Nanostructured materials provide new and exciting approaches to the development of supercapacitor electrodes for high-performance electrochemical energy storage applications. One of the biggest challenges in materials science and engineering, however, is to prepare the nanomaterials with desirable characteristics and to engineer the structures in proper ways. This dissertation presents the successful preparation and application of very promising materials in the area of supercapacitor energy storage, including manganese dioxide and its composites, polyaniline and activated carbons. Attention has been paid to understanding their growth process and performance in supercapacitor devices. The morphological and electrochemical cycling effects, which contribute to the understanding of the energy storage mechanism of MnO2 based supercapacitors is thoroughly investigated. In addition, MnO2 based binary (MnO2-carbon nanocoils, MnO2-graphene) and ternary (MnO2-carbon nanotube-graphene) nanocomposites, as well as two novel electrodes (MnO2-carbon nanotube-textile and MnO2-carbon nanotube-sponge) have been studied as supercapacitor electrode materials, showing much improved electrochemical storage performance with good energy and power densities. Furthermore, a general chemical route was introduced to synthesize different conducting polymers and activated carbons by taking the MnO2 nanostructures as reactive templates. The electrochemical behaviors of the polyaniline and activated nanocarbon supercapacitors demonstrate the morphology-dependent enhancement of capacitance. Excellent energy and power densities were obtained from the template-derived polyaniline and activated carbon based supercapacitors, indicating the success of our proposed chemical route toward the preparation of high performance supercapacitor materials. The work discussed in this dissertation conclusively showed the significance of the preparation of desirable nanomaterials and the design of effective nanostructured electrodes for supercapacitor energy storage applications.

The diploma thesis deals with the study of the process of grinding aggregates of particles of a mixture of powdered lanthanide oxides in the dowanol solvent. The formed dispersions were characterised and used for the preparation of printing inks and subsequently for the printing of labels with chemical codes readable by XRF spectrometry. The aim was to study the milling process, to verify the reliability of reading and recognition of marks with the appropriate codes and to monitor the influence of the additive of the up-conversion powder on the resulting relative intensities of the elements in the chemical code. The statistical significance of the differences in the averages of relative intensities was assessed based on the Student's t test.

A research report submitted in fulfilment of the requirements for the degree of Master of Science in Engineering (50/50) to the Faculty of Engineering and the Built Environment, University of the Witwatersrand, Johannesburg, 2018 / Metal dusting (MD) is a severe form of corrosion in which iron, steels, and nickel (Ni) and cobalt (Co) based alloys disintegrate into a metal or carbide powder with a coke deposit when exposed to strongly carburising gases (carbon activity, ac>1) at elevated temperatures (400800°C). Temperature affects both the driving force and rate of the reaction, represented by gas phase supersaturation with carbon, and the rates of the various processes involved in converting that energy difference into the dusting process. Therefore, process streams such as reformer gas can be benign when hot, but becomes aggressive below critical temperatures. There are different views in literature about the effect of temperature on metal dusting of different materials and alloys. Alloy 800 experiences metal dusting (MD) at 525°C, which is the temperature of the tube sheet of reformers in petrochemical industry. This alloy is specifically used for tube ferrules in the reformers. The reformer trains can reach a critical (highest) internal temperature of 650°C. Therefore, these two temperatures were compared. The effect of temperature and exposure time on the metal dusting of Alloy 800 were investigated in terms of the form of attack and the degradation mechanism. From the results obtained, it was observed that the longer exposure periods result in more carbon deposition and the carbon filaments in the coke become finer as compared to the nanotubes obtained after shorter exposure periods. The alloy suffered metal dusting attack after a relatively short exposure period of three days (72 hours) at both temperatures of 525°C and 650°C, with very little coking. / TL2019

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Iron oxyhydroxides are ubiquitous in surface environments, playing a key role in many biogeochemical processes. Their characterization is made challenging by their nanophase nature. Magnetometry serves as a sensitive non-destructive characterization technique that can elucidate intrinsic physical properties, taking advantage of the superparamagnetic behaviour that nanoparticles may exhibit. In this work, synthetic analogues of common iron oxyhydroxide minerals (ferrihydrite, goethite, lepidocrocite, schwertmannite and akaganéite) are characterized using DC and AC magnetometry (cryogenic, room temperature), along with complementary analyses from Mössbauer spectroscopy (cryogenic, room temperature), powder X-ray diffraction and scanning electron microscopy. It was found that all of the iron oxyhydroxide mineral nanoparticles, including lepidocrocite, schwertmannite and akaganéite were superparamagnetic and therefore magnetically ordered at room temperature. Previous estimates of Néel temperatures for these three minerals are relatively low and are understood as misinterpreted magnetic blocking temperatures. This has important implications in environmental geoscience due to this mineral group’s potential as magnetic remanence carriers. Analysis of the data enabled the extraction of the intrinsic physical parameters of the nanoparticles, including magnetic sizes. The study also showed the possible effect on these parameters of crystal-chemical variations, due to elemental structural incorporation, providing a nanoscale mineralogical characterization of these iron oxyhydroxides. The analysis of the intrinsic parameters showed that all of the iron oxyhydroxide mineral nanoparticles considered here have a common magnetic moment formation mechanism associated with a random spatial distribution of iv uncompensated magnetic spins, and with different degrees of structural disorder and compositional stoichiometry variability, which give rise to relatively large intrinsic magnetization values. The elucidation of the magnetic nanostructure also contributes to the study of the surface region of the nanoparticles, which affects the particles’ reactivity in the environment.

<p> The partitioning of niobium to slag and gaseous niobium oxide vapourizing from metal/slag may cause niobium losses and erratic recovery rates in steelmaking practices. Knowledge of the volatility and activities of niobium oxides in slag melts are of great value for both theoretical evaluation and practical applications in niobium microalloyed steels. Because of the multi-valence state of niobium ions in slags, the behaviour of niobium in metallurgical slags is complicated. So far, little systematic attempts have been made and activity data of niobium oxides in slags are extremely scarce. The aim of this study is to determine precise data on the vapour pressures of niobium oxides, and consequently, to obtain information on thermodynamic quantities of niobium oxides in slag melts.</p> <p> The thermodynamic properties of niobium oxide in CaO-SiO2-NbOx and CaOSiO2-Al2O3-NbOx slag melts were determined by employing the transpiration method from 1800-1873K under a controlled atmosphere. To confirm the validity of the transpiration method for the measurement of thermodynamic properties, the binary alloy system silver-gold was chosen for a comparison with the same property which has been measured by other recognized procedures. The agreement with literature results confirmed that the measurement yields reliable results for thermodynamic activity data by the transpiration method.</p> <p> The vapourization of liquid Nb2O5 was studied as a function of partial pressure of oxygen in the system and this confirms that atmosphere control is the essential condition for the vapourization study. The gaseous niobium oxide species was verified to be NbO2; hence, Nb2O5 vapourizes by the reaction Nb2O5(1) = 2NbO2(g)+1/2O2(g). Heat of vapourization was estimated by applying the second law method and comparison with the literature showed a fairly good agreement.</p> <p> The thermodynamic properties of niobium oxide in the slag system of CaO-SiO2-NbOx and CaO-SiO2-Al2O3-NbOx were measured by varying the experimental conditions of slag basicities, slag compositions, temperature and oxygen partial pressures. From the basicity dependency of the activity coefficient for each oxide in this study, it is proposed that niobium oxide behaves as an amphoteric oxide and niobium pentoxide as an acidic oxide. On the other hand, it was observed in the redox equilibrium experiment that NbO2.5 becomes predominant as the slag basicity increases. However, insufficient interaction parameters as well as parameter conversions prevent the application of the regular solution model. The co-relationship between the ionic diameter and ionic energy was discovered and shows good agreement with calcium oxide and silicon oxide. With the interaction parameter and converting parameter attained, the regular solution model shows good agreement for the activity coefficients between measurement and calculation.</p> / Thesis / Doctor of Philosophy (PhD)

<p> The crystal structures of five ternary oxides and fluorides have been determined. It is shown that the gross features of these structures and the coordination of the atoms can be described in terms of the theory of close-packing of spheres. However, in each of the structures there appear cations whose coordination cannot be uniquely predicted, as the cation-anion radius ratios are close to the critical value for transition from one coordination to another.</p> / Thesis / Doctor of Philosophy (PhD)

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