The current thesis takes a step forward into understanding the intergranular stress corrosion cracking (IGSCC) by applying a relatively new micro-mechanical technique to look at the crack growth rate of individual grain boundaries in 304 stainless steel (SS) and to measure fracture toughness for different grain boundaries in Ni Alloy 600. In addition, a model is tested and proposed that could predict crack initiation in 304 SS. Pentagonal cross-section cantilevers 5 μm wide by 25 μm long were milled at individual grain boundaries in both 304 SS and Ni Alloy 600. The cantilevers milled in 304 SS were tested in-situ in a customised stage, using the nanoindenter. Crack growth rate was measured for two different cantilevers to be approximately 40 μm/s (K = 1.1 MPa(m)^(1/2)) and 120 μm/s (K = 1.7 MPa(m)^(1/2)). Cantilevers were milled in Ni Alloy 600 for three different samples: samples that were exposed to simulated pressurized water reactors (PWR) environment for 4500 h, for 1500 h and un-oxidised samples. The fracture toughness calculated for the fractured cantilevers in samples that were exposed for 4500 h was measured to be between 0.73 and 1.82 MPa(m)^(1/2). No intergranular fracture occurred in the samples that were exposed for 1500 h and in the un-oxidised samples. The grain boundary misorientation was measured for the tested cantilevers but no direct correlation was observed between the misorientation angle and the fracture toughness. A Schmid-modified grain boundary stress (SMGBS) model previously used to study the intergranular behaviour of irradiated 316L steel in supercritical water was applied to predict crack initiation in 304 stainless steel. The model was successfully applied and accurately predicted crack initiation. To extend the model, sensitisation was also included. In addition, different areas of the specimen, including the initiation site were analysed using High resolution electron backscatter diffraction (HR-EBSD) technique to measure the geometrically necessary dislocations (GNDs) density. It was observed that the boundary average GNDs is lower for the intact boundaries and higher for the cracked grain boundaries.

Using a Panasonic MG-72 Micro Electro-Discharge Machine, techniques and procedures are developed to fabricate complex microstructures in conductive materials and engineered ceramics.

We calculate the stress response, or rheology, of a micro-mechanical model suspension of rigid, Brownian spheroids in a Newtonian fluid in an oscillatory shear flow. The straining and rotation components of a linear flow affects the microstructure, or particle orientation in space and time, and thus, the suspension stress. A statistical description of the microstructure is given by an orientation probability distribution function, which quantifies the likelihood of a particle possessing a particular orientation at an instance in time. The evolution of the microstructure results from the memory of the material, advection from the flow, and rotational Brownian motion. The macroscopic stress response is calculated from ensemble averages of the stresslet weighted by the orientation distribution function. First, we calculate the linear stress response of a dilute suspension of rigid, spheroidal, self-propelled particles under a small-amplitude oscillatory shear deformation using regular perturbation theory. The particle activity leads to a direct contribution to the material stress, via self-propulsion, and an indirect contribution due to correlated tumbling events. The mechanism and strength of self-propulsion and correlation between tumbling events can be determined from the linear stress response of an active suspension. Next, we develop a framework for determining the relaxation moduli of a viscoelastic material through the combination of a memory integral expansion and a multimode-frequency oscillatory shear flow. We analytically determine the first nonlinear relaxation modulus of the model suspension through a comparison of the second normal stress difference from the microstructural stress response, calculated via regular perturbation theory, and a co-rotational memory integral expansion. The stress response of the system is reconstructed for the start-up and cessation of steady simple shear and uniaxial extension. Finally, we numerically calculate the nonlinear viscoelasticity of the model system subject to a large-amplitude oscillatory shear flow. In a sufficiently strong flow with oscillation frequency comparable to the material relaxation rate, secondary overshoots in the stress response occur. We attribute the origin of secondary overshoots to particles undergoing a Jeffery orbit during a (half) cycle of the oscillation, analogous to the case of non-Brownian spheroids in steady shear flow.

Micro-mechanical Raman spectroscopy is an excellent tool for direct stress measurements in the structure. The presence of mechanical stress changes the Raman frequency of each Raman modes compared to the Raman frequencies in absence of stress. This difference in Raman frequency is linearly related to stress induced and can be calibrated to stress by uniaxial or biaxial tension/compression experiments. This relationship is not generally linear for non-linear behavior of the materials which limits its use to experimentally study flow stress and plastic deformation behavior of the material. In this work strontium titanate ceramic particles dispersed inside epoxy resin matrix were used to measure stress in epoxy resin matrix with non-linear material behavior around it. The stress concentration factor between stress induced inside ceramic particles and epoxy resin matrix was obtained by non-linear constitutive finite element model. The results of finite element model were used for training a machine learning model to predict stress in epoxy resin matrix based on stress inside ceramic particles. By measuring stress inside ceramic particles using micro-mechanical Raman spectroscopy, the stress inside epoxy matrix was obtained by pre-determined stress concentration factor.

The mechanical response of geomaterials is highly influenced by geometrical and material heterogeneity. To date, most modelling practices consider heterogeneity qualitatively and the choice of input parameters can be subjective. In this study, a novel approach to combine detailed micro-scale characterization with modelling of heterogeneous geomaterials is presented. The influence of micro-scale heterogeneity and microcracks on the mechanical response and brittle fracture of a crystalline rock was studied using numerical and experimental tools. An existing Combined Finite-Discrete element (FEM/DEM) code was extended to suit heterogeneous, discontinuous, brittle rocks. By conducting grid micro-indentation and micro-scratch tests, the Young's modulus and fracture toughness of the constituent phases of the rock were obtained and used as accurate input parameters for the numerical models. The models incorporated the exact phase mapping obtained from a MicroCT-scanned specimen and the existing microcrack density obtained from thin section analysis. The results illustrated that by incorporating accurate micromechanical input parameters and the intrinsic rock geometric features, the numerical simulations could more accurately predict the mechanical response of the specimen, including the fracture patterns and tensile strength. The numerical simulations illustrated that microstructural flaws such as microcracks should be included in the models to more accurately reproduce the rock strength. In addition, the differential elastic deformations caused by rock heterogeneity altered the stress distribution in the specimen, creating zones of local tensile stresses, in particular, on the boundaries between different mineral phases. As a result, heterogeneous models exhibited rougher fracture surfaces. MicroCT observations emphasized the influence of heterogeneity and, in particular, biotite grains on the fracture trajectories in the specimens. Favourably oriented biotite flakes and cleavage splitting significantly deviated the cracks. The interaction of the main crack with perpendicular cleavage planes of biotite caused strong crack deviation and termination. Considering heterogeneity and the strength degradation caused by microcracks, the simulations captured reasonably accurate mechanical responses and failure mechanisms for the rock, namely, the nonlinear stress-strain relationships. The insights presented in this study improve the understanding of the role of heterogeneity and microstructure on damage and mechanical behaviour of brittle rock.

The mechanical response of geomaterials is highly influenced by geometrical and material heterogeneity. To date, most modelling practices consider heterogeneity qualitatively and the choice of input parameters can be subjective. In this study, a novel approach to combine detailed micro-scale characterization with modelling of heterogeneous geomaterials is presented. The influence of micro-scale heterogeneity and microcracks on the mechanical response and brittle fracture of a crystalline rock was studied using numerical and experimental tools. An existing Combined Finite-Discrete element (FEM/DEM) code was extended to suit heterogeneous, discontinuous, brittle rocks. By conducting grid micro-indentation and micro-scratch tests, the Young's modulus and fracture toughness of the constituent phases of the rock were obtained and used as accurate input parameters for the numerical models. The models incorporated the exact phase mapping obtained from a MicroCT-scanned specimen and the existing microcrack density obtained from thin section analysis. The results illustrated that by incorporating accurate micromechanical input parameters and the intrinsic rock geometric features, the numerical simulations could more accurately predict the mechanical response of the specimen, including the fracture patterns and tensile strength. The numerical simulations illustrated that microstructural flaws such as microcracks should be included in the models to more accurately reproduce the rock strength. In addition, the differential elastic deformations caused by rock heterogeneity altered the stress distribution in the specimen, creating zones of local tensile stresses, in particular, on the boundaries between different mineral phases. As a result, heterogeneous models exhibited rougher fracture surfaces. MicroCT observations emphasized the influence of heterogeneity and, in particular, biotite grains on the fracture trajectories in the specimens. Favourably oriented biotite flakes and cleavage splitting significantly deviated the cracks. The interaction of the main crack with perpendicular cleavage planes of biotite caused strong crack deviation and termination. Considering heterogeneity and the strength degradation caused by microcracks, the simulations captured reasonably accurate mechanical responses and failure mechanisms for the rock, namely, the nonlinear stress-strain relationships. The insights presented in this study improve the understanding of the role of heterogeneity and microstructure on damage and mechanical behaviour of brittle rock.

Following the continually increasing demand for high-density interconnection and multilayer packaging for chips, solder bump size has decreased significantly over the years, this has led to some challenges in the reliability of interconnects. This thesis presents research into the resulting effects of miniaturization on the interconnection with Sn-solder, especially focusing on the full intermetallics (IMCs) micro-joints which appear in the 3D IC stacking packaging. Thereby, systematic studies have been conducted to study the microstructural evolution and reliability issues of Cu-Sn and Cu-Sn-Ni IMCs micro-joints. (1) Phenomenon of IMCs planar growth: The planar IMCs interlayer was asymmetric and composed of (Cu,Ni)6Sn5 mainly in Ni/Sn (2.5~5 μm)/Cu interconnect. Meanwhile, it was symmetric two-layer structure in Cu/Sn (2.5~5 μm)/Cu interconnect with the Cu3Sn fine grains underneath Cu6Sn5 cobblestone-shape-like grains for each IMCs layer. Besides, it is worth noticing that the appearance of Cu-rich whiskers (the mixture of Cu/Cu2O/SnOx/Cu6Sn5) could potentially lead to short-circuit in the cases of ultra-fine ( < 10 μm pitch) interconnects for the miniaturization of electronics devices. (2) Microstructural evolution process of Cu-Sn IMCs micro-joint: The simultaneous solidification of IMCs interlayer supressed the scalloped growth of Cu6Sn5 grains in Cu/Sn (2.5 μm)/Cu interconnect during the transient liquid phase (TLP) soldering process. The growth factor of Cu3Sn was in the range of 0.29~0.48 in Cu-Cu6Sn5 diffusion couple at 240~290 °C, which was impacted significantly by the type of substrates. And the subsequent homogenization process of Cu3Sn grains was found to be consistent with the description of flux-driven ripening (FDR) theory. Moreover, Kirkendall voids appeared only in the Cu3Sn layer adjacent to Cu-plated substrate, and this porous Cu3Sn micro-joint was mechanically robust during the shear test. (3) Microstructural evolution of Cu-Sn-Ni IMCs micro-joint: There was obvious inter-reaction between the interfacial reactions in Ni/Sn (1.5 μm)/Cu interconnect. The growth factor of (Cu,Ni)3Sn on Cu side was about 0.36 at 240 °C, and the reaction product on Ni side was changed from Ni3Sn4 into (Cu,Ni)6Sn5 with the increase of soldering temperature. In particular, the segregation of Ni atoms occurred along with phase transformation at 290 °C and thereby stabilized the (Cu,Ni)6Sn5 phase for the high Ni content of 20 at.%. (4) Micro-mechanical characteristics of Cu-Sn-Ni IMCs micro-joint: The Young s modulus and hardness of Cu-Sn-Ni IMCs were measured by nanoindentation test, such as 160.6±3.1 GPa/ 7.34±0.14 GPa for (Cu,Ni)6Sn5 and 183.7±4.0 GPa/ 7.38±0.46 GPa for (Cu,Ni)3Sn, respectively. Besides, in-situ nano-compression tests have been conducted on IMCs micro-cantilevers, the fracture strength turns out to be 2.46 GPa. And also, the ultimate tensile stress was calculated to be 2.3±0.7 GPa from in-situ micro-bending tests, which is not sensitive with the microstructural change of IMCs after dwelling at 290 °C.

No description available.

UV-LIGA is a microfabrication process realzed by material deposition through microfabricated molds. UV photolithography is conducted to pattern precise thick micro molds using UV light sensitive materials, mostly SU-8, and electroforming is performed to fabricate micro metallic structures defined by the micro molds. Therefore, UV-LIGA is a bottom-up in situ material-addition process. UV-LIGA has received broad attention recently than LIGA – a micro molding fabrication process using X-ray to pattern the micro molds. LIGA is an expansive and is limited in access. In comparing to LIGA, the UV-LIGA is a cost effective process, and is widely accessible and safe. Therefore, it has been extensively used for the fabrication of metallic micro-electro-mechanical-systems (MEMS). The motivation of this research was to study micro mechanical systems fabricated with nano-structured metallic materials via UV-LIGA process. Various micro mechanical systems with high-aspect-ratio and thick metallic structures have been developed and are presented in this desertation. A novel micro mechanical valve has been developed with nano-structured nickel realized with UV-LIGA fabrication technique. Robust compact valves are crucial for space applications where payload and rubstaness are critically concerned. Two types of large flow rate robust passive micro check valve arrays have been designed, fabricated and tested for robust hydraulic actuators. The first such micro valve developed employs nanostructured nickel as the valve flap and single-crystal silicon as the substrates to house inlet and outlet channels. The Nano-structured nickel valve flap was fabricated using the UV-LIGA process developed and the microchannels were fabricated by deep reactive etching (DRIE) method. The valves were designed to operate under a high pressure (>10MPa), able to operate at high frequencies (>10kHz) in cooperating with the PZT actuator to produce large flow rates (>10 cc/s). The fabricated microvalves weigh 0.2 gram, after packing with a novel designated valve stopper. The tested results showed that the micro valve was able to operate at up to 14kHz. This is a great difference in comparison to traditional mechanical valves whose operations are limited to 500 Hz or less. The advantages of micro machined valves attribute to the scaling laws. The second type of micro mechanical valves developed is a in situ assembled solid metallic (nickel) valves. Both the valve substrates for inlet and outlet channels and the valve flap, as well as the valve stopper were made by nickel through a UV-LIGA fabrication process developed. Continuous multiple micro molds fabrication and molding processes were performed. Final micro mechanical valves were received after removing the micro molds used to define the strutures. There is no any additional machining process, such as cutting or packaging. The alignment for laminated fabrication was realized under microscope, therefore it is a highly precise in situ fabrication process. Testing results show the valve has a forward flow rate of19 cc/s under a pressure difference of 90 psi. The backward flow rate of 0.023 cc/s, which is negligible (0.13%). Nano-structured nickel has also been used to develop laminated (sandwiched) micro cryogenic heater exchanger with the UV-LIGA process. Even though nickel is apparently not a good thermal conductor at room temperature, it is a good conductor at cryogentic temerpature since its thermal conductivity increases to 1250 W/k·m at 77K. Micro patterned SU-8 molds and electroformed nickel have been developed to realize the sandwiched heat exchanger. The SU-8 mold (200mm x 200mm x50mm) array was successfully removed after completing the nickel electroforming. The second layer of patterned SU-8 layer (200mm x 200mm x50mm, as a thermal insulating layer) was patterned and aligned on the top of the electroformed nickel structure to form the laminated (sandwiched) micro heat exchanger. The fabricated sandwiched structure can withstand cryogenic temperature (77K) without any damages (cracks or delaminations). A study on nanocomposite for micro mechanical systems using UV-LIGA compatible electroforming process has been performed. Single-walled carbon nanotubes (SWNTs) have been proven excellent mechanical properties and thermal conductive properties, such as high strength and elastic modulus, negative coefficient of thermal expansion (CTE) and a high thermal conductivity. These properties make SWNT an excellent reinforcement in nanocomposite for various applications. However, there has been a challenge of utilizing SWNTs for engineering applications due to difficulties in quality control and handling – too small (1-2nm in diameter). A novel copper/SWNT nanocomposite has been developed during this dissertational research. The goal of this research was to develop a heat spreader for high power electronics (HPE). Semiconductors for HPE, such as AlGaN/GaN high electron mobility transistors grown on SiC dies have a typical CTE about 4~6x10-6/k while most metallic heat spreaders such as copper have a CTE of more than 10x10-6/k. The SWNTs were successfully dispersed in the copper matrix to form the SWNT/Cu nano composite. The tested composite density is about 7.54 g/cm3, which indicating the SWNT volumetric fraction of 18%. SEM pictures show copper univformly coated on SWNT (worm-shaped structure). The measured CTE of the nanocomposite is 4.7 x 10-6/°C, perfectly matching that of SiC die (3.8 x 10-6/°C). The thermal conductivity derived by Wiedemann-Franz law after measuring composit's electrical conductivity, is 588 W/m-K, which is 40% better than that of pure copper. These properties are extremely important for the heat spreader/exchanger to remove the heat from HPE devices (SiC dies). Meanwhile, the matched CTE will reduce the resulted stress in the interface to prevent delaminations. Therefore, the naocomposite developed will be an excellent replacement material for the CuMo currently used in high power radar, and other HPE devices under developing. The mechanical performance and reliability of micro mechanical devices are critical for their application. In order to validate the design & simulation results, a direct (tensile) test method was developed to test the mechanical properties of the materials involved in this research, including nickel and SU-8. Micro machined specimens were fabricated and tested on a MTS Tytron Micro Force Tester with specially designed gripers. The tested fracture strength of nanostructured nickel is 900±70 MPa and of 50MPa for SU-8, resepctively which are much higher than published values.

No description available.