This thesis looks at the effect of micro segregation of Nb, generated from the continuous casting on grain structure development during reheating and deformation. The amount of segregated material present in the microstructure has been quantified in the as-cast condition and that has been used to model grain size distribution after reheating and deformation which is required for subsequent toughness prediction in 0.045 wt % Nb steel. The limits of validity of the original Dutta-Sellars model for predicting the amount of recrystallisation; investigating the influence of the variables such as starting grain size distribution, strain and Nb content has been examined. A modified Dutta-Sellars model considering the starting grain size distribution has been found to be more accurate in quantifying the amount of recrystallisation. This approach has been used to model grain size distribution after deformation both in the homogenised and in presence of Nb segregation. The effect of AlN, to replace Nb(C,N), on pinning the austenite grain boundaries during reheating has been investigated, as the segregation tendency of Al is much less compared with Nb.

The defect structure of single crystal tantalum with orientation 001, 011 and 111 after a 6 GPa shock loading with lateral and back release waves were characterised using scanning electron microscopy (SEM) and transmission electron microscopy. The SEM images were filtered using ImageJ script to determine the type and fraction of deformation twins. A methodology of imaging dislocations in the tantalum single crystals using electron channelling contrast was made with the assistance of the dislocation contrast profile simulation based on the dynamical theory of electron diffraction. The dislocation density distribution was measured using electron channelling contrast imaging (ECCI) technique. The nucleation and growth of the deformation twins are discussed with the aid of finite element simulation of the wave propagation in the material. The defect evolution and response of the single crystals are found to be highly dependent on the loading orientation of the shock wave. The effects of the lateral release wave and back release waves on the deformation mechanisms are also discussed.

In-situ TEM compression testing is able to probe quantitatively the mechanical response of materials with simultaneous imaging of the deformation microstructure evolution. Ti-6Al-4V (Ti64), known for high strength, is the most widely used Ti alloy. A better understanding of the plastic deformation micro-mechanisms is sought using in-situ TEM studies. This project investigates the dislocation characterization of bulk Ti64 and the dislocation activities in micro-pillars during in-situ TEM compression.

The purpose of this work was to determine the microstructure and secondary phase distribution in the TiB2 particulate reinforced Al-4.5Cu A205 alloy. This was extended to sand, investment and die casting techniques with the overall aim of optimising the existing solution heat treatment protocol for a variety of possible starting conditions. Additional work was aimed at determining a relationship between TiB2 additions and the observed globular microstructure. Hardness testing, DSC analysis, EDS and tensile testing were used to determine the effectiveness of heat treatment. It was found that a 4hr solution treatment at 538oC did not produce significantly different results from a 44hr, four step treatment process. As the diffusion behaviour of Cu was judged to be the most important factor affecting solution heat treatment, a simple microstructural model of typical A205 grain structures was proposed. The model was found to operate on similar timescales to those observed from experimental testing of A205 but was limited by idealised phase structures. The castability of A205 was determined using fluidity and hot tearing experiments. The better than expected castability was attributed to enhanced feeding brought about by the globular structure of A205.

A requirement for online monitoring has emerged owing to the susceptibility of fibre reinforced composite materials to sub-surface damage. Acoustic emission (AE) monitoring is understood to detect damage well before catastrophic failure; research in AE sensing therefore continues to attract significant attention. The research presented herein provides a review of a fibre-optic-based AE sensor design. Developmental work was performed to evaluate both sensor fabrication and packaging-related issues. The characteristics of the sensor were found to be influenced by: (i) the type of optical fibre used for fabrication; and (ii) preparation of optical fibres prior to sensor fabrication. The use of a small-diameter packaging substrate revealed improvements in sensor performance. The fibre-optic AE sensor was successfully embedded in a uni-directional composite laminate that was fabricated using autoclave processing. The embedded fibre-optic sensor was found to provide higher sensitivity to simulated AE compared with a surface-mounted sensor. Sensor characterisation trials were performed using simulated AE; a low directional sensitivity was observed. Modal analysis revealed a preferential sensitivity to the A0 wavemode; this sensor design may therefore be suited to the detection of delamination in FRCs. Finally, the sensor was shown to successfully detect interlaminar crack propagation under Mode-I loading.

This thesis describes hydrodynamic studies of the leach and solvent extraction stages of a Platinum Group Metal (PGM) hydrometallurgical flowsheet. The studies were motivated by the need to increase PGM throughput in Johnson Matthey’s PGM refining business. In the leach stage, key components in the feed are selectively dissolved using acids in a stirred tank before they are recovered by liquid-liquid (L-L) solvent extraction and finally purified. The work described in this thesis tackles four main areas: hydrodynamic studies of L-L PGM solvent extraction in both mixer and settler stages, whilst for the leach stage, studies of particle behaviour in gas evolving solid-liquid (S-L) reactions and gas-liquid-solid (GLS) characterisation by a novel Electrical Resistance Tomography (ERT) technique are performed. In the mixer-settler, the effects of impeller diameter, D, to vessel diameter, T, ratio (D/T), the phase flow ratio, cφ/dφ; (where cφis the continuous phase flow fraction and dφ is the dispersed phase flow fraction) and the specific power input,Tε, upon the droplet size distribution in a L-L system and their phase separation were investigated. Changing a smaller D/T impeller for a larger D/T impeller at constant P/V and cφ/dφincreased droplet size because the maximum shear rate decreased as a result of increasing ratio of impeller pumping capacity (Q) with tip speed (Utip). Changing a larger cφ/dφfor smaller cφ/dφat a fixed P/V and D/T impeller increased droplet size because turbulent dampening increased since the average density, ρ ∝ dφ. Meanwhile, Kolmogoroff-Hinze’s theory was shown to apply for the measured relationship between Tε and droplet size. A settler design criterion, which relates the dispersed phase concentration (Ca) in the dispersion band to the dispersed phase throughput (Qd/A) agreed with the model by Ryon et al. (1959). Ca was significantly dependent on P/V and Qd/A, whilst the effects of Qc/Qd (where Qc is the continuous phase flowrate and Qd is the dispersed phase flowrate) and D/T were minimal. Droplet size analysis of the sedimenting region of the dispersion band and dense packed layer revealed a transitional distribution of droplet sizes due to the counteracting effects of droplet sedimentation, hindered settling and droplet-droplet coalescence. Particle behaviour in gas evolving S-L systems were quantified using the Zwietering ‘just-suspended’ impeller speed (Njs) condition in a sponge nickel® and sodium hypochlorite system. The presence of gas caused Njs to increase, however a coherent relationship between Njs in an ungassed and gassed system 3 could not be easily ascertained. Further work with Positron Emission Particle Tracking (PEPT) was advised to quantify the relationship. A well-known electrical concept called skin effect, which describes how the effective resistance of an electrical conductor varies as the frequency of an alternating current (AC) increases and decreases, was used to investigate GLS behaviour via a novel ERT spectroscopic technique. The process relies on the change in effective resistance of conducting objects with changing AC frequency to selectively detect different phases. The concept was initially validated with static phantoms of a stainless steel and plume of gas before being applied to dispersible stainless steel particles and gas. ERT spectroscopy showed that two AC frequencies (0.3 kHz and 9.6 kHz) could successfully isolate and simultaneously detect the gas and solid phases at a fixed current. By subtracting solids and gas conductivity, the change in solids and gas holdup were obtained.

Due to high hydrogen capacity, good reversibility and low cost, magnesium hydride is one of the most promising hydrogen storage materials. However, the high desorption temperature and slow hydriding kinetics hinder the application of magnesium hydrides. To improve the hydrogen storage characteristics of magnesium hydrides, many effective treatments have been developed and applied, such as ball milling, melt spinning, alloying with other metals, adding catalysts and using thin film technique. In this work, melt spinning and alloying with Ni were the main sample modification methods used to improve hydrogen storage properties for magnesium hydrides. At the beginning of this project, it was found that it was difficult to repeat the methodology of sample preparation in the literature. Therefore, sample synthesis method was developed after numerous preliminary trials and a series of Mg-Ni alloys were melt-spun successfully. The structural characterization and analysis of hydrogen storage property were performed on the melt-spun Mg-Ni samples in a range of compositions. It was found that a nanocrystalline / amorphous structure was produced by melt spinning, and a metastable intermediate phase, Mg\(_6\)Ni, was discovered in the melt-spun materials. The melt-spun Mg-Ni ribbons exhibited fast kinetics of both absorption and desorption at 300 °C, with a high capacity. Moreover, they exhibited low temperature and even room temperature hydrogen sorption, with slow kinetics.\(\gamma\)-MgH\(_2\) phase, which forms usually under high pressure, has been found in the samples, which probably caused the ambient hydrogen absorption.

This work investigated the effect of transition metal additions on the double oxide film defects in Al alloys. A bubble trapping experiment was initially conducted, which deliberately trapped an air bubble inside the aluminium melt for a period of time in three different Al alloys (Commercial purity aluminium, 2L99(Al-7Si-0.35Mg) and Al-5Mg alloy), as an analogy of the consumption of the entrapped atmosphere in double oxide film defects in castings. Several elements, namely, Mo, Ti, Zr, Hf, Sc were selected and added into the aluminium melt. The result suggested that the three different alloys behaved differently with regard to the consumption of the entrapped bubble and the different oxide/nitride layers formed. Only the addition of Sc and Mo altered the structure of the oxide surface and promoted the consumption of the air in the trapped bubble in the 2L99 aluminium alloy melt. Sand casting was subsequently conducted for 2L99 alloy with different element additions. Mo and W were found to improve the Weibull moduli of the UTS. Statistical analysis confirmed that such improvement was significant. For the castings with Mo addition, a nitride was found in some double oxide film defects, on the fracture surface of the tensile testbars. This was unusual, as bi-film defects in aluminium castings usually have a short solidification time and do not have enough time to consume the majority of their entrapped oxygen. The formation of the nitride on the surface of bi-film defects in +Mo castings, suggested that the majority of the oxygen was depleted and a reaction was going on between nitrogen and liquid aluminium. The formation of the permeable nitride surface layer on the bifilm defect might promote the consumption of the entrapped gas. This should lead to reductions in the bi-film size and an improvement in mechanical properties. For +W casting, W containing intermetallic compound might be nucleated on the sides of the bifilm and drag the bi-film to the bottom of the casting, resulting in a clean melt and improving mechanical properties. The effect of Si modifier addition on the bi-film defect (Na, Sr and Ba) in 2L99 sand castings was also investigated, which suggested the addition of modifiers resulted in a reduction in the mechanical properties of the 2L99 castings while the bi-film defect content in the casting was high but significantly improved the Weibull moduli of the UTS of 2L99 castings while the bi-film defect content was reduced. The results suggested that the modifier addition tended to aggravate the effect of bi-film defects on mechanical properties by increasing the defect size. Ti and Mn additions into 2L99 alloy were found to not significantly affect the mechanical properties of the casting. A porous oxide structure was found on only one of the fracture surfaces (out of ten) of Ti containing testbar examined, which hardly affect the mechanical properties of the casting. For the +Mn casting, the composition and structure of the oxide was not affected by the addition. The reduction of the mean value of the UTS for both element additions could be due to bi-film defects being introduced during master alloy preparation, master alloy addition and during degassing before casting.

Synthetic hydroxyapatite (HA) has been widely used for biomedical applications, in particular as a bone substitute and coating for implants, due to its similarity to the inorganic component of human bone. The aim of this study was to incorporate three divalent cations (silver, zinc and magnesium) into the hydroxyapatite structure via a wet chemical precipitation method to enhance its antibacterial properties, to avoid the need for the use of antibiotics. Material characterisation techniques such as XRD and Raman Spectroscopy confirmed that these ions were substituted within the crystal structure of HA, though did not follow the expected reaction stoichiometry and substitution ratios. HA material properties, such as crystal size, crystallinity and solubility were shown to change after ion substitution. Metal-substituted HA showed varying strengths of antibacterial properties against two bacterial strains of \(E\).\(coli\) and \(S\).\(epidermidis\), which was attributed to different type of ions and substitution ratios and also different release profiles from the solid phase to the culture medium. The results from cell biological studies confirmed that the rate of osteoblast cell proliferation and cell differentiation were improved after cells being incubated with disks of substituted HA.

Grain size refinement can be achieved by recrystallisation during hot deformation, with multiple deformation steps during rolling or forging being used to generate fine grain sizes. Whilst the mode (or average) grain size after recrystallisation can be determined from standard equations the full grain size distribution is required for predicting a range of mechanical properties. In this work an approach has been proposed to allow prediction of the full grain size distribution by varying the value of the D’ parameter value in the Dutta - Sellars equation developed to predict the recrystallised mode/average grain sizes. It has been found that D’ is a function of strain at high strain values (above 0.3) and the relative position of the grain size in the grain size range (D*). Results for recrystallised grain size distributions for a range of steel grades (including model Fe - Ni steels, commercial Nb-microalloyed plate and high alloy (9Cr) forging steel) with different initial grain sizes and following deformation to different deformation strains, show that the predictions give good agreement with the experimental data except for samples with larger mode grain sizes deformed to a strain of 0.15.