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 diffraction 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 performances de la micro-électronique, en empilant les différents 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. Afin de maîtriser leurs procédé 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), ainsi qu'une haute résolution (50 nm). De plus, afin 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 étudiés 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 tomographies réalisées sur la ligne de lumière ID16A de l'ESRF a été adapté, afin de limiter au maximum l'intervention humain et le temps global d'analyse.Des mesures de déformations ont également été menées à l'ESRF, sur une ligne de nano-diffraction, 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 textit{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 existante peuvent permettre des analyses routinières à haute résolution pour le milieu de la micro-électronique. / This PhD thesis aims at developing new characterization techniques for 3D integration in microelectronics. More specifically, the focus is set on recent ESRF (European Synchrotron Radiation Facility) beamlines, both for 3D imaging by tomography and for strain measurements by Bragg diffraction.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 measure of the strain inside them. Those measurements must be conducted on large areas (100 µm2), 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 workflow 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 textit{in situ} measurements in copper.In this work, we show the possibilities of synchrotron based techniques (here, tomography and Bragg diffraction) for the chacracterization of 3D integration devices. We show that, provided some adjustments, these techniques can be used routinely for the microelectronics field.

This project is in collaboration with the Hydro-Quebec Research Institute (IREQ) and the Canadian Centre for Electron Microscopy (CCEM) on the mechanical test performance of miniature-scale micro-tensile specimens. The objective of the thesis project is to create an efficient and reliable fabrication route for producing micro-tensile specimens and to validate the accuracy of a newly custom-built micro-tensile bench at IREQ. The fabrication techniques developed and outlined in this thesis use the underlying fundamental physical mechanisms of secondary electron microscopy (SEM), focused-ion beam (FIB), and the femtosecond (fs)-laser machining for producing optimal quality micro-tensile specimens. The mechanical testing of the specimens is geared towards studying the localized deformation occurring in the microstructure when the size of the specimen only limits a number of grains and grain boundaries in order to target the specific detailed measurement of the mechanical behaviour of individual grains and interfaces. The goal for creating an optimal fabrication route for micro-tensile specimens is to carry out micro-mechanical testing of the primary turbine steels of 415 martensitic stainless steel used in the manufacture of Francis turbine components at Hydro-Quebec. The mechanical testing of single phase and interphase interface 415 steel micro-tensile specimens are considered building blocks to developing digital twin models of the steel microstructure. The experimental data from the mechanical tests would be fed into the crystal plasticity finite element models (CPFEM) that are currently being developed by researchers at IREQ. With the development of digital twin models, engineers at IREQ would be able to predict crack initiation at the microstructure level (prior to crack propagation into macro-scale cracks) by observing the evolution of the grain’s crystallographic orientation and morphology, as well as deformation mechanisms such as martensite formation and twinning produced from localized induced strains in the microstructure. In addition, self-organized dislocation processes such as dislocation nucleation and dislocation escape through the free surface can also be studied using the CPFEM models for size-limited mechanical deformation behaviour of miniature-scale mechanical test specimens. The fabrication routes studied in this thesis project use the combination of the fs-laser and plasma focused ion beam (PFIB) to machine the micro-tensile specimens. (100) single crystal copper was the ideal material chosen to validate the accuracy of the micro-tensile bench and quality of the fs-laser-machined tensile specimens, due to its ductile nature and well-characterized properties studied in literature. A mechanical size effect was studied for single crystal copper specimens with different gauge thicknesses. It was observed from the micro-tension testing that the strength of the specimens increased with decreasing gauge thickness occurring in the size-limited tensile gauges. In addition, it was determined there was negligible differences in the size effect seen between the PFIB-machined copper micro-tensile specimens and the fs-laser-machined micro-tensile specimens, demonstrating that the fs-laser is a reliable machining route for the micro-tensile specimens. X-ray computed tomography was used to validate the correct geometry of the machined gauge section produced from an innovative gauge thinning method adopted from IREQ’s research collaborator, Dr. Robert Wheeler. As well, finite-element analysis (FEA) was performed to determine the deformation behaviour under both linear-elastic and non-linear elastoplastic conditions of (100) copper and 415 steel models simulated in pure tension, prior to the fabrication of the micro-tensile specimens, respectively. Furthermore, significant progress has been made towards targeting martensite grains in the 415-steel microstructure using electron backscattered diffraction (EBSD) analysis to produce single crystal and interphase interface micro-tensile specimens. A workflow towards grain targeting using EBSD analysis has been developed, as well as for the relocation of grains using reference fiducial marks for future fabrication of the single crystal and interphase interface 415 micro-tensile specimens. / Thesis / Master of Applied Science (MASc) / Hydro-Quebec is an energy utilities company that operates the design of Francis hydro-turbines to supply hydroelectric power across the province of Quebec. The hydro-turbines have an expected service life of 70 years. Unfortunately, the turbines can get replaced by new ones prior to reaching half of its service life, due to the development of severe fatigue crack growth in the primary components of the turbines. A solution proposed by the researchers at the Hydro-Quebec Research Institute (IREQ) is to determine a linkage between the turbine’s steel’s microstructure and the mechanical behaviour of the turbine steels. Deformation of the material starts at the microstructure level, where dislocations glide through the material lattice, causing both reversible (elastic) and irreversible (plastic) deformation. Therefore, a solution was proposed by the researchers at IREQ to create computational models of the steel microstructure to predict the deformation of the steel’s microstructure. Being able to predict the deformation mechanisms through the simulation models of the microstructures allows for engineers at Hydro-Quebec to schedule regular maintenance of the turbines more efficiently and provide metallurgists the knowledge on what is occurring at the microstructure level and what can be done to improve the chemical and physical composition of the steel. To develop the digital twin models, experimental data must be collected through mechanical testing of miniature mechanical test specimens of the turbine steels. The mechanical properties of the single phases and interphase interface specimens are fed into the models as building blocks to building a microstructure map of the turbine steels. Micro-tension testing of micro-tensile specimen provides direct information about the material’s mechanical properties. In this work, a reliable and efficient fabrication route for micro-tensile specimens was developed for the purpose of extracting mechanical properties of single phase and interphase interface turbine steel specimens using focused ion beam (FIB) and femtosecond laser machining.