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Le collage direct consiste en la mise en contact de deux surfaces suffisamment lisses et propres pour qu'une adhésion puisse se créer sans ajout de matière à l'interface. Ce procédé réalisable à l'échelle industrielle trouve son intérêt dans l'empilement de structures ou de matériaux pour la microélectronique ou les microtechnologies. Il s'avère alors important de maîtriser ce procédé et cela passe notamment par la compréhension des mécanismes physico-chimique se produisant lors du collage. Le but de ce travail de thèse est donc l'étude des mécanismes mis en jeu dans le collage hydrophobe de silicium et le collage hydrophile d'oxydes de silicium déposés.Dans cette étude, des procédés de collage direct hydrophobe de plaques de silicium (100) reconstruit ont été développés, ainsi que des collages de surfaces hydrophiles d'oxyde de silicium déposés préparées par des activations plasma azote ou oxygène ou par un procédé de polissage mécano-chimique. Le comportement de toutes ces structures a été étudié à plusieurs stades du procédé, en particulier lors des traitements thermiques de consolidation de l'interface de collage. Pour ce faire, différentes techniques de caractérisation ont été mises en oeuvre comme la mesure d'énergie de collage, l'observation de la défectivité par microscopie acoustique, la spectroscopie infrarouge et la réflectivité des rayons X. Cela a ainsi permis de suivre la fermeture de l'interface de collage en température d'un point de vue chimique et mécanique et des mécanismes de collage ont alors pu être proposés pour toutes les structures étudiées. Des recommandations ont également pu être faites pour l'obtention de collages d'oxydes de silicium déposés efficaces et de qualité. / Direct wafer bonding refers to a process by which two mirror-polished wafers are put into contact and held together at room temperature by adhesive force, without any additional material. This technology feasible at an industrial scale generates wide interest for the realization of stacked structures for microelectronics or microtechnologies. In this context, a precise understanding of bonding mechanisms is necessary. Consequently, the aim of this work is to study the bonding mechanisms for hydrophobic silicon reconstructed surfaces and hydrophilic deposited silicon oxides surfacesIn this study, bonding of hydrophobic silicon reconstructed surfaces and bonding of hydrophilic deposited silicon oxides prepared either by plasma activation or chemical-mechanical polishing were analyzed, as a function of post-bonding annealing temperature. For this, several characterization techniques have been used: bonding energy measurement, acoustic microscopy in order to observe defectivity, infrared spectroscopy and X-Ray reflectivity. Thus the bonding interface closure has been analyzed from a chemical and mechanical point of view and bonding mechanisms have been proposed for the studied bonded structures. Finally the study of deposited silicon oxide bonding prepared either by plasma activation or by chemical-mechanical polishing has lead to some recommendations for efficient and high quality deposited silicon oxides bonding.

Safe, effective hydrogen fuel cells are one of the contenders for the next shift in mobile power technology. One of the solutions to the inherent risks of high pressure hydrogen fuel cells is an outer low pressure container with an inner high pressure containers containing a micro-electromechanical systems (MEMS) valve which regulating the pressure. These MEMS valves consist of several etched Si-chips stacked and bonded, which shall withstand the pressure and temperature range in the high pressure fuel cell as well as the embrittlement caused by the hydrogen gas. Hydrogen embrittlement is a phenomena where materials, mostly metals, lose their ductility due to diffusion of hydrogen atoms into their grain boundaries. A suitable method for stacking the chips is needed and thus a literature study was conducted. Several chip-to-chip bonding methods were investigated in the purpose of finding the most suitable methods tolerating temperatures between -40 to 85°C, pressure up to 1000 bar, hermetically sealing, withstanding hydrogen embrittlement and still bond with particulate contaminations caused by testing each chip. The method found to be best fitting for the purpose was anodic bonding with an alkali glass. Alternatively anodic bonding with a ceramic glass system could be considered if technique from alkali glass is adaptable.

Wafer bonding is important in microelectromechanical systems (MEMS) manufacturing, enabling wafer-level encapsulation and packaging. In this project, different pre-treatments of the polycrystalline silicon surface for eutectic gold-silicon (AuSi) bonding were studied with respect to the resulting bond strength. Native oxides or other surface layers can decrease the interaction between Au and Si, leading to weaker bonds. Different etching methods were investigated to remove native oxide. Spectroscopic ellipsometry (SE), water contact angle measurements and Fourier transform infrared spectroscopy (FTIR) were used to analyze the surfaces. SE measurements showed that the oxide layer grew 5 Å the first 4 hours after HF etch, rinse and dry, but then grew less than this during the following 6 weeks. The measured oxide growth was similar for wafers with other pre-treatments. Through contact angle measurements, it was demonstrated that the different etching methods resulted in different outermost surface layers. None of the contact angles were changed much over several weeks, indicating subsequent oxide growth occurred below a stable outermost layer. For wafer bonding, wafers with bond frame structures were used. After wafer bonding, the bond frames were analyzed with infrared (IR) microscopy and the bonds were shear tested for bond strength. The shorter the exposure time to ambient air atmosphere before bond, the stronger the bond in general. Furthermore, the wafers stored in nitrogen atmosphere exhibited higher bond strengths than the wafers stored in air for the same amount of time, confirming that the growing oxide was the reason for the decreased bond quality during wafer storage. HF (wet/vapor) etched wafers in general had slightly stronger bonds than the other wafers and the wafers etched with HF vapor had the highest average bond strength of all. The IR images showed that white areas in the bond frames were related to decreased bond strength, and that wafers that had longer storage time on average had more white in the bond frames. As a conclusion, to achieve as strong bonds as possible, the waiting time between wafer pre-treatments and bonding should be minimized, and in the waiting time it is beneficial to store the wafers in nitrogen atmosphere. In this study most wafers stored 2 weeks in nitrogen had good bond quality and even wafers stored 3 days in air had acceptable bond strengths. However, using HF to etch away the oxide before bond is preferable compared to the other etching methods, not only to have larger average bond strength, but also to have less bond strength decrease during waiting time before bond. / I tillverkning av mikroelektromekaniska system (MEMS) är skivbondning viktigt för inkapsling och förpackning av mikrosystem på skivnivå. I detta projekt studerades olika förbehandlingar av polykristallina kiselytan, inför eutektisk AuSi-bondning, med avseende på resulterande bondstyrka. Nativoxid eller andra ytskikt kan minska interaktionen mellan guld (Au) och kisel (Si), vilket leder till svagare bond. Flera olika etsmetoder undersöktes för att ta bort nativoxid. Spektroskopisk ellipsometri (SE), mätningar av vattenkontaktvinkel och Fouriertransform infraröd spektroskopi (FTIR), användes för att analysera ytorna. Resultaten från SE-mätningarna visade att oxiden växte 5 Å under de 4 första timmarna efter HF-ets, skölj och tork, men växte sedan mindre än detta under de följande 6 veckorna. Den uppmätta oxidtillväxten var liknande för skivorna med andra förbehandlingar. Kontaktvinklarna var olika för olika förbehandlingsmetoder, vilket visar att de hade olika yttersta ytskikt. Ingen av kontaktvinklarna ändrades mycket under flera veckor, vilket indikerar att den följande oxidtillväxten skedde under ett stabilt yttersta lager. För skivbondning andvändes skivor med bondramar längs chip-kanterna. Dessa bondramar var gjorda av polykristallint Si respektive Au på skivorna som skulle bondas. Efter bondning analyserades bondramarna med infraröd (IR) mikroskopi och skjuvtester gjordes för att bestämma bondstyrkan. Ju kortare tid skivorna exponerades till omgivande luft, desto starkare bond i allmänhet. Dessutom uppvisade skivorna som lagrats i kväveatmosfär högre bondstyrkor än de skivor som lagrats i luft, vilket bekräftar att den växande oxiden var orsaken till den minskade bondkvaliteten under skivlagring. HF-etsade skivor (HF- dipp och HF-ånga) hade något starkare bond än de andra skivorna och de skivor som etsats med HF-ånga hade allra högst genomsnittlig bondstyrka. IR-bilderna visade att vita områden i bondramarna var relaterat till minskad bondstyrka och att skivor som hade längre lagringstid i genomsnitt hade mer vitt i bondramarna. Slutsatsen är att för att uppnå så hög bondstyrka som möjligt ska tiden mellan förbehandlingar och bond minmeras, och under väntetiden är det till fördel att skivorna förvaras i kväveatmosfär. I den här studien hade skivor som förvarats 2 veckor i kväve bra bondkvalitet och även skivor som stått 3 dagar i luft hade godtagbara bondstyrkor. Att använda HF för att etsa bort oxid är dock bättre än att använda någon av de andra etsmetoderna, inte bara för att få högre genomsnittliga bondstyrkor, utan också för att få mindre minskning av bondstyrkan under väntetiden inför bondning.