abstract: Increasing demand for high strength powder metallurgy (PM) steels has resulted in the development of dual phase PM steels. In this work, the effects of thermal aging on the microstructure and mechanical behavior of dual phase precipitation hardened powder metallurgy (PM) stainless steels of varying ferrite-martensite content were examined. Quantitative analyses of the inherent porosity and phase fractions were conducted on the steels and no significant differences were noted with respect to aging temperature. Tensile strength, yield strength, and elongation to fracture all increased with increasing aging temperature reaching maxima at 538oC in most cases. Increased strength and decreased ductility were observed in steels of higher martensite content. Nanoindentation of the individual microconstituents was employed to obtain a fundamental understanding of the strengthening contributions. Both the ferrite and martensite hardness values increased with aging temperature and exhibited similar maxima to the bulk tensile properties. Due to the complex non-uniform stresses and strains associated with conventional nanoindentation, micropillar compression has become an attractive method to probe local mechanical behavior while limiting strain gradients and contributions from surrounding features. In this study, micropillars of ferrite and martensite were fabricated by focused ion beam (FIB) milling of dual phase precipitation hardened powder metallurgy (PM) stainless steels. Compression testing was conducted using a nanoindenter equipped with a flat punch indenter. The stress-strain curves of the individual microconstituents were calculated from the load-displacement curves less the extraneous displacements of the system. Using a rule of mixtures approach in conjunction with porosity corrections, the mechanical properties of ferrite and martensite were combined for comparison to tensile tests of the bulk material, and reasonable agreement was found for the ultimate tensile strength. Micropillar compression experiments of both as sintered and thermally aged material allowed for investigation of the effect of thermal aging. / Dissertation/Thesis / M.S. Materials Science and Engineering 2011

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.

Owing to continuous miniaturization, many modern high-technology applications such as medical and optical devices, thermal barrier coatings, electronics, micro- and nano-electro mechanical systems (MEMS and NEMS), gems industry and semiconductors increasingly use components with sizes down to a few micrometers and even smaller. Understanding their deformation mechanisms and assessing their mechanical performance help to achieve new insights or design new material systems with superior properties through controlled microstructure at the appropriate scales. However, a fundamental understanding of mechanical response in surface-dominated structures, different than their bulk behaviours, is still elusive. In this thesis, the size effect in a single-crystal Ti alloy (Ti15V3Cr3Al3Sn) is investigated. To achieve this, nanoindentation and micropillar (with a square cross-section) compression tests were carried out in collaboration with Swiss Federal Laboratories for Materials Testing and Research (EMPA), Switzerland. Three-dimensional finite element models of compression and indentation with an implicit time-integration scheme incorporating a strain-gradient crystal-plasticity (SGCP) theory were developed to accurately represent deformation of the studied body-centered cubic metallic material. An appropriate hardening model was implemented to account for strain-hardening of the active slip systems, determined experimentally. The optimized set of parameters characterizing the deformation behaviour of Ti alloy was obtained based on a direct comparison of simulations and the experiments. An enhanced model based on the SGCP theory (EMSGCP), accounting for an initial microstructure of samples in terms of different types of dislocations (statistically stored and geometrically necessary dislocations), was suggested and used in the numerical analysis. This meso-scale continuum theory bridges the gap between the discrete-dislocation dynamics theory, where simulations are performed at strain rates several orders of magnitude higher than those in experiments, and the classical continuum-plasticity theory, which cannot explain the dependence of mechanical response on a specimen s size since there is no length scale in its constitutive description. A case study was performed using a cylindrical pillar to examine, on the one hand, accuracy of the proposed EMSGCP theory and, on the other hand, its universality for different pillar geometries. An extensive numerical study of the size effect in micron-size pillars was also implemented. On the other hand, an anisotropic character of surface topographies around indents along different crystallographic orientations of single crystals obtained in numerical simulations was compared to experimental findings. The size effect in nano-indentation was studied numerically. The differences in the observed hardness values for various indenter types were investigated using the developed EMSGCP theory.

Dans l’industrie, les traitements mécaniques de surface métalliques permettent d’améliorer les conditions de service des pièces mécaniques. Les effets de contact de ces types de procédés engendrent une forte déformation plastique du matériau et par conséquent une transformation microstructurale en sous-surface. Cette transformation se manifeste dans le raffinement progressif de la microstructure dans une couche de quelques dizaines de micromètres. Celle-ci est souvent dénommé "surface tribologiquement transformée" (en anglais : Tribologically Transformed Surface - TTS). Une telle transformation microstructurale conduit à une augmentation des propriétés mécaniques en extrême surface et rend le matériau plus résistant aux conditions de frottement, usure et fatigue.Dans le cadre de cette étude, deux procédures de transformation microstructurale ont été employées sur un matériau modèle : le fer-α. Pour la première technique (grenaillage), la surface est impactée de façon répétitive avec des billes métalliques projetées à grande vitesse. Concernant la deuxième méthode (micro-percussion), la surface est impactée répétitivement à un endroit précis avec un indenteur conique rigide.L’objet de ce projet se centre sur trois aspects principaux : (i) déterminer les gradients mécaniques et microstructuraux induits sur les deux types de surfaces transformées (grenaillage et micro-percussion), (ii) établir un lien quantitatif entre les mesures faites par deux types d’essais micromécaniques (nano-indentation et micro-compression de piliers) et (iii) mettre en évidence les effets microstructuraux impliqués (taille de grain, densité de dislocations, etc...) dans l’augmentation des propriétés mécaniques par hyper-déformation de surfaces. / The mechanical surface treatments confer better local mechanical properties against wear or fatigue service conditions. In the case of impact-based treatments, the material is exposed to repeated mechanical loadings, producing a severe plastic deformation in the near-surface. It leads to a local and progressive refinement of the microstructure into the affected zone, commonly known as Tribologically Transformed Surface (TTS). For this project, two mechanical surface treatments are used in a model material (pure α-iron): (i) shot-peening and (ii) micro-percussion.The resulting surfaces are characterized by a mechanical property gradient in-depth as a consequence of the microstructural transformation over a few tens of microns. Nowadays, it is well-known that this rise of local mechanical properties could improve the service lifetime of materials. However, a simple micro-hardness test is not quite enough to quantify precisely the engendered variation of mechanical properties and understand the influence of several microstructural effects. For this purpose, two micro-mechanical tests are considered: (i) nano-indentation and (ii) in situ micro-pillar compression.The main issue of this work is to characterize the mechanically-induced transformed surfaces and correlate the mechanical properties gradients with the local microstructural evolutions. Indeed, three main goals are considered: (i) quantify the mechanical and microstructural gradients induced by the surface treatments (shot-peening and micro-percussion), (ii) correlate the results obtained by the means of both mechanical tests (nano-indentation and micro-pillar compression) and finally (iii) investigate the influence of several microstructural effects related with the graded strengthening of hyper-deformed surfaces.

Fundamental understanding of high strain rate deformation behavior of materials is critical in designing new alloys for wide-ranging applications including military, automobile, spacecraft, and industrial applications. High entropy alloys, consisting of multiple elements in (near) equimolar proportions, represent a new paradigm in structural alloy design providing ample opportunity for achieving excellent performance in high strain rate applications by proper selection of constituent elements and/or thermomechanical processing. This dissertation is focused on fundamental understanding of high strain-rate deformation behavior of several high entropy alloy systems with widely varying microstructures. Ballistic impact testing of face centered cubic Al0.1CoCrFeNi high entropy alloy showed failure by ductile hole growth. The deformed microstructure showed extensive micro-banding and micro-twinning at low velocities while adiabatic shear bands and dynamic recrystallization were seen at higher velocities. The Al0.7CoCrFeNi and AlCoCrFeNi2.1 eutectic high entropy alloys, with BCC and FCC phases in lamellar morphology, showed failure by discing. A network of cracks coupled with small and inhomogeneous plastic deformation led to the brittle mode of failure in these eutectic alloys. Phase-specific mechanical behavior using small-scale techniques revealed higher strength and strain rate sensitivity for the B2 phase compared to the L12 phase. The interphase boundary demonstrated good stability without any cracks at high compressive strain rates. The Al0.3CoCrFeNi high entropy alloy with bimodal microstructure demonstrated an excellent combination of strength and ductility. Ballistic impact testing of Al0.3CoCrFeNi alloy showed failure by ductile hole growth and demonstrated superior performance compared to all the other high entropy alloy systems studied. The failure mechanism was dominated by micro-banding, micro-twining, and adiabatic shear localization. Comparison of all the high entropy alloy systems with currently used state-of-the-art rolled homogenous armor (RHA) steel showed a strong dependence of failure modes on microstructural features.