SiGe 25% substrates were treated with aqueous solutions of ammonium sulfide with and without added acid to understand the adsorption of sulfur on the surface. X-ray photoelectron spectroscopy showed no sulfide layer was deposited from aqueous (NH4)(2)S alone and instead both Si and Ge oxides formed during immersion in the sulfur solution. The addition of hydrofluoric and hydrochloric acids dropped the pH from 10 to 8 and deposited sulfides, yet increased the oxide coverage on the surface and preferentially formed Ge oxides. The sulfur coverage grew with increasing concentrations of acid in the aqueous (NH4)(2)S. The simultaneous deposition of O and S is suspected to be the result of oxidized sulfur species in solution. Metal-insulator-semiconductor capacitor (MISCAP) devices were fabricated to test the electrical consequences of aqueous ammonium sulfide wet chemistries on SiGe. MISCAPs treated with acidic ammonium sulfide solutions contained fewer interface defects in the valence band region. The defect density (D-it) was on the order of 10(+12) cm(-2) eV(-1). The flat band voltage shift was lower after the acidic ammonium sulfide treatment, despite the presence of surface oxides. Adsorption of S and potentially O improved the stability of the surface and made it less electrically active. (C) 2017 American Vacuum Society.

The results of three very different studies are presented. X-ray diffraction has been utilized for single-crystal structure determinations, fiber diffraction analyses, and in conjunction with molecular modeling of Cellulose IIII. Although each technique is different in its sampling, data acquisition, data treatment, and identification, the common denominator has been the use of x-rays. The single-crystal structure determination of ethylene glycol bis(tropane-3-carboxylate) is presented as an example of the use of modern single-crystal x-ray instrumentation including the use of coupled charged devices (CCDs) as detectors for accurate data collection and rapid elucidation of crystal structures. The structure determination of Cellulose IIII by x-ray diffraction and computer modeling is presented to show how the use of x-rays in weakly diffracting materials can generate a reliable structure and be a key component in model building. Finally, a study is presented in which x-ray fiber diffraction data is utilized to investigate possible correlations between the crystallite orientation, crystallinity, crystallize size and the strength properties of cotton fibers collected from various countries.

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The practice of using X-Ray fluorescence analysis as a method in ar-chaeological, forensic and osteological studies have resulted in a vast amount of data. It is time and cost efficient, and the method of µXRF element analysis has been of great use to archaeologists, forensic an-thropologists and osteologists to understand dietary customs, techno-logical trade patterns, understanding of diagenesis, elemental accumu-lation in bone and more. Moreover, the method has been crucial due to its non-destructive nature since bones and ancient artifacts are fragile and thus a nonde-structive method is preferable. This essay will give the reader an intro-duction to the basics of micro X-Ray fluorescence analysis and will explore the possibilities of trace elements in right (dexter) and left (sinister) thighbones (femur) on a medieval population in Visby Got-land, namely Sankt Hans. The reader will also come to know the fun-damental principles, applications, strengths and weaknesses of mi-croX-Ray fluorescence, as well as its limitations. Keywords: µXRF, non-destructive, data, method, left, right, thigh-bone, elements, analysis.

Abstract Layered inorganic-organic hybrid compounds have been widely studied as new potential sources of semiconductors and other optical devices. They simulate natural quantum well materials, where the inorganic part acts as semiconductors, separated by an organic part. This class of hybrid materials has no covalent bonds between the inorganic and organic parts; instead, weak hydrogen bonds and van der Waals forces bind and stabilise the overall structure. The inorganic part is made up of layers of corner-sharing metal halide octahedra, MX6, where the metal must be in a divalent state and the halides are Cl, Br or I. The 2-D layers extend infinitely in two directions and are separated themselves by layers of primary ammonium cations, with only one ammonium group at one end of the chain, [(R-NH3)2MX4], or two ammonium groups at either of the chain, [(H3N-R-NH3)MX4]. Due to its similarity to the cubic perovskite structure, this inorganic motif is referred to as "layered perovskite-type". Depending on the choice of the organic ammonium cation, the materials can display phase transitions and / or have optical and electronic properties. Various investigations of inorganic-organic hybrids have concentrated on the phase transitions of the hybrids of general formula [(CnH2n+1NH3)2MX4] and [(NH3CnH2nNH3)MX4] (n = 1-18; X = Cl, Br, I; M = Cu2+, Mn2+, Cd2+) to elucidate their mechanism. There are two types of displasive transitions, a minor one were small conformational changes within the alkylammonium chain occurs, and a major one, when the entire alkylammonium chain becomes disordered along its long axis. The interlayer spacing between the inorganic layers increases with temperature and during the major phase transition. The methods used to identify the temperatures and the enthalpies of the phase transitions are Differential Scanning Calorimetry (DSC); and Single Crystal X-ray Diffraction (SC-XRD) as well as Powder X-Ray Diffraction (P-XRD) to follow the structural changes. In contrast, only a few reports on investigations of the lead iodide hybrids, [(CnH2n+1NH3)2PbI4] were found in the literature, with only two single crystal structures previously reported. Due to the difficulty in growing good quality crystals, the previous studies on the lead iodide hybrids have been only researched using DSC and P-XRD. The phase transition behaviour has been found to show the same trends as the previous hybrids. The primary aim of this study was to follow the same phase transitions via SC-XRD, ideally single-crystal to single-crystal, and to determine the detailed structural changes with the hopes of elucidating their detailed phase transition mechanism. A secondary aim was to synthesize as many inorganic-organic hybrids as possible using a variety of primary ammonium cations to find different inorganic motifs apart from the layered perovskite-type. Other inorganic motifs can have purely corner-, edge or face-sharing octahedra or combinations thereof to give 2-D net-type networks or 1-D extended chains. The effect that the identity of the ammonium cation has on the type of inorganic motif and the effect on the detailed structural geometry within the inorganic motif are investigated. Examples of structural geometries within the layered perovskite-type inorganic motif that can differ from compound to compound are the relative positions of the inorganic and organic moieties; the N---H….X hydrogen bonding geometry between the halides and the ammonium group; and the relative positions of successive inorganic layers.

M.Med. (Radiology), Faculty of Health Sciences, University of the Witwatersrand, 2011 / Lymphobronchial tuberculosis (LBTB) is tuberculous lymphadenopathy involving the airways, which is particularly common in children. AIM: To describe the CT findings of LBTB in children, the parenchymal complications and associated abnormalities. METHOD: CT scans of 98 children with LBTB were retrospectively reviewed. Lymphadenopathy, bronchial narrowing, parenchymal complications and associations were documented. RESULTS: Infants comprised 51% of patients. The commonest lymphadenopathy was subcarinal (97% of patients). Bronchial compressions (259 in total) were present in all patients, of which 23% were severe / complete stenoses and 28% affected bronchus intermedius. Parenchymal complications were present in 94% of patients, including consolidation (88%), breakdown (42%), air trapping (38%), expansile pneumonia (28%), collapse (17%) and bronchiectasis (9%), all predominantly right-sided (63%). Associations included oval focal bodies, miliary nodules, pleural disease and intracavitory bodies. CONCLUSIONS: The most important CT finding of children with LBTB is visible airway compression as a result of lymphadenopathy. CT of children with LBTB showed that airway compressions were more severe in infants and most commonly involved bronchus intermedius. Numerous parenchymal complications were documented, all showing rightsided predominance. Several associations were identified.

PhD, Faculty of Engineering and the Built Environment, University of the Witwatersrand, 2010 / Dual Energy X-Ray Transmission (DE-XRT) Imaging is a multi-sensor technique employed to conduct particle-by-particle sorting. The system makes use of a dual energy x-ray line scan sensor, which generates images of the transmitted x-rays, similar to images generated for suitcase inspection in airport security applications. The dual energy x-ray system allows for rapid approximation of atomic number range, which is utilised to evaluate the mineral and maceral content of a variety of minerals, including coal. The process is independent of particle surface condition, and can thus be utilised as a dry process. A unique application of this technology is in the removal of torbanite from a coal deposit located in Mpumalanga, South Africa. The separation of coal from torbanite has been a problem for the coal industry for a long time. The separation of coal and torbanite by conventional gravity separation techniques is difficult, due to the overlapping densities of torbanite and coal. The commercial value of both commodities is significantly compromised if contaminated with the other, thus impacting negatively on the financial viability of mining such a deposit. Preliminary laboratory DE-XRT testwork results on high quality coal and torbanite products were promising. In order to evaluate the separation of typical Run of Mine (ROM) material on pilot scale, a production scale Mikrosort X-Tract Sorter was purchased. This was the first DE-XRT sorter available in South Africa, and was housed at Mintek in Johannesburg. A 150t sample was provided from a box cut adjacent to the coal deposit under investigation in order to conduct bulk and pilot sorting tests, the focus of which was on obtaining coal products of low ash and torbanite content. Clear distinctions between the coal, torbanite and shale fractions were observed using this technique. The sorter feed (-80mm+20mm) could be upgraded from a CV of 22MJ/kg to 28MJ/kg. Ash content could be reduced from 26% to 10%, which meets export quality standards. Petrographic analysis of the coal product indicated that a high purity coal product (in terms of torbanite and ash content) was attainable (91% by volume) at a mass yield of 42.9% to the coal product, with shale and mixed humic/sapropelic coal as contaminants. Under these conditions, torbanite contamination was marginal. It was demonstrated that shale could be removed from the torbanite product via a second sorting stage. This however was not the primary focus of the study, and was not optimised for this investigation. Two major limitations of the sorting process were identified, viz.; poor liberation and limited sorter feed size range. These impacted on the process as follows:- • The effects of poor liberation on coal quality could be counteracted by adjusting the sorting criteria of the algorithm to reject additional material. This would result in a lower coal product mass yield. In addition, interlocked coal/shale particles would report to the torbanite fraction. • A significant proportion of the ROM feed reported to the -20mm size fraction, and therefore did not fall part of the sorter feed. This resulted in a very low coal mass yield as a proportion of the ROM feed. If this process were to be adopted, means of minimizing fines production during mining and crushing would need to be investigated to improve overall yield to coal product. The capability to process coarse materials (-80mm+20mm) allows for throughputs in excess of 40t/hr. Consequently, this technique may be applied in simpler coal upgrading processes, such as coal deshaling in arid regions.

FAculty of SCience School of Cheistry 9910913j messai@auvum.chem.wits.ac.za / The monodentate phosphine complexes bui3PMX (2a: M = Cu, X = Cl, 2b: M = Cu, X = I, 2c: M = Ag, X = Cl, 2d: M = Au, X = Cl) were synthesised in high yields from bui3P and MX. Their reaction with [Li{μ-N(R)C(but)C(H)R}]2 (R = SiMe3) gave the monomeric complexes bui3PCuN(R)C(but)=C(H)R (3a) and bui3PMC(H)RC(but)=NR (3b: M = Ag, 3c: M = Au) in moderate to high yields. The bonding mode in the 1-aza-allyl complexes 3a-c was found to depend strongly on the metal ion, with 3a being an enamide complex and 3b and 3c iminoalkyl complexes. The reaction of bidentate ligand dpmaaH2 (2,3-bis(diphenylphosphino)maleic acid) with R2Sn-precursors led to novel dialkyl tin dpmaa complexes (R2Sn)(O,O dpmaa) (6) (where 6a, R = Me; 6b, R = Bu) were synthesized. Complexation of the tin/phosphine complexes led to the heterobimetallic complexes {Au[(dpmaaO,O)(SnR2)]2}Cl (7a and 8a) {Au[(dpmaaO,O)(SnR2)][dpmaaH2]}Cl (7b and 8b) (where 7a and 8a, R = Me; 7b and 8b, R = Bu) and the mixed metal complexes {Au[(dpmaaO,O)(RuCl)]2}Cl (9a) {Au[(dpmaaO,O)(SnBu2)(dpmaaO,O)RuCl)]}Cl (9b) and {Au[(dpmaaO,O)(RuCl)][dpmaa]}Cl (9c). All compounds were fully characterised by multinuclear NMR spectroscopy and microanalysis (not 3a, 3b, 4 and 5) solid state IR spectroscopy (KBr-pellets) (4-9) and mass spectrometry (6-8). The solid state structures of complexes 2c, 2d, 3c, 6a and 6b (two polymorphs) have been determined by X-ray crystallography revealing the presence of rare trimeric macrocycles in the case of 6a and 6b. The anti-tumour activity of the metal complexes (6b and 7-9) was tested on a single cell-line (except 7a and 8a which were on eight cell-lines) and their activity was compared to cisplatin.

A estrutura da florencita foi refinada pelo método de mínimos quadrados, utilizando dados experimentais obtidos através do método de Debye-Scherrer. A coleta dos dados das intensidades integradas foi feita através da leitura do difratograma de pó por um microdensitômetro óptico automático, e empregando métodos de análise numérica para fazer a integração da função (2&#952,Y), tabelada a pontos eqüidistantes. Foram observados 14 picos de difração e as reflexões que se superpunham contribuindo para as intensidades dos picos foram identificadas e suas contribuições levadas em conta através de seus fatores de multiplicidade. O refinamento foi feito com o programa POWLS (Powder Least Squares) e inicialmente foram fornecidos os parâmetros posicionais dos átomos da Goyazita, que é isomorfa com a florencita. As intensidades observadas foram corrigidas pelos fatores de Lorentz-polarização e adsorção. O índice de discordância R atingido para os 14 picos de difração observados foi de 0.097. A fórmula molecular da florencita é CeAl3(PO4)2(OH)6. O composto cristaliza no sistema hexagonal com parâmetros de rede ao=6.96Å co=16.33Å &#945= &#946 = 90° &#947=120° V=685.07&#1973. O grupo espacial é R3m com Z=3 e densidade calculada igual a 3.67g.cm-3. / The crystal structure of the florencita was refined by least squares using experimental data obtained with the Debye-Scherrer method. An automatic optical microdensitometer was used for the data collection from powder difractogram and numerical analysis methods for the integration of the function (2&#952,Y) which is tabulated at equidistant points. 14 diffraction peaks were observed, reflections which superpose contributing to the same peak were identified and their contributions were taken in account using multiplicity factors. The program POWLS (Powder Least Squares) was used for the refinement and initially the positional parameters of the atoms of the Goyazite, which is isomorfous with the florencita were used. Intensities were corrected for the Lorentz, polarization and absorption factors. The final R factor for the 14 peaks was of 0.097. The molecular formula of the florencitais CeAl3(PO4)2(OH)6. It crystallizes in the hexagonal system, space group R3m with cell ao=6.96Å co=16.33Å &#945= &#946 = 90° &#947=120° V=685.07&#1973.

Neste trabalho apresenta-se inicialmente algumas considerações sobre a difração de raios-X, suas principais leis, fatores de correção dos dados experimentais, uma revisão sobre os principais Métodos Diretos de resolução da estrutura, e considerações sobre o refinamento da estrutura obtida. A seguir descreve-se a determinação da estrutura cristalina do produto natural 5,4\'-Dihidroxi-3\', 5\' -dimetoxi- 6,7 -(2\",2\" -dimetilpirano) flavona de fórmula molecular C22H20O<sub<7, isolado de plantas da espécie Neoraputia paraensis, que cristaliza-se no sistema monoclínico, grupo espacial C2/c, com os seguintes parâmetros de cela unitária: a = 13,651(1), b= 23,428(2),c= 13,725(1) &#197; &#946= 119,528(4)&#176, V=3819,6(5)A&#9463 , Dc = 1,366g cm-3 e Z =8 moléculas por cela unitária. A estrutura foi resolvida através da aplicação de Métodos Diretos. Os índices de discordância finais são: R= 0,0509, Rw = 0,0530 para 1743 reflexões com I &#8805 3&#963(I) e Ra11=0,157. A estrutura foi refinada fazendo uso dos cálculos de Fourier Diferença e pelo método de mínimos quadrados usando matriz completa. A molécula apresenta duas ligações de hidrogênio intramoleculares, de força média (distâncias O-O 2,558(3) e 2,674(4) &#946). O empacotamento cristalino apresenta duas outras ligações de hidrogênio intermoleculares, mais fracas, sendo feitas com as moléculas geradas pelo espelho c (distâncias O-O 2,830(3) e 2,992(3) &#946). O efeito destas ligações intermoleculares é o da formação de cadeias ao longo da direção [101]. / Initially, some considerations about X-ray diffraction, its laws, the factors for the correction of experimental data, a revision of the main Direct Methods for structure resolution, and comments on the refinement of the resulting structure are presented. Next, the structure determination of the compound 5,4\' -dihydroxy-3\'-5\'- dimethoxy-6,7(2\",2\' \')dimethylpyran)flavone is described The compound is isolated from plants of the species Neuroputia paraenesis and has the molecular formula C22H20O<sub<7. It crystallizes in the monoclinic system, space group C2/c, with the following unit cell parameters: a = 13.651(1), b= 23.428(2), c= 13.725(1) &#197; &#946= 119,528(4)&#176, V=3819,6(5)A&#9463 , Dc = 1,366g cm-3 e Z =8molecules per unit cell. The structure was solved applying Direct Methods. The final disagreement indices are: R= 0.0509, Rw= 0.0530 for 1743 reflections with &#8805 3&#963(I) and Ra11=0,157. The structure was refined applying Fourier difference calculations and full matrix least squares methods. The molecule shows two intramolecular hydrogen bonds of medium strength (distances O-O 2.558(3) and 2.674(4) &#946). The crystal packing shows also two weaker hydrogen bonds; these are formed between the molecules generated by the c mirror (distances O-O 2.830(3) and 2.992(3) &#946). The result of these intermolecular hydrogen bonds is the formation of chains in [10 1] direction.