Nano-grained nickel produced by electroforming technique was investigated for its microstructure evolution and mechanical properties upon annealing. It was found that during low temperature annealing (T<250 oC), electroformed nano-grained nickel showed scattered and isolated abnormal grain growth, followed by a major abnormal grain growth at 320 oC. A secondary abnormal grain growth, featuring faceted grain boundaries, was observed at a higher annealing temperature (T=528 oC). A semi-in-situ observation using optical microscopy was conducted to track the movement of the faceted grain boundaries, and it was found that these boundaries were mostly immobile. The mechanical properties under various annealing conditions were studies using hardness and tensile testing. The hardness was observed to decrease with increasing annealing temperature. The material became very brittle after annealing at 320 oC or higher temperatures. Fractography investigation showed that the brittleness is caused by intergranular fracture.

Nano-grained nickel produced by electroforming technique was investigated for its microstructure evolution and mechanical properties upon annealing. It was found that during low temperature annealing (T<250 oC), electroformed nano-grained nickel showed scattered and isolated abnormal grain growth, followed by a major abnormal grain growth at 320 oC. A secondary abnormal grain growth, featuring faceted grain boundaries, was observed at a higher annealing temperature (T=528 oC). A semi-in-situ observation using optical microscopy was conducted to track the movement of the faceted grain boundaries, and it was found that these boundaries were mostly immobile. The mechanical properties under various annealing conditions were studies using hardness and tensile testing. The hardness was observed to decrease with increasing annealing temperature. The material became very brittle after annealing at 320 oC or higher temperatures. Fractography investigation showed that the brittleness is caused by intergranular fracture.

Commercially available polycrystalline Ni (Ni200; grain size: 32 μm) and electrodeposited nanocrystalline Ni (grain size: 57 nm), Ni-2.6%Fe (grain size: 25 nm) and Ni-8.5%Fe (grain size: 20 nm) were analyzed for the phenomena of stress-induced heat generation and strain localization during plastic deformation at room temperature (i.e. 250C). Tensile specimens according to ASTM E8 standard dimensions were tested at strain rates of 10-2/s and 10-1/s, respectively, to record the amount of heat dissipated and the change of localized strain using a high resolution infrared (IR) detector and digital image correlation (DIC) camera, respectively. Results have shown that the maximum temperatures that were recorded in nanocrystalline Ni and Ni-Fe alloys were at least 300C lower than the onset temperatures for subgrain coalescence previously measured through differential scanning calorimetry. It can be concluded that thermally activated grain growth during tensile testing of nanocrystalline Ni and Ni-Fe alloys is not likely to occur.

Commercially available polycrystalline Ni (Ni200; grain size: 32 μm) and electrodeposited nanocrystalline Ni (grain size: 57 nm), Ni-2.6%Fe (grain size: 25 nm) and Ni-8.5%Fe (grain size: 20 nm) were analyzed for the phenomena of stress-induced heat generation and strain localization during plastic deformation at room temperature (i.e. 250C). Tensile specimens according to ASTM E8 standard dimensions were tested at strain rates of 10-2/s and 10-1/s, respectively, to record the amount of heat dissipated and the change of localized strain using a high resolution infrared (IR) detector and digital image correlation (DIC) camera, respectively. Results have shown that the maximum temperatures that were recorded in nanocrystalline Ni and Ni-Fe alloys were at least 300C lower than the onset temperatures for subgrain coalescence previously measured through differential scanning calorimetry. It can be concluded that thermally activated grain growth during tensile testing of nanocrystalline Ni and Ni-Fe alloys is not likely to occur.

With the recent development of in situ transmission electron microscopy (TEM) characterization techniques, the real time study of property-structure correlations in nanomaterials becomes possible. This dissertation reports the direct observations of deformation behavior of Al2O3-ZrO2-MgAl2O4 (AZM) bulk ceramic nanocomposites, strengthening mechanism of twins in YBa2Cu3O7-x (YBCO) thin film, work hardening event in nanocrystalline nickel and deformation of 2wt% Al doped ZnO (AZO) thin film with nanorod structures using the in situ TEM nanoindentation tool. The combined in situ movies with quantitative loading-unloading curves reveal the deformation mechanism of the above nanomaterial systems. At room temperature, in situ dynamic deformation studies show that the AZM nanocomposites undergo the deformation mainly through the grain-boundary sliding and rotation of small grains, i.e., ZrO2 grains, and some of the large grains, i.e., MgAl2O4 grains. We observed both plastic and elastic deformations in different sample regions in these multi-phase ceramic nanocomposites at room temperature. Both ex situ (conventional) and in situ nanoindentation were conducted to reveal the deformation of YBCO films from the directions perpendicular and parallel to the twin interfaces. Hardness measured perpendicular to twin interfaces is ~50% and 40% higher than that measured parallel to twin interfaces, by ex situ and in situ, respectively. By using an in situ nanoindentation tool inside TEM, dynamic work hardening event in nanocrystalline nickel was directly observed. During stain hardening stage, abundant Lomer-Cottrell (L-C) locks formed both within nanograins and against twin boundaries. Two major mechanisms were identified during interactions between L-C locks and twin boundaries. Quantitative nanoindentation experiments recorded during in situ experiments show an increase of yield strength from 1.64 to 2.29 GPa during multiple loading-unloading cycles. In situ TEM nanoindentation has been conducted to explore the size dependent deformation behavior of two different types (type I: ~ 0.51 of width/length ratio and type II: ~ 088 ratio) of AZO nanorods. During the indentation on type I nanord structure, annihilation of defects has been observed which is caused by limitation of the defect activities by relatively small size of the width. On the other hand, type II nanorod shows dislocation activities which enhanced the grain rotation under the external force applied on more isotropic direction through type II nanorod.

Plastic deformation of metals and alloys are invariably accompanied by the development of texture. The origin of texture is attributed to the deformation micro-mechanisms associated with processing. The face-centered cubic (FCC) metals and alloys are known to exhibit two distinct types of textures when subjected to large strain rolling deformation, namely, (i) Cu-type texture, commonly seen in high/medium stacking fault energy (SFE) materials, (ii) Bs-type texture in low SFE materials. The circumstances that could result in the formation of Bs-type texture in low SFE materials still remains an open question and no definite mechanism has been uniquely agreed upon. Apart from the SFE, grain size could also influence the deformation mechanism and hence the deformation texture. It is well known that in materials with grain sizes less than 100 nm (referred to as nano-crystalline materials), the microstructures contain large fraction of grain boundaries. This subsequently introduces a variety of deformation mechanisms in the microstructure involving grain boundary-mediated processes such as grain boundary sliding and grain rotation, in addition to slip and twinning. A clear understanding of texture evolution in nano-crystalline materials, particularly at large strains, is a topic that remains largely unexplored. The present work is an attempt to address the aforementioned issues pertaining to the evolution of deformation texture, namely, (i) the effect of SFE and (ii) the effect of grain size, in FCC metals and alloys. Nickel-cobalt alloys are chosen as the model system for the present investigation. The addition of cobalt to nickel leads to a systematic reduction of SFE as a function of cobalt content. In this thesis, three alloys of Ni-Co system have been considered, namely, nickel – 20 wt.% cobalt, nickel – 40 wt.% cobalt and nickel – 60 wt.% cobalt. For a comparison, pure nickel has also been subjected to similar study. Chapter 1 of the thesis presents a detailed survey of literature pertaining to the evolution of rolling textures in FCC metals and alloys, and chapter 2 includes the details of the experimental techniques and characterization procedures, which are commonly employed for the entire work. Chapter 3 addresses the effect of stacking fault energy on the evolution of rolling texture. The materials subjected to study in this chapter are microcrystalline Ni-Co alloys. The texture evolution in Ni-20Co is very similar to pure Ni, and a characteristic Cu-type rolling texture is observed. The evolution of texture in these materials is primarily attributed to the intense dislocation activity throughout the deformation stages. In Ni-40Co, a medium SFE material, the rolling texture was predominantly Cu-type up to a strain of ε = 3 (95% thickness reduction). However, beyond this strain level, namely at ε = 4 (98%), the texture gets transformed to Bs-type with orientations maxima predominantly close to Goss ({110} <001>) position. Simultaneously, the Cu component which was dominant until 95% reduction has completely disappeared. The analysis of microstructures indicate that deformation is mostly accommodated by dislocation slip up to 95%, however, at ε > 3, Cu-type shear bands get initiated, preferably in the Cu-oriented ({112} <111>) grains. The sub-grains within the shear bands show preferred orientation towards Goss, which indicates that the Cu component should have undergone transformation and resulted in high fraction of Goss component. In Ni-60Co alloy, Bs-type texture forms in the early stages of deformation (ε ~ 0.5) itself and further deformation results in strengthening of the texture with an important difference that the maximum in orientation distribution has been observed at a location close to Goss component, rather than at exact Bs-location. The development of Bs-type texture is accompanied by the complete absence of Cu and S components. Extensive EBSD analyses show that the deformation twinning gets initiated beyond 10% reduction and was found extensively in most of the grains up to 50% reduction. At higher strains, tendency for twinning ceases and extensive shear banding is observed. A non-random distribution of orientations close to Goss orientation was found within the shear bands. The near-Goss component in the Ni-60Co alloy can be explained on the basis of deformation twinning and shear banding. Thus, a reasonable understanding of the deformation texture transition in the extreme SFE range has been developed. In chapter 4, the effect of fine grain size on the evolution of rolling texture has been addressed. Nanocrystalline (nc) nickel-cobalt alloys with a mean grain size of ~20 nm have been prepared by pulse electro-deposition method. For a comparison, nc Nickel (without cobalt) with similar grain size has also been deposited. For all the materials, a weakening of the initial fiber texture is observed in the early stage of room temperature rolling (ε ~ 0.22). A combination of equiaxed grain microstructure and texture weakening suggests grain boundary sliding as an operative mechanism in the early stage of rolling. At large strain (ε = 1.2), Ni-20Co develops a Cu-type texture with high fractions of S and Cu components, similar to pure Ni. The texture evolution in Ni-40Co and Ni-60Co alloys is more towards Bs-type. However, the texture maximum occurs at a location 10° away from the Goss. The evolution of Cu and S components in nc Ni-60Co alloy takes place simultaneously along with the α-fiber components during rolling. Microstructural investigation by TEM indicates deformation twinning to be more active in all the materials up to 40% reduction. However, no correlation could be drawn between the texture evolution and the density of twins. The deformation of nc Ni-20Co alloy, is also accompanied by significant grain growth at all the stages of rolling. The increase in grain size, subsequently, renders the texture to be of Cu-type. However, Ni-40Co and Ni-60Co alloys show high grain stability. The absence of strain heterogeneities such as shear bands, and the lack of significant fraction of deformation twins indicate that the observed Bs-type texture could be due to planar slip. The increase in deformation beyond 70% reduction caused a modest reduction in the intensity of deformation texture. The microstructural observation indicates the occurrence of restoration mechanisms such as recovery/ recrystallization at large strains. The overall findings of the investigation have been summarized in chapter 5. The deformation mechanism maps relating stacking fault energy with amount of strain and with grain size are proposed for micro- and nano- crystalline materials respectively.