drwk of hving zero rossings for given frequenies f of the pourier dominF o overome this issueD rdiogrphs n e quired t di'erent smpleEtoEdetetor distnes nd ompiled to provide one projetionF he distnes will hve to e hosen suh s the zero rossings do not our for the sme frequeniesF enother pproximtionD the rnsport of sntensity iqution @siA WVD is more dpted to prllel ems nd smll propgtion disE tnesF e mixed pproh etween the two o'er the possiility to retrieve the phse from soring mterilsD suh s the ones enountered in Qh integrtionD pled in one emF he method onsisting in the quisition of four di'erent projetionsD when omined with tomogrphyD is lled holoEtomogrphy WWD IHHF st is illustrted in pigure QFISF pigures QFITEd present n exmple of four rdiogrphs quired y holoEtomogrphyD nd the (nl projetion otined fter the phse retrievl proeE dureF es presented in this setionD phse ontrst is oservle on sorption rdioE grphsD provided oherent enough soure nd su0ient distne of propgtion etween the smple nd the detetorF hose re onditions hievle oth on the shITe nd shIW emlinesF diogrphs otined on shITe re usully E quired using the fourEdistne sheme nd used fter phse retrievl proedureF he fousEtoEdetetor distne ws typilly I meterD while the fousEtoEsmple disE tnes were kept round I neF he rdiogrphs otined on shIW were diretly used during this workF sn suh projetionsD the phse ontrst minly ppers on the edges of mterilsD s the sttering is higherF he rdiogrphs n therefore e onsidered s sorption projetionsD with n edge enhnement due to the phse ontrstF his improves the imging of voids in opper pillrs nd opper pds for exmpleF 3.3.1.3 Fluorescence imaging es depited in setion QFIFPD the sorption of n inident photon y n tom n trigger the emission of nother photonD whih energy will e hrteristi of the tomF his gives rise to the )uoresene tehniqueD illustrted in pigure QFISF he pigure QFISX sllustrtion of the Qh imging setups presented in this setionF A esorptionEsed tomogrphyF A rolotomogrphy @propgtionEsed phse onE trst imgingAF A pluoresene tomogrphyF dA vminogrphyF pigure QFITX EdA w rdiogrphs on opper pillr otined on the shITe emlineD t four di'erent distnesF eA rojetion otined fter the phse retrievl proedureD omining imges D D D nd dF ide is to illuminte the smple with the xEry em nd to detet the exiting photonsF fy seleting them y their energyD one otins spetrum presenting ll the present elementsF e (tting proessD where peks of the spetrum re linked to their origin mterilD provides n informtion on the hemistry of the smple in the re illuminted y the emF he pixel size is limited y the size of the em rossE setion on the smpleF sn synhrotronD it is possile to fous the em down to severl tens of nnometersF his llows one to otin hemil mp of the smpleD y shifting it inside the fousD in plne @xDyA orthogonl to the xEry emF pei( (tting tools re implemented to otin n urte distriution of elementsF sn ftD severl side e'ets must e tken into ountD mong whih the reEsorption of emitted photons y the smple itselfF sn ddition to reEsorption numeri models tht improve the (ttingD for the mesure to e onsidered quntittiveD the smple must e smll enough to limit reEsorptionF he )uoresene quisitions relized in this work were performed t the shITe emlineF wo detetors ollet the exiting photonsF hey re pled on opposite sides of the smpleD in order to ollet s mny photons s possileF he vessel in whih the smples re pled is under vuumD whih improves the qulity of the nlysis s it redues sorptionF prom dt set of the Ph projetion imgesD one n reonstrut n urte enough Qh volumeD provided some onditions on the setup geometryD the numer nd distriution of the quired projetionsD nd the use of n dpted reonstrution lgorithmF ell those fetures re desried in the next setionF 3.3.2 Obtaining a 3D reconstruction sn the previous setionD severl wys of otining Ph projetion of smple were explined nd illustrtedF hose projetions n e omined together in order to otin Qh reonstrution of the ojetF rere we present two experimentl setups to do so E tomogrphy nd lminogrphyF hey re illustrted respetively in pigure QFISE nd QFISdF eonstrution lgorithms re lso presented nd disussed in this setionF por lerer visuliztionD ll exmples re presented for Ph reonstrution with quisitions mde with prllel emF xottions from the previous setion re keptX the xEry em propgtes long zD nd the imged ojet is de(ned in the plne @xDzA y funtion f F f is usully tken s µD ut it hs een shown the equtions given here lso pply to δ IHIF he smple9s orienttion in the plne is de(ned y the ngle θD s given in pigure QFIPF he Ih detetor is therefore de(ned y line zaonstntF hey n e esily dpted to Qh situtionF he don trnsformD here noted RD de(nes the reltionship etween the funE tion f nd the signl otined on the detetorF he trnsformD when pplied to the funtion f nd for projetion long pth of length LD is de(ned sX

Rf = L f (x, z)dz @QFPSA
st n e shown tht this trnsform is diretly linked to the pourier trnsform of the ojetF sn ftD the pourier slie theorem sttes tht the Ih pourier trnsform of n ojet9s projetion t n ngle θ is equl to the Ph pourier trnsform of the ojet long line forming n ngle θ with the siss nd pssing through the originF hereforeD the don trnsform o'ers smpling of the ojet in the pourier dominF end sine the pourier trnsform is ijetiveD y quiring enough projetions @t di'erent ngles θA of the ojetD on n reonstrut the ojet in the pourier dominD nd then in the rel speF 3.3.2.1 Experimental setups: tomography, holo-tomography, and laminography o otin reonstrution of the ojetD projetions must e quired regulrlyD with evenly distriuted ngles θ long IVH • or QTH • F o do soD (rst experimentl setup is the tomogrphy oneD illustrted in pigure QFISF he smple is pled in the xEry emD nd is rotted round the xis yD orthogonl to the emF sn the se of holoEtomogrphyD this proedure will e dptedX the whole rottion will e performed t R fousEtoEsmple distnesD s illustrted in pigure QFISF por those setupsD it is possile to perform lol @or zoomEinA tomogrphyF st onsists in pling the smple suh s it is lrger thn the (eld of viewF his llows to improve the resolution without thinning the smpleD ut my lso trigger some rtefts IHPF pluoresene tomogrphy n lso e performed using the tomogrphy setupD y pling the smple in the fous @see pigure QFISAF por those experimentl setupsD n issue rises in the se of lminr smple @typilly piee of wferAF e Ph smple de(ned y dimensions E nd F is lled lminr when one of its dimensions @for exmple EA is muh smller tht the other @hereD F AF por given nglesD when diretion F is prllel to the xEry emD the em will e highly soredD muh more thn when the diretion F is orthogonl to the emF heir will e lk of informtionD lled missing wedgeD oming from this @thoseA ngle@sAD whih will redue the resolution of the reonstrutionF o void thisD seond setup n e set for lminr smplesF st is lled lminogrphy nd is illustrted in pigure QFISdF he rottion is mde round n xis whih is slightly tilted from the y xisD in the @yzA plneF his wyD projetions n e quired without rehing the sitution of missing wedge desried erlierF sn this workD tomogrphy hs een performed on the rdi tomogrphD nd on the shITe nd shIW emlinesF vminogrphy ws lso performed in shIWF he Qh reonstrution lgorithms rely on the sme priniples for ll setupsF hey re presented in next setionF

Reconstruction algorithms

Analytical methods e (rst reonstrution lgorithm n e diretly deduted from the pourierEslie theorem IHQF st sttes tht the Ih pourier rnsform of the projetion t ngle θ of n ojet is equl to the Ph pourier trnsform of the sid ojetD evluted on line pssing through the origin nd forming n ngle θ with the xisF hereforeD it is possile to reonstrut the ojet in the pourier dominD nd pply n inverse pourier trnsformF nfortuntelyD this requires to perform n interpoltion in the pourier dominD whih leds to serious distortionF roweverD the theorem expression lso leds to more intuitive reonstrution lgorithmD lled the piltered fk rojetion @pfA lgorithmF ih projetion is (rst (lteredD nd kEprojetedF he ddition of ll kEprojetions provides the (nl imgeD s n e seen in pigure QFIUF he kEprojetion proess implies to pss from polr oordintes @rDθA to rtesin ones @xDyAF his tends to highlight low frequeniesF e (lter @typilly rmp oneA ensures ll the frequenies re eqully represented in the (nl reonstrutionF pigure QFIUX hemti view of the piltered fk rojetion reonstrution proessF smge soureX dpted from IHR es pf relies on the smpling of the pourier dominD it ides y smpling rules nd demnds mny projetionsF sn ftD s the projetions re smpling of the pourier dominD nd if the detetor pixel size ∆r is onsidered the resolution limitD then the ngulr step etween projetions should e ∆θ • δrF yn hlfEirle rottionD this risesX N ∆θ = πr @QFPTA with N the numer of quired projetions nd r the ojet rdiusF por n ojet imged on detetor hving M pixelsD r n lso e written s r = ∆r(M -1) 2 F he theoretil vlue of N is therefore given yX

N = π 2 M
@QFPUA por PHRV pixel lrge detetorD the numer of projetions should therefore e N = 3200F ith this mount of projetionsD the pf lgorithm is onsidered to pigure QFIVX hemti view of the itertive reonstrution proessF Image source: [105]F provide n urte reonstrution of the ojetF sn prtieD QPHH projetions re indeed quired on shIWD while reonstrutions on the shITe emline were sed on PHHH projetions or even ISHHF sn order to limit the numer of projetions needed @nd lso to limit the reonE strution sensitivity to noiseAD other reonstrution lgorithmsD known s itertiveD hve een developedF Algebraic iterative methods pf is n nlytil methodD sine the disretizE tion of the dt ours when implementing the reonstrutionF yn the ontrryD lgeri methods suh s itertive ones diretly use disrete dtF hey rely on the disretiztion of the spe nd the smpleF he smple is no longer de(ned y funtion f@xDyAD ut y set of disrete vlues f i D lled pixelsF he don trnsform is represented y projetor mtrix RD nd the quired projetion P n e written sX P = Rf @QFPVA rovided the geometry of the experimentl setup @in prtiulr the shpe of the emAD the mtrix n e knownF he diret inversion of the mtrix D in order to otin f from D is theoretilly possileD ut given the size of the mtriesD impossile to implementF stertive minimiztion methods re therefore ppliedD only using the knowledge of nd the implementtion of the forwrd projetion it leds toF et the (rst itertionD the funtion f 0 is usully tken s the null mtrixF et eh itertionD the mtrix f will e lulted reltively to its vlue t the previous itertion IHTX

f (n+1) i = f (n) i + λ (n) ∆f (n) i @QFPWA here λ (n) is relxtion prmeterD nd ∆f (n)
i the lulted normlized difE ferene etween the urrent reonstrution forwrd projetion nd the tul experE imentl dtD s illustrted in pigure QFIVF he wy this di'erene is lulted is the min distintion etween the existing itertive lgorithmsF st will hve n imE pt on the onvergene riterion of the lgorithmD nd on the numer of itertions neededF wny itertive lgorithms existD here only the ones used in this work re presentedF sn the e @elgeri eonstrution ehniqueA lgorithmD the distne is lulted for eh pixelD projetion fter projetionF ih pixel is therefore modi(ed severl times during one itertionF es every pixel is delt with seprtelyD the e lgorithm is little roust to noiseF s @imultneous stertive eonstrution ehniqueAD on the ontrryD ompres the whole quired projetions with the ones generted from the urrent reonstrutionF his mkes the lgorithm slower thn eD ut more roustF he gqEv @gonjugte qrdient E vest qureA lgorithm is very similr to sD ut lultes distnes using the L 1 norm insted of L 2 F he e lgorithm modi(es the reonstrution fter kEprojeting ll the pixels @like sA from one projetion @like eAF he e lgorithm therefore ene(ts from the stility from s nd the fst lultion of eF es mentioned erlierD itertive lgorithms hve minly een developed for eleE tron tomogrphyD nd hve een pplied to xEry tomogrphy sine IHUD IHSD IHVF sn this workD some of them hve een tested on shITe dtF he results re preE sented in setion SFQF 3.3.3 Sample Preparation rere we present the onstrints on the smples shpes nd sizes linked to the exE perimentl setupsF e (rst onstrint omes from the penetrtion depth of xEry inside the smpleF rnsmission imging relies on the ft tht the photons Et lest some of themE re le to exit the smple nd reh the detetorF e too E soring mteril or too low energy will led the low signl to noise rtio nd poor reonstrutionsF qiven mteril nd n energyD the size of the smple must e dptedF he seond origin for those onstrints is the (eld of view rehle y given experimentl setupF his is diretly linked to the setup geometry nd the size of the detetorF vet9s (rst fous on the energies nd penetrtion depthsF he xEry ttenution length L p is de(ned s the distne in the smple fter whih the proportion of nonEsored nd nonEsttered photons is e -1 F le QFQ provides the vlues of the xEry ttenution length L P for silion nd opperD t the energies used in the experimentl setups from this setionF he vlues of β re otined using y softwre VWD nd µ re derived from them @see eqFQFWAF he feerEvmert lw then rises L p = 1 µ F 17keV 19 keV 26.5 keV 33.6 keV gopper PI PW TT IRH ilion SWW VPT PIUR RHHH le QFQX lues of xEry ttenution length L p @in µmA in silion nd opperD for energies used during this hhF prom tle QFQD it is visile tht for the onsidered energiesD smple must e quite smllF hepending on the mount of opperD n experiment t QQFT ke @s performed tody t shITeA my require smples elow PHH µm for exmpleF por n experiment t shIW onduted t n energy of PTFS keD smples should e elow IHH µm for tomogrphyF es mentioned previouslyD in the se of )uoreseneD sine reEsorption is posE sileD one hs to tke into ount not only the inident em energyD ut lso the emitted photons energyF he size of the smple my hve to e redued in order to llow the photons emitted inside the smple to reh the detetorF hotons n e emitted from di'erents shells of the eletroni lyer @uD vD or wAF roweverD the rightest is usully the Kα 1 emissionD nd it is the one onsidered here when dimenE sioning smple for )uoresene imgingF le QFR summrizes the Kα 1 emission energies for the mterils looked for during this workF elthough silver nd tin emit t rther high energies @PP keAD silionD opperD nd nikel demnd rther smll smple @`20µmAF woreoverD the smller the smpleD the more quntittive the dt will eD s reEsorption will e smllerF sn this workD Ph )uoresene imges were quired with I µm thik smpleD while Qh quisitions where quired on U µm lrge opper pillrF Si Cu Sn Ag Ni Kα 1 @keA IFUR VFHS PSFQ PPFP UFRV le QFRX lues of the Kα 1 emission energies for mterils usully imged in this workF he (eld of view tht n e quired y given setup is further onstrintF sn the se of the shITe emlineD given the setup geometryD experiments re typilly performed with pixel size of PS nmF es the detetor is PHRV pixels x PHRV pixels oneD the smple should e out SH µm lrge to (t the (eld of viewF yn shIWD severl optis n e hosen to redue the pixel sizeD whih hs n impt of the (nl (eld of viewF ypillyD for pixel size of ITS nmD the (eld of view will e of RPH µm @using PSTH pixel lrge Ph detetorAF o otin smples elow SH µm for shITe experimentsD the psf ws usedD pplying the liftEout proedure presented in setion PFRFP to set the smple on luminum pinF his method ws dpted to sttistil nlysis during this hhD s will e detiled in SFPF le QFSX reprtion tehniques used in this workD for the di'erent experimentl setupsF por tomogrphy performed on shIWD limittions linked to the penetrtion depth re similr to the ones on shITeF he (eld of view however is lrger in the onditions of our experimentsD s the pixel size ws lrgerF mple prepred for shITe re therefore perfetly suitle for tomogrphy on shIWD where lrger smples n lso e imgedF por exmpleD P mm wide hips ould e leved nd imgedF he sme thoughts pply to the rdi tomogrphD whih is designed for smples of severl cm 3 F sn the se of lminogrphyD performed on shIWD only the thikness of the smpleD tht the xEry will hve to rossD will hve n imptF por lminogrphy mesures of wfersD the typil smple will mesure less thn P mm in widthD in order to get high enough signl to noise rtioF he dimensions in the plne re of less importneF sn order to e pled nd (xed into the setupD they ould e leved @typilly to IS ne x IS ne squreAF por the imging setups presented hereD the smple preprtion methods used re summrized in tle QFSF

Strain measures by Bragg diraction

es presented in prgrph QFIFPD xEry n e di'rted y rystlF he di'rtion ptterns tht result from suh n intertion n e ptured y detetorF hey led to rystllogrphi informtion out the smpleF everl tehniques hve een implemented in order to retrieve suh informtionF rere we fous on monohromti frgg di'rtionD tht llows to mesure the interplnr distne inside rystlD nd therefore otin n informtion out strin in smpleF st hs een pplied here to silion nd opper stksF 3.4.1 Monochromatic Bragg Diraction e perfet rystl n e seen s periodi lyout of given lttieD desried y three dimension prmeters nd three nglesD s illustrted in pigure QFIWF rereD the onsidered mterils re silion nd opperD whih oth hve ui lttieD so a = b = c nd α = β = γ = 90 • F he lttie is therefore only de(ned y aD lled the lttie spingF eny Q points inside the lttie de(ne plneD s illustrted in pigure QFIWF he plne n e desried y the willer indies @hklAF e fmily of equivlent plnes @prllel nd equidistntA is written {hkl}F he interplnr distne is noted d hkl ndD for ui lttieD is lulted y eqF QFQHF

d hkl = a √ h 2 + k 2 + l 2 @QFQHA
pigure QFIWX A vttie prmeters of rystlF A sllustrtion of rystllogrphi plne inside rystlD together with its willer indies @hklAF sn rel rystlsD toms n e shifted with respet to their idel positionF his is interpreted s strin inside the mterilD nd n e due to the presene of defets inside the rystlD suh s dislotionsD grin oundriesD or stking fultsD or to n pplied externl foreD suh s mehnil stressD n eletri (eldD or hnge of tempertureF he outEofEplne strinD whtever its originD is de(ned for given fmily of plnes y eqF QFQIX

ε hkl (%) = d hkl -d ref d ref • 100 @QFQIA
where a is the lttie sping of the mterilD nd d ref is referene vlue for the interplnr distneD otined y lultion or mesured on n unstrined region of the mterilF trin mesurement therefore relies on the mesurement of the interplnr distneD for given fmily of plnesF vet9s now onsider n xEry em forming n ngle θ with rystlline smple9s surfeD s presented in pigure QFPHF st is here ssumed tht the surfe is prllel to the plne fmily of interestF es explined in setion QFIFPD frgg lw providesX 2d • sin θ = λ with d the interplnr distneD nd λ the xEry wvelengthX xEry di'rtion is therefore sensitive to the interplnr distneF frgg di'rtion n lso e desried using the propgtion vetorsF k i is de(ned s the propgtion vetor of the inident emD nd k f s the propgtion vetor of the sttered em towrds the detetor positionF fy de(nitionD

|k i | = |k f | = 2π
λ F he momentum trnsfer vetor si de(ned s Q = k f -k i F hi'rtion eing n elsti proessD frgg lw n e written sX

|Q| = |k f -k i | @QFQPA = 2 • sin(θ) @QFQQA = 2π d @QFQRA
pigure QFPHX en illustrtion frgg lwD expressed with propgtion vetors k i nd k f fy hnging the ngle θD one n therefore ess di'erent interplnr distnes nd proe the reiprol speF his onlusion leds to one of the experimentl setups used in shHIF st relies on frgg lw nd is performed with monohromti wve @with ∆E/E = 10 -4 AF he ide is to tilt the smple round the theoretil frgg ngle vlue nd to oserve the displement of the frgg pek on the detetorF he (tting of these displements provide the interplnr distne for the onsidered plnesD nd therefore the strin underwent y the mterilF 3.4.2 The ID01 workow 3.4.2.1 Experimental setup: the K-map scanning technique o set this ide in prtieD n experimentl setup suh s the one shown in pigE ure QFPI is implementedF he smple is pled in the fous of the xEry emF st n e tiltedD so the ngle η reted etween the em nd the smple n e dpted to the oserved mteril nd plneF en hexpod llows the smple to sty in fous while doing soF sn the se where the oserved plnes re prllel to the smple surfeD one otins η = θF he detetor is pled on rotle rmD nd n e set t n ngle 2θ so it ptures the di'rtion ptternsF o otin strin mp of the smpleD it is snned in the nd rel spe diretionF por eh pointD the di'rtion pttern is reorded on detetorF he Ph wess ultrEfst detetorD reently developedD mkes it possile to quire the dt fst enough to relize suh n experiment VVF he smple is tilted long roking urve round the theoretil frgg ngle nd snned for eh ngleF frgg ngles nd some relevnt vlues re given in tle QFT for the mterils nd plnes studied nd energies used during this workF pigure QFPIX ixperimentl setup for xEry frgg di'rtion experimentsD iming t strin mesuresF X nd Y re the rel spe dimensions of the snD η is the ngle etween the inident em nd the smple surfe @here supposed to e prllel to the oserve plne fmilyAD nd X d nd Y d re the oordintes on the Ph detetorF

d hkl @nmA q 0 @Å -1 A η @ • A V ke W ke Cu 222

HFIHS TFHQ RVFVH RIFVI

Si 004 HFSRQ RFTQ QRFVI QHFSH le QFTX elevnt vlues for Si 004 nd Cu 004 plnes oservtion sn order to perform the sn nd the roking urve of the smple in resonle timeD snning tehnique lled uEmp @quiu mppingA ws developped in shHIF st is fully desried in refF VU nd is sed on the ontinuous quisition of dtD thus sving time on the hrdwre ommunition of dtF pinl sn times n e redued y s muh s P orders of mgnitudeF his tehnique genertes tremendous mount of dtF e typil quisition n over QH µm x QH µm re with snning steps of QHH nmD nd with rokE ing urve ontining QH pointsF his leds to QHH HHH Ph di'rtion ptternsF o del with this quntity of dtD softwre lled EygD for xEry trin yrienE ttion glultion oftwreD ws developed nd implemented in shHI @httpsX GGgitE lFesrfFfrGkmpGxsosAF he next setion desries its min feturesD while further detils n e found in VUF 3.4.2.2 Post-processing: the X-SOCS software he proess desried in the previous setion genertes S dimensionl dtF sn ft the snning in the X nd Y diretions re two dimensionsD to whih θ dds dimensionF ell quired dt re Ph imges @with dimensions X d nd Y d AD thus ringing S dimensionsF his llows for n unmiguous determintion of the lttie strin nd orienttion @tiltAF sn this setionD only the strin mps genertion is desriedF por eh point @XDY A of the smpleD the roking urve genertes Qh volume in the reiprol speD whih is de(ned y diretions Q x D Q y D nd Q z expressed in Å -1 F uh volumeD showing frgg pek otined for Si 004 oservtionD is presented in pigure QFPPF he min prt of the postEproessing is to (nd the oordintes of the frgg pek for every point of the smpleF yne this is doneD one otins mps suh s the ones presented in pigure QFPQED showing respetively Q x D Q y D nd Q z for every point of the nlyzed smpleF pinllyD the outEofEplne strin ε hkl is otined y eqF QFQSF fy inluding this formul into eqF QFQID the softwre provides strin mpD suh s the one presented in pigure QFPQdF huring the experiments performed hereD ptterns overed the whole wfer surfeF here were no unstrined regionsD therefore theoretil vlues were tken s d ref F heir vlues re given in tle QFTF st is notiele tht the otined strin mps re highly dependent on the hosen referene vlueD nd the vlues they ontin should therefore e onsidered s reltiveF pigure QFPPX @A hreeEdimensionl representtion of the i HHR frgg pek for given rel spe position on the smpleF woEdimensionl uts of the frgg pek in reiprol spe s funtion of x nd y @AD x nd z @AD nd y nd z @dAF Image source: [87]

d hkl = 2π |Q| @QFQSA = 2π √ Q 2 x +Q 2 y +Q 2 z @QFQTA
pigure QFPQX ttering vetor oordintes @A xD @A y nd @A zD nd @dA outE ofEplne strin s funtion of rel em position on the smpleF Image source: [87] wo resolutions must e disussed when referring to the kEmp tehniqueF pirstD the sptil resolutionF st is limited y the footprint of the em on the smpleD nd is therefore linked to the size of the fousD thus the size of the soureF ypillyD the sptil resolution hievle on this emline is out PHH E VHH nmF st must lso e tken into ount tht the otined vlue is verged through the depth rehed y the emF et V keD if not limited y the thikness of the smple itselfD this depth will e out UH to IHH µm in silionF he strin nd tilt sensiility is the resolution in the reiprol speF st is linked to the divergene of the emD nd n go down to ∆ε ε = 10 -5 F 3.4.3 Sample Preparation es presented in this hpterD the experiments re rried y di'rtionD in frgg @re)etionA on(gurtionF st does not require spei( smple dimensionsD s the em does not hve to go through the smpleF roweverD one of the dvntges of using xEry is their penetrtion depthD nd the ft tht uried strutures n e oservedF sn the se were suh ojets re to e nlyzedD the smple must e thinned in order for enough photons to reh the struturesD e sttered y themD nd exit the smpleF por exmpleD s will e presented in hpter TD here silion nd opper stks were nlyzedF por the V ke em to reh the lower lyer of the stkD sorption hd to e tken into ountD nd the upper lyer of the stk hd to e thinned down to Q µmF Méthodes d'imagerie par rayons X Résumé du chapitre ge hpitre présente en détils quelques possiilités des ryons pour l rE téristion de mtériuxD et les dispositifs expérimentux ssoiésF gomme dns le hpitre préédentD quelques soures de ryons sont déritesD ve leurs priniE ples rtéristiquesF ves deux types mjeurs sont les soures de lortoire et les soures synhrotronsD ien plus verstilesF ges dernières sont détilléesD en prennt omme exemple l9ip @iuropen ynhrotron dition pilityAD où les expériE enes présentées ii ont été réliséesF ves di'érentes intertions possiles entre les ryons et l mtière sont déritesD ve un intérêt prtiulier pour elles exploitées pendnt ette thèseF ves dispositifs expérimentux permettnt l9imgerie pr ryons sont églement déritsF xotmmentD trois lignes de lumières de l9ip sont présentéesD et leur rtéristiques spéi(ques mises en vntF v9imgerie Qh pr ryons @pr tomogrphie ou lminogrphieA est ensuite présentéeF ves di'érentes tehniques d9imgerie Ph omptiles sont déritesF sl s9git de l9imgerie d9sorptionD de l9imgerie pr ontrste de phseD et de l9imgerie pr )uoreseneD permettnt d9otenir une informtion himiqueF pinlementD les prinipes et l mise en prtique de l mesure de déformtionD sée ii sur l di'rtion de frggD sont présentésF gette desription est supportée pr le prinipe de fontionnement de l ligne shHIF lie nd view tehniquesD desried in setion PFRFIFP hve een used for long time nd re still under developmentF elthough they o'er gret insight into the mtterD nd the possiility to imge seleted regions of interest t resolutions rehing severl nmD their implementtion in dul em psfGiw mirosopes shows some limitsF he min one is the quite low sputtering rte of Ga + ion ems @SFR µm 3 .s -1 AF o overome this issueD dul em psfGiwD originlly developed for lrge smple preprtionD hve een pplied to lie nd iew imging QHD TVF hey o'er the possiility to imge volumes s lrge s 100 3 µm 3 with voxel size of IHH nmF imilrly to psfGpsf tehniques desried in setion PFRD it is possile to impleE ment psfGpsf lie nd iew proedureF e single em psf ene(ts from the high rsion rte of the xenon plsm ion em @QHH µm 3 .s -1 AD nd would therefore llow for higher imged volumes thn psfGiw nd psfGpsf proeduresF his mhine is however originlly designed exlusively for smple preprtionD nd numer of djustments re required for it to e omptile with Qh imgingF sn this hpterD we present the development of suh proedureD implemented inside singleEem lsm psfF e (rst setion is dedited to the utomtion of the dt quisition inside the pis ion lsmEpsfF sn seond setionD the postEproessing sriptD written spei(lly for these dtD is desried nd explinedF pinllyD results otined with suh setup re presented nd disussedF he tehE nique is illustrted throughout the hpter using imges quired on the psfD ll of them hving een otined in the frme of this hh thesisF 4.1 Automation of the data acquisition he lie nd iew proedure ws implemented on single olumn pis ion lsm psfF his mirosope o'ers S degrees of lierty to the smpleF he stge is le to move the smple in the DD nd diretionsD s illustrted in pigure RFIF purtherE moreD rottion round xis nd entered on ny smple point n e ppliedF e tilt round xis D rnging etween EIP • nd TH • n lso e usedF pigure RFI lso presents the fetures de(ning the region of interest @ysA to e imgedF he ys is onsidered to e retngleD de(ned y dimensions X ROI nd Y ROI D nd whih enter is lled P 0 F sn this hpterD diretions D D nd re de(ned regrding the smpleX t H • tiltD disussed diretions re nd D while the quired imges re de(ned in the @A plneF pigure RFIX xottions used in this hpter to designte the degrees of lierty @D D D rottionD tiltA llowed y the single olumn psfD nd the nottions regrding the smple itselfF he ys to e imged is onsidered to e retngleD de(ned y its dimensions X ROI nd Y ROI nd its enter P 0 F 4.1.1 The iFast software he whole dt quisition ws utomted using the pis ipst softwre IHWF st is visul sripting softwre whih enles the triggering of suessive tions on the psfD without humn interventionF he progrmming of tions onsists in onneting grphi oxes togetherD s presented in pigure RFP whih illustrtes some funtionlities of the softwreF wore generllyD the tions progrmmle using ipst inludeX Stage movements tge movements n e de(ned with solute or reltive oE ordintesF he (nl position is urte up to severl tens of nnometersF pigure RFPX ixmple of visul sript produed in ipstF st this sriptD nmed 4reprtifsITmin4D the em prmeters @urrentD fousD rightnessD ontrstA re (rst setD nd n imge is quiredF henD qs @qs snjetion ystemA is inserted nd stys in the hmre until the endF he em prmeters re modi(ed @the urrent is hngedAD nd retngleEshped pttern is depositedF

Beam shift movements hose movements llowD with no move from the stgeD to dpt the imged reD in the limit of SH µm in ll diretionsF he (nl position is urte up to severl nnometersF gompred to lssil dul em setupsD the single em requires the smple to move etween the sliing nd imging stepsF his rises issues regrding the smple lignment nd the time needed for the whole proedureF rere we present the di0E ulties metD the solutions rought in the se of psfGpsf imgingD nd the (nl work)ow they led toF fetween the milling nd imging stepsD the smple must e moved regrding the emF wo possiilities existF pirstD the smple n e simply tiltedF st is quite esy to implement solutionD tht does not need ny spei( toolF roweverD s the tilt of the psf is limited to TH • D the imging is not performed orthogonlly to the rossEsetionX quired rossEsetions hve to e reEsmpled for the dimensions to e orret in oth diretionsF e seond possiility is to set the smple on RS • preEtilted supportF he sliing is then performed t psf tilt of RS • D so tht the em rrives orthogonlly to the smple surfeF por the em to imge the rossEsetionD the smple is tilted k to H • nd rotted y IVH • F he imging is then performed t RS • D whih llows to imge the rossEsetion orthogonllyF sn this studyD the (rst solutionD s it ws simpler nd did not require supplementry smple supportD ws hosenF fesidesD s will e presented in the postEproessing desriptionD reEsmpling is needed in most ses fter lie nd iew proedureD nd is performed in dul em solutionsD sine the two ems do not form WH • ngleF he reEsmpling required y the dt quisition mde t TH • ours t little supplementry omputtion ostF es the stge is moved etween two suessive sliing proeduresD seond hlE lenge is to ensure the sliing step remins onstnt through the whole proedureF o do soD t the eginning of eh suessive stepD the psf stge is progrmmed to go to point P 0 D situted t the enter of the ysF es mentioned eforeD this stge movement is not very preiseF o improve the lotion of the referene pointD n lignment step is neededF o do soD n lignment ross is milled t the top of the ysD t distne h of the ys edgeD s illustrted in pigure RFQF he enter of this ross is the referene pointX t the eginning of every itertionD the pttern reognition lgorithm implemented in ipst sets the enter of the imge on the enE ter of the rossD using only em shiftF etullyD this proedure is done twieD with two di'erent (elds of viewF he (rst proedure is relized with lrge (eld of view imge @typilly IQH µmA suh s the one presented in pigure RFQF he lrge (eld of view ensures the ross n e found on the quired imgeF efter this (rst stepD more preise lignmentD sed on smller (eld of view imge @typilly PH µmAD is ppliedF e typil referene imge for this smller (eld of view is presented in pigure RFQF yne the enter of the imge is ligned with the enter of the lignment rossD (nl em shift moves the enter of the imge to the edge of the previouslyE slied rossEsetionF woreoverD ontrol imges re quired during the proedureF hey llow for the mesurement of the tul sliing step during the postEproessing proedureF his will e detiled in setion RFPF pigure RFQX ypil referene imgesD ontining the lignment rossD used for the lignment stepF A smge with lrge (eld of view @IHH µmY A imge with smller (eld of view @IQ µmAF pinllyD supplementry di0ulty is to keep the region of interest @usully prE llel to the smple surfeA inside the (eld of view imged during the proedureF e (rst step to do so is to dpt the position of the smple for the ys to e on the tilt xisD s illustrted in pigure RFRF fy doing so howeverD the region of interest tends to drift towrds the top of the imged re long the suessive lie nd iew stepsD s shown in pigure RFRF his is due to the ft tht the stge is still pigure RFRX smged regions of the ys during the proedureD depending on the tilt xisF he purple lyer of the smple is the region ot e imgedF A he tilt is relized round n xis pssing through point P 0 D t the egining of the proedureF he imged re is dpted to ontin the purple lyerF A efter severl itertionsD the tilt round the sme xis P 0 does not gurnty the purple lyer to e in the imged reF A he smple is tilted round prllel xisD pssing through the point P 1 D situted on the edge of the ysF he purple lyer is imgedF he tilting xis must therefore e hnged long the proedureD nd lwys ontin point from the edgeF entered on point P 0 D nd not on the edgeD sine only em shifts hve een perE formedF o overome this issueD the lst em shift is repledD fter the end of the rossEsetion millingD y stge movement of the sme mplitudeF yn pigure RFRD the tilt is performed round point P 1 D situted on the edgeF es illustrtedD this ensures the region of interest is lwys pled t the enter of the imged regionF por some smplesD further em shift @triggered y n imge lignment lgorithm or user de(nedA ould lso e pplied fter the shift in order to set the rossEsetion region of interest on the enter of the imged regionF 4.1.2.2 PFIB/PFIB acquisition workow ROI preparation fefore eginning the quisition of dtD preprtion of the region of interest is neessryF he ys preprtion steps re summrized nd illustrted in pigure RFSF pirstD protetive t lyer of typilly Q to S µm thikness is deposited on region ontining the ys @f RFSAD using the son fem sndued heposition method desried in setion PFQFPF henD lrge trenhes re milled round the ysD in order to limit future redepositionF e (rst milling step is mde high ion urrent @typilly P µAAD using regulr rossEsetion pttern @f RFSAF henD softer pttern @lening ross setionD f RFSA is ppliedD t lower urrent @HFIV µAAF pinllyD the edge of the ys is de(ned y soft lening ross setion @performed t SW ne urrentAD nd the lignment ross is milled @f RFSdAF Acquisition preparation yne the preprtion step is overD the dt quisition must e on(guredF he numer of lie nd iew steps is de(ned y the numer xD nd eh itertion is designted y its numer nF he sliing step required y the user is noted pF pigure RFT presents the generl work)ow for ny itertion n of the proessF he user relizes the (rst itertion mnullyD while setting the prmeters for the utomti dt quisitionF pirstD the user djusts nd sves the fousD rightnessD nd ontrst prmeters for imging t H • F hese vlues will e used throughout the whole proessF his ensures tht the imges lwys look similrD nd therefore ensures the suess of the pttern reognition lgorithm to omeF he distne h is then mesured nd input into the softwreF henD the two referene imgesD t lrge nd smll (eld of viewD re reorded nd svedF efter the lignment stepD em shift of h is ppliedF wore generllyD t eh itertionD the movement from the enter of the ross to the edge of the ys will e de(ned y distne hEnp in the diretionF he milling pttern n then e de(ned y the userD s lening ross setion tht is to e pled on the edge of the ysD s shown in pigure RFTdF he user then tunes the position of the smpleD for the region of interest of the ross setion to e in the enter of the imged re fter the TH • tiltF he user n lso dd nd sve em shift tht will e pplied t eh itertionD for etter imgeF he smple is then moved k to H • tiltD nd the P 0 position n e sved into the softwreD given the new vlue of F sf neededD the fousD rightness nd ontrst prmeters t H • n e updtedF pigure RFSX teps of the ys preprtion for the proedureF A heposition of protetive lyer on the ysF A egulr rossEsetion milling round the ysF A glening rossEsetion milling round the ysF dA elignment ross nd (nl lening ross setion millingF pigure RFTX eutomti lie nd iew tions ourring during step @noted nAF he tions relted to em prmeters pper in orngeD while imging ppers in greenF Automatic acquisition efter the setting of ll the prmetersD it is possile to lunh the lie nd iew proedure for numer x of suessive stepsF ih step n onsists in severl tionsD depited nd illustrted using di'erent smples in pigure RFTF sn this (gureD tions referring to em prmeters pper in orngeD while imging proeduresD e it for ontrol purposes or the tul imging of the ysD re presented in greenF es illustrtedD eh step n e seprted into four suEstepsX 1. Positioning of the beam and the sample at 0 • he (rst tion of the proE edure is to move the stge towrds P 0 @see pigure RFTAF he positioning of the em then relies on the pplition of previously sved em prmetersD together with the lignment of the em on the enter of the lignment rossF e ontrol imge @see pigure RFTA is quired thenF his (rst lignment llows to set the em on the edge of the smple @see pigure RFTAF 2. Slicing of the sample he sliing is performed using the milling pttern preE viously de(nedD situted on the enter of the imge @see pigure RFTdAF efter the sliing step nd hnge of urrentD sved em prmeters re ppliedF 3. Positioning of the beam and sample at 60 • es explined previouslyD eE fore tilting the smpleD the lst em shift is suppressed @see pigure RFTeA nd repled y stge movementF he tilt is then relized @see pigure RFTfAF 4. Imaging the cross-section pinllyD fter pplying em prmetersD the wnted imge of the rossEsetion n e quired @see pigure RFTgAF

Data post-processing

efter the dt quisitionD two sets of dt re villeF hey re illustrted in pigure RFUF he ontrol imges @see pigure RFUA llow to retrieve the tul vlue of the sliing stepF heir dimensions in pixels re noted X control nd Y control D nd x of them hve een quiredF he x rossEsetions dimensions in pixels re noted X im nd Z im F he pixel sizes in the nd diretions re noted p X nd p Z D respetivelyF pigure RFU fetures the rw volume nd two orthogonl views otined y simply stking those x imges togetherF es n e oserved on the @redA orthogonl view of the volumeD the rossE setions re not perfetly ligned with one notherD whih leds to plnr interfes tht do not pper s suh in the reonstrutionF sn order to otin the (nl volumeD the rossEsetions therefore hve to e registeredF woreoverD let us note p X nd p Z the pixel sizes of the ross setions in the nd diretionsF ine the rossEsetions re not imged orthogonllyD p X nd p Z re not equlF edditionllyD the sliing step p Y is set independently from those two vluesD nd is therefore not equl to themF o otin (nl volumeD with ui voxelsD reEsmpling step is therefore neededD preeded y the lultion of the tul sliing step p Y F pigure RFUX ht otined fter the dt quisition nd the postEproessingD respetivelyF A gontrol imges quired for sliing step lultionF A w volume generted y stking rossEsetionsF A pinl volumeD otined fter the postE proessingF he slies hve een registeredD nd the volume reEsmpled in order for the dimensions to e isotropiF he following setions im t desriing the postEproessing steps leding to wellEregisteredD isotropi reonstruted volumeF he min steps re presented in pigure RFVF pigure RFVX teps of the dt postEproessing developed for psf dtF 4.2.1 Calculation of the actual slicing step he (rst step of the postEproessing is to retrieve from the dt the tul vlue of the sliing stepD noted p Y F o do soD the sript uses the ontrol imgesF he ontrol imges re entered on the lignment rossF es shown in pigure RFWD the edge of the ys gets loser to the lignment ross with the itertionsF ht the sript mesures is the position of the edge in the imge for eh itertionD nd therefore its dvne in pixels nd lter in nnometersF es the edge ppers s very right horizontl line in the imgeD its position n e found using the pro(le of the imge in the vertil diretionD possily lulted on ys @identil for ll slies nd mnully de(nedAF pigures RFWdD eD n f show suh pro(lesD lulted on the ys de(ned on imges D D nd D respetivelyF sn this exmpleD the mximum vlue orresponds to the edge of the smple nd llows to follow the sliing step throughout the proedureF hepending on the smpleD the lultion of the pro(le9s grdient n provide etter resultsD s it will help spotting the shrp hnge of grey level tht is the edgeD nd leve out the other possily right fetures of the imgeF his method is illustrted in pigures RFWgD hD nd iF he hoie of the method nd of the ys re up to the userF yne the edge position is known for ll the sliesD the sript drws grph presenting the evolution of the position vs the numer of the slieF he grph should represent lineD whih slope provides the sliing stepD s will e presented in setion RFQF et the end of this stepD the vlue p y of the sliing step is known nd expressed in pixelsF es the pixel size of the ontrol imge is knownD the onversion to sliing step in nnometers is strightforwrdF 4.2.2 Slices registration e seond step in the postEproessing is to red ll the sliesD to register them with one notherD nd to stk them into volumeF elthough the shifts etween the di'erent slies re quite smllD due to the e'orts mde during the dt quisition stepD the slies hve to e perfetly or registered for the volume to e of good qulityF pigure RFWX gontrol imges quired during lie nd iew proedureD fter A IHH itertionsY A QHH itertionsY A SHH itertionsF he sliing step ws set to SH nmF dD eD fA pro(les lulted on the ys respetively shown on D D nd F gD hD iA grdients of pro(les dD eD nd fD respetivelyF he sript lultes nd pplies shifts to the slies in diretions nd F st llows for di'erent optionsX

• wo di'erent registrtion methods re villeF he (rst one is the regis-ter_translation funtion from the skimage.feature pkge from ythonF he seond one relies on the sme pro(le lultion s the sliing step evlutionF st is fster thn the registrtion funtionD ut only works for very spei( smplesD hving right spot tht n e identi(ed through the smpleF

• he lignment is either performed on ll slies regrding the (rst oneD or for ll slies regrding the previous oneF his seond method is less preiseD nd often leds to liner shift throughout the volumeD ut llows to minimize the impt of possile high mgnitude shifts during the quisitionF

• he lignment n e performed on given ys of the quired imgeD mnE ully de(nedF

• sn most sesD no or little movement ours in the horizontl @A diretionF st is possile then to limit the registrtion lultion to the vertil @A diretionF his is dvised when the hosen registrtion method is the pro(leEsed oneF por ll the sets of possile optionsD the sript drws grph showing the luE lted shiftsF huring the tests performed on this experimentl setupD these di'erent options were implemented on the goD in order to dpt to the tested smplesF es will e presented in the next setionsD it llowed to imge wide pnel of smple typesF he set of options must e dpted to the studied smpleD nd no prmeters hve een found to work on every smpleF hile registering the sliesD the sript reds themD shifts them in the nd diretionD ordingly to the shift vlues foundD nd normlizes their ontrstF st n then stk them into volumeF his volume hs to e reEsmpledD in order for the voxels to e ui nd the mesures to e urte in ll diretionsF 4.2.3 Volume re-sampling sn the setup presented hereD two reEsmpling tions re neededF he horizontl rossEsetion pixel size p X is tken s refereneD nd the other pixel sizes re dpted to itF pirstD ll slies re distorted given the quisition setupX sine the imging is done t TH • insted of WH • D (rst reEsmpling must e mde in the diretion @y ftor sin(30 • ) a HFVUAF his llows to otin isotropi rossEsetionD of pixel size p XZ @typilly QH nm for n imging (eld of view of TH µmAF he sliing step p Z is however typilly of SH nmD or even IHH nmF e seond reEsmpling must then e performed in the diretionD y ftor mag de(ned s mag = p Y p XZ F hese proedures re performed using the zoom funtion from the ython scipy.ndimage.interpolation pkgeD nd render n isotropi volumeF he (nl volumeD otined fter ll the postEproessing stepsD is illustrted in pigure RFUF lies hve visily een lignedD sine the interfes now pper s lerly plnrF he reEsmpling is lso visileD on the ross setions @whih re smller in the diretionAD nd on the orthogonl viewsX mag is here tken superior to I @whih will usully e the seAD whih enlrges the volume in the diretionF

Results

por the psfGpsf lie nd iew tehnique to e relileD it is ritil tht the dt quisition step n e performed utomtillyF he quisition eing quite longD the proess must remin stle for severl tens of hoursF his hs een hievedD minly y sving the imging prmeters t H • X this mde the pttern reognition step more roustF he experiment setup is now le to quire dt for tens of hours uninterruptedX RH hours of unsupervised dt quisition were hieved so frF he proess ould lst even longerD if neededF he experimentl setup presented here did llows for the reonstrution of vrE ious smples of di'erent nturesD with di'erent sliing stepsD imging pixel sizesD nd (elds of viewF es n illustrtion of the presented setupD (gure RFIH presents three exmples of smples imged on this setupX stk ontining severl lyers of opperD opper pillrD nd ermis used in olid yxide puel gells @ypgAF wore generllyD pigure RFII presents the volumes nd voxel sizes of some smples nlyzed on this setupD together with the type of mteril studiedF he voxel size in this se ws hosen to e the sliing stepD s it is the limiting ftor to the resolutionF es n e seenD the psfGpsf imging llows to inrese the nlyzed volume ompred to psfGiw imgingD sine the nlyzed volumes rehed 50 3 µm 3 D with typil slie size of TH x PH µm 2 for stksF he previously detiled sript utomtilly provides the sliing step vlue in few minutesF pigure RFIPA presents suh grphD for demnded sliing step of SH nm quired on stk smple suh s the one presented in pigure RFIHF he reltionship etween the itertions nd the position of the edge is lerly linerD nd ws (tted y line of oe0ient EHFQWW pxlGitertionD with oe0ient of determintion R 2 a WWFWR7F hereforeD the sliing step is found to e SHFU nm nd quite regulrF his regulrity ws lso found for the other smples nd sliing stepsF he sliing steps minly tested were SH nmD IHH nmD nd PHH nmF he SH nm sliing stepD omined with n imge quisition mde with po of IHH µmD o'ered the dvntge to render volumes tht needed little reEsmpling to e isotropiF por most smplesD the slie registrtion n e mde utomtilly in out IH minutesF pigure RFIP shows typil movements pplied to the slies during the registrtion proess for stk smple suh s the one shown in pigure RFIHF es n e seenD the movements of the smple re quite smll @elow IH pixelsAD ut still need to e orretedX the dt quisition setup ensures the ys remins in the imged reD ut does not provide perfet lignment of the sliesF roweverD it is worth notiing tht the registrtion softwre works very well on stksD ut is less e0ient on opper pillrs for exmpleF por these smplesD mnul registrtion using other tools suh the piji tkeg plugin n e requiredF sn tht seD the postEproessing is more likely to require out one hour per smpleF he dt quisition time itself vries with the sliing stepD the imged volumeD nd the sliing urrentF pigure RFIQ shows some of the times needed for the imging of vrious smples tested in this studyF he quisition time vries from U hours @for the imging of 19 3 µm 3 A to RP hours @for n imged volume of 54 3 µm 3 AF yn vergeD the time per slie is of RFS minutesF he psf llows for fst millingD nd the sliing time is only of TH seonds on vergeD whih represents PH7 of the step timeF pigure RFIQ presents the verge ontriution of every tion performed during lie nd iew stepF es n e seenD high resolution ion imging requires long time @out IFS minutesAD nd tkes out one third of the overll timeF woreoverD the two min tions during step @imging nd sliingA only ount for SS7 of the timeD the rest eing spent in hnging the urrentD setting the em nd stge prmetersD nd tilting the smpleF pigure RFIHX esults otined y psfGpsf Qh imgingF ell results re presented through one view @the imged ross setionA nd two orthogonl views @ nd AD otined from the (nl reonstrutionsF A e opper C silion stkY A e SH µm lrge opper pillrY A e ermi for ypg @olid yxide puel gellsAF pigure RFIIX smged volumes nd voxels sizes otined for vrious smples nlyzed in this studyF pigure RFIPX qrphs shown during the postEproessing of the dt quired from hyrid onding stkD whih progrmmed sliing step ws SH nmF A he grph showing the position of the edge regrding the numer of the itertionF he slope oe0ient is EHFQWW @lulted with oe0ient of determintion of WWFWR7AD whih leds to sliing step of SHFU nmF A he grph showing the shift pplied to every slieD in the horizontl nd vertil diretionsF pigure RFIQX ime onsidertions regrding the psfGpsf dt quisitionF A equisition times vs imged volumes for vrious smplesF A eltive time needed for every tion during lie nd iew stepF 4.4 Limits of the technique and possible improvements es disussed previouslyD the dt quisition nd postEproessing hve een designed nd implemented to demnd little user interventionF e step further in the develE opment of this setup would e to improve its utomtionF he dt quisition itself is fully utomtiD ut requires the user to spend out one hour on verge to set the prmetersF por known smplesD this time ould e redued y the use of sved reipesD dpted to spei( mterilsF purthermoreD the experiments ould ene(t from user interfeF sn suh n interfeD it would e possile for the user to only set the wnted ys nd the sliing step desiredD nd the softwre ould set the trenhesD the position of the lignment ross etF roweverD the setting of the position of the smple would still e up to the userD together with the setting of fousF uh n interfe should e le to redue the user intervention to out PH minutesF egrding the postEproessingD the utomtion is more hllengingF es menE tioned previouslyD the registrtion of slies does not work on ll smplesD nd in ny se the hoie of the method nd the ys on whih the registrtion is mde re left up to the userF he postEproessing softwre ould however ene(t from the imE plementtion of other registrtion methodsD suh s sp @le snvrint petures rnsformAD whih is sed on the reognition of feturesD for exmpleF he user would therefore still hve to mke hoies during the postEproessingD ut would e provided with more optionsF es oserved previouslyD the dt quisition still requires muh timeF elthough the use of xenon ion plsm soure llows for very fst millingD the other steps of the proedure require more time thn in lssi psfGiw setup for exmpleD sine the smple hs to e tilted nd the urrent hngedF woreoverD s the mhine ws not ment for imging originllyD the detetor requires long quisition times to produe high qulity imgeF he dt quisition time ould therefore e redued y ting on those prmetersF elthough the use of dul em mirosope or etter detetor ould solve some of these prolemsD we here present solutions pplile with the given single em mirosopeD s it is le to provide vlule results with no hrdwre hngeF efter the sliing stepD the urrent is hngedD nd the stge is tiltedF hose two steps require lmost one minute togetherF he ipst softwre does not llow the two to hppen simultneouslyF sf this ws mde possileD QH seonds ould e sved per itertionF woreoverD the tilt itself ould e improved y hnging its speed prmeters in the psf softwreF e Qh postEproessing deEnoising step ould lso llow to quire imge of less qulityD thus sving timeF gomining these di'erent feturesD it should e possile to redue the time per slie to PFS minutesF he resolution nd (eld of view ould lso e improved without inresing the quisition timeF sn ftD the psf is le to operte EIP • tiltF sf the smple ws slied t stge position of EIP • D the rossEsetion would e imged t n ngle of UP • insted of TH • F his would inrese the imge qulityD s the further reE smpling would e of lower mplitudeF roweverD the implementtion of this ide would require new tehniques to mintin the region of interest in the imged zoneX the ross setion would not e orthogonl to the smple surfe nymoreF his ould e done inside the softwreX sine the ngle of the preEtilt is knownD the softwre n ompenste for it y moving the stge or the emF en even simpler wy would e to ple the smple on IP • preEtilted supportF his wyD the rossEsetion would e orthogonl to the smple surfeD even when sliing the smple t EIP • tilted stge positionF he imged volume isD s of todyD limited in the diretion to IHH µmF sn ftD the work)ow relies on the ft tht the movement etween the enter of the lignment ross nd the edge of the ys is performed y the em shiftF yn the psfD the vertil em shift is limited to SH µm in oth diretions @positive nd negtive vlues of AF he distne h etween the enter of the lignment ross nd the edge must therefore e inferior to IHH µmF he point P 0 is pled on the enter of the ys preisely to mximize the essile regionF st is worth mentioning tht IHH µm ws more thn enough in the smples studied hereF roweverD if higher length is neededD it should e esy to implement dt quisition in severl prtsD with severl lignment rosses ligned on the xis nd used one fter the otherF ith suh tehniqueD the length of the imged volume should e virtully in(niteF he psfGpsf imging presents drwk enountered in psfGpsf imgingD ut voided in psfGiw imgingF es explined in hpter P @setion PFQFQAD if the positive hrges nnot espe the smple @eFgF the re is n insultor or surrounded y n insultorAD they will umulte t the surfeD preventing ny hrge rriving in this re to leve the surfeF hereforeD the re will pper in lkF sf smple ontins ondutive res @opper pds for exmpleA tht re isolted from other ondutive zones @for exmple in the se of dummiesAD they will not pper on the quired volumeF his phenomenon is illustrted in pigure RFIRF sn ftD on the top view presented in pigure RFIRD otined y milling retngle pttern from the surfe of the smpleD di'erent strutures re visileF emong themD pds overing grid pttern n e oservedF pigure RFIR presents view of the reonstrution nd two orthogonl viewsD quired on the psfGpsf setupF yn the one leled ID the pds re lerly visile nd the re from (gure is lerly identi(edF roweverD the grid pttern is not visileF hen exploring the smple is the diretionD this pttern does not pperD s illustrted y the slie leled PF his is due to the ft tht during the ys preprtion stepD the milling of trenhes round the ys ut the grid from the rest of the wferF heir imging ws no long possileF o overome this issueD negtive hrges should e projeted on the surfeF his is only possile in dul em mirosopeF pinllyD the psfEsed lie nd iew proedure enounters ll the typil issues of lie nd iew proeduresF ine the imging tehnique is sensitive to rystlline orienttionD the segmenttion n e di0ultX polyrystlline mteril will feture severl grey levelsF woreoverD s for every proedureD the segmenE ttion of porous mterils is very hrdF en exmple is given in pigure RFISF st presents n histogrm lulted on suvolume of dt quired y psfGpsf from SH µm opper pillr @see pigure RFISAF he suvolume ws tken round pigure RFIRX sllustrtion of the onsequenes of hrge umultion on the psfGpsf imgingF A opEview of silion C opper stkD quired on the psf nd feturing pds on the whole surfeF A eonstruted slieD using the psf Qh imgingD where the entrl pds nnot e seenF the interfeD whih mens it ontins ll the voidsF he histogrm is quite smoothD nd does not llow for diret segmenttion sed on thresholdD s shown in pigure RFISX threshold level set t SU leds to seletion @in redA tht does not ontin ll the voidsD wheres WV threshold level leds to seleting intermetlli lloy nd prt of opperD while the voids re still not ompletely segmentedF his issue ws lso enountered when imging porous ermis suh s the one shown in pigure RFIHF st is wellEknown prolem IIHD inherent to lie nd iew proeE duresF elthough some solutions re eing foundD it remins hllenge in the se of porous medi IIID IIPF he di0ulty minly relies on the high depth of (eld of the Ph imging tehniquesF sndeedD deep enough void will pper s lk spotD sine the seondry eletrons reted in it will not e le to ome k t the surfe nd hit the detetorF efter few slies howeverD when the void is shllowerD some seondry eletrons will ome k to the detetor nd the void will pper in lighter grey levelF efter the volume retionD the otined void will not pper in uniform grey levelF he segmenttion will require dvned tools nd severl hours per smpleF pigure RFISX A ristogrm of ys of opper pillrsD ontining intermetlli lloys nd voidsF A wo ttempts for the segmenttion of voids @in redA inside this ysD using two di'erent threshold levelsF 4.5 Conclusion sn this hpterD the implementtion of lie nd iew proedure inside single olumn psf hs een presentedF he min gol of suh n implementtion ws to inrese the hievle imged volume y lie nd iew proedureD using the high sputtering rte of xenon plsm ion soureF es the psf mhine ws originlly designed for smple preprtionD its ppliE tion to Qh imging rose severl issuesF hey hve een identi(ed nd nswered in this hpterD nd the implementtion they led to hs een presentedX omplete work)owD inluding ys preprtionD dt quisitionD nd postEproessingD hs een provided nd detiledF es resultD the setup now llows for the Qh imging of vrious smplesD s illustrted throughout the hpterF he quisition proess hs een shown to e stle nd relileD s it ould run unsupervised for RH hoursF he postEproessing provides the user with informtion on the sliing stepD nd renders registered nd reEsmpled reonstruted volume for most smplesF vimits of the setupD inluding those regrding the quisition timeD hve lso een disussedF es expetedD the hievle volumes re higher thn the ones quired in psf mirosopesX xenon sliing llows to otin rossEsetions of RH x QH µm 2 in less thn one minuteD leding to imged volumes etween 15 3 nd 50 3 µm 3 F es the mirosope only fetures one olumnD time is lost in urrent hnge nd tilt opertionsD whih leds to longer quisition times thn those otined with dul em psfF qiven this nlyses nd the experiments relized during this workD pigure PFUD presenting the volumes nd voxel size hievle y lie nd iew tehniques @nd presented in setion PFRAD hs een updtedF e new version is provided in pigure RFITX results of psfGpsf imgingD implemented for the (rst time during this hhD o'er (elds of view nd voxel sizes pled etween the ones o'ered y psfEsed e nd y dul em psf proeduresF pigure RFITX pdted version of pigure PFUD presenting the hievle volumes nd voxel sizes using di'erent lie nd iew tehniquesX psfGiw @in lkAD psfGpsf @in light lueAD psfGiw @in redAD nd psfGpsf @in purple nd quired in the frme of this hhAF st is worth mentioning tht the setup presented here o'ers voxel sizes @SH nmA nd (elds of view @SH µmA whih re not only omptile with the Qh integrtion requirementsD ut lso similr to the ones otined on the shITe emline of the ipF he tehniques re of ourse very di'erentD nd so re the otined resultsF roweverD omprison etween those tehniques remins interesting nd is mde possile y those similritiesF Développement d'une technique d'imagerie 3D dans un PFIB Résumé du chapitre hns e hpitreD nous présentons le développement d9une tehnique d9imgerie Qh destrutiveD implémentée u sein d9un psf à une seule olonneF gette tehE niques est sée sur l9imgerie lie nd iewD typiquement implémentée dns un psfGiwF ves di0ultés liées à l présene d9une seule olonne et à l9utomtistion de l9quisition des données sont dérites une à uneD et des solutions sont proposéesF v proédure d9quisition des données en résultnt est dérite et justi(éeF ve sript de postEtritement érit pour ette proédureD et les di'érentes étpes le onstituntD sont ensuite déritsF ves résultts otenus grâe à ette tehniqueD tnt u niveu de l9implémenttion elleEmême que des mtériux imgésD sont ensuite fournisF v9quisition des données est un proédé ujourd9hui stleD qui peut tourner plusieurs dizines d9heures sns intervention humineF ve postEtritement permet d9otenir utomtiquement @pour l pluprt des éhntillonsA un volume ligné et reonstruitF sl fournit de plus une mesure du ps e'etif de déoupeF ves mtériux testés inluent des piliers de uivreD des empilements à plusieurs niveux de uivre et de siliiumD et des érmiques poreusesF in(nD les limites et possiles méliortions de l tehnique sont disutéesF ves limites portent priniplement sur le temps d9quisition des donnéesD ujourd9hui ssez longF hes solutions sont proposéesD telles que l9utilistion d9un mirosope omportnt deux olonnesD et l9optimistion des prmètres du mirosope utiliséD omme le mouvement de l9éhntillonF ne disussion plus lrge sur les prolèmes renontrés pr les proédures lie nd iew est menéeF ille porte notmment sur l9imgerie des mtériux poreuxD toujours di0ileF ves possiilités d9imgerie du psfGpsf sont en(n mises en reltions ve elles d9utres implémenttions similiresD telles que le psfGiwD le psfGpsfD et le psfGiwF gette étude est sée sur l littérture et les résultts otenus u ours de e trvilF ve psfGpsf permet omme espéré d9ugmenter les volumes imgésD pr rpport u psfGiw ou u psfGpsfF sl est ien sûrD en ontreprtieD limité pr s résolutionF gompré u psfGiwD il est moins rpideD don les volumes tteints sont moins importntsF v tille de pixels qu9il propose @QH nmA en imgerie Ph est ependnt ssez omptile ve son ps de déoupe @SH nmAD e qui en fit une tehnique essentiellement QhF es explined in setion QFPFID the shITe emline of the ip is reent emlineD uilt during the (rst phse of the ip upgrdeF st is ment for suESHnm resolution Qh imgingD nd is the (rst hrd xEry nnoEtomogrphy emlineF es of todyD it o'ers the possiility to perform holoEtomogrphyD )uoresene tomogrphyD nd ptyhogrphyD on smples rnging from iology to miroeletronisF sn this hpterD we minly fous on the holoEtomogrphy tehniqueD nd more prtiulrly on strtegies llowing to inrese the smple throughput on this emE lineD in order to perform sttistil studies for the industryF o do soD (rst setion will e dedited to the originl nlysis work)ow on shITeD going from the smple preprtion to the dt quisition nd the dt proessingF he three next setions desrie solutions to redue the overll time of the whole proedureD using new smple preprtion shemeD the redution of the numer of projetionsD nd the utomtion of the postEproessingD respetivelyF he new work)ow thus otined is lso disussedF pinllyD setion presents those results in the lrger ontext of Qh integrtion hrteriztionD y pling them next to results otined on other wellEestlished Qh imging tehniquesD suh s the psfGiw or the shIW emline of the ip @presented in setion QFPFPAF mpleEsed exmples re given throughout the hpterD in order to illustrte the di'erent steps of the proedure nd the otined resultsF nless spei(ed othE erwiseD those imges were quired in the frme of this hh thesis 1 F 5.1 Original ID16A workow he omplete work)ow of n experiment on shITe goes from the originl smple in the form of wfer to the (nl reonstruted volumeF es one n expetD it forms into mny stepsF sn this setionD the min ones re presentedD from user point of viewD together with the time they requireF Sample preparation es explined in setion QFQFQD the shITe is quite demnding in terms of smple dimensionsD s they should e elow SH µm in width to (t the (eld of view @for pixel size of PS nmAF he originl work)ow to do thisD in the se of miroeletronis smplesD is to prepre the smple inside psf nd ple it on top of n luminum pinD using the liftEout proedure desried in setion PFRFPF he luminum pin is then pled inside rss ylinder @ ruer pinAD tht n e introdued inside holder whih is spei( to the emlineF he smple preprtion step requires out one hour of millingD whih is perE formed without humn interventionD fter userEperformed setting tht tkes out hlf n hourF he extrtion of the smple requires out hlf n hour s wellF lE ing the luminum pin inside the ruer pin tkes out (ve minutesF Data acquisition yne the smple is mounted on the holderD it is pled under vuumD in smple hngerF en utomti rm gets it nd puts it inside the emF he stge is then movedD for the smple to e inside the (eld of view during the rottionF efter the dt quisitionD the smple is repled outside of the emD in the smple hngerD nd the next one n e fethedF he time etween the end of one quisition nd the egining of the next one is ounted y dding the time to retrieve the (rst smpleD ple it k inside the smple hngerD to feth the seond oneD ple it in the emD nd to lign the stgeF st is estimted to out one hourF ht quisition relies on the quisition of referene imges @drk imgesD with no emD nd referene imgesD with no smple in the (eld of viewA nd rdiogrphs for numer N proj of nglesD for four di'erent fousEtoEsmple distnesF rereD eh rdiogrph will e designted y the ouple @d rad D n rad AD with d rad < 4D nd n rad < N proj F ypillyD N proj a PHHHD for n exposure time of HFS seondsF his leds to n quisition time of four hours per tomogrphyD inluding the time of stge stiliztion nd mer redEoutF Post-processing he postEproessing of the dt is mde of severl stepsD eh one set nd triggered y the userX IF por eh ngle n proj D the orresponding rdiogrphs @d rad D n rad = n proj A must e ligned togetherF pirstD they re resmpledD for the smple to mesure the sme size on ll of themF his resmpling is mde knowing four fousE toEsmple distnesD nd therefore the mgni(tion pplied to the smpleF he tul registrtion n e mde in rel spe or pourier speF st is usully mde every IHH nglesD nd the movements of the rdiogrphs re (tted for the remining nglesF his proedure requires out QH minutes for PHHH nglesF his step must e triggered y the userD ut is quite trnsprent to themX the user only hooses the registrtion method nd heks mnully if the rdiogrphs re wellElignedF por some smplesD di'erent registrtion methods n e pplied suessively for etter preisionF PF yne the projetions re registeredD the phse n e retrieved for eh ngleF ih projetion otined then is hrterized y the numer n proj @n Ǹproj AF everl phse retrievl lgorithms re villeD mong whih the gp @gontrst rnsfert puntionAD the si @rnsport of intensity equtionAD nd mixed pproh etween them @see setion QFQFIFP for desription of those lgorithmsAF sn the se of Qh integrtion smplesD the gp method ws the most often ppliedF his proedure requires out V hours for PHHH quired nglesF QF efter the phse retrievlD the rottion xis is mnully lultedF o do soD the (rst projetion of the dt set is registered with the lst oneD )ipped horizontllyF he shift found this wy is noted sF he rottion xis is then provided y the formulX RotationAxis = 1024 -s 2 F sullyD the user reonE struts one slie of the smple with rnge of rottion xis round this vlueD nd ompres the results visullyD in order to selet the etter suited rottion xisF his requires out PH minutes of humn interventionF RF pinllyD the volume n e reonstrutedD using the pf @piltered fk roE jetionA lgorithmF his requires less thn one hourD in the se of PHHH proE jetionsD eh one mesuring PHRV x PHRV pixels2 F he otined volume is PHRV pixels wide ueF pigure SFI summrizes nd illustrtes ll the steps depited in this setionD toE gether with their time ontriution during the work)owF hose times re given sed on the experiene quired long this workF yf ourseD omputtion times depend widely on the onsidered mhineF sn the se of experiments performed on the shITe emlineD phse retrievl nd reonstrution steps re performed on ip lustersD mnged y the ye th sheduler IIRF he glol omputE tion time n of ourse vryD depending on the vilility of the mhines nd their performnesD nd the given vlues re men onesF st is worth mentioning tht lthough the overll time from wfer to volume is importntD the redution of some steps is more relevnt thn othersF sn ftD in the frme of this workD the fous ws set on limiting minly the em time nd the pigure SFIX he shITe work)ow nd the time needed for eh stepD in the se of dt quisition of PHHH projetionsF humn intervention timeF o limit the em timeD two strtegies re possileF he (rst one would e to derese drstilly the quisition time per projetionF his is done on severl emlinesD nd n even led to ultrEfst quisitions nd possily to inEsitu mesures IISF roweverD this derese in time omes t the ost of the resolutionF rereD the gol is to mintin the resolutionD nd mke the most out of the em timeF o do soD the pplied strtegy is to utomte s muh s possile the work)owF por lrity purposesD the humn intervention time is represented in red in the (gureD while long enough @one hour nd moreA utomti proedures pper in greenF qiven the previous golsD three strtegies hve een set in ple nd tested on the shITe emlineD s will e presented in the next setionsF es the high resolution rehed y the shITe emline is quite demndingD little hnge hs een rought to the tehnique itselfD nd the min fous ws to limit the time of the surrounding tions without deresing the resolution of the (nl reonstrutionsF 5.2 New sample preparation scheme es n e seen in pigure SFID the smple preprtion nd instlltion require quite some timeD nd re minly mde mnullyF e (rst pproh therefore fouses on those two stepsF 5.2.1 New sample supports es mentioned in the work)ow presenttionD fter the smple preprtionD the luE minum pin hs to e pled into ruer pin nd glued to itD s illustrted in pigure SFPF wore importntly thn the time tken y this stepD the issue is tht there is risk to dmge the smple while doing thisF o void this stepD new smE ple supports were therefore designedF he new smple supports feture the exterior spet of ruer pinsD in order to (t the shITe emlineF snsted of eing hollow howeverD they feture pin on whih the smple n e pledD s shown in pigE ure SFPF his llows for smll gin in timeD nd more importntly dereses the risk to lose the smple during the smple preprtionF hose smples support hve een suessfully tested on the shITe emlineF pigure SFPX mple support designs for the shITe emlineF A en luminum pin on whih the smple is mountedD whih hs to e pled inside ruer pinF A e new design of smple supportD lredy feturing the externl dimensions of the ruer pinF 5.2.2 Making the most of the sample preparation and installation sn order to utomte the instlltion of the smple inside the emD severl emE lines hve een equipped with roots whih utomtilly hnge the smpleF his is the se of the fwHS nd shIW emlines t the ipF his solution is however expensiveD nd introdues n dditionl risk of filureF et shITeD n rtiulted rm llows for the hnge of smple without opening the experimentl owl pled under vuumF his tion however still requires humn tionF he strtegy deE veloped here is to limit the numer of times this mnipultion hs to e done during n experimentF st is therefore to mke the most out of every smple instlltionD y putting lrge numer of smples on every supportF uessive tomogrphy n e lunhed y mro on the shITe emlineD nd the stge llows vertil movement @ diretionA of S mmD whih mkes the imging of mny suessive smE ples possileF o do soD di'erent smple preprtion methods hve een developedD depending on the type of smple to e imgedF por tomogrphy experimentsD opper pillrs re usully isolted nd mounted on n luminum pin using psfF he (nl on(gurtion is shown in pigure SFQF sn the se of opper pillrs sttistil nlysisD the hosen strtegy is here to sw IHH µm lrge support out of the wfer supporting the opper pillrsF uh on(gurtion is presented in pigure SFQF yne in the emD the opper pillrs re imged one fter the otherD with only n utomti shift in the diretion etween the tomogrphy quisitionsF pigure SFQX wo smple orgniztions for opper pillrsF A e opper pillr pled on n el pinF A IP opper pillrs pled on swn silion lmellF e omprison etween the imging of opper pillr pled on pin nd on multiEsmple support hs een performed on PS µm wide opper pillrsD frited with the sme proessF esults re shown in pigures SFRD D nd @respF dD eD nd fA for opper pillr pled on pin @respF on swn supportAF por ehD n slie reonstruted y the lgorithm is shown @pigures SFR nd SFRdD respetivelyAD together with orthogonl view @pigures SFR nd SFReD respetivelyAF pigures SFR nd SFRf re zoomEin views of the interfe etween the opper ylinder nd the umpF es shown on this (gureD the min fetures to spot n esily e identi(ed in oth smplesF ettention n e rought here on the zoomEin viewsD nd the voids ppering on themF sn pigure SFRD voids pper little strEshpedF hose re movement rtifts nd mke the further segmenttion of the voids di0ultF yn pigure SFR howeverD voids pper perfetly roundF his n e explined y the orienttion of the projetions nd thus the reonstrutionX the strEshped rtifts re orn y the originlly reonstruted sliesD those eing orthogonl to the em during the experimentX for opper pillr pled on pinD the rtifts will therefore pper on slies of interest @the interfeAD wheres for opper pillr on silion supportD they will e present on one of the orthogonl views @nmely pigure SFRdAF fy pling the opper pillr smples of vertil supportD more thn one hour per smple is sved during preprtionD s the silion support is only swnD nd out I hour per smple in instlltionD s this proedure is done one for ll smplesF purE thermoreD no loss in resolution is notiele y doing soD nd even n improvement n e seen in the slies of muh interestF por smples whih re yss tken from wferD two smples preprtion shemesD dpted from the lssi liftEout proedureD hve een developedF sn the se of stks presenting di'erent regions of interest situted next to one notherD it is posE sile to dpt the previously shown tehnique nd to prepre lrge smples @IHH µm lrge for exmpleAD whih ontin severl yssF he gol here is twofoldF pirstD lrge smple llows to otin lrge (eld of view imge of the ysD t lower ut still elow IHH nm resolutionF e more resolved quisition of the sme re n lso e otined using lol tomogrphyD whih fouses on one re of the smpleF o test this smple preprtionD prllelepipedEshped smple ws extrted nd pled on pinD using liftEout tehnique lose to the one used for ylindril smplesF he steps of the smple preprtion re illustrted in pigure SFS in the se of hyrid onding smpleD in whih the interfe etween opper pds ws to e oservedF he two smple preprtion shemes desried so fr n sve time during the smple preprtion nd instlltionF roweverD they only pply to the imging of regions of interest @hereD the opper pillrsA situted next to one nother on the originl wferF por ys situted fr wy from one notherD seond method hs een developedF e smple support is (rst prepredD y pplying n nnulr milling to the top of n luminum pinD using the psfF e ylinder of severl hundred of mirometersD suh s the one illustrted in pigure SFTD is otined in out hlf n hourF he smple is isolted nd extrted extly s previouslyF he deposition of the smple on the support is quite similrD lthough the smple is not mounted on the top of the supportD ut rther on its sideD s shown in pigures SFTD D nd F his proedure n e repeted with other smplesD s illustrted in pigure SFTdD whih fetures support where IP smplesD extrted from di'erent diesD hve een mountedF imilrly to opper pillrsD suessive tomogrphies re performed on the smplesF pigure SFRX gomprison of the results otined when imging opper pillrs pled lone on n el pin @D D nd A or on multiEsmple i support @dD eD nd fAF A yriginlly reonstruted slie of the pillrD presenting the interfe etween the ump nd the ylinderY A yrthogonl view of the pillrY A oomEin view of (gure F dA yriginlly reonstruted slie of the pillrD presenting the whole opper pillrY eA yrthogonl view of the pillrD ontining the interfeY fA oomE in view of (gure eF pigure SFSX mple preprtion llowing for lrge smpleD ontining severl regions of interest or ment for lrge (eld of view imgingF A he region round the ys is milledF A en re under the ys is milledF A he prt of the wfer supporting the ys is prtlyEmilledF dA e miromnipultor is soldered to the ysF he remining wfer prt supporting the ys is then milledD nd the miromnipE ultor rings the ys to n luminum pinF he ys is then soldered to the el pinD nd the solder join with the miromnipultor is removedF eA he smple thus otinedF pigure SFTX mple preprtion shemeD iming t pling severl smples on one single supportF he support is n luminum pinD milled in order to hve ylindril shpeD severl hundred of µm wideF he ys is isolted nd soldered to miromnipultorD s in lssi liftEout tehniqueF A he ys pprohes the supportF A he ys is pled on the support nd solder join is deposited etween themF he miromnipultor is removedF A he smple remins on the supportF dA he (nl smple supportD fter this proedure @D D A hs een performed for severl @hereD IPA smplesF hose psfEsed smples preprtion methods hve een tested on hyrid onding smplesF he gol ws to ompre the tehniquesD when it omes to imging the voids t the interfe etween the opper pdsF o do soD (rst lrge smpleD illustrted in pigure SFSeD hs een prepred in the psfF sn this smpleD the upper region hs een thinned down to PH µmD in order to imge the pds non lollyF his upper region is lter lled rt eD nd is the referene region for further imgingF rt fD on the ontrryD mesures SH µm in width nd is intended oth for lrge (eld of view nd lol imgingF rt eD de(ned in pigure SFSD hs een imged with pixel size of IH nmF rt f hs een imged lollyD t pixel size of IH nmD nd nonElollyD t pixel size of PS nmF enother smple ws lso prepred nd pled on supportD following the psfEsed multiEsmple support sheme presented previouslyF sn this exmpleD the support ws mde of IHH µm wide nd USH µm thik swn silion lmellD nd the quisition ws mde with pixel size of PS nmF ell quisitions were mde t n energy of QQFT ke nd PHHH projetionsF esults of the psfEsed smples preprtion shemes presented here re proE vided in pigure SFUD in whih spei( slie ontining the interfe etween opper pds is shownF pigure SFU is the referene imgeD quired with smll pixel size @IH nmA without lol tomogrphyF es n e seen in the orresponding zoomEin view @pigure pigure SFUeAD the morphology of the pdsD together with some voidsD n e oservedF sn the lol tomogrphy reonstruted slie @see pigures pigE ure SFU nd pigure SFUfAD the sme fetures n e oservedD without ny ovious rtift due to the lollyEquired dtF sn the lrge (eld of view slie @see pigures pigure SFU nd pigure SFUgAD more pds re visileD nd their morphology n e ssessedF roweverD the pixel size is too ig to spot ll the voids spotted using lol tomogrphy @s the pds presented in pigures pigure SFUf nd pigure SFUg re the smeD this omprison is strightforwrdAF pinllyD the slie otined from the smE ple pled on i support fetures lerly visile voidsF his tehnique is therefore shown to provide good resultsF yn ll the reonstrutionsD it is visile tht the voids present t the interfe etween opper pds remin elow SH nm in widthF hey re still in the eptne rngeD from proess point fo viewF es shown in this setionD pling severl smples on one support llows for n ovious gin in time in the shITeEsed nlysisD oth during smple preprtion nd instlltionF st hs lso een shown to provide good qulity reonstrutionD y omprison with smples pled on individul pinsF e vriety of smple preprtion methods hs een thought of nd re illustrted hereF emong these tehniquesD pling severl ys on support using psf is the more verstile methodD s it does not require regions of interest pled lose to one notherF st hs therefore een used extensively during this hhD minly for sttistil studies @see setion SFTFIAF sn the next setionsD only this method will e onsidered when disussing the gin in time of the smple preprtionF yne must however er in mind the other methods exist nd hve een proven e0ientF hey n e more relevnt for other smplesD with regions of interest situted next to one notherF pigure SFUX lies t the interfe etween the diesD otined with di'erent experE imentl orgniztionsX A PH µm wide smple @prt eAD pixel size IH nmD no lol tomogrphy @referene imgeAY A SH µm wide smple @prt fAD pixel size IH nmD lol tomogrphyY A SH µm lrge smple @prt fAD pixel size PS nmD nonElol toE mogrphyY dA smple pled on silion supportD pixel size PS nmF eADfAD gAD nd hA re zoomEin views of one pd tken respetively from AD AD AD nd dAD resled to mke omprison possileF oids re irled in redF st should e noted tht fA nd gA feture the very sme pdF 5.3 Reduction of the number of projections es explined in setion QFQFPFPD the piltered fk rojetion lgorithm o'ers mthE emtilly ext reonstrution of the imged ojetD provided lrge numer of projetionsF sn our seD ISHH to PHHH projetions were typilly quired for every distne on the shITe emlineF he quisition of those projetions requires sevE erl @typilly RA hoursF rereD we tried to redue the numer of quired projetions y using itertive reonstrution lgorithms 2 F e here tested numer of itertive lgorithms on xEry projetions nd omE pred the results to pf reonstrutionsF ell reonstrutions were performed using the estr toolox IHUF he study ws performed on slie of opper pillrD pled on vertil support suh s the one presented previouslyD with other pillrsF e referene reonstrution ws mde with PHHH projetionsD using pfD nd ll other reonstrutions were mde from the sme set of dtF his referene imge is shown in pigure SFVF pigure SFVX eonstrutions of the sme opper pillr slie using two di'erent reonstrution lgorithmsF A pf using PHHH projetionsF A gqEv using SHH projetions @nd PQ itertionsAF he sw vlue rised y the omprison of those two imges is HFVIF he imge qulity ws ssessed y (gure of merit @powAF rereD the sw @truturl swilrityA funtion IIU ws usedF he min dvntge of this funtion is tht the omprison is not lolD ut onerns generl fetures of the imgeF es our gol is to distinguish ojets in the imgeD this is of high vlueF he generl expression of the funtionD for omprison of two imges e nd fD is given in eqution SFIF

SSIM (A, B) = 2µ A µ B +C 1 µ 2 A +µ 2 B +C 1 • 2σ A σ B +C 2 σ 2 A +σ 2 B +C 2 • σ AB +C 3 σ 2 A +σ 2 B +C 3 @SFIA = l(A, B) • c(A, B) • s(A, B) @SFPA
where µ A @respF µ B A is the verge vlue of imge e @respFfAD σ 2 A @respF σ 2 B A its vrineD nd σ AB the ovrine of e nd fF C 1 D C 2 D nd C 3 re onstntsF he three frtions refer to di'erent hrteristis of the imgesX l(A, B)D the luminneD c(A, B)D the ontrstD nd s(A, B)D the struture of the imgesF he prmeters of the funtion @nmelyD C 1 D C 2 D nd C 3 A hve een tuned in order to (t the requirements of the opper pillr slies omprisonF e omprison of two identil imges rises the vlue ID nd the funtion is little impted y hnge in overll luminneF e hnge in ontrstD on the ontrryD dereses the funtion drstillyF he (nl funtion rises vlues etween EI nd ID EI eing rised when ompring n imge with totlly lurred version of itselfF ell omprisons were then mde with the sme sw prmetersD etween the referene imge @pfD PHHH projetionsA nd the ssessed imgeF pigure SFW shows sw vlues for pf reonstrutions regrding the numer of projetions usedD together with ys of the otined sliesF es n e seenD the sw vlue drops quite fst when the numer of projetions deresesF por exmpleD the sw vlue for SHH projetions is HFRSF es omprisonD (gures SFWD D nd d present the sw vlues otined with the eD sD nd gqEv lgorithmsD respetivelyD for vrious numers of projetions nd itertionsF es expetedD the vlues for PHHH projetions re lose to ID while still remining elow itX itertive lgorithms do not rise extly the sme results s pfF roweverD the vlues derese more slowly thn with pf reonstrutionsX they ll remin ove HFUD even for PSH projetionsF e ys of the opper pillr slie is presented for eh reonstrution performedD for visul omprisonF es n illustrtionD pigure SFV shows two di'erent reonstrutions of the sme slie of opper pillrF he reonstrution SFV ws performed using the pf lgorithm nd PHHH projetions @referene imgeAD while the slie SFV ws reonstruted from only SHH projetionsD using the itertive lgorithm gqEvF he sw vlue otined when ompring those imges is HFVIF isullyD one n retrieve the sme fetures from the two imgesX intermetlli lloys re lerly visileD nd voids nd eg preipittes n lso e spottedF he use of n itertive reonstrution lgorithms therefore llows to redue the numer of projetions y ftor R with little loss of imge qulityD ording to the sw (gure of meritF he dt quisition time is therefore divided y the sme ftorD going from four hours of dt quisition to only oneF pigure SFWX sw vlues for di'erent reonstrution lgorithmsD when ompring the otined slie with referene oneD otined when reonstruting the slie with PHHH projetionsD using n pf lgorithmF A sw vlues otined for pfD reE grding the numer of projetionsY sw vlues otined regrding the numer of projetions nd the numer of itertionsD for A eY A sY dA gqEvF 5.4 Automation of the post-processing sn the originl work)owD every step is mnully set nd triggeredF hen deling with similr smples @typilly opper pillrs or silionCopper stksAD the user often uses the sme prmetersF hereforeD it is possile to enter those prmeters t the eginning of the postEproessingD nd let the omputer trigger the proessing steps one fter the otherF rere we desrie ython wrpping mde round the postEproessing lgoE rithms implemented on shITeF st requires the informtion listed elowX

• votion of the dt setD nme of the smple • xumer of projetions • inergy of the em • pousEtoEmple distne • pousEtoEhetetor distne • δ/β rtio for the onsidered mteril es the proess ims t eing utomtiD prmeters hve een hosen to e the more likely to provide good resultsF hereforeD the lignment step is mde twieD s is usully done mnullyX the (rst lignment etween rdiogrphs is mde in the pourier dominD nd the seond one in rel speF he rottion xis lultion is performed utomtillyD following the sme priniple s in the mnul proedureX the (rst projetion is registered with the lst oneD )ipped horizontllyD nd the rottion xis is provided y the formulX RotationAxis = 1024 -s 2 D s eing the shift found etween the two projetionsF he sriptD desried here for one smpleD n proess di'erent dt sets in prllelD eh dt set eing proessed y n independent thredD whih llows for fster resultsF he utomti reonstrution of volumes hs een implemented nd tested with the pf lgorithmF st hs shown to e le to postEproess whole th of smples @ mximum of IP hs een tried so frA without humn interventionF he sript lso provides report llElong the postEproessingD whih llows to follow the di'erent steps of the proedureF uh reportD otined for one smple @with ISHH projetionsAD is shown in pigure SFIHF st lso fetures sttistis out the postEproessingD y giving the time tken y eh step of the proedureF pigure SFIHX eport rendered y the utomti postEproessing sript during the proedureD otined for one smple pled on n luminum multiEsmple supportF st provides informtion on the di'erent steps of the postEproessingD together with (nl ssessment of the time they tookF

Time gain and discussion

sn the previous setionsD di'erent strtegies hve een set in ple in order to redue the overll time of the tomogrphy setup on shITeD with fous on the redution of humn intervention nd the em timeF hey ll hve een shown to redue the nlysis timeD with no or little loss in resolutionF rereD we present n updted version on the shITe work)owD tking into ount those strtegiesF e disussion on their (eld of pplition nd their limits is lso proposedF pigure SFII presents the updted work)ow of shITeD with the time required for eh stepF he new vlues hve een lulted with the psfEsed smple preprtion shemeD nd dt quisition sed on SHH projetionsF he (gure lso ssumes n utomti postEproessingF he vlues re given for one smple nd lulted s the men time per smpleD ssuming the smple is pled on support ontining IH smplesF pigure SFIIX pdted version of the shITe work)owD tking into ount the methods iming t inresing its throughputF he vlues re verge onesD given for I smpleD ssuming it ws pled on support ontining IH smples in totlF st should e noted tht the time sle is not the sme s in the originl (gure @pigure SFIAD nd the overll time presented is now out U hours insted of ITF his is minly due to the redution of the numer of projetionsD whih redues the dt quisition time from R hours to ID together with the phse retrievl timeD whih psses from V hours to PF woreoverD more steps re now utomtiD s ompred with the originl (gureX the whole postEproessing therefore ppers in greenF he smple preprtion time is reduedD sine the psf setting n usully e mde for whole th of smpleF he sme pplies to the smple instlltionD whih lsts n hour ut n e done one for IH smplesF gomined togetherD these strtegies therefore llow for drsti redution of the timeD espeilly the one n opertor hs to spend on the experimentF st should e reminded tht this (gure hs een relized in spei( onditionsF elthough we elieve the methods presented here n pply to mny smples nd situtionsD they might not trigger s good resultsF pirstD the smples must e E soring enoughF sn ftD lthough the support is mde of lowEsoring mteril suh s silion or luminumD it is possile tht for lowEsoring smplesD the toE mogrphy will e onsidered lol @sine the support ppers on some projetions ut not llAD reting rtiftsF sn the se of miroeletronis nd more spei(lly of opper oservtionD this issue is not enounteredF hen onsidering the diminution of the numer of projetionsD numer of ssumptions hve een mdeF he reonstrutions hve een mde from dt set of PHHH phse mpsD from whih numer of projetions @PSHD SHHD IHHHD or PHHHA hve een usedF his mens tht the originl lignment etween the four distnes ws performed using the PHHH x R rdiogrph dt setF es the lignment relies on the tul lignment of every 100 th ngle nd (ttingD it is possile tht the lignment would e poorer with only SHH projetions quiredF roweverD this issue should e solved y inresing the numer of projetions the tul registrtion is sed onF pinllyD the omplete utomti postEproessing hs een proven to work so fr only with the pf reonstrution lgorithmF st is however likely to work with ny lgorithmD sine it is n independent step of the proessF he time vlue given in (g SFII for the phse retrievl is P hoursD sine the numer of slies is redued y ftor R nd so does the lultion timeF he reonstrution time hs een @overEAestimted to e Q times the time needed for n pf reonstrutionD tht is to sy out one hourF e further investigtion of the postEproessing timeD requirE ing the implementtion of itertive reonstrution lgorithmsD would e possile improvement of this studyF yther improvements of the utomti postEproessing ould e implementedF ine severl prmeters @suh s the positionsD energyD nd numer of projetionsA re sved in the dt quisition frmeworkD the postEproessing sript ould feth themD whih would limit the numer of prmeters the user hs to enter to the dt set lotion nd the δ/β rtioF woreoverD intermedite (gures ould e shown during the proessingD for the user to hek its qulity efore going furtherF e grphi interfe ould llow to do so in userEfriendly wyF es seen in this setionD the shITe emline o'ers high resolution reonstrutions nd pplies to Qh integrtion deviesF e set of methodsD rnging from smple preprtion to postEproessingD hve een shown to limit the needed time for the omplete imging proessD without deresing the imge qulityF sn the next setionD set of smples from the Qh integrtion (eld re shownD in order to illustrte the possiilities of shITe on suh smplesD nd when possile to ompre it with other Qh imging tehniquesF 5.6 Application to 3D integration imaging sn this setionD three illustrtions of the possiilities nd limits of shITe re givenD with the help of other Qh imging resultsF e (rst prgrph presents study on lrge numer of smplesD mde possile y the new shITe smple preprtion shemeF e seond prgrph is dedited to the imging of opper pillrs y di'erent tomogrphy setupsF e omprison of the di'erent tehniques is providedD tking into ount not only the otined resolutionD ut lso the time needed for the imging proessD the retrievle informtionD nd the vilility of the equipmentF pinllyD disussion is onduted out the possiility to enlrge the (eld of view of tomogrphy imgingF 5.6.1 Imaging of a large number of post-electromigration samples rereD we present n illustrtion of the new shITe work)owD when pplied to lrge numer of smplesD in order to otin sttistil informtionF he onsidered smples re hyrid onding ones PD with disy hin strutureF e top view of the strutureD quired y infrred @sA imgingD is presented in pigure SFIPF he smples re stressed @QIW¦gGIS meA until the filure riterion is rehed @reltive resistne inrese of IH 7AF he ime o pilure or p is then mesuredF huring this testD opper is displed y eletromigrtion mehnismsD whih results in the retion of voidD situted t lotion identi(ed in previous work IIVF his re is irled in pigure SFIPF he gol of the experiene is to study whether there is orreltion etween the volume of the void nd the pF elthough the lotion of the void is knownD lssi imging methods suh s iw or psfGiw only provide Ph informtionD nd the Qrd dimension dimension of the void is in generl ssumed to e equl to its line widthF fy omining the lrge (eld of view nd high resolution hievle on the shITe emline with the new work)owD n tul Qh mesure ould e otined for PH smplesD providing sttistil informtionF wo luminum supports were prepredD nd respetively IP nd V smples were pled on themD s illustrted in pigure SFIQ nd F he smples of eh support were suessively imged y tomogrphyD withE out ny humn interventionF he IP smples on the (rst support @pigure SFIQA were imged with ISHH projetionsD whih led to out RH hours of unsupervised quisitionF por the seond support @pigure SFIQAD IWHH projetions were quired for eh smpleD nd the entire quisition lst for QR hoursF he reonstrution ws then performed utomtillyD one ll the quisitions were overF pigure SFIPX snfrred top view of one ysD where the void due to eletromigrtion ppers fter n eletromigrtion testF he preise lotion of the void retion is irled in redF pigure SFIQX wo luminum supports ontining respetively A IP nd A V smE plesF e slie ontining the reserhed void is presented for eh smple in pigE ure SFIRF he sme ys of the smple n e identi(ed on every slieD nd the void ppers lerly in lk on ll @exept for the two referene smplesD whih did not undergo the eletromigrtion testAF prom those reonstruted volumesD the void n e segmented quite esilyD given the high ontrst of the reonstrutionF yne exmE ple of suh segmented volume is presented in pigure SFIRF he segmenttion is done independently for every smple with lol threshold tool nd tkes out IS minutes per smpleD using the evizo softwre @nd the wgi wnd toolAF prom the segmented voidsD the depleted volumes of opper ould e mesured nd ompred to the pF he result is presented in pigure SFIRF e ler orreltion etween depleted volumes nd p is highlighted thnks to sttistil dt nlysisF he orreltion ftor of erson is equl to HFVS3 F he high resolution hievle on the shITe emlineD omined with new smple preprtion shemeD therefore llowed to perform Qh sttistil studyF 5.6.2 Morphology study on copper pillars huring this hhD opper pillrs were imged with lrge pnel of tehniquesF rereD we present the results otined on SH µm wide opper pillrsD with Q tomogrphy setupsX shITeD shIWD nd eiss rdi l tomogrph4 F hose setups hve een presented in setions QFP nd QFQF emong the possile setup prmetersD preliminry quisitions hve llowed for n optimiztion of the quisition setupsF por the shITe emlineD n energy of QQFT ke ws hosenD nd the hosen smple orgniztion ws swn silion supportD on whih opper pillrs were pled next to one notherF he sme support ws used t the shIW emlineD where the energy ws IW ke during this experimentF sn the se of the l tomogrphD pling the opper pillr on luminum pin showed etter results thn the silion supportF he remining experimentl prmetersD suh s the pixel sizeD the numer of projetionsD nd the exposure timeD re provided in le SFIF HFS HFP TH le SFIX ixperimentl onditions for the imgig of opper pillrsD using three di'erent tomogrphy setupsX shITeD shIWD nd l tomogrph e pigure of werit @lter lled powA is de(ned in order to pproh the resolution nd ompre the resultsF st is sed on the width of n edge on Ph imge of interestF his esyEtoEuse method relies on the mesurement of the numer of pixels pigure SFIRX A lie of interestD ontining the enter of the depleted volumeD for the PH nlyzed smplesF he (rst two smples eing referenesD no opper ws depletedF sn the other smplesD the depleted volume ppers in lkF A en exmple of the segmented depleted volumeF A lues of the depleted volumes regrding the ime o pilureF he plin line is the otined (tD whih is liner @with orreltion ftor of HFVSAD while the dshed lines de(ne the on(dene intervl t WS 7F pigure SFISX eonstruted volumes of opper pillrsD otined with A shITeY A shIWY A v tomogrphF por eh setupD slie reonstruted y the softwre is shown @AD together with one orthogonl view @AF e zoomEin view of the interfe ontining the voids is lso presentedF he otined pow vlue is lso providedF enlosed in n edge of the smple @here the edge of lrge enough voidAF he width of suh n edge is otined y mesuring the full width t hlf mximum @prwA of the pro(le9s derivtiveF his vlue is then multiplied y the pixel sizeF his riteri oviously does not provide the resolutionD ut gives ommon ground for imging tehniques omprisonX it tkes into ount the pixel size rehle y the tehniquesD the shrpness of drsti ontrst hngeD nd to some extent the ontrst sensitivity of the tehniqueF sn order to limit the impt of the hoie of the voidD the vlue is lulted on numer @etween IH nd ISA of voids in the whole volume nd is given with n error mrginF pigure SFIS provides seleted slies from the otined reonstrutionsD together with zoomEin view of the interfe nd the lulted powF e lrge rnge of pow is visileX while the pow of the l tomogrph is out IFQ µmD tomogrphy performed in synhrotron n hieve pow of RUH nm @shIWA or even PPS nm @shITeAF st is notiele tht voids even smller thn those vlues n e spotted @respF IFP µmD RIH nm nd IPH nm for respF the l tomogrphD shIW nd shITeD those vlues eing lulted with the prw vlue of void pro(leAF hile voids lerly pper on ll three reonstrutionsD the intermetlli lloys re rely visile on the l tomogrph reonstrutionF he synhrotron sed tomogrphiesD s they re sensitive to phse shifts nd therefore more sensitive to edges even etween similr mterilsD llow for etter visuliztion of those feturesF yn the shIW mirotomogrphy zoomEin viewD light irles surrounding voids re visileX they re the e'et of phse whih enhnes the edges nd mke them more visileF his lso 'ets the pow vlueX euse of this edge enhnementD the pro(le seems pigure SFITX ime required for three tomogrphy setups for the imging of opper pillrsD split into their di'erent stepsF shrper thn it relly isD nd the pow vlue presented here n e it optimistiF elthough this imge o'ers high ontrst of voids nd even intermetllisD etter ontrst nd resolution re provided y the nnoEtomogrphy performed on shITeD s n e seen when ompring the two zoomEin viewsF st is lso worth mentioning tht shITe o'ers the possiility to dpt the pixel size to the onsidered smple lmost ontinuouslyD s it only depends on the position of the smpleF shIW is dependent on the ville lensesF hen ompring suh hrteriztion tehniques in n industril ontextD it is importnt to tke into ount the time required for the glol imging proessF pigure SFIT presents the time needed for eh step of the onsidered experimentl setupsF st is notiele tht the vlues presented for shITe di'er from the ones given erlier @pigure SFIIAD euse the smple instlltion di'er @here the support is simply swnAD nd so does the dt quisition @IRSH projetions re quired insted of SHHAF he shIW emline is designed for industril needsF he dt quisition is mde in out QH minutesD nd so does the postEproessingF his is enhned in the se of this experimentD where no phseEretrievl lgorithm is pplied to the dtF his setupD omined with fst smple preprtion shemeD leds to very quik imging proessF sn order to reh resolutions omptile with the opper pillr imgingD the exposure time of the l tomogrph hs een inresedD together with the numer of projetionsF his leds to long @V hoursA dt quisition stepF woreoverD the hosen smple preprtion sheme @psf liftE outA is long oneD ut ims t improving the resolutionF shIW is wellEestlished tomogrphy emlineF st indeed o'ers wellEresolved reonstrution in little time @out I hourAD nd is omptile with the new smE ple preprtion sheme proposed hereF shITe o'ers lerly etter resolution nd ontrstD s disussed erlierD ut t the ost of severl hours per smpleF sn ftD even y pplying n itertive reonstrution lgorithmD whih would llow for the quisition of only SHH projetionsD the overll time for the shITe work)ow would e out T hoursF e trdeEo' must lerly e found etween the two emlinesF prom pigure SFITD it is ovious tht the l tomogrph nnot ompete with the synhrotron emlines on this prtiulr smple typeD neither when onsidering the resolutionD nor the experimentl timeF roweverD one must er in mind tht it is l equipmentD whih o'ers the possiility to imge the smple t ny momentD whih is not the se fo synhrotron experimentsF untul nlysis ould therefore e onduted on the l tomogrphD while mesurements mpign would ene(t from the synhrotron sed tomogrphiesD performed on either lineD depending on the wnted resolution nd ville timeF 5.6.3 Towards a larger eld of view he new shITe work)ow llows to redue the nlysis timeF roweverD it is still muh longer thn on shIWD nd the (eld of view remins elow IHH µmF elthough it o'ers high resolutionD it is not wellE(tted for the imging of omplete stks or pkgesF por these feturesD experiments hve een onduted on shIWD oth in tomogrphy nd lminogrphyF sllustrtions of the possiilities of this emline for opper pillrEsed stks re presented hereF he imging experiments primrily ims t spotting voids inside opper pillrsF sing tomogrphy on shIW with pixel size of HFTS µmD omplete stks ould e imgedF he smple presented here is stkingD mde y the use of IH µm lrge opper pillrsF e polymer ws then injeted in the re remining etween the two wfersD nd the top wfer ws thinned down to Q µmF he gol is here to see the voids inside the pillrsD nd possily some defets inside the polymerF et this mgni(tionD the shIW emline should llow for (eld of view of IFQ mmF roweverD method hs een implemented on this emlineD in order to inrese the poX y shifting the rottion xis from the enter of the quired imgesD nd rotting the smple y QTH • insted of IVHD lrger prt of the smple n e imgedF his inreses the (eld of view y SH 7D llowing for P mm wide smplesF he smples were therefore swn into this dimensionF he tomogrphy quisition ws performed with SRHH projetions @to over QTH • AD with n exposure time of HFHS seF he energy of the em ws PTFS keF enother smple ws imged using lminogrphyF his tehniqueD s explined erlierD presents the dvntge of limiting the smple preprtionD s it n remin in it originl wfer formF he onsidered smple is lso stkD ontining PH µm lrge opper pillrsF he lminogrphy quisition ws performed t n energy of PS keD with pixel size of HFTS µmF por eh lminogrphyD QTHH projetions were quiredD t n exposure time of HFHS seF pigure SFIUX olume reonstruted y lrge (eld of view Qh imging setupsX A omogrphy performed t shIW with pixel size of HFTS µmY A vminogrphy performed t shIW with pixel size of HFTSµmF he (gure fetures one slie reonE struted y the softwre @A nd two orthogonl viewsD ll entered on the imging of opper pillrsF pigure SFIU presents the volumes otined y tomogrphy nd lminogrphy performed on shIWF por oth setupsD the quisition of dt requires out IH minutesF he reonstrution itself tkes out QH minutes in oth sesF roweverD for tomogrphy it is utomtiD while lminogrphy tody requires mnul lignment tht lst out PH minutes per smpleF es n e on the resultsD the otined (eld of view is fr lrger tht the one tht n e otined on shITeX out I mm ould e imgedD oth y tomogrphy nd lminogrphyF his llows for lrge sttistis on opper pillrsF his of ourse hs n inidene on the resolutionF sn oth reonstrutionsD only lrge voids @out I µmA n e imgedF hey pper in lk nd present good ontrstD whih mens their segmenttion is quite esyF st is worth mentioning tht for tomogrphyD the resolution is limited y the quisition methodD nd is the sme is ll three dimensionsF sn lminogrphy howeverD the resolution is lower in the diretionD due to lk of informtionF e trdeEo' etween resolution nd (eld of view must then e foundD nd those two tehniques will provide gret sttistis for lrge @ few millimetersA ojetsF vminogrphy in prtiulr o'ers the possiility to void smple preprtion of ny kind for thinned stksF sn the experiment onduted hereD with the energy of PS keD it ws however not possile to imge omplete pkged die relilyD s the smple ws too thikF roweverD it ppers quite lerly tht the shIW emline @used in tomogrphy or lminogrphyA remins n dpted tool for fst filure loliztionD espeilly sine it o'ers fst quisition nd lrge poF roweverD when it omes to the hrteriztion of smll @`SHH nmA defetsD the shITe emline is etter suitedD nd llows for e0ient imgingF pigure SFIVX olumes nd voxel size of smples nlyzed on shITe during this workD together with their typeF he provided volume is the one of the (nl ysF 5.7 Conclusion sn this hpterD the shITe emline hs een presentedD in wy it n e used s routine tool for the Qh imging of Qh integrtion deviesF he work)ow urrently implemented on the emline hs een shown nd desriedF e new work)owD relyE ing on new smple preprtion shemeD the redution of the numer of projetionsD nd the utomtion of the postEproessingD hs een depitedF st hs een shown to workD nd llows for the redution of the overll nlysis time y ftor PF wore importntlyD it redues the humn intervention time drstillyD s the user now minly ts during the smple preprtion nd the instlltion of whole th of smplesF sn seond prt of the hpterD exmples of possile pplitions of the shITe emlineD omined with the previously introdued work)owD hve een givenF hey inlude omprison of di'erent tomogrphy setups pplied to the imging of opper pillrsD nd sttistil study mde possile y the new smple preprtion shemeF sn order to give n overview of the smples tht n e imged using the shITe emlineD pigure SFIV presents the volumes nd voxel sizes of numer of smples pigure SFIWX olumes nd voxel size of smples nlyzed on shITeD shIW @tomogE rphy nd lminogrphyAD nd the eiss l tomogrph during this hhF nlyzed during this hhD together with their typeF he presented volume is the (nl ys volumeD nd not the volume of the whole reonstruted ueD s this is more relevnt informtionF st is worth pointing out tht the (eld of view o'ered y shITe is still limitedD whih is usully the prie for high resolutionF e lst prgrph of the hpter presents shIW tomogrphy nd lminogrphy s wys to inrese the imging (eld of viewD while limiting the smples preprtionF st must however e notied tht these positive e'ets re possile here t the expense of the resolutionF sn order to ompre the possiilities of shITe tomogrphy to the ones of more estlished tehniquesD pigure SFIW presents lrger seletion of smplesD imged respetively on shITeD shIW tomogrphyD shIW lminogrphyD nd the rdi l tomogrphF st n e seen tht shIT is pled in the leftElower ornerD orresponding oth to low voxel sizes nd quite smll imged volumesF hen ompring this imge to the one otined t the end of hpter RD one n see the tomogrphy performed on shITe mkes the link etween the psfGiw destrutive tehnique nd otherD not so wellEresolvedD nonEdestrutive tomogrphy tehniquesF e spei( set of smplesD mong whih Qh integrtion si ojetsD will therefore highly ene(t from this tehniqueF es mentioned eforeD the gol here is not ultrEfst tomogrphyD nd the shITe emline is not ment for in situ tomogrphyF roweverD the proessing time ould e reduedD in order to (t some industril needsF Contribution à l'imagerie par tomographie sur ID16A appliquée à l'intégration 3D Résumé du chapitre ge hpitre est onsré ux développements menés sur l ligne de lumière shITeD visnt à son utilistion dns un ontexte industrielF out d9ordD le proédé glol d9nlyse de tomogrphieD pour des éhntilE lons de miroEéletroniqueD est détilléD depuis l préprtion d9éhntillons jusqu9à l9otention du volume reonstruitF ve temps que néessite hque étpe est donnéD sé sur une expériene utilisteurD et sépré en di'érentes tégoriesD selon qu9il s9gisse d9un temps néessitnt une mhine telle que le psfD le fiseu synE hrotronD ou une intervention humineF ves uts de l9étude sont rppelés X il s9git de limiter le temps glolD mis surtout de réduire le temps de fiseu et de mxE imiser l9utomtistion (n de limiter l9intervention humineF our elD trois strtégies sont mises en plesF out d9ordD un nouveu modE èle de préprtion d9éhntillons est développéF ves éhntillons sont plés sur des supports vertiuxD les uns à ôté des utresD e qui permet de lner des toE mogrphies suessives sns intervention humineF ve nomre de projetions est ussi réduitD grâe à l9utilistion d9lgorithmes de reonstrution itértifsF in(nD un sript est érit (n d9enhiner toutes les étpes du postEtritement utomtiqueE mentF hns e hpitreD nous montrons que es strtégies permettent de réduire le temps d9nlyse glol @d9un fteur PAD le temps de fiseu @d9un fteur RAD et le temps d9intervention humine @d9un fteur QAD sns perdre en résolutionF in(nD des exemples d9pplitions de l ligne de lumière shITe sont donnésD sur des éhntillons d9intégrtion QhF sl est montré que le nouveu proédé d9nlyseD et notmment l nouvelle préprtion d9éhntillonD permet de réliser une nlyse sur un grnd nomre d9éhntillonsD ve très peu d9intervention humineD mennt à une informtion sttistiqueF ne seonde étudeD menée sur des piliers de uivreD ompre les performnes en temps et en résolution de di'érents dispositifs de tomogrphie X shITeD shIWD et un tomogrphe de lortoireF shIW est dpté pour de grnds nomres d9éhntillons r l9nlyse y est rpideD mis des nlyses à hute résoluE tion néessitent l9utilistion d9shIeF ve tomogrphe de lortoire n9o're dns e s ni l résolution ni l rpiditéD mis permet de réliser ette mesure sns déliD ontrirement ux lignes synhrotronF in(nD une ré)exion sur le hmp de vueD qui reste ssez file sur shITeD est menée à l9ide de résultts de tomogrphie et de lminogrphie otenus sur shIWF Chapter 6

Local strain measurements in hybrid and direct bonding stacks sn the lst two hptersD pnel of Qh imging tehniques hs een depited nd shown to pply to Qh integrtionF hose tehniques provide numer of informtion on the Qh integrtion ojets morphologyD tht n e orrelted with future filure of the devieF roweverD in some sesD the morphology is hrd to link diretly to the devie mehnil ehviorF sn order to otin more omplete hrteriztion of Qh integrtion deviesD experiments were rried on shHID whih is nnoEdi'rtion emlineF he emline setup ws presented in setion QFPFQD while the tul experiment priniple nd work)ow were desried in setion QFRF hi'rtion is ommonly used for miroeletronis hrteriztionD nd shHI o'ers the possiility to otin lol informtionD s the em rehing the smple hs width of PHH nm @t n energy of W keAF rere we present two illustrtions of the possiilities of shHI for the hrterizE tion of Qh integrtion smplesF pirstD the in)uene of hyrid onding opper pds on the lower nd upper wfers of silion ws investigtedF he shHI emline llowed for simultneous investigtion of the two silion lyersD with little smple prepE rtionF he strin results otined for those ptterned smples re orrelted with oservtions of the smple inner morphologyD otined y tomogrphy on shITeF sn seond prtD muh simpler smple is investigtedD in order to otin strin mps in opper grinsD efore nd fter RHH • g nnelingF he smple is only onstituted of silion wferD on top of whih fullEsheet of opper is deposited 1 F 6.1 Hybrid bonding stack strain measure in silicon rereD we present the possiilities of shHI frgg di'rtion imgingD when pplied to hyrid onding stkF he onsidered smple is mde of two wfers of @HHIAE oriented silionD topped with two lyers of ptterned opper pdsD linked together with opper vis surrounded y Si0 2 F he wfers re then ssemled togetherD using the k )ip ondingD s lredy illustrted in pigure IFS @setion IFPAF he onsidered region of interest in this smple ontins prtiulr strutureD lled disyhinsF uh ys is presented in pigure TFIF he (nl step of the smple frition is the thinning of the top wfer down to Q µmF st is mde y polishing nd hemil ttkF elthough it is not smple preprtion stepD it is however ruil for the experimentD whih is performed t n energy of W keDwith em size of PHH nm x SHH nm @horizontl x vertilAF et this energyD the ttenution length of xEry is WVFP µm in i nd QFWS µm in guF por the em to reh the silion sustrteD the originl thinning of the top lyer is therefore ritilF woreoverD the thinning (nl step is hemil ttkD whih llows the ssumption tht the thinning does not indue supplementry strinF pigure TFIX A tk ontining disy hinsF snsetX view of one unit of the opper designF e tomogrphy of similr smple ws lso relizedD in order to orrelte the otined mps with the tul smple morphologyF he smple used for this nlysis is the one presented in pigure SFSe @setion SFPFPAD imged t n energy of QQFT keF he imged re is prt fD with pixel size of PS nmF 6.1.1 Simultaneous observation of two silicon layers sn the hyrid onding smpleD the strin in the two lyers of silion ws mesuredF he thinning of the top lyer ensures tht the em rehes oth the top lyer nd the silion sustrteF sn this studyD the @HHRA plnes of IHH x IHH µm 2 re were nlyzed @with smpling step of SHH nm in oth diretionsAD the ngles of the roking urve going from QHFRU • to QHFWU • with HFHI • stepF he smple @DDA oordintes re de(ned suh s the xEry rrive in the plne @see pigure TFPAF pigure TFPX A shemti view of the two silion lyers nlyzed in the ptterned smple nd the trjetory of the xEry inside it for given ngle ηF snside the top lyerD toms nd rystlline diretions re representedF por understnding purposesD toms re not represented in the sustrte representtionF A e Qh representtion of the detetor quisitionD mde y stking the Ph quisitions for ll the ngles ηF pigure TFP provides shemti view of the silion lyers of the ptterned smE pleD nd more preisely the rystlline plnes inside themF prom the mnufturing proessD the lyers re known to e prllelF his hs een veri(ed y diret miE rosopy oservtionF he @HHRA rystlline plnes from one lyer however re not neessrily prllel to the @HHRA plnes of the other lyerF sn ftD the two wfers tht form the top lyer nd the sustrte ould e ut from two di'erent i monoE rystlsD nd the utting plnes re likely to e di'erent from the @HHIA plneF sn (gure TFPD the top lyer rystlline plnes re ssumed to e perfetly ligned with the smple sed @DDA oordintesF he sustrte plnes however present three ngles (α, β, γ) regrding these oordintesF his leds to two di'erent signls on the detetorX one omes from the silion sustrteD the other one from the top lyerF pigure TFP presents Qh representtion of the otined dtF he Qh view is mde y stking together Ph imges of the detetorD for ll ngles η forming the roking urveF por understnding purposesD projetions of the dt re given on the plnes @X d Y d A nd @Y d ηAF es nnounedD two distint peks re oservleF hey hve di'erent shpesD nd re seprted on the detetor y distnes ∆X nd ∆Y F woreoverD they do not pper for the sme ngle ηX they re seprted in the Qh representtion y distne ∆ηF sn the se of the ptterned smpleD the sustrte pek ppers for η = 30.81 • D while the lyer pek ppers for η = 30.65 • F imple geometry onsidertions estlish qulittive links etween the mislignE ment of the rystlline plnes nd the reltive positions of the peksF he qunti(E tion of those linksD whih hs to tke into ount the refrtion of xEry inside the smpleD is not onduted hereF he di'erentition etween the two peks is performed using their shpeX the lrger the lyerD the shrper the ptternF his distintion llows for the de(nition of two ys on the detetorD eh orresponding to silion ontriutionF 6.1.2 Strain maps and morphology correlation he seprtion of the two lyers ontriution to the di'rted signl leds to two strin mpsD presented in pigure TFQ with ommon olor sleF hue to the ngle η etween the surfe nd the emD s well s the tul depth of the di'erent feturesD originlly the two mps re not perfetly ligned in the diretionX there is shift etween fetures from the top lyer nd from the sustrteF his is due to the ft tht for eh mpD the @DA point is ssumed to e the point where the em hits the smple surfeF por the sustrte mp howeverD the vlue situted t the point @DA reltes to informtion gotten t the point @DC∆Y AD s illustrted in pigure TFPF por n esier omprisonD the presented mps were shifted in the diretion in order for the fetures to e lignedF st is notiele tht while the top lyer mp is diretly interpretleD the nlysis of the sustrte is not so diretD s multiple refrtion nd sorption e'ets our efore nd fter the intertion of the em with the sustrteF he vlues re therefore rther to e tken s reltive vlues inside eh mpD insted of solute vluesF he mps show reltively low nd equl outEofEplne strin in silion in oth lyersD s the verge vlues for respetively the top lyer nd the sustrte re < ε zz,layer >= 0.06% nd < ε zz,substrate >= 0.07%F e higher strin level drws retngulr shpeD tht n e interpreted s lrge opper pd imprintF he mximum strin is otined lose to those retngles edgesF pigure TFQ presents slies of the disy hins reonstruted from nnoEtomogrphy experimentsF nd views show the pro(les of disy hinsD while the pds re fully visile on the two viewsD t two di'erent levelsF hose views show the opper pds lose pigure TFQX esults of the oservtions performed on the hyrid onding imgerF A trin mps of the i top lyer @on the leftA nd the i sustrte @on the rightA with ommon olor mpF he lk retngles drw the shpes of lrge opper pdsF A eleted slies of the volume reonstruted y nnoEtomogrphyF nd views of the disy hins @on the top nd on the rightAD slies on the lrge pdsD respetively lose to the top lyer nd the sustrteF he shpe of the regions of interest presented in pigure is reported in pigure for morphology orreltionF to the top lyer @on the leftD in plin greenA nd the ones lose to the sustrte @on the rightD in dshed redAF es stressed y the frmes of (gure TFQ reported in pigure TFQD the shpes oserved on the strin mps orrespond extly to the morphology of the lrge pds present on the smpleF his on(rms the ft tht higher strin is oserved in the silion lose to lrge opper pdsD nd tht the highest strin is oserved on the pd edgesD where the pds re onneted to the lower levelD using opper visF he onstrint underwent y those smllEdimension vis is likely to e the origin of the strin inside the silion lyersF 6.2 Direct bonding in-situ strain measure in copper sn order to mesure the strin in opper during the proessD nd more preisely during nnelingD seEstudy smple ws relizedX SHH nm of fullEsheet opper were deposited on top of USH µm thik silion sustrteD nd only lyer of SiO 2 ws pled on top of the opper in order to protet it from oxidtionF en illustrtion of suh smple is proposed in pigure TFRF xo smple preprtion ws needed for the mesure of strinF pigure TFRX tk mde of silion wfer topped y fullEsheet lyer of opper nd proteted y lyer of SiO 2 F sn this nonEfuntionl fullEsheet smpleD the strin in the opper lyer ws meE suredF lnes @RRRA were oserved using the uEwp method t room temperture s well s t RHH • gF he smple ws pled inside homemde eryllium dome hot stge IIW in oth situtionsD llowing to het the smple when needed with little sorption of the xEry emF e (rst experiment ws rried out t room temperE ture @A under vuumF en re of TH x IHH µm 2 ws nlyzedD with smpling of @horizontl x vertilA RPV nm x UIR nmF he ngles of the roking urve were hosen from η a RHFST • to η a RIFST • with HFHS • stepsF yne the experiment ws overD the smple ws heted progressively up to QWR • gD while dpting its position in order to keep the sme grins inside the (eld of viewF e seond strin mp of @RRRAEoriented grins ws then quired t QWR • gD with the sme snned re s previously nd roking urve going from η a RHFUT • to η a RIFPT • with HFHS • stepsF pigure TFS shows two strin mps of the @RRRAEoriented grins of the gu sheetD t room temperture nd t RHH • gF sndividul grins n e oserved nd it is visile tht the sme grins hve een imged during the two experimentsF he verge vlues from those two mps re < ε 444,RT >= -0.27% nd < ε 444,400 • >= 0.47%F hereforeD the nneling indued strin ∆ε = 0.74%F sf the strin in opper is only due to temperture @iFeF therml strinAD its theoretil vlue is given using eqution TFIF ith α = 17 • 10 -6 K -1 nd ∆T = 370KD it rises ∆ε = 0.63%D whih is quite lose to the experimentl dtF ∆ε = α.∆T @TFIA st is notiele tht the nlysis ws mde on plne @RRRAD so the three direE tions ontriute to the (nl vlues of strinF roweverD when ompring the verge vlues of the omponents of in this seD it ppers tht Q Z is predominnt for oth experimentsX the deformtion is minly in the diretionF he silion does not onstrin the opper in tht diretionD whih mens it is norml for the opper to follow its nturl ehvior during hetingF edditionl mesures in di'erent plnes ould e interesting nd give us more informtion on the intertion etween silion nd opperF pigure TFSX trin mps of @RRRAEoriented opper grins inside SHH nm thik opper lyer deposited on top of silion wferD A t room tempertureY A t RHH • gF golor mps re dpted in order for the stronger strin @either in tension or ompressionA to pper in redF 6.3 Conclusion sn this hpterD strin hs een mesured for two silion nd opper stksD imed for the (eld of Qh integrtionF shHI ws shown to e wellE(tted for the simultneous mesurement of lol strin in two silion lyersD onded with hyrid ondingF st ws lso possile to omine the sid mps with morphology oservtionsD nd on(rm tht the shpes oserved in the strin mps were the opper pds present in the smpleF o study the strin in onding opper efore nd during hetingD nonEfuntionnl nd muh simpler smple ws lso nlyzedF he experiment setup llowed to meE sure the strin in @RRRAEoriented grins of opperD nd to follow the grins during RHH • g nnelingD in order to mesure the strin in those sme grinsD t RHH • gF shHI is long emlineD whih hs lredy een used for miroeletronisD in prtiulr for the nlysis of hough ilion is @A IPHD IPID IPPF his study enlrges the possiilities of shHI to multiElyered stksF st llows for quisitions or lrge res of the smple @IHH x IHH µm 2 AD together with sptil resolution of severl hundred of nnometersD providing lol informtionF hereforeD it lE lows for sttistil nd possily inEsitu nlysesF woreoverD orreltion etween two tehniques @shHI di'rtion imging nd shITe tomogrphyA is here shown to e possileD nd ould led to etter understnding of the links etween strin nd morphology inside Qh integrtion stksF sn the se of strin mesurements in opperD sine it is here polyrystllineD one ould ene(t from vue nlysis of the smpleD whih would provide more generl informtionD regrding the strin in ll the grinsF he tehnique used here is however simpler to postEproessD nd still provides n pproximtion of the strin in opper lyerD together with n informtion out the grin sizeF

Mesure locale de déformations au sein d'empilements

Résumé du chapitre hns e hpitreD nous dérivons deux mesures loles de déformtionsD rélisées pr nnoEdi'rtion sur l ligne de lumière shHI de l9ipF hns une première mesureD un empilement rélisé pr ollge hyride est nlyséF sl est omposé de deux wfers de siliiumD entre lesquels se situent des strutures de uivreF ve ut de ette étude est l mesure simultnée des déformtions des deux ouhes de siliiumF our elD les files délges des plns ristllins des deux ouhes sont exploités X sur le déteteur PhD deux tâhes de di'rtion distintes pprissentD permettnt d9otenir deux rtes de déformtions indépendntes en un seul sn de l9éhntillonF v orréltion entre les déformtions et l morphologie de l9éhntillon pu être étlie grâe à des mesures de tomogrphieD otenues sur shITeF ne seonde expériene été menée sur un éhntillon plus simpleD destiné lui ussi u ollgeF sl s9git d9un wfer de siliiumD sur lequel une ouhe de uivre été déposéeF yn herhe ii à oserver les déformtions dns le uivreD à tempérture minte et à RHH • gF ve fiseu étnt monohromtiqueD une seule fmille de grins @orientée @RRRAA pu être oservéeF intre les deux tempérturesD les grins de uivre ont pu être suivisD et les mêmes grins ont don été imgés à tempérture minte et à RHH • F gette tehnique nous donne une informtion sur l tille des grinsD insi que sur l déformtion glole dns une telle ouhe de uivreD vnt et près reuitF hns es deux expérienesD de grndes zones de l9éhntillon ont pu être nlyséesD typiquement IHH x IHH µm 2 D ve un ps d9éhntillonnge de moins de SHH nmD e qui permet d9otenir une informtion loleF i le tritement des données reste ssez long @quelques heuresAD il est prole qu9il soit réduit pr l nouvelle interfe utilisteur développée sur shHID e qui permettr une utilistion routinière de ette ligneF

Concluding remarks and perspectives

sn this workD we explored the requirements of Qh integrtion devies in terms of hrteriztionD nd more spei(lly in terms of imgingF sn ftD it provides upstrem informtion out the smplesD nd llows for the understnding of the mehnisms hppening during the frition proessD nd therefore monitoring of the sid proess over timeF o do soD severl experimentl setups hve een investigted nd developedD in order to otin lrge enough (eld of viewD with optiml resolution villeF he fous ws set on the utomtion of ll those proeduresD for the tehniques to e used s routine hrteriztion mens for the industryF he (rst three hpters of this mnusript re dedited to the presenttion of the ontext of the studyF he (rst one desries Qh integrtion priniplesD toE gether with the spei( ojets of interest nd their hrteriztion needsF he seond hpter presents the physil priniples of eletron nd ion sed snning mirosopesF pinllyD hpter Q fouses on xEry sed hrteriztion methodsD presenting oth lortory nd synhrotron experimentl setupsF he next hpters rely on those sis to present the work done during this hh thesisF he min development performed during this hh thesis onerns xEry tomogrE phy nd is widely disussed in hpter SF he shIW emline of the ip @iuropen ynhrotron dition pilityA provides tomogrphy reonstrutions in little time @less thn one hourAD mking it wellEsuited for sttistil mesurementsD nd thereE fore of gret interest for industryF he experiments onduted on this emline showed the possiility to imge smples s lrge s P mm y tomogrphy nd sevE erl entimeters y lminogrphyD for (nl voxel size rehing HFTS µmF elthough smller voxel sizes @ISH nmA n e rehedD smll fetures suh s voids in opper pillrs nd opper pdsD whih re severl tens of nnometer lrgeD nnot e imged on this emlineF wuh higher resolution n e hieved on shITeF his newlyEuilt long emE line ims t nnoEtomogrphy with suESH nm resolutionD y exploiting the high oherene of the soureF sts llows for (eld of view of severl tens of mirometersF uh n experiment howeverD from the smple preprtion to the (nl reonstruted volumeD required too muh time nd humn intervention for n industril ppliE tionF e mjor result of this work is the redution of this overll experimentl time y ftor PD nd more spei(lly of the required humn intervention y ftor QF yur ontriution to the shITe work)ow mkes it possile to routinely perform sttistil mesures on smples suh s opper pillrs nd hyrid onding stksD with little humn intervention during the whole proessF eutomti postEproessing hs een shown possileD nd it should e pplile during the experiment itself in the futureD in order to otin redy to proess reonstruted volumes t the end of the emtimeF en insight on other possile hrteriztion methods o'ered y synhrotron setup ws provided in hpter TF yn the shHI emlineD lol strin mesurements ould e ondutedD thnks to fst snning tehnique llowing for quisitions on lrge res @IHH x IHH µm 2 A with reltively high sptil smplingD s the em n e foused down to PHH nmF e (rst study exploited the xEry penetrtion depth nd simultneously mesured the strin in two silion lyers of the sme stkD with no smple preprtionF e seond study ws onduted in situD on the opper used for wfer ondingF he otined strin only onerns fmily of grinsD ut still provides informtion out verge strin efore nd fter nnelingF he use of monohromti em suh s the one ville t shHI is prtiuE lrly wellEsuited for studies performed on monorystlsD nd one n imgine suh studies performed on multiElyer stksD with no need of smple preprtionF por polyrystlline mterils suh s opper hereD other methods suh s vue di'rE tion would seem more relevntD lthough the quired dt seem more tedious to postEproess nd interpretF por oth experimentsD the postEproessing of the dt requires severl hours of humn interventionD ut the user interfe ltely developed on the emline should pve the wy for more user friendly proedureF ynhrotron hrteriztion methodsD e they y morphology or di'rtion imgE ingD therefore o'er gret possiilities for Qh integrtion smplesD nd n e dpted for routine hrteriztion proeduresF et the ipD their glol performnes re likely to inrese in the next few yersD thnks to the seond phse of the ip upE grdeF his phseD whih follows the one during whih shITe nd shHI were uiltD represents n investment of ISH millions of euros etween PHIS nd PHPPF he min gol is to limit the emittne @espeilly the horizontl oneA of the eletron soureF his will llow for higher )ux nd more oherent emsD whih will improve oth imging nd di'rtion resultsD nd derese experimentl timesF xewly developed tehniquesD suh s ptyhogrphyD will ene(t from this improvementD nd their deE velopment ould led to industryEomptile ptyhoEtomogrphyD onept lredy shown relevnt for miroeletronis y roller et lF IPQF es mentioned in this rE tileD the high resolution hievle y ptyhogrphy @elow PH nmA ould even e omined with lminogrphyD in order to otin lrge (eld of view imgingD with no or little smple preprtionF uh djustments would mke synhrotron soures @nd mye future l onesA even more relevnt for routine sttistil hrteriztion of Qh integrtion deviesD nd more generlly of miroeletronis onesF ogether with those tehnil improvementsD shift in pereption hs een ourring in the lst few yersF he ip ims t o'ering more routine servies to industry tors in the futureD through diret ess emtime or for exmple through progrms suh s the s xnoeleD for more upstrem studies nd proofs of oneptF he work presented here lso ontriutes to new vision of synhrotronEsed hrterizE tion tehniquesD tht n e omptile with the industry e0ieny nd retivity requirementsF sn prllel to the synhrotron developmentD lortory sed equipment is lso improvingF es tleEtop synhrotrons pper on the mrketD one n hope tht results otined tody in synhrotron my e pprohed in the future in the lF elthough todyD lortory equipment still either lk (eld of view @in the se of iw or slie nd viewA or resolution @in the se of l tomogrphs or di'rtometersAD they still o'er the gret dvntge of eing ville t ll timeD with no or little time notieF por this resonD during this workD lortoryEsed Qh imging proedure hs een implemented inside singleEem psf @lsm poused son femAF he detils of this implementtionD together with the otined resultsD re presented in hpter RF st ws shown to o'er oth resolutions nd (elds of view omptile with Qh integrtionF sts utomtion ws mde possile nd it hs een shown to e stle for severl tens of hours long dt quisitionsD with sliing step down to SH nmF ome limitsD minly regrding the required quisition timeD re imposed y the mhine itselfF sn ddition to the redution of the dt quisition timeD mde y the use of dul em mirosope or y tuning the stge nd em prmeters of the single em oneD this tehnique ould e improved y the ddition of new feturesF sn ftD the tehnique ould esily ene(t from n dditionl ih detetor for exmpleD whih would provide Qh hemil informtion on lrge volumesD whih tody is hrd to otinF sn this workD we hd the opportunity to work on mny reent setupsD for the hrteriztion of Qh integrtion deviesD s they rise new hllengesF hen possiE leD omprison hve een mde etween the di'erent tehniquesD in order to point out their ssets nd drwksD from user nd industril point of viewF ome development hve een mde to mke those tehniques possile to use routinely for miroeletronis filure nlysisF wny foreseele developments re likely to strengthen this trendF

Conclusion générale et perspectives

hurnt le trvil présenté iiD ertins esoins de rtéristion d9une nouvelle tendne en miroEéletroniqueD ppelée intégrtion QhD ont été étudiésF lus prtiE ulièrementD nous nous sommes intéressés à son imgerieD qui fournit une informE tion mont sur l9éhntillonD pemettnt à l fois une meilleure ompréhension des ménismes guidnt son proédé de frition et un suivi dudit proédé dns le tempsF our répondre à es esoins de rtéristionD plusieurs dispositifs expériE mentux ont été testés et développésD (n d9otenir un lrge hmp de vueD tout en mximimisnt l résolution tteignleF ne ttention prtiulière été portée sur l9utomtistion des toutes es proéduresD pour que les tehniques onsidérées puissent être utilisées de mnière routinière dns l9industrieF ves trois premiers hpitres présentent le ontexte de l9étudeF ve premier présente les grnds prinipes de l9intégrtion QhD insi que ses esoins de rtéristion spéi(quesF n seond hpitre présente les mirosopes à lyge @életroniques et ioniquesA insi que leur utilistion u ours de e trvilF ve hpitre Q introduit les méthodes de rtéristion utilisnt les ryons D qu9ils soient issus d9une soure synhrotron ou de lortoireF ges hpitres posent les ses physiques sur lesquelles s9ppuient les hpitres suivntsF ves prinipux développements rélisés durnt e trvil de thèse onernent l toE mogrphie pr ryons D et sont disutés en détils u hpitre SF v ligne de lumière shIW de l9ip @iuropen ynhrotron dition pilityA est ple de fournir en peu de temps @moins d9une heureA des reonstrutions tomogrphiquesD e qui en fit une tehnique dptées ux mesures à grnde éhelleD et don à l9industrieF ves mesures rélisées sur ette ligne ont montré s pité à imger des éhnE tillons reltivement grnds pr tomogrphhie @P mmA et lminogrphie @quelques entimètresAD ve une tille de voxel de HFTS µmF fien que des tilles de voxels plus petites puissent être otenues @ISH nmA u détriment du hmp de vueD de petits défuts u sein des strutures étudiéesD omme des trous ux interfes entre pdsD ne peuvent être oservés sur ette ligneF ne résolution ien plus importnte peut être otenue sur l ligne de lumière shITeF sl s9git d9une ligne réenteD visnt une résolution de SH nm en tomogrphieF our elD elle exploite l forte ohérene du fiseu de ryons F ve hmp de vue qu9elle permet lors est de quelques dizines de miromètresF gependntD le proédé d9nlyse originl de ette ligne néessitit de nomreuses heuresD et surtout euoup d9intervention humineF e(n de rendre ette ligne omptile ve les exigenes de l9industrieD un nouveu proédé d9nlyse à été mis en pleF n résultt mjeur de e trvil est l rédution pr un fteur P du temps glol d9nlyseD ve une rédution pr un fteur Q du temps d9intervention humineF ge développement sur shITe permet de réliser des mesures sttistiques sur ette ligne sur des éhntillons tels que les piliers de uivre et des empilements de plusieurs niveux de uivre et de siliiumD de mnière utomtiséeF ve postEtritement été utomtiséD et il devrit être possile dns un futur prohe d9otenir les volumes reonstruits pendnt le temps de fiseu llouéF ne illustrtion d9utres rtéristions rélisles à l9ip est donnée u hpitre TF in e'etD sur l ligne shHID des mesures de déformtions ont pu être rélE iséesD en utilisnt une tehnique de sn rpide permettnt d9nlyser des zones lrges de l9éhntillon @typiquement IHH x IHH µm 2 AF v tille du fiseu étnt de PHH x SHH nm 2 D il été possile sur ette ligne d9otenir des mesures lolesF ne première étude présentée ii permisD en exploitnt l grnde profondeur de pénéE trtion des ryons dns le siliium et le uivreD d9nlyser simultnément deux ouhes de siliium d9un même empilementF ne seonde étude été rélisée in situD sur un éhntillon destiné à un ollge diret pleine plqueF ves déformtions dns le uivre ont pu être mesurées à tempérture minte insi qu9à RHH • gF ves résultts otenus ne onernent qu9une fmille de grinsD mis fournissent tout de même une informtion sur l déformtion moyenne vnt et près reuitF v ligne shHI présentnt un fiseu monohromtiqueD elle est prtiulièreE ment ien dptée à l9étude d9un mtériu monoristllin tel que le siliiumF sl est même possile d9imginer l mesure de déformtions dns le siliium telle que elle présentée iiD mis rélisée sur un empilement ontennt plus de deux niveux de siliiumD sns uune préprtion d9éhntillonF hns le s de mtériux polyE ristllins tels que le uivreD d9utre méthodes telles que l di'rtion vue semlent plus pertinentes que l di'rtion de frgg dérite iiF gependntD elle néessite un tritement de données et une interpréttion des résultts plus fstidieuxF ur shHID le postEtritement des données néessite ujourd9hui plusieurs heures d9intervention humineF gependntD l9interfe grphique réemment développée devrit permettre de rendre ette étpe plus simple pour l9utilisteurF ves méthodes de rtéristion essiles dns un synhrotronD qu9il s9gisse d9imgerie ou de mesure des ontrintesD ont mnifestement euoup à o'rir pour l rtéristion d9éhntillons d9intégrtion QhD d9utnt plus qu9elles peuvent être dptées pour une utilistion routinièreF e l9ipD les performnes de es tehE niques vont être menées à s9méliorer dns les nnées à venirD u vu de l deuxième phse du progrmme 4pgrde4F gette phse représente un investissement d9une huteur de ISH millions d9euros entre PIHS et PHPPD et pour ut mjeur de limiter l9emittne @surtout horizontleA de l soure primire d9életronsF ge hngement v se réperuter sur l9ensemle des hemins optiques X un )ux plus importnt ser essileD de même que des soures seondires plus ohérentesD mennt à une réE dution du temps d9nlyse pour une ugmenttion de l qulité des résulttsF hes tehniques en ours de développementD telles que l ptyhogrphieD onE nitront prolement un essor grâe à es méliortionsF in e'etD en limitnt le temps d9quisitionD des expérienes de ptyhoEtomogrphie pourront être rélisées dns des temps omptiles ve l9industrieF gette tehnique d9illeurs déjà été testée sur des éhntillons issus de l miroEéletronique pr roller et lF IPQF gomme mentionné dns et rtileD il pourrit même être possile de ominer l hute résolution de l ptyhogrphie @PH nmA ve l lminogrphieD (n d9otenir un lrge hmp de vue tout en limitnt l préprtion d9éhntillonsF outes es évoE lutions permettront ux soures synhrotron de s9imposer omme des outils possiles pour l rtéristion d9éhntillons issus de l9intégrtion QhD et plus générlement de l miroEéletroniqueF in prllèle de es développements tehniquesD un réent hngement de perepE tion des synhrotrons est à noterF in e'etD l9ip pr exemple herhe ujourd9hui à développer son o're pour les industrielsD que e soit pr l9ht de temps de fisE eu ou pr des projets tels que l9s xnoeleD orienté vers ds études mont et des tests de fisilitéF he son ôtéD le trvil présenté ii prtiipe à hnger l pereption du milieu de l miroéletronique onernnt les soures synhrotronD en les présentnt omme un outil de rtéristion qui peut être routinierD rétifD et e0eF r illeursD de nomreux développements ont ussi été rélisés sur les équipements de lortoireF hes soures de ryons dites 4synhrotron de lortoire4 sont ujourd9hui ommerilisésD et des résultts ujourd9hui seulement essiles en synhrotron le seront peutEêtre demin en lortoireF eujourd9hui ependntD les équipements de lortoire sont toujours limités soit pr l résolution @dns le s de tomogrphes de lortoireAD soit pr le hmp de vue @dns le s du wi ou du psfGiwAF sl ne fut ps oulier ependnt qu9ils o'rent l9vntge indénile d9être disponiles à tout momentD ontrirement ux expérienes en synhrotronF our ette risonD une tehnique d9imgerie Qh en lortoire églement été développée during ette thèseF sl s9git d9une proedure lie nd iew implementée dns un psf @lsm poused son femAF ves détils de e développementD insi que les résultts otenusD sont présentés u hpitre RF ves hmps de vue et l résolution teignles sur un tel dispositif sont omptiles ve l rtéristion pour l9intégrtion QhF v9quisition des données été rendue utomtique et stle pendnt plusieurs dizines d9heuresD ve un ps d9éhntillonge dns l diretion de déoupe pouvnt ller jusqu9à SH nmF ves limites de ette tehnique ont été identi(ées et disutéesF illes onernent surtout le temps d9quisitionD qui pourrit ien sûr être réduit pr l9utilistion d9un mirosope équipé de deux olonnesD une pour l oupe et l9utre pour l9imgerieF eu delà de es onsidértionsD il peut être intéressnt de noter que l9jout de nouvelles fontionnlités à ette méthode pourrit être d9un grnd intérêtF in e'etD l9jout d9un déteteur ih pr exemple pourrit permettre d9otenir une informtion himique tridimensionnelle sur une lrge région d9intérêtD e qui est ujourd9hui di0ileF ge trvil de thèse été l9osion de réliser des expérienes sur on nomre de dispositifs expérimentux réentsD et de les ppliquer à des éhntillons en plein développementF vorsque el été possileD des omprisons et orréltions ont été rélisées entre es di'érentes tehniquesD (n de mettre en lumière leurs vntges et inonvénientsD d9un point de vue industrielF ges tehniques ont été dptées pour le milieu de l miroéletroniqueD (n de fournir rpidement et filement des informE tions sttistiquesD rpides à triterF he nomreuses évolutions à venirD ertines évoE quées iiD sont à même de ontinuer dns ette diretion et d9instller le synhrotron en tnt que tehnique de rtéristion prfitement dptée à l9industrieF pges U!IQD PHHVF @gited on pges PR nd PWFA QR eF rF F n eenD gF F rgenD tF iF frthD nd F uruitF edued rightE ness of the ryG shottky eletron emitterF Journal of Vacuum Science and Technology B: Microelectronics and Nanometer StructuresD IW@TAXPHQV!PHRRD PHHIF @gited on pges PT nd PVFA QS wF fronsgeestF Physics of Schottky electron sources: Theory and optimum operationD pges I!PSTF hysis of hottky iletron ouresX heory nd yptimum ypertionF n tnfordD PHIRF @gited on pge PVFA QT rF uwnoF i'etive work funtions for ioni nd eletroni emissions from monoE nd polyrystlline surfesF Progress in Surface ScienceD VQ@IEPAXI! ITSD PHHVF @gited on pge PVFA QU hF F uggleD tF F viD nd vF F wnsonF oint thodes for use in virtul soure eletron optisF Journal of microscopyD IRH@QAXPWQ!QHID IWVSF @gited on pge PVFA QV wF tF prnsenD wF rF pF yverwijkD nd F uruitF frightness mesurements of ryG hottky eletron emitter in trnsmission eletron mirosopeF Applied Surface ScienceD IRT@IAXQSU!QTPD IWWWF @gited on pge PVFA QW vF F wnsonD qF eF hwindD F wF uelloggD nd uF viuF gomputer modeling of the shottky eletron soureF RV F rrn£í°nd vF rldíkF pst nd preise Qh tomogrphy of y using e plsm psfF sn Conference Proceedings from the International Symposium for Testing and Failure AnalysisD pges PU!QPD PHIQF @gited on pges QR nd RHFA TI eF nkelD tF gnerD nd F oeltF eril setioning methods for Qh investiE gtions in mterils sieneF MicronD TPXTT!UVD PHIRF @gited on pge QUFA TP eF uirunndhmD sF vujnEegldoD F llhneniD nd xF ghwlF hree dimensionl hrteriztion of tin rystllogrphy nd Sn 6 Sn 5 interE metllis in solder joints y multisle tomogrphyF JOMD TV@IIAXPVUW!PVVUD PHITF @gited on pge QUFA TQ wF sto nd tF utoF Qh nlysis of opper )ipEhip interonnetion using psfEiw slie nd viewF Electronic Device Failure AnalysisD IV@IAXIR!PHD PHITF @gited on pge QUFA TR wF hF hiD vF rolzerD fF tF snksonD iF vF rinipeD nd F wunroeF hreeE dimensionl mirostruturl hrteriztion using foused ion em tomogE rphyF MRS BulletinD QP@SAXRHV!RITD PHHUF @gited on pge QWFA TS wF gntoni nd vF rolzerF edvnes in Qh foused ion em tomogrphyF MRS BulletinD QW@RAXQSR!QTHD PHIRF @gited on pge QWFA TT uF uimD xF qreenD nd F qri0thsF poused ion em milling nd imgE ingX en dvned method to detet (ne inlusions in st luminium lloysF Materials Science ForumD UTSXISH!ISRD PHIQF @gited on pge QWFA TU F wiymurD F ekiguhiD tF ghenD tF F viD uF tneD uF uumgiD nd eF ygurF poused ion em imging of defets in multirystlline i for photovolti pplitionF Acta Physica Polonica AD IPS@RAXWWI!WWQD PHIRF @gited on pge QWFA TV F rrn£í°D vF rldíkD nd wF drzilF pst Qh tomogrphy t pkge level y using e plsm foused ion emF sn Proceedings of the International Symposium on the Physical and Failure Analysis of Integrated Circuits, IPFAD pges IIP!IISD PHIQF @gited on pges RH nd VSFA TW vF eF qinnuzziD tF vF hrownD F F frownD F fF srwinD nd pF eF tevieF poused ion em milling nd miromnipultion liftEout for site spei( rossE setion iw speimen preprtionF sn Materials Research Society Symposium -ProceedingsD volume RVHD pges IW!PUD IWWUF @gited on pge RHFA UH vFeF qinnuzziD fFF uemshllD FwF hwrzD tFuF vomnessD fFsF renitzerD nd pFeF tevieF FIB lift-out sample preparation techniques -in situ and ex situ methodsD hpter IHF pringerD PHHSF @gited on pge RHFA UI hF omus nd rF F xgF sn situ liftEout dedited tehniques using (Esem system for tem speimen preprtionF MicronD RR@IAXIIS!IIWD PHIQF @gited on pge RHFA UP qF hivitiniD yF tenzelD eF qhdirzdehD F qurnerD F ussoD gF F gsriD eF vF fssiD eF etrozzD pF hi ponzoD F hmidtD nd gF hutiF xnosle nlysis of hierrhil hyrid solr ell in QhF Advanced Functional Mate-rialsD PR@PHAXQHRQ!QHSHD PHIRF @gited on pge RHFA UQ tF whmidD F hmpersD rF ersoonD eF eF rymnD F fumeisterD nd tF wF litzkoF e foused ion em milling nd liftEout pproh for siteEspei( preprtion of frozenEhydrted lmells from multiellulr orgnismsF Journal of structural biologyD IWP@PAXPTP!PTWD PHISF @gited on pge RHFA UR F tF ros nd hF tF vrsonF wodern fousedEionEemEsed siteEspei( speimen preprtion for tom proe tomogrphyF pges SVQ!SVSD PHITF @gited on pges RH nd RPFA UW tF elsExielsen nd hF wworrowF Elements of Modern X-ray Physics: Second EditionF ileyD PHIIF @gited on pges RTD RUD RV nd SQFA VH vF eF qomes eriniD F fleuetD tF pilevihD F rkerD fF fuijsseD nd vF pF zF uwkmnF hevelopments on iwEsed Ery tomogrphy systemX tiE liztion sheme nd performne evlutionF Review of Scientic InstrumentsD VV@TAXHTQUHTD PHIUF @gited on pge RWFA VI ten hygi nd tosé fegrivF yonnement synhrotron et ppliE tionsF Techniques de l'ingénieur CND: méthodes globales et volumiquesD se doumentireX sfSVShyF@refF rtileX pPUHHAD PHIIF freF @gited on pges SP nd SQFA VP iFfF odgorskF Radiation Oncology PhysicsF sxixesyxev eywsg ixiq eqixgD iennD PHHSF @gited on pge SSFA VQ ipF UPBL4 Nano-Imaging and Nano-Analysis -Technical Design ReportD PHIHF @gited on pge SWFA VR F uirkptrik nd eFF fezF pormtion of optil imges y xErysF Journal of the Optical Society of AmericaD QV@WAXUTT!UURD IWRVF ited fy UVWF @gited on pge SWFA VS gF worweD F frrettD F gloetensD fF vntelmeD tEghF e'enD nd eF ivoF qrded multilyers for (gured kirkptrikEez mirrors on the new ip end sttion shITeF sn Proceedings of SPIE -The International Society for Optical EngineeringD volume WSVVD PHISF ited fy QF @gited on pge SWFA VT tulio gesr h ilvD elexndr urenuD ng ngD ylvin fohiD ghrisE tin worweD ymond frrettD nd eter gloetensF i0ient onentrtion of highEenergy xErys for di'rtionElimited imging resolutionF OpticaD R@SAXRWP! RWSD wy PHIUF @gited on pge SWFA VU qF eF ghhineD wF ihrdD F eF romsEegojoD F xF rnEglisteD hF grE oneD F vF F tquesD F qrifoneD F foesekeD tF utzerD sF gostinD rF hjE zouliD F hroederD nd F F hülliF smging of strin nd lttie orienttion y quik snning xEry mirosopy omined with threeEdimensionl reiproE l spe mppingF Journal of Applied CrystallographyD RU@PAXUTP!UTWD PHIRF @gited on pges TID VHD VI nd VPFA VV gF onhutD tFwF iglD tF glémentD iF pillonD eF romsD nd F etitE demngeF wxipixD fst redout photonEounting xEry re detetor for synhrotron pplitionsF Journal of InstrumentationD T@IAD PHIIF ited fy UVF @gited on pges TI nd UVFA VW oger tF hejus nd wnuel nhez del ioF yX e grphil user interE fe for spetrl lultions nd xEry optis utilitiesF Review of Scientic InstrumentsD TU@WAXQQST!QQSTD IWWTF @gited on pges TT nd USFA WH F fonse nd wF rrtF en xEry interferometerF Applied Physics LettersD T@VAXISS!ISTD IWTSF ited fy UQVF @gited on pge TRFA WI hF ghpmnD F homlinsonD FiF tohnstonD hF shurnD iF isnoD xF qmürD F hongD F wenkD pF erfelliD nd hF yersF hi'rtion enhned xEry imgingF Physics in Medicine and BiologyD RP@IIAXPHIS!PHPSD IWWUF ited fy VRTF @gited on pge TRFA WP eF womoseF hseEsensitive imging nd phse tomogrphy using xEry inE terferometersF Optics ExpressD II@IWAXPQHQ!PQIRD PHHQF ited fy IVSF @gited on pge TRFA WQ eF ylivo nd FhF pellerF e novel xEry imging tehnique sed on oded pertures mking phse ontrst imging fesile with onventionl souresF sn IEEE Nuclear Science Symposium Conference RecordD pges IRRU!IRSHD PHHVF ited fy HF @gited on pge TRFA WR tFF qoodmnF Introduction to Fourier opticsF xew orkX oerts nd gompny ulishersD PHHSF @gited on pge TTFA WS tFF quigyF pourier trnsform nlysis of fresnel di'rtion ptterns nd inE line hologrmsF Optik (Jena)D RW@IAXIPI!IPSD IWUUF ited fy IPRF @gited on pge TTFA WT enn furvllD lf vundströmD er eF gF kmnD hniel rF vrssonD nd rns wF rertzF hse retrievl in xEry phseEontrst imging suitle for tomogrphyF Opt. ExpressD IW@IIAXIHQSW!IHQUTD wy PHIIF @gited on pge TUFA WU vF eerD wF vngerD F vellD eF uggiuD nd pF eyrinF untittive evlution of regulrized phse retrievl lgorithms on one s'olds seeded with one ellsF Physics in Medicine and BiologyD TI@WAXxPIS!xPQID PHITF @gited on pge TUFA WV wihel eed egueF srrdine momentsX heir propgtion nd use for unique retrievl of phseF J OPT SOC AMD UP@x WAXIIWW!IPHWD IWVPF ited fy IRHF @gited on pge TUFA WW eter gloetensF Contribution to Phase Contrast Imaging, Reconstruction ans Tomography with Hard Synchrotron RadiationF hh thesisD rije niversiteit frusselD IWWWF @gited on pge TUFA IHH F gloetensD F vudwigD tF fruhelD hF n hykD tF n vnduytD tF F quigyD nd wF hlenkerF rolotomogrphyX untittive phse tomogrphy with mirometer resolution using hrd synhrotron rdition x rysF Applied Physics LettersD US@IWAXPWIP!PWIRD IWWWF @gited on pge TUFA IHI pF eyrinD F gloetensD w lomeEteyronD t fruhelD nd F pnneF eonE strution Qh en tomogrphie pr ryonnement synhrotron oherentF Seizième colloque GRETSID IWWUF @gited on pge UHFA IHP rF uD F uD F wouD nd qF ngF eent progress in lol reonstrutionF sn Proceedings of SPIE -The International Society for Optical EngineeringD volume UVHRD PHIHF ited fy IF @gited on pge UIFA IHQ eF gF uk nd fF eF oertsF eonstrution from projetionsX pplitions in omputerized tomogrphyF Handbook of pattern recognition and image pro-cessingD pges TRW!TWQD IWVTF @gited on pge UIFA IHR teven F mithF the scientist and engineer's guide the digital signal process-ingF gliforni ehnil uFD IWWUD IWWUF @gited on pge UPFA IHS wF feisterD hF uolditzD nd FeF ulenderF stertive reonstrution methods in xEry gF Physica MedicaD PV@PAXWR!IHVD PHIPF ited fy PPPF @gited on pges UQ nd URFA IHT evinsh uk nd wlolm lneyF Principles of Computerized Tomographic ImagingF oiety for sndustril nd epplied wthemtisD IWVVF @gited on pge URFA IHU F n erleD F tF lenstijnD tF he feenhouwerD F eltntzisD F flsD uF tF ftenurgD nd tF ijersF he ee tooloxX e pltform for dvned lgorithm development in eletron tomogrphyF UltramicroscopyD ISUXQS!RUD PHISF @gited on pges UR nd IPQFA IHV helei ghenD frt qorisD polkert fleihrodtD rmed reidri wezerjiD r flsD uees toost ftenurgD qijsertus de ithD nd reiner priedrihF he properE ties of sD wD nd he for Qh imging of tuulr domins in nnoomE posite thinE(lms nd setionsF UltramicroscopyD IRUXIQU ! IRVD PHIRF @gited on pge URFA IHW pisF ifstF @gited on pge VTFA IIH wF lzerD F hieleD F engerleD nd F hmidtF yn the importne of (Esem spei( segmenttion lgorithms for porous mediF Materials Charac-terizationD WSXQT!RQD PHIRF @gited on pge IHTFA III F rillD uF hlditzD hF teulinD wF pesselD nd gF ieserF worphologil segmenttion of (Esem dt of highly porous mediF Journal of MicroscopyD PSH@PAXUU!VUD PHIQF @gited on pge IHTFA IIP riroshi swiD xoki hikzonoD oshiki wtsuiD risnori eshimD wsshi uishimotoD yo uishidD hisuke ryshiD utsuhis wtsuzkiD hisuke unnoD wotohiro itoD riroki wuroymD uoihi iguhiD xouhide usgiD nd rideo oshidF unti(tion of sof node mirostruture sed on dul em (Esem tehniqueF Journal of Power SourcesD IWS@RAXWSS ! WTID PHIHF @gited on pge IHTFA IIQ eF przkiewizD iF gpriD F gloetensD tF h ilvD eF touveD F vhostisD pF vorutD F wourierD nd F fleuetF righ resolution xEry omputed tomogE rphyX wht synhrotron soures n ring to Qhi devies filure nlysisF Conference Proceedings from the International Symposium for Testing and Failure Analysis 2016D PHITF @gited on pge IIPFA IIR x gpitD q h gostD qeorgiouD q rurdD g wrtinD q wounieD xeyronD nd y ihrdF e th sheduler with high level omponentsF sn 2005 IEEE INTERNATIONAL SYMPOSIUM ON CLUSTER COMPUTING AND THE GRID, VOLS 1 AND 2D pges UUT!UVQD PHHSF @gited on pge IIQFA IIS F hudinD F erziD F vhuissierD tF myoD wF heelD xF rri fuD hFqF iskinD nd vF lvoF rtileEindued morphologil modi(tion of el lloy equixed dendrites reveled y suEseond in situ mirotomogrphyF Acta MaterialiaD IPS@upplement gAXQHQ ! QIHD PHIUF @gited on pge IIRFA IIT FEyF eutrnF eméliortion des lgorithmes de reonstrution d9imges d9ojets QdD fournis pr le synhrotronF @gited on pge IPQFA IIU ng houD eln gonrd fovikD rmid him heikhD nd iero imonelliF smge qulity ssessmentX from error visiility to struturl similrityF IEEE transactions on image processing: a publication of the IEEE Signal Processing SocietyD IQXTHH!TIPD epril PHHRF @gited on pge IPQFA IIV F woreuD hF fouhuD F flnD eFEvFvF ferrigoD eF touveD F renrionD gF fessetD hF evolD F vhostisD pF quyderD iF helo'reD F wermozD nd tF ruvostF wss trnsportEindued filure of hyrid ondingEsed integrE tion for dvned imge sensor pplitionsF sn Proceedings -Electronic Components and Technology ConferenceD volume PHITEeugustD pges IWRH!IWRSD PHITF ited fy IF @gited on pge IQHFA IIW F qF ivnsD qF ghhineD F qrifoneD F vF F tquesD tF F plenkD nd F F hülliF gompt ultrhigh vuum smple environments for xEry nnoem di'rtion nd imgingF Review of Scientic InstrumentsD VR@IIAD PHIQF @gited on pge IRVFA IPH fF inneD F isousD gF urussD wF F ihrdD F vtD qF ghhineD tF F wihD F hülliD F pioriD eF pryD nd yF homsF emperture depenE deny of the strin distriution indued y tsvs in silionX e omprtive study etween miroElue nd monohromti nnoEdi'rtionF Microelectronic EngineeringD ISTXSW!TRD PHITF @gited on pge ISIFA IPI hF pF nhezD F eohD wF vF hF eleguelD tF F wihD yF ohD F wourierD F qergudD nd F fleuetF snEsitu xEry µlue di'rtion study of opper throughEsilion visF Microelectronics ReliabilityD STXUV!VRD PHITF @gited on pge ISIFA IPP eFF fudimnD rFEeFEF hinD fFEtF uimD FErF rwngD rFEF onD wFEF uhD FErF ghungD uFEF fyunD xF murD wF uunzD nd FEgF tooF wesureE ment of stresses in n nd i round throughEsilion vi y synhrotron xEry mirodi'rtion for QEdimensionl integrted iruitsF Microelectronics Reli-abilityD SP@QAXSQH ! SQQD PHIPF peil setion on snterntionl eminr on ower emiondutors PHIHF @gited on pge ISIFA IPQ wirko rollerD wnuel quizrEiirosD isther rF F siD oerto hinpoliD iliseth wullerD yliver funkD torg eD nd qriel eeppliF righE resolution nonEdestrutive threeEdimensionl imging of integrted iruitsF NATURED SRQ@UTRSAXRHPCD we IT PHIUF @gited on pges ISR nd ISWFA

2

  Electron and Ion based microscopes 23 PFI qenerl overview nd relevnt vlues F

  pigure IFRX ro(le illustrtion of A diret ondingF Image source: [15]Y A hyrid ondingF Image source: [2]F A ro(le view of the disyhin strutureD otined with xEry tomogrphyF pigure IFSX impli(ed hyrid onding proessF Image source: [2]

  of x-ray physics . . . . . . . . . . . . . . . . . . . . 46 3.1.1 Obtaining an x-ray beam . . . . . . . . . . . . . . . . . . . . 46 3.1.2 X-ray/matter interactions . . . . . . . . . . . . . . . . . . . . 53 3.2 Experimental setups . . . . . . . . . . . . . . . . . . . . . . . . 57 3.2.1 ID16A: a nano-tomography beamline . . . . . . . . . . . . . . 58 3.2.2 ID19: a versatile tool for coherent imaging and diraction . . 60 3.2.3 ID01: Local strain measurement . . . . . . . . . . . . . . . . 61 3.3 X-ray transmission 3D imaging . . . . . . . . . . . . . . . . . 62 3.3.1 2D image formation . . . . . . . . . . . . . . . . . . . . . . . 62 3.3.2 Obtaining a 3D reconstruction . . . . . . . . . . . . . . . . . 70 3.3.3 Sample Preparation . . . . . . . . . . . . . . . . . . . . . . . 74 3.4 Strain measures by Bragg diraction . . . . . . . . . . . . . . 76 3.4.1 Monochromatic Bragg Diraction . . . . . . . . . . . . . . . . 76 3.4.2 The ID01 workow . . . . . . . . . . . . . . . . . . . . . . . . 78 3.4.3 Sample Preparation . . . . . . . . . . . . . . . . . . . . . . . 82

  n(x, y, z) = 1 -δ(x, y, z) + iβ(x, y, z) @QFIIA pigure QFIPX xottions regrding the spe oordintes used in this setionF he xEry em propgtes long diretion zD nd the projetion plnes re @xDyAF he distne etween the end of the smple nd the detetor is noted hF 3.3.1.1 Absorption contrast imaging

  Saving of beam parameters rmeters suh s the fousD the rightness nd ontrstD n e sved during the settingsD nd used lter in the experimentF Imaging he imge quisition prmetersD suh s the (eld of view nd the E quisition timeD n e tunedF Change of current he hnge of urrent n e triggered y ipstF Milling willing n e performed with ll shpesD urrentsD nd generl settings ville on the psfD nd the ptterns n e svedF Matter deposition sfsh is villeD the insertion of gs eing lso triggered y the ipst softwreF Pattern recognition he ipst softwre is le to ompre referene imge preE viously sved with newly quired oneF st then ligns the two imgesD nd moves @y em shift or stge movementD depending on the user hoieA toE wrds the position t whih the originl imge ws tkenF 4.1.2 Data acquisition workow 4.1.2.1 Main issues and answers

  ID16A workow . . . . . . . . . . . . . . . . . . . . . 112 5.2 New sample preparation scheme . . . . . . . . . . . . . . . . 114 5.2.1 New sample supports . . . . . . . . . . . . . . . . . . . . . . 115 5.2.2 Making the most of the sample preparation and installation . 115 5.3 Reduction of the number of projections . . . . . . . . . . . . 123 5.4 Automation of the post-processing . . . . . . . . . . . . . . . 126 5.5 Time gain and discussion . . . . . . . . . . . . . . . . . . . . . 128 5.6 Application to 3D integration imaging . . . . . . . . . . . . . 130 5.6.1 Imaging of a large number of post-electromigration samples . 130 5.6.2 Morphology study on copper pillars . . . . . . . . . . . . . . 133 5.6.3 Towards a larger eld of view . . . . . . . . . . . . . . . . . . 137 5.7 Conclusion . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 139

  Contents 6.1 Hybrid bonding stack strain measure in silicon . . . . . . . 144 6.1.1 Simultaneous observation of two silicon layers . . . . . . . . . 144 6.1.2 Strain maps and morphology correlation . . . . . . . . . . . . 146 6.2 Direct bonding in-situ strain measure in copper . . . . . . . 148 6.3 Conclusion . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 151

  two types of imging experimentl setupsX the trnsmission imgingD where the smple is pled in the propgting emD nd snning imgingD where the smple is pled inside the fous of the emF he former will e illustrted y )uoresene imgingD while the ltter will led to sorption nd phse ontrst imgingF he expression of the omplex refrtion index is reminded in eqF QFUD s it leds oth to sorption nd phse ontrst imgingF pigure QFIP provides the nottions used in this setion regrding the spe oordintesF his (gure n e seen s the followEup of (g QFIH pituring shITe9s optil pthF es those nottions re ommon to Ph nd Qh imgingD n ngle θ is lredy present in this (gure nd in the next equtionsD s they foresee smple rottionF

	shITe shIW rdi	Absorption contrast Phase contrast Absorption contrast tomography tomography laminography ossile IU keY QQFT ke gone em xot possile IW keY PTFS ke rllel em ossile PTFS ke rllel em UH k gone em xot implemented xot implemented	Fluorescence tomography QQFT ke pous size `QH nm xot possile xot possile
	le QFPX ixperimentl Qh trnsmission imging tehniques nd experimentl seE tups used in this workF
	3.3.1 2D image formation
	rere we present

  Automation of the data acquisition . . . . . . . . . . . . . . . 86

	Chapter 4
	Development of 3D imaging in a
	single column PFIB
	Contents
	4.1

4.1.1 The iFast software . . . . . . . . . . . . . . . . . . . . . . . . 86 4.1.2 Data acquisition workow . . . . . . . . . . . . . . . . . . . . 88 4.2 Data post-processing . . . . . . . . . . . . . . . . . . . . . . . 94 4.2.1 Calculation of the actual slicing step . . . . . . . . . . . . . . 96 4.2.2 Slices registration . . . . . . . . . . . . . . . . . . . . . . . . . 96 4.2.3 Volume re-sampling . . . . . . . . . . . . . . . . . . . . . . . 98 4.3 Results . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 99 4.4 Limits of the technique and possible improvements . . . . . 104 4.5 Conclusion . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 107

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ITSD PHHSF ited fy URF @gited on pge PHFA PW F hurhD F owlndD F frdleyD nd F ithersF gomprison nd omiE ntion of imging tehniques for three dimensionl nlysis of eletril treesF IEEE Transactions on Dielectrics and Electrical InsulationD PP@PAXUHW!UIWD PHISF @gited on pge PIFA QH F vF furnettD F uelleyD fF inirskiD vF gontrersD wF hlyD eF qholiniD wF qF furkeD nd F tF ithersF vrge volume seril setion tomogrphy y xe plsmpsf dul em mirosopyF UltramicroscopyD ITIXIIW!IPWD PHITF @gited on pges PID QRD RH nd VSFA QI tF qoldsteinD hF xewuryD hF toyD gF vymnD F ihlinD iF vifshinD vF wyerD nd tF wihelF Scanning Electron Microscopy and X-ray Microanalysis, Third editionF vuwer edemi Glenum ulishersD xew orkD PHHQF @gited on pges PR nd QIFA QP vFeF qinnuzziD fFF uemshllD FwF hwrzD tFuF vomnessD fFsF renitzerD nd pFeF tevieF Introduction to Focused Ion Beams -Instrumentation, Theory, Techniques and PracticeF pringerD PHHSF @gited on pges PRD QQ nd QTFA QQ F eshD xF mithD xF wrtinD nd hF uinionF righ urrent foused ion em instrument for destrutive physil nlysis pplitionsF sn Conference Proceedings from the International Symposium for Testing and Failure AnalysisD

  Journal of Vacuum Science and Technology B: Nanotechnology and MicroelectronicsD QH@TAD PHIPF @gited on pge PVFA RH xF F mithD F F kozylsD F wF uelloggD hF iF uinionD F F eshD yF utherlndD eF eneslndD nd F F foswellF righ rightness indutively oupled plsm soure for high urrent foused ion em pplitionsF Journal of Vacuum Science and Technology B: Microelectronics and Nanometer StructuresD PR@TAXPWHP!PWHTD PHHTF @gited on pge PWFA RI F mith nd tFEwF llsF Ion erosion in surface analysisD hpter PD pges PH!STF ilsevier iene vtdD IWWHF @gited on pge PWFA RP tF uellerD xF mithD F foswellD vF ipioniD gF ghrlesD nd yF utherlndF wgnetilly enhnedD indutively oupled plsm soure for foused ion em systemF @gited on pge PWFA RQ F igmundF sputtering proessesX ollision sdes nd spikesF sn xFrF yvuD tFgF vvD F risvexhD nd gFF rsiD editorsD Inelastic Ion Surface CollisionsD pges IPI ! ISPF edemi ressD IWUUF @gited on pge QQFA RR unov nd wunroeF psfEindued dmge in silionF JOURNAL OF MICROSCOPY-OXFORDD PIR@QAXPIQ!PPID tx PHHRF weeting on edvnes in poused son fem wirosopy @xnopsf PHHQAD gorpus ghristi gollegeD gmridgeD ixqvexhD e HRD PHHQF @gited on pges QQ nd QRFA RS F rrn£í°D wF ikulD yon § tFEFD nd F qounetF row to hieve rtiftE free psf milling on polyimide pkgesF sn Proceeding of ISTFA 2016D PHITF @gited on pge QQFA RT F woreuD hF fouhuD nd qF eudoitF pst nd esy smple preprtion with redued urtining rtifts using EpsfF sn 2014 IEEE 21ST INTERNA-TIONAL SYMPOSIUM ON THE PHYSICAL AND FAILURE ANALYSIS OF INTEGRATED CIRCUITS (IPFA)D siii snterntionl ymposium on the hysil nd pilure enlysis of sntegrted giruitsD pges PQI!PQSF siiiY pis go eY siii ingpore elil gw ih ghpterY ilet hevies oY elil oD PHIRF PIst siii snterntionl ymposium on the hysil nd pilure enlysis of sntegrted giruits @speAD sxqeyiD tx QHEtv HRD PHIRF @gited on pge QQFA RU vF uwkmnD qF prnzD wF wF F kloD eF ulumppD nd F mmF ghrterE iztion nd filure nlysis of Qh integrted systems using novel plsmEpsf systemF sn AIP Conference ProceedingsD volume IQWSD pges PTW!PUQD PHIIF @gited on pge QRFA

  Microscopy and Micro-analysisD pges I!ITD PHIUF ertile in ressF @gited on pge RHFA US F dlkrD tF F ileyD F viD qF F ngD nd vF tF vuhonF viftEout proedures for tom proe tomogrphy trgeting nnosle fetures in oreE shell nnowire heterostruturesF Physica Status Solidi (C) Snrrent Topics in Solid State PhysicsD II@QERAXTST!TTID PHIRF @gited on pge RHFA UT F fleuetD qF eudoitD tF F frnesD tF fertheuD F hinD rF hnssD tF F pE riD fF plorinD F qergudD eF qrenierD qF rerfehlnerD iF vyD tF vureninD F errD nd tF illnovF pei(tions for hrd ondensed mtter speE imens for threeEdimensionl highEresolution tomogrphiesF Microscopy and MicroanalysisD IW@QAXUPT!UQWD PHIQF @gited on pge RHFA UU wF ruertD tF vureninD F gloetensD tF gF d ilvD pF vefevreEtoudD F fleuetD eF xkjoD nd iF ieertF ole of mirostruture on eletrode opE erting mehnisms for mixed ioni eletroni ondutorsX prom synhrotronE sed Qh reonstrution to eletrohemil modelingF Solid State IonicsD PWRXWH!IHUD PHITF @gited on pge RHFA UV qF eudoitD F fleuetD qF helpyD nd vF uwkmnF lsmE( smple prepE rtion for xEry tomogrphy of QhEsg interonnetsF sn Conference Proceedings from the 42nd International Symposium for Testing and Failure AnalysisD

Institut de Recherche Technologique

PlateForme de NanoCaractérisation, the nano-characterization platform at CEA

Chapter 2. Electron and Ion based microscopes

Chapter 4. Development of 3D imaging in a single column PFIB

The changes brought to the ID16A workow described in this chapter have been the object of two contributions to the ISTFA conference, in

and

[113].

This work has been made in the frame of an internship realized by Pierre-Olivier Autran [116].

A more detailed version of this study is to be published in 2018.

A more complete study on the imaging of copper pillars, using both tomography and Slice and View techniques, has been submitted to Ultramicroscopy in 2017.

This chapter is a slightly modied version of a paper to be submitted to Microelectronics Reliability under the title "In-situ local strain measurement and morphology correlation in hybrid bonding stacks using nano-focused x-ray and electron microscopy."

RW xs utoF eduing foused ion em dmge to trnsmission eletron miE rosopy smplesF JOURNAL OF ELECTRON MICROSCOPYD SQ@SAXRSI! RSVD PHHRF @gited on pge QRFA SH qF poldiD F feuerD wF ommelD F nevD eF tF fuerD nd rF ysselF ixperimentl oservtion of psf indued lterl dmge on silion smplesF Microelectronic EngineeringD VT@RETAXSRV!SSID PHHWF @gited on pge QRFA SI wF ommelD qF poldiD F nevD F feuerD fF emonD tF tmrekD F eE tersenD eF tF fuerD nd vF preyF gomprehensive study of foused ion em indued lterl dmge in silion y snning proe mirosopy tehniquesF Journal of Vacuum Science and Technology B: Nanotechnology and Microelec-tronicsD PV@QAXSWS!THUD PHIHF @gited on pge QRFA SP rF eilerF eondry eletron emission in the snning eletron mirosopeF Journal of Applied PhysicsD SR@IIAXI!IVD IWVQF @gited on pge QTFA SQ tF yrlo'D vF wnsonD nd wF tlutF High Resolution Focused Ion Beams:

FIB and its ApplicationsF pringer D (rst editionD PHHQF @gited on pge QTFA SR tefn e'erer nd xhidExor ilhmiF heory nd pplition of eletron hnnelling ontrst imging under ontrolled di'rtion onditionsF Acta MaterialiaD USXPH ! SHD PHIRF @gited on pge QTFA SS vFeF qinnuzzi nd tFF wihelF son hnneling vsF eletron hnneling imE ge ontrstF Microscopy and MicroanalysisD IVXTWR!TWSD U PHIPF @gited on pge QTFA ST gF vngloisD F houillrdD rF unD xF F flnhrdD eF hesmpsEwndineD fF n de woortèleD gF igottiD nd F ipiierF grystl orienttion mpping vi ion hnnelingX en lterntive to ifhF UltramicroscopyD ISUXTS!UPD PHISF @gited on pge QTFA SU xF fssimD uF ottD nd vF eF qinnuzziF eent dvnes in foused ion em tehnology nd pplitionsF MRS BulletinD QW@RAXQIU!QPSD PHIRF @gited on pge QUFA SV F henk nd rF rorstmnnF eril lokEfe snning eletron mirosopy to reonstrut threeEdimensionl tissue nnostrutureF PLoS BiologyD P@IIAD PHHRF @gited on pge QUFA SW vF rolzerD pF sndutnyiD hF qsserD fF wünhD nd wF egmnnF hreeE dimensionl nlysis of porous fiy 3 ermis using psf nnotomogrphyF Journal of microscopyD PIT@IAXVR!WSD PHHRF @gited on pges QU nd QWFA TH wF eF wngnD F hF vurenD nd qF tF hi)etF hreeEdimensionl reonE strution of widmnsttten pltes in peEIPFQwnE HFVgF Journal of microscopyD IVV@IAXQT!RID IWWUF @gited on pge QUFA

Scientic contributions

Communications in conferences A. Fraczkiewicz, E. Capria, P. Cloetens, J. Da Silva, P. Gondcharton, A. Jouve, F. Lorut, T. Mourier, P. Bleuet, Tomographie par rayons X appliquée à l'intégration 3D: vers une information statistique sub-50 nm poster, RX et matière 2015, Grenoble, France A.Fraczkiewicz, E.Capria, G.Chahine, P.Cloetens, J.Da-Silva, A.Jouve, F.Lorut, S.Lhostis, M-I. Richard, P.Bleuet, 3D morphological and structural nanocharacterization for microelectronics: the potential of recent, long synchrotron beamlines, poster, XRM 2016, Oxford, UK A.Fraczkiewicz, E.Capria, P.Cloetens, J.Da Silva, A.Jouve, S.Lhostis, F.Lorut, T.Mourier, P.Bleuet, High resolution x-ray computed tomography: what synchrotron sources can bring to 3Di devices failure analysis, oral presentation and published proceeding, 42nd International Symposium on Testing and Failure Analysis 2016, Fort Worth, Texas, US A.Fraczkiewicz, P.-O. Autran, E.Capria, P.Cloetens, J.Da Silva, S.Lhostis, F.Lorut, S. Moreau, T.Mourier, P.Bleuet, Making synchrotron tomography a routine tool for 3D integration failure analysis through a limited number of projections, an adapted sample preparation scheme, and a fully-automated post-processing, oral presentation and published proceeding, 43rd International Symposium on Testing and Failure Analysis 2016, Pasadena, California, US Articles submitted to peer-reviewed journals A.Fraczkiewicz, F.Lorut, G.Audoit, E.Boller, E.Capria, P.Cloetens, J.Da Silva, A.Farcy, T.Mourier, F.Ponthenier, P.Bleuet, 3D high resolution imaging for microelectronics: a multi-technique survey on copper pillars, Ultramicrosopy, submitted A.Fraczkiewicz, M.-I. Richard, E. Capria, G. Chahine, P. Cloetens, J. Da Silva, A. Jouve, S. Lhostis, F. Lorut, P. Bleuet, In-situ local strain measurement and morphology correlation in hybrid bonding stacks using nano-focused x-ray and electron microscopy, to be submitted Résumé Ce travail de thèse vise à développer de nouvelles techniques de caractérisation pour l'intégration 3D en micro-électronique. Plus précisément, ce travail porte sur l'imagerie 3D de tels objets et la mesure des contraintes par diraction de Bragg, réalisées sur de récentes lignes de lumière de l'ESRF (European Synchrotron Radiation Facility).

L'intégration 3D a pour but de répondre aux besoins de performance de la micro-électronique, en empilant les diérents éléments constituant les puces au lieu de les placer les uns à côté des autres; ceci permet de limiter la place qu'ils occupent et la longueur des connections. Pour ce faire, de nouvelles connections entre puces ont du être développées, telles que les piliers de cuivre et les pads de cuivre, utilisés dans le cas du collage hybride. An de maîtriser leurs procédés de fabrication, il est important de pouvoir caractériser ces objets, à la fois par des moyens d'imagerie et de mesure de la déformation dans les puces. Ces mesures doivent permettre un large champ de vue (100 µm 2 ), ainsi qu'une haute résolution (50 nm). De plus, an de satisfaire les besoins en temps de l'industrie micro-électronique, les techniques choisies doivent être aussi rapides et automatiques que possible.

Pour satisfaire ces besoins, plusieurs techniques ont été étudiées durant ces travaux de thèse. Une technique d'imagerie 3D par Slice and View, inspirée de la technique classique du FIB/SEM et implémentée dans un PFIB (Plasma Focused Ion Beam), a été développée durant ces travaux de thèse. Elle permet aujourd'hui l'acquisition de larges volumes de manière automatique. De même, le procédé d'analyse des mesures de tomographie réalisées sur la ligne de lumière ID16A de l'ESRF a été adapté, an de limiter au maximum l'intervention humaine et le temps global d'analyse.

Des mesures de déformations ont également été menées à l'ESRF, sur une ligne de nano-diraction, ID01. Ces expériences ont été réalisées sur des empilements dédiés au collage, hybride ou direct. Il a été possible de mesurer en une seule expérience les déformations présentes dans deux couches de silicium, et de réaliser des mesures in situ dans le cuivre.

Dans les travaux de thèse présentés ici, nous montrons les possibilités de techniques synchrotron (imagerie et mesure de déformations) pour la caractérisation d'objets issus de l'intégration 3D. Nous montrons que certaines adaptations des techniques existantes peuvent permettre des analyses routinières à haute résolution pour le milieu de la micro-électronique.

Mots clés :

Synchrotron, Tomographie, Intégration 3D, Imagerie 3D, Slice and View, Plasma FIB, Diraction, Piliers de cuivre, Collage hybride, Analyse de défaillance Abstract This PhD thesis aims at developing new characterization techniques for 3D integration in microelectronics. More specically, the focus is set on recent ESRF (European Synchrotron Radiation Facility) beamlines, both for 3D imaging by tomography and for strain measurements by Bragg diraction.

3D integration aims at reducing the global microelectronics devices footprint and connections length, by stacking the dies on top of one another instead of setting them one to another. This new geometry however requires new connections, such as copper pillars (CuP) and copper pads, used in hybrid bonding. The monitoring of their fabrication process requires their imaging in three dimensions, and the measurement of the strain inside them. Those measurements must be conducted on large areas (100 µm 2 ), with high resolution (500 nm for strain and 100 nm for imaging). Moreover, given the industrial context of this study, the characterization methods must be as routine and automatic as possible.

To answer those needs, several techniques have been developed in this work. Two 3D imaging techniques have been made compatible with the requirements of 3D integration characterization. A Slice and View procedure has been implemented inside a single beam PFIB, leading to large volumes 3D automated imaging. The tomography workow accessible on the ID6A beamline of the ESRF has been adapted, in order to limit the human intervention and beam times. This leads to possible statistical measurements on this beamline.

Strain measurements have been conducted on the ID01 beamline of the ESRF, on silicon and copper stacks meant for direct and hybrid bonding. They allowed for simultenous local strain measurements in two independent layers of silicon, and in situ measurements in copper.

In this work, we show the possibilities of synchrotron based techniques (here, tomography and Bragg diraction) for the chacracterization of 3D integration devices. We show that, provided some adjustments, these techniques can be used routinely for the microelectronics eld.