The intercalation of surfactant anions, namely sodium dodecyl sulphate, sodium benzene sulphonate and lauric acid, into commercial layered double hydroxides (LDH-CO3) with approximate composition [Mg0.654AI0.346 (OH)2](CO3)0.173.0.5H2O] was explored. LDH-CO3 is commercially available in bulk form owing to its large scale applications as a PVC stabiliser and acid scavenger in polyolefins. It is therefore of interest to investigate intercalation methods using LDH-CO3 as starting material. The intercalation method used was compared with the pre existing procedures, for instance the co-precipitation, ion exchange and regeneration methods. Due to the tenacity with which the carbonate ion is held in LDH-CO3, direct ion exchange is an intricate matter. Hence, in the regeneration method the carbonate ion is removed by thermal treatment and the LDH-surfactant is obtained by reaction of the LDH and surfactant in an aqueous medium. Nevertheless, the resulting products are impure and poorly crystallised, and only partial intercalation is achieved. The underlying principle of the current method is protonation of the carbonate anion to a monovalent anion that is easily exchanged with surfactant anions. Improved results were obtained when water-soluble organic acids were used, the most suitable being lower aliphatic carboxylic acids, e.g. acetic, butyric and hexanoic acid. In contrast, higher linear aliphatic carboxylic acids are preferentially intercalated to the anionic surfactants. In both cases the carboxylic acids are assumed to assist intercalation by facilitating the elimination of the carbonate ions present in the anionic clay galleries. X-ray diffraction analysis, thermal analysis and infrared spectroscopy confirmed the monolayer intercalation of LDH-dodecyl sulphate and LDH-dodecylbenzene sulphonate. In contrast, LDH-laurate featured a bilayer structure. / Dissertation (MSc)--University of Pretoria, 2009. / Chemistry / unrestricted

<p> Understanding the function and structure of a protein is crucial for informing on rational drug design and for developing successful drug candidates. However, this understanding is often limited by the protein pipeline, i.e. the necessary steps to go from developing protein constructs to generating high-resolution structures of macromolecules. Because each step of the protein pipeline requires successful completion of the prior step, bottlenecks are often created and therefore this process can take up to several years to complete. Addressing current limitations in the protein pipeline can help to reduce the time required to successfully solve the structure of a protein. </p><p>The field of nonlinear optical (NLO) microscopy provides a potential solution to many issues surrounding the detection and characterization of protein crystals. Techniques such as second harmonic generation (SHG) and two-photon excited UV fluorescence (TPE-UVF) have already been shown to be effective methods for the detection of proteins with high selectivity and sensitivity. Efforts to improve high throughput capabilities of SHG microscopy for crystallization trials resulted in development of a custom microretarder array (μRA) for depth of field (DoF) extension, therefore eliminating the need for z-scanning and reducing the overall data acquisition time. Further work was done with a commercially available μRA to allow for polarization dependent TPE-UVF. By placing the μRA in the rear conjugate plane of the beam path, the patterned polarization was mapped onto the field of view and polarization information was extracted from images by Fourier analysis to aid in discrimination between crystalline and aggregate protein. </p><p>Additionally, improvements to X-ray diffraction (XRD), the current gold standard for macromolecular structure elucidation, can result in improved resolution for structure determination. X-ray induced damage to protein crystals is one of the greatest sources of loss in resolution. Previous work has been done to implement a multimodal nonlinear optical (NLO) microscope into the beamline at Argonne National Lab. This instrument aids in crystal positioning for XRD experiments by eliminating the need for X-ray rastering and reduces the overall X-ray dosage to the sample. Modifications to the system to continuously improve the capabilities of the instrument were done, focusing on redesign of the beam path to allow for epi detection of TPE-UVF and building a custom objective for improved throughput of 1064 nm light. Furthermore, a computational method using non-negative matrix factorization (NMF) was employed for isolation of unperturbed diffraction peaks and provided insight into the mechanism by which X-ray damage occurs. This work has the potential to improve the resolution of diffraction data and can be applied to other techniques where X-ray damage is of concern, such as electron microscopy.</p><div><br></div>

A comprehensive study on growth of ferrimagnetic manganese zinc ferrite (Mn0.5Zn0.5Fe2O4) films on single crystalline strontium titanate(001) (SrTiO3) substrates was carried out. Under the optimized conditions, a thin film with a layer thickness of 200 nm was deposited, and the structural properties were investigated. Contrary to data published in literature, no buffer layer was necessary to achieve epitaxial growth of a poorly lattice-matched layer. This was confirmed for Mn0.5Zn0.5Fe2O4(001) on SrTiO3(001) by x-ray diffraction and the adjoined phi scans, which also revealed a lattice compression of 1.2% of the manganese zinc ferrite film in the out-of-plane direction. Using x-ray photoelectron spectroscopy, the near surface stoichiometry of the film could be shown to agree with the intended one within the uncertainty of the method. X-ray absorption spectroscopy showed an electronic structure close to that published for bulk samples. Additional x-ray magnetic circular dichroism investigations were performed to answer detailed structural questions by a comparison of experimental data with the calculated ones. The calculations took into account ion sites (tetrahedral vs. octahedral coordination) as well as the charge of Fe ions (Fe2+ vs. Fe3+). Contrary to the expectation for a perfect normal spinel that only Fe3þ ions are present in octahedral sites, hints regarding the presence of additional Fe2+ in octahedral sites as well as Fe3+ ions in tetrahedral sites have been obtained. Altogether, the layer could be shown to be mostly in a normal spinel configuration.

The main content of this master's thesis is a determination of the fatigue properties by using non-destructive testing methods – the acoustic emission technique and the X-ray diffraction. The reactor steel, that is named GOST 15Ch2NMFA, is used as a model material and is used to manufacture VVER-1000 reactor pressure vessels. The supplied material was made of two different steel melting, designated as H and S. For the basic measurement of the fatigue properties the stress-cycle asymmetry R = -1 was used. Some of the samples were used for approximate determination of the fatigue strength stress-cycle asymmetry R = 0. During the loading process the resonance frequency of the loading machine and acoustic emission signals were recorded. The changes in microstructure were estimated from the record of acoustic emissions during the whole fatigue life. The change of the microstructure was experimentally observed by X-ray diffraction analysis. The mechanism of the fatigue can be described by the observation of the microstructural processes as well as the relevant bifurcation with sufficient sensitivity. The results of the used methods indicate a decay and re-growth of mosaic blocks during the whole loading process. Therefore, it is important to find a correlation of these two non-destructive methods, or to use other non-destructive testing methods in the future.

京都大学 / 0048 / 新制・課程博士 / 博士(農学) / 甲第18340号 / 農博第2065号 / 新制||農||1024(附属図書館) / 学位論文||H26||N4847(農学部図書室) / 31198 / 京都大学大学院農学研究科森林科学専攻 / (主査)教授 木村 恒久, 教授 西尾 嘉之, 教授 髙野 俊幸 / 学位規則第4条第1項該当 / Doctor of Agricultural Science / Kyoto University / DFAM

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Today's society is currently developing lithium-ion batteries to eventually replace the use of fossil fuels. High entropy oxides is a new type of material to use as an anode in the lithium-ion battery. These high entropy oxides may consist of a few different transition metals including lithium and oxygen. In this report was (MgCoNiZn)1-xLixO synthesized with a method called Pechini with a molar fraction of x=0.35. This study compares the results from a reference study that has shown the potential of the electrochemical characteristics of (MgCoNiZn)1-xLixO for application as anode in a lithium-ion battery.  The synthesis starts with a heating step to remove all the organics in the composition. The powder consists of several structures and, therefore goes through a calcination step to dissolve all of the intermediate phases into the rock-salt structure. The structure of the powder had a lattice constant of 4,138Å. The powder was made into a slurry containing Carbon black, PVDF and NMP to later get coated by a Dr. Blade. After drying the coating the cell was then assembled with lithium as metal cathode and 1M LiPF6 in 1:1 EC/DMC as electrolyte. After the cell was assembled it, went through electrochemical properties test using a potentiostat and the cell being inside a in a climate chamber at 25°C.  7 cycles were done to plot a cyclic voltammetry graph as well as a discharge-charge test was performed. The cyclic voltammetry and discharge-charge test was run with a voltage range of 0,053 V. The discharge-charge test was run at a current density of 100 mA/g and a constant current of 42,68 mA. / Dagens samhälle genomgår en stor utveckling av litium-jon batterier för att kunna ersätta användningen av fossila bränslen. Höga entropi oxider är ny typ av material som används som anod material för litiumjonbatterier. Dessa höga entropi oxider kan bestå av en rad olika övergångsmetaller inklusive litium och syre i sammansättningen. I den här rapporten var (MgCoNiZn)1-xLixO syntetiserad med en metod som heter Pechini med ett molbråk på x=0,35. En studie har visat potentialen i dem elektrokemiska beetenden av (MgCoNiZn)1-xLixO till applicering som en anode i ett litiumjon batteri.  Syntetiseringen började med ett uppvärmningsteg för att bränna bort alla organiska föreningar. Resulterade pulvret bestod av olika strukturer, och till ett kalcinerings steg för att lösa upp mellanfaserna till NaCL-struktur. Strukturen på pulvret hade en gitter constant på 4,138 Å. Pulvret gjordes till en slurry som innehåller amorft kol, PVDF och NMP för att sedan belägga elektroden med en Dr.Blade. Efter beläggningen har fått torka monterades cellen med litium som katod och 1M LiPF6 in 1:1 EC/DMC som elektrolyt. Tester utfördes på cellen med hjälp av en potentiostat medans cellen var förvaren i en klimatkammare i 25°C.  7 stycken cykler kördes för att plotta en cyklisk voltametri graf samt en urladdning-laddning prov utfördes. Cykliska voltametrin och urladdning-laddnings prov utfördes med ett spänningsintervall på 0,05-3,0V. Urladdning-laddnings provet hade en strömtäthet på 100 mA/g och en konstant ström på 42,68 mA.

Electrostatic interactions such as halogen bonding and pnictogen bonding interactions have gained a lot of interest in the field of crystal engineering and pharmaceutical science. In the first part of this thesis, we expand our knowledge on anion coordinated halogen bonded cocrystals by looking at a series of cocrystals made from 3-iodoethynyl pyridine and 3-iodoethynylbenzoic acid. We utilize the power of mechanochemistry to create the new cocrystals made with phosphonium salts and use multinuclear solid-state nuclear magnetic resonance spectroscopy and X-ray diffraction and characterize them. We found that mechanochemistry is a fast and powerful tool to explore and synthesize new halogen bonded cocrystals and ³¹P solid-state NMR is a rapid way to identify the formation of a cocrystal. In the second part, we look at the versatility of the pnictogen atom, specifically antimony, as a pnictogen bond donor and a halogen bond acceptor. We evaluate these electrostatic interactions with nuclear quadrupolar resonance and found that nuclear quadrupole resonance is a strong spectroscopy tool to probe these types of electrostatic interactions.