Sn-based solder alloys are extensively used in electronic devices to form interconnects between different components to provide mechanical support and electrical path. The formation of a reliable solder interconnects fundamentally relies on the metallurgic reaction between the molten solder and solid pad metallization in reflowing. The resultant IMC layer at the solder/pad metallization interface can grow continuously during service or aging at an elevated temperature, uplifting the proportion of IMCs in the entire solder joint. However, the essential mechanical properties of interfacial IMC (i.e. Cu6Sn5, Cu3Sn) layers, such as Young s modulus and hardness, are drastically different in comparison with Sn-based solder and substrate. Therefore, the increasing fraction of interfacial IMCs in the solder joint can lead to significant deformation incompatibility under exterior load, which becomes an important reliability concern in the uses of solder joints for electronic interconnects. In the past decades, extensive research works were implemented and reported regarding the growth of interfacial IMC layers and its effect on the mechanical integrity of solder joints. But, the following fundamental issues in terms of mechanical and microstructural evolution in the uses of solder joints still remain unclear, demanding further research to elaborate: (1) The protrusion of IMCs: Though the growth of interfacial IMC layers along the diffusion direction in solder joints were studied extensively, the growth of IMCs perpendicular to the diffusion direction were reported in only a few papers without any further detailed investigation. This phenomena can crucially govern the long-term reliability of solder interconnects, in particular, in the applications that require a robust microstructural integrity from a solder joint. (2) Fracture behaviour of interfacial IMC layers: The fracture behaviour of interfacial IMC layers is a vital factor in determining the failure mechanism of solder joints, but this was scarcely investigated due to numerous challenges to enable a potential in-situ micro-scale tests. It is therefore highly imperative to carry out such study in order to reveal the fracture behaviour of interfacial IMC layers which can eventually provide better understanding of the influence of interfacial IMC layers on the mechanical integrity of solder joints. (3) Volume shrinkage: The volume shrinkage (or solder joint collapse) induced by the growth of interfacial IMC layers was frequently ascribed as one of the main causes of the degradation of mechanical reliability during aging due to the potentially resulted voids and residual stress at the solder/substrate interface. However, very few experimental works on the characterisation of such type of volume shrinkage can be found in literatures, primarily due to the difficulties of observing the small dimensional changes that can be encountered in the course of IMCs growth. (4) Residual stress: The residual stress within solder joints is another key factor that contributes to the failure of solder joints under external loads. However, the stress evolution in solder joints as aging progresses and the potential correlation between the residual stress and the growth of interfacial IMC layers is yet to be fully understood, as stress/strain status can fundamentally alter the course of total failure of a solder joint. (5) Crack initiation and propagation in solder joints: Modelling on the mechanical behaviour of solder joints is often undertaken primarily on the stress distribution within solder joints, for instance, under a given external loading. But there is lack of utilising numerical analysis to simulate the crack initiation and propagation within solder joints, thus the effect of interfacial IMC layers on the fracture behaviour of the solder joints can be elaborated in further details. In this thesis, the growth of interfacial IMCs in parallel and perpendicular to the interdiffusion direction in the Sn99Cu1/Cu solder joints after aging was investigated and followed by observation with SEM, with an intention of correlating the growth of IMCs along these two directions with aging durations based on the measured thickness of IMC layer and height of perpendicular IMCs. The mechanism of the protrusion of IMCs and the mutual effect between the growth of IMCs along these two directions was also discussed. The tensile fracture behaviour of interfacial Cu6Sn5 and Cu3Sn layers at the Sn99Cu1/Cu interface was characterised by implementing cantilever bending tests on micro Cu6Sn5 and Cu3Sn pillars prepared by focused ion beam (FIB). The fracture stress and strain were evaluated by finite element modelling using Abaqus. The tensile fracture mechanism of both Cu6Sn5 and Cu3Sn can then be proposed and discussed based on the observed fracture surface of the micro IMC pillars. The volume shrinkage of solder joints induced by the growth of interfacial IMC layers in parallel to the interdiffusion direction in solder joint was also studied by specifically designed specimens, to enable the collapse of the solder joint to be estimated by surface profiling with Zygo Newview after increased durations of aging. Finite element modelling was also carried out to understand the residual stress potentially induced due to the volume shrinkage. The volume shrinkage in solder joints is likely to be subjected to the constraint from both the attached solder and substrate, which can lead to the build-up of residual stress at the solder/Cu interface. Depth-controlled nanoindentation tests were therefore carried out in the Sn99Cu1 solder, interfacial Cu6Sn5 layer, Cu3Sn layer and Cu with Vickers indenter after aging. The residual stress was then evaluated in the correlation with aging durations, different interlayers and the locations in the solder joint. Finally, finite element models incorporated with factors that may contribute to the failure of solder joints, including microstructure of solder joints, residual stress and the fracture of interfacial IMC, were built using Abaqus to reveal the effect of these factors on the fracture behaviour of solder joints under applied load. The effect of growth of IMC layer during aging on the fracture behaviour was then discussed to provide a better understanding of the degradation of mechanical integrity of solder joints due to aging. The results from this thesis can facilitate the understanding of the influence of interfacial IMC layers on the mechanical behaviour of solder joints due to long-term exposure to high temperatures.

Small-scale fracture behavior of four model alloy systems were investigated in the order of increasing microstructural complexity, namely: (i) a Ni-based Bulk Metallic Glass (Ni-BMG) with an isotropic amorphous microstructure; (ii) a single-phase high entropy alloy, HfTaTiVZr, with body centered cubic (BCC) microstructure; (iii) a dual-phase high entropy alloy, AlCoCrFeNi2.1, with eutectic FCC (L12) -BCC (B2) microstructure; and (iv) a Medium-Mn steel with hierarchical microstructure. The micro-mechanical response of these model alloys was investigated using nano-indentation, micro-pillar compression, and micro-cantilever bending. The relaxed Ni-BMG showed 6% higher hardness, 22% higher yield strength, and 26% higher bending strength compared to its as-cast counterpart. Both the as-cast and corresponding relaxed BMGs showed stable notch opening and blunting during micro-cantilever bending tests rather than unstable crack propagation. However, pronounced notch weakening was observed for both the structural states, with the bending strength lower by ~ 25% for the notched samples compared to the un-notched samples. Deformation behavior of HfTaTiVZr was evaluated by micropillar compression and micro-cantilever bending as a function of two different grain orientations, namely [101] and [111]. The [111] oriented micropillars demonstrated higher strength and strain hardening rate compared to [101] oriented micropillars. The [111] oriented micropillars showed transformation induced plasticity (TRIP) in contrast to dislocation-based planar-slip for the [101] oriented micropillars, explaining the difference in strain hardenability for the two orientations. These differences in deformation behavior for the two orientations were explained using Schmid factor calculations, transmission electron microscopy, and in-situ deformation videos. For the dual-phase AlCoCrFeNi2.1 high entropy alloy, the L12 phase exhibited superior bending strength, strain hardening, and plastic deformation, while the B2 phase showed limited damage tolerance during bending. The microstructure and deformation mechanisms were characterized for a few different medium-Mn steels with varying carbon (0.05-0.15 at%) and manganese (5-10 at%) content. The alloy with 10 at% Mn and 0.15 at% C (1015 alloy) showed hierarchical microstructure of retained austenite and ferrite with lamellae 200 nm to 300 nm wide. Micro-pillar compression at different strain levels for this alloy revealed that deformation in austenite is primarily accommodated through transformation to martensite, thereby increasing the strain hardening rate.

The aim of the presented work was to deposit cubic boron nitride thin films by magnetron sputtering under simultaneous stress relaxation by ion implantation. An in situ instrument based on laser deflectometry on cantilever structures and in situ ellipsometry, was used for in situ stress measurements. The characteristic evolution of the instantaneous stress during the layered growth of cBN films observed in IBAD experiments, could be reproduced for magnetron sputter deposition. To achieve simultaneous stress relaxation by ion implantation, a complex bipolar pulsed substrate bias source was constructed. This power supply enables the growth of cBN thin films under low energy ion irradiation (up to 200 eV) and, for the first time, the simultaneous implantation of ions with an energy of up to 8 keV during high voltage pulses. It was demonstrated that the instantaneous stress in cBN thin films can be released down to -1.1 GPa by simultaneous ion bombardment during the high voltage pulses. A simultaneous stress relaxation during growth is possible in the total investigated ion energy range between 2.5 and 8 keV. These are the lowest ion energies reported for the stress relaxation in cBN. Since such a substrate bias power supply is easy to integrate in existing process lines, this result is important for industrial deposition of thin films, not only for cubic boron nitride films. It was found that the amount of stress relaxation depends on the number of atomic displacements (displacements per atom: dpa) that are induced by the high energy ion bombardment and is therefore dependent on the ion energy and the high energy ion flux. In practise, this means that the stress relaxation is controlled by the product of the pulse voltage and the pulse duty cycle or frequency. The cantilever bending measurements were complemented on microscopic scale by x-ray diffraction (XRD). The analysis of the cBN (111) lattice distances revealed a pronounced biaxial compressive state of stress in a non-relaxed cBN film with d(111) being larger in out-of-plane than in in-plane direction. Post deposition annealing at 900 ° C of a sample with an ion induced damage of 1.2 dpa, resulted in a complete relaxation of the lattice with equal in-plane and out-of-plane lattice parameters. In the case of medium-energy ion bombardment, the in-plane and out-of-plane lattice parameters approach the value of the annealed sample with increasing ion damage. This is a clear evidence for stress relaxation within the cBN lattice. The stability of cBN under ion bombardment was investigated by IR spectroscopy and XRD. The crystalline cBN was found to be very stable against ion irradiation. However a short-range ordered, sp3/sp2 - mixed phase may exist in the films, which could be preferably converted to a sp2 -phase at high damage values. From the analysis of the near surface region by XANES, it can be concluded the stress relaxation by the energetic ion bombardment is less at the surface than in the bulk film. This is explained with the dynamic profile of the ion induced damage, that reaches the stationary bulk value in 15-20 nm depth, whereas it is decreasing towards the surface. This fits with the results that the stress relaxation is dependent on the amount of ion induced damage. Comparing the results from substrate curvature measurement, XRD, XANES, and IR spectroscopy possible mechanisms of stress relaxation are discussed. Concluding the results, it can be stated that using simultaneous ion implantation for stress relaxation during the deposition it is possible to produce BN films with a high amount of the cubic phase and with very low residual stress.

The aim of the presented work was to deposit cubic boron nitride thin films by magnetron sputtering under simultaneous stress relaxation by ion implantation. An in situ instrument based on laser deflectometry on cantilever structures and in situ ellipsometry, was used for in situ stress measurements. The characteristic evolution of the instantaneous stress during the layered growth of cBN films observed in IBAD experiments, could be reproduced for magnetron sputter deposition. To achieve simultaneous stress relaxation by ion implantation, a complex bipolar pulsed substrate bias source was constructed. This power supply enables the growth of cBN thin films under low energy ion irradiation (up to 200 eV) and, for the first time, the simultaneous implantation of ions with an energy of up to 8 keV during high voltage pulses. It was demonstrated that the instantaneous stress in cBN thin films can be released down to -1.1 GPa by simultaneous ion bombardment during the high voltage pulses. A simultaneous stress relaxation during growth is possible in the total investigated ion energy range between 2.5 and 8 keV. These are the lowest ion energies reported for the stress relaxation in cBN. Since such a substrate bias power supply is easy to integrate in existing process lines, this result is important for industrial deposition of thin films, not only for cubic boron nitride films. It was found that the amount of stress relaxation depends on the number of atomic displacements (displacements per atom: dpa) that are induced by the high energy ion bombardment and is therefore dependent on the ion energy and the high energy ion flux. In practise, this means that the stress relaxation is controlled by the product of the pulse voltage and the pulse duty cycle or frequency. The cantilever bending measurements were complemented on microscopic scale by x-ray diffraction (XRD). The analysis of the cBN (111) lattice distances revealed a pronounced biaxial compressive state of stress in a non-relaxed cBN film with d(111) being larger in out-of-plane than in in-plane direction. Post deposition annealing at 900 ° C of a sample with an ion induced damage of 1.2 dpa, resulted in a complete relaxation of the lattice with equal in-plane and out-of-plane lattice parameters. In the case of medium-energy ion bombardment, the in-plane and out-of-plane lattice parameters approach the value of the annealed sample with increasing ion damage. This is a clear evidence for stress relaxation within the cBN lattice. The stability of cBN under ion bombardment was investigated by IR spectroscopy and XRD. The crystalline cBN was found to be very stable against ion irradiation. However a short-range ordered, sp3/sp2 - mixed phase may exist in the films, which could be preferably converted to a sp2 -phase at high damage values. From the analysis of the near surface region by XANES, it can be concluded the stress relaxation by the energetic ion bombardment is less at the surface than in the bulk film. This is explained with the dynamic profile of the ion induced damage, that reaches the stationary bulk value in 15-20 nm depth, whereas it is decreasing towards the surface. This fits with the results that the stress relaxation is dependent on the amount of ion induced damage. Comparing the results from substrate curvature measurement, XRD, XANES, and IR spectroscopy possible mechanisms of stress relaxation are discussed. Concluding the results, it can be stated that using simultaneous ion implantation for stress relaxation during the deposition it is possible to produce BN films with a high amount of the cubic phase and with very low residual stress.