The stress corrosion cracking (SCC) condition for Alloy 600 was determined for various stress modes: constant-strain standard C-ring, and indentation, used to localize cracks for interrogation with x-ray techniques such as micro Laue diffraction (MLD). The SCC cracks nucleated on both the indentation edge, where finite element analysis showed that the maximum residual tensile stresses lie, and the surface in tension (bulge) on 150-kgf conically indented mill-annealed specimens (0.02 wt% C) in de-aerated solution of 10% caustic at 150 mVRE (pseudo-reference: A600), 315 OC for 48 hr. On the C-rings, the cracks nucleated at the lateral outer surface of apex, where maximum tensile stresses lie, in less than 12 hours, and propagated into the cross section. Also, corrosion tests on as-received A600 30-min ZrO2 surface mechanical attrition treated (SMAT) specimens suggested an intergranular attack type of behavior in 50% caustic at 210 mVRE (pseudo-reference: A600), 280°C for 24 hr.

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.

Multilayered iron electrodeposits composed of alternating layers of coarse-grained iron (grain size: 1.87 μm; (110) texture; hardness: 177 VHN) and fine-grained iron (grain size: 132 nm; (211) texture; hardness: 502 VHN), with layer thicknesses ranging from ~0.2-7 μm were successfully synthesized. The average hardness of the multilayered electrodeposits increased from 234 VHN to 408 VHN with decreasing layer thickness, consistent with a Hall-Petch type behaviour. In three-point bending tests, they failed in a macroscopically brittle manner although local ductility was observed in certain layers. Fractography analysis has shown that strain incompatibility between alternating layers contributes to the brittle nature of these materials. This study has demonstrated the possibility of applying a multilayered structure design to tailor the microstructure and mechanical properties of electrodeposited iron.

The grain-size dependences of thermal conductivity and electrical resistivity of polycrystalline and nanocrystalline nickel were measured by the flash method and four-point probe method, respectively. Nanocrystalline nickel was made by the pulsed-current electrodeposition process, while polycrystalline nickel was commercially available Ni 200 in annealed condition. The grain sizes of the materials examined ranged from 28 nanometers to 57 micrometers. Noticeable changes in thermal conductivity and electrical resistivity with grain size were observed in particular for samples with grain sizes less than 100 nm. These results can be explained on the basis of the rapid increase in the intercrystalline grain boundary and triple junction volume fractions at very small grain sizes. The relationship between thermal conductivity and electrical resistivity of nanocrystalline nickel follows the classic Wiedemann-Franz law.

This thesis describes the synthesis and assembly of metal and semiconductor nanoparticles (NPs). The two research topics include i) hetero-assembly of metal and semiconductor NPs, ii) effect of ionic strength on homo-assembly of gold nanorods (GNRs). First, we present hetero-assembly of GNRs and semiconductor quantum dots (QDs) in a chain using biotin-streptavidin interaction. We synthesized alloyed CdTeSe QDs and modified them with mercaptoundecanoic acid to render them water-soluble and to attach streptavidin. We synthesized GNRs by a seed-mediated method and selectively modified the ends with biotin. Hetero-assembly of QDs and GNRs depended on the size, ligands, and ratio of QDs and GNRs. Second, we controlled the rate of homo-assembly of GNRs by varying the ionic strength of the DMF/water solution. The solubility of polystyrene on the ends of GNRs depended on the ionic strength of the solution, which correlated with the rate of assembly of GNRs into chains.

Red mud is a waste product of alumina production and has an adverse effect on environment. About 90 million tonnes of red mud are produced annually throughout the world and little is recycled for useful applications. The world nickel reserves consist of approximately 30% sulphide ores and 70% oxide ores. Despite the relative abundance of oxide ores, 55% of nickel and nickel alloys produced today are derived from sulphide ores. However, with the production of nickel and its alloys from low-grade oxide ores becoming increasingly important, a major concern is high sulphur level in the resultant alloy. For this reason, desulphurization of the ferronickel becomes an important consideration. In the present study, experiments were conducted to determine if red mud could be used as a major ingredient of custom designed fluxes for the desulphurization of ferronickel alloy. Factors investigated included desulphurization rates, contact angle measurements and flux-refractory interactions.

The stress corrosion cracking (SCC) condition for Alloy 600 was determined for various stress modes: constant-strain standard C-ring, and indentation, used to localize cracks for interrogation with x-ray techniques such as micro Laue diffraction (MLD). The SCC cracks nucleated on both the indentation edge, where finite element analysis showed that the maximum residual tensile stresses lie, and the surface in tension (bulge) on 150-kgf conically indented mill-annealed specimens (0.02 wt% C) in de-aerated solution of 10% caustic at 150 mVRE (pseudo-reference: A600), 315 OC for 48 hr. On the C-rings, the cracks nucleated at the lateral outer surface of apex, where maximum tensile stresses lie, in less than 12 hours, and propagated into the cross section. Also, corrosion tests on as-received A600 30-min ZrO2 surface mechanical attrition treated (SMAT) specimens suggested an intergranular attack type of behavior in 50% caustic at 210 mVRE (pseudo-reference: A600), 280°C for 24 hr.

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.

Multilayered iron electrodeposits composed of alternating layers of coarse-grained iron (grain size: 1.87 μm; (110) texture; hardness: 177 VHN) and fine-grained iron (grain size: 132 nm; (211) texture; hardness: 502 VHN), with layer thicknesses ranging from ~0.2-7 μm were successfully synthesized. The average hardness of the multilayered electrodeposits increased from 234 VHN to 408 VHN with decreasing layer thickness, consistent with a Hall-Petch type behaviour. In three-point bending tests, they failed in a macroscopically brittle manner although local ductility was observed in certain layers. Fractography analysis has shown that strain incompatibility between alternating layers contributes to the brittle nature of these materials. This study has demonstrated the possibility of applying a multilayered structure design to tailor the microstructure and mechanical properties of electrodeposited iron.

The grain-size dependences of thermal conductivity and electrical resistivity of polycrystalline and nanocrystalline nickel were measured by the flash method and four-point probe method, respectively. Nanocrystalline nickel was made by the pulsed-current electrodeposition process, while polycrystalline nickel was commercially available Ni 200 in annealed condition. The grain sizes of the materials examined ranged from 28 nanometers to 57 micrometers. Noticeable changes in thermal conductivity and electrical resistivity with grain size were observed in particular for samples with grain sizes less than 100 nm. These results can be explained on the basis of the rapid increase in the intercrystalline grain boundary and triple junction volume fractions at very small grain sizes. The relationship between thermal conductivity and electrical resistivity of nanocrystalline nickel follows the classic Wiedemann-Franz law.