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In-situ study of crack propagation in patterned structures of microchips using X-ray microscopy
(2023)
The motivation of this thesis was to control crack steering into regions of engineered 3D-nanopatterned structures with high fracture toughness and to determine the local critical energy release rate for crack propagation in 3D-nanopatterned systems. On-chip copper interconnect structures of advanced microchips, insulated by organosilicate glasses, were chosen as an example system to study fracture on small scale, since this is a well-defined 3D- nanopatterned system and since a high mechanical robustness is requested for microchips. An experiment for in-situ high-resolution 3D imaging of the fracture behavior of 3D-nanopatterned structures and of the kinetics of microcrack propagation in solids was designed and applied, combining a miniaturized micromechanical test and high-resolution X-ray imaging. Particularly, a miniaturized piezo-driven double cantilever beam test set-up (micro- DCB) was integrated in a laboratory X-ray microscope, and nano X-ray computed tomography was applied for high-resolution 3D imaging of the microcrack evolution in the on-chip interconnect stack of microchips manufactured in the 14 nm technology node. The measured geometry of the microcrack at several loading steps during the micro-DCB test and the subsequent data analysis based on linear elastic fracture mechanics and the Euler-Bernoulli beam model were the basis for the development and application of a new methodology to determine the critical energy release rate for crack propagation in sub- 100 nm regions of a processed wafer quantitatively. It was experimentally proven that specially designed metallic guard ring structures at the rim of the microchips dissipate energy in such a way that the microcrack propagation is efficiently slowed down and eventually stopped, i.e. they are effective to prevent mechanical damage of microchips. It was demonstrated that it is possible to steer the microcrack in a controlled way by tuning the fracture mode mixity locally at the crack tip. The established concept for a controlled crack propagation provides the basis for further fundamental studies of the fracture behavior of nanoscale materials and structures. The results have significant effects for the understanding of fracture mechanics at small scales, e.g. in microchips, but also in other nanopatterned materials, e.g. in bio-inspired, hierarchically structured engineered materials. The experimental results gathered at realistic microelectronic products provide valuable information to control the crack path in on-chip interconnect stacks for design-for-reliability in semiconductor industry and to manufacture mechanically robust microchips in leading-edge technology nodes. The experimental study of controlled microcrack steering into regions with high fracture toughness provides knowledge for the design of guard ring structures in microchips to stop the propagation of microcracks, e.g. generated during the wafer dicing process.
The powder metallurgically produced beta titanium alloys (traditional PM beta Ti-alloys) have long been plagued by high impurities contamination. For binder-based powder technologies, they originate from the sintering atmosphere, the debinding processes and the starting powders. In general, a normal carbon residual of binder-based powder technologies is capable of incurring the formation of aligned TiCx particles along beta grain boundaries (GB-TiCx) in most classes of beta Ti-alloys. Whereas, oxygen atoms are likely to deteriorate the ductility of PM Ti alloys by promoting the formation of diverse brittle phases and/or altering the deformation modes. Such materials exhibiting rather low toughness to strain ratios are not an option for critical structural applications, where catastrophic damage is completely unacceptable.
In this study, biotolerant metastable beta Ti-20Nb-10Zr alloys, containing a certain amount of carbon, oxygen residuals originated from materials processing and consequently 0.5 vol.% in situ synthesized TiCx particles, were fabricated via metal-injection-molding (MIM). With varying yttrium (Y) addition, the effects of Y-induced oxygen scavenging, beta-grain refinement and porosity increment on tensile properties were systematically investigated. To scavenge oxygen from the beta Ti-matrix, the Y elemental powder with a maximum particle size of 15 µm (e.g. <12 µm or 1200 mesh) is more appropriate than the commonly used <45 µm (i.e. 325 mesh) sized powder or larger ones and without significant detrimental effect on the as-sintered density of beta Ti-alloys.
A novel toughening strategy was proposed by regulating TiCx precipitation evolution and resultantly adjusting particles distribution pattern. Synchrotron radiation identified that two separate TiCx precipitation-type reactions occurred at the beta phase region and the alpha/beta region. In a narrow temperature range between these two precipitation reactions, dissolution of carbides was observed just below alpha/beta transus. Y addition can postpone TiCx precipitation. On the basis of those mechanisms, adjusting TiCx particle distribution was proposed for the first time, specifically a combination of yttrium addition (Y) and carbide spheroidization reprecipitation annealing (CSRA). As a result, aligned GB-TiCx particles were adjusted to dispersed intragranular TiCx particles. An apparent toughening effect (≈ 113% increment reaching elongation = 8.3%) was achieved after TiCx redistribution, while non-optimally aligned TiCx pattern seriously limited tensile toughness of materials. Here, the mechanisms of TiCx redistribution behavior and its toughening are elucidated systematically.