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A dissertation submitted to the Faculty of Engineering and the Built Environment, University of the Witwatersrand, in fulfilment of the requirements for the degree of Master of Science in Engineering 15 October 2016 / The alloys Ti-52.5Al-10.0Ni (at.%) and Ti-52.5Al-10.0Ni-0.2Ru (at.%) were made by mixing, and melting their powders in a button arc furnace under an argon atmosphere. The high temperature oxidation and room temperature corrosion of behaviour of the alloys was investigated. Isothermal oxidation in air at 950°C for 120 hours and 720 hours was done. Cyclic oxidation behaviour of the alloys was also investigated in air and in a hot salt (Na2SO4) environment. The corrosion tests were conducted in 5 wt% and 25 wt% HCl. All the samples were characterised using scanning electron microscopy with energy dispersive X-ray spectroscopy, X-ray diffraction and hardness measurements. On solidification, the Ti-52.5Al-10.0Ni (at.%) alloy formed dendrites of γ-TiAl (~55 at.% Al) surrounded by a eutectic of γ-TiAl + Ti2NiAl3 (τ3) phases. Most of the nickel was found in the Ti2NiAl3 (τ3) phase (~12 at.%) with trace amounts in the dendrites (~0.5 at.%). The Ti-52.5Al-10.0Ni-0.2Ru (at.%) alloy formed dendrites of γ-TiAl (~53 at.% Al) surrounded by a eutectic of γ-TiAl + Ti2NiAl3 (τ3). Most of the nickel (~15 at.%) and ruthenium (~0.3 at.%) were in solid solution in the Ti2NiAl3 (τ3) phase, although small amounts of both metals were present in the dendrites (~1 at.% Ni and 0.1 at.% Ru). Under isothermal oxidation conditions, both alloys showed good oxidation resistance with a low mass gain (< 2%). The alloys formed a continuous scale of TiO2 and Al2O3 with good adherence to the substrate, but as exposure time increased, the scale was severely degraded and exfoliated from the surface. Cyclic oxidation conditions were more aggressive for both alloys. The Ti-52.5Al-10.0Ni-0.2Ru (at.%) alloy was more resistant and formed a nickel-rich sub-surface zone between the substrate and intermixed oxide layer. Both alloys had a fairly good corrosion resistance in HCl due to the presence of nickel. They formed a thin and non-continuous Al2O3 oxide scale on the surface of the γ-TiAl dendrites, with Ti3NiAl2O on the γ-TiAl + Ti2NiAl3 (τ3) eutectic regions. The acid mainly corroded the τ3 phase, thus attacking the eutectic and leaving the γ-TiAl dendrites exposed. / MT2017

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M.S. / Materials Science and Engineering / The goal of this thesis is to determine the corrosion behavior of a new class of advanced materials, namely: titanium carbide reinforced iron composites containing chromium (Fe-Cr-TiC) and chromium and manganese (Fe-Cr-Mn-TiC). TiC has excellent physical properties, such as high melting point, low density, high Vickers hardness value, high electrical resistivity and low thermal expansion. Due to their great wear resistance characteristics and toughness, these materials show potential applications in pulp and paper industries, mining and mineral processing industries, metallurgical industries, cement industries, and electric industries. Some components made of these materials may work under a combined action of corrosion and wear. This study is aimed at determining the corrosion behavior using electrochemical methods such as potentiodynamic and potentiostatic. Two different electrolytes were used in this research: 1N (0.5 M) sulfuric acid (H2SO4) and 1N (0.5 M) sodium sulfate (Na2SO4). The experiments were performed on the following materials; Fe-TiC, Fe-Cr-TiC, Fe-Cr-Mn- TiC and their matrix materials.

Thesis (M.S.)--University of North Texas, Dec., 2009. / Title from title page display. Includes bibliographical references.

Organically modified sol-gel coatings have been investigated as potential replacements for chromate conversion coating of AA1050 and AA2024 aluminium alloys. The coatings were prepared by a combination of a completely hydrolysable precursor of tetra-n-propoxyzirconium (TPOZ), with a partially hydrolysable precursor of glycidoxypropyltrimethoxysilane (GPTMS). GPTMS contains organic functional groups, which are retained in the sol-gel coatings after the hydrolysis-condensation process. Different process parameters, e.g. GPTMS/TPOZ ratios, withdrawal speeds, solvent water concentrations, and curing temperatures were studied. Coatings produced using a low GPTMS/TPOZ ratio and a high withdrawal speed generated significant cracks due to the shrinkage of the coatings. It was found that increase of organic moieties reduced the shrinkage of the coatings and the tendency for crack formation. By controlling process parameters and ratios of organic and inorganic moieties, crack-free sol-gel coatings from 0.1 μm to 9 μm thick can be achieved. The sol-gel coatings formed are amorphous and contain organic epoxy-ether retained silicon oxide, silicon hydroxide, zirconium oxide, zirconium hydroxide, and zirconium acetate. The Si/Zr ratios of resultant sol-gel coatings are proportional to the initial GPTMS/TPOZ ratio. Cerium oxide nanoparticles were successfully incorporated into sol-gel coatings with a single layer and double layer sol-gel process. Through the dip coating process, crack-free sol-gel coatings, of varied thickness, were developed on different aluminium substrate, including electropolished superpure aluminium, magnetron sputtered aluminium with varied copper contents from 0 to 30 wt.%, and commercial AA1050 and 2024 aluminium alloys. Sol-gel coatings formed on commercial AA1050 and 2024 aluminium alloys revealed a significant passivation in 3.5 wt.% sodium chloride solution during anodic polarisation when the sol-gel coating is more than 1 µm thick and proper surface pretreatments of the alloys were used. Corrosion tests by immersion in 3.5 wt% sodium chloride solution and by salt spray in 5 wt.% sodium chloride solution revealed that sol-gel coatings successfully protected AA2024 aluminium alloy against the aggressive environment and have the potential to replace chromate containing coating systems.

A comparative study of the fatigue crack growth rate (FCGR) behaviour of five alloys in air and in aqueous environments has been performed. The alloys tested include: mild steel as a reference material, a corrosion resistant dual phase steel, 3CR12, a proprietary martensitic stainless steel, AISI 431, a newly developed 8% Cr martensitic steel, Alloy 825, and a newly developed corrosion-abrasion resistant metastable austenitic alloy, 1210. Tests were conducted in laboratory air, distilled water at rest potential, 500 ppm chloride solution at rest potential, 1000 ppm chloride solution at rest potential, and 1000 ppm chloride solution at -1200 m V see; solution temperatures were maintained at 25⁰ C. Crack growth rate tests were performed using sinusoidal loading at a load ratio R = 0.1, a frequency of 3Hz in the laboratory air, and a frequency of 1 Hz in the aqueous environments. At the completion of testing, fracture surfaces were studied using a scanning electron microscope. In air, the mild steel and 3CR12 display comparable rates of cracking and exhibit a greater resistance to fatigue crack propagation than the martensitic AISI 431 and Alloy 825; Alloy 825 shows the least resistance to fatigue crack propagation. The deformation induced transformation in 1210 gives this alloy the greatest resistance to fatigue crack propagation in air. Fatigue crack growth rates were all enhanced in the aqueous environments. The greatest overall rate of environmentally assisted cracking was shown by alloy 825 while the lowest was shown by the mild steel. Although the rate of cracking of 1210 in the aqueous environments was less than that of Alloy 825, 1210 was influenced the most by the aqueous environments. An environmentally assisted cracking index shows that the rate of fatigue crack propagation in 1210 is increased by 32 times in the 500 ppm chloride solution at low stress intensities. The fatigue crack growth rates of mild steel and AISI 431 were significantly influenced by the cathodically polarised conditions in the 1000 ppm chloride solution, compared to the rest potential conditions. In these cases hydrogen was seen to be evolved from the specimen surfaces. Changes in the fatigue crack growth rate behaviour were accompanied by changes in the fracture surface morphologies. The observed changes varied for each alloy and for each environment, and were manifest by the degree of intergranular cracking, cleavage, quasi cleavage, and increased coarseness of the transgranular cracking. The fracture surface morphologies are reported and discussed in detail. In general, the fracture surface morphologies could be directly related to the relative degrees of environmental influence on the rate of cracking; results are explained in terms of existing hypotheses. It is suggested that the environmentally assisted cracking of mild steel and AISI 431 at cathodic potentials in the 1000 ppm chloride solution could only be attributed to hydrogen assisted cracking. Similarly, it is suggested that the large crack growth rate acceleration of 1210 in the aqueous environments could also be attributed to hydrogen. The similar fracture surface morphologies observed on the other specimens after tests in the aqueous environments suggests-that hydrogen could be responsible for the environmentally assisted cracking of all the steels in aqueous environments.

Bibliography: pages 96-103. / The mechanisation of the working stapes in South African gold mines has required the introduction of a fundamentally new technology, hydro-power, in which machines are powered hydraulically using mine water fed from above ground. Mine water is aggressive and has a variable acidity and pH, and contains high concentrations of sulphate, chloride and nitrate ions. In order to minimise the pitting corrosion of piping and stoping machinery a compromise between selecting a suitable corrosion resistant material and treating the mine water to an acceptable level of corrosiveness is being sought.

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The current work is part of the EPSRC MUZIC project, which established the collaboration among several universities to carry out a multidiscipline study on the breakaway oxidation of zirconium alloys. The overall goal of the project is to further understand the mechanisms of the oxidation and breakaway process of zirconium alloys. This thesis describes the nano/micro-structural study and nano-analysis of the corroded zirconium alloys using up-to-date TEM and 3D focused ion beam (FIB) slicing and reconstruction techniques. The work mainly focused on the characterization of ZIRLO. The oxide morphology in general comprises an inner columnar layer and an outer equiaxed layer, except for a post-second transition oxide grown on a Zr-Nb-Ti test alloy with a very poor corrosion resistance, which exhibits generally only equiaxed grains throughout the whole oxide scale. Detailed investigation reveals oxides in a slower oxidation stage exhibit better developed columnar grain structure. All the oxides, independent of different corrosion stages and alloy types, contain predominantly monoclinic oxide and a small amount of tetragonal oxide. Defects at different length scales were examined. In stead of a sudden burst of crack nucleation at the kinetic transition, a gradual introduction of cracks parallel to the metal/oxide interface throughout the pre-transition stage is found, suggesting no direction correlation between the formation of cracks and the transition. Besides cracks, the oxide also contains different forms of nano-porosity: isolated pores of 1-3 nm or interconnected pores at grain boundaries. The density of interconnected porosity, especially those along the oxide growth direction, increases towards the oxide surface, evolving over time. It is suggested that the kinetic transition is related to the development of an interconnected porosity down to the metal/oxide interface, providing easy pathways for the transportation of oxidation species. The metal-oxide interface has a wavy morphology both in the micrometer and nanometer scale. The roughness develops to a maximum just before the first kinetic transition. An intermediate suboxide layer with complex 3D morphology between the bulk oxide and the metal substrate is found. Quantitative EELS analysis shows the composition of this layer to be 40-50 at. % oxygen. The suboxide appears to develop in thickness with increasing oxidation time for the pre-transition oxides, while is very thin or absent in the post-, and post-second transition oxides. In the suboxide region, multiple phases including &alpha;-Zr, &omega;-Zr, tetragonal oxide and a phase with an unidentified structure were found, suggesting different structures can coexist in the suboxide layer. Second-phase particles (SSPs) of &beta;-Nb and hexagonal Zr(Fe,Nb)₂ types were found in ZIRLO samples and FCC Zr(Fe,Cr)₂ was the predominant type in Zircaloy-4. The SPPs showed delayed oxidation compared to surrounding Zr. In ZIRLO, those containing high Fe contents were found to be oxidized and transform into an amorphous state much earlier than &beta;-Nb. Hydrides of different types (&gamma;, &sigma; and &epsilon;) were observed in the metal and metal/oxide region for both Zircaloy-4 and ZIRLO samples. A higher density of hydrides was seen in post-transition oxides of ZIRLO than in pre-transition oxides.