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The aim of the presented work was to deposit cubic boron nitride thin films by magnetron sputtering under simultaneous stress relaxation by ion implantation. An in situ instrument based on laser deflectometry on cantilever structures and in situ ellipsometry, was used for in situ stress measurements. The characteristic evolution of the instantaneous stress during the layered growth of cBN films observed in IBAD experiments, could be reproduced for magnetron sputter deposition. To achieve simultaneous stress relaxation by ion implantation, a complex bipolar pulsed substrate bias source was constructed. This power supply enables the growth of cBN thin films under low energy ion irradiation (up to 200 eV) and, for the first time, the simultaneous implantation of ions with an energy of up to 8 keV during high voltage pulses. It was demonstrated that the instantaneous stress in cBN thin films can be released down to -1.1 GPa by simultaneous ion bombardment during the high voltage pulses. A simultaneous stress relaxation during growth is possible in the total investigated ion energy range between 2.5 and 8 keV. These are the lowest ion energies reported for the stress relaxation in cBN. Since such a substrate bias power supply is easy to integrate in existing process lines, this result is important for industrial deposition of thin films, not only for cubic boron nitride films. It was found that the amount of stress relaxation depends on the number of atomic displacements (displacements per atom: dpa) that are induced by the high energy ion bombardment and is therefore dependent on the ion energy and the high energy ion flux. In practise, this means that the stress relaxation is controlled by the product of the pulse voltage and the pulse duty cycle or frequency. The cantilever bending measurements were complemented on microscopic scale by x-ray diffraction (XRD). The analysis of the cBN (111) lattice distances revealed a pronounced biaxial compressive state of stress in a non-relaxed cBN film with d(111) being larger in out-of-plane than in in-plane direction. Post deposition annealing at 900 ° C of a sample with an ion induced damage of 1.2 dpa, resulted in a complete relaxation of the lattice with equal in-plane and out-of-plane lattice parameters. In the case of medium-energy ion bombardment, the in-plane and out-of-plane lattice parameters approach the value of the annealed sample with increasing ion damage. This is a clear evidence for stress relaxation within the cBN lattice. The stability of cBN under ion bombardment was investigated by IR spectroscopy and XRD. The crystalline cBN was found to be very stable against ion irradiation. However a short-range ordered, sp3/sp2 - mixed phase may exist in the films, which could be preferably converted to a sp2 -phase at high damage values. From the analysis of the near surface region by XANES, it can be concluded the stress relaxation by the energetic ion bombardment is less at the surface than in the bulk film. This is explained with the dynamic profile of the ion induced damage, that reaches the stationary bulk value in 15-20 nm depth, whereas it is decreasing towards the surface. This fits with the results that the stress relaxation is dependent on the amount of ion induced damage. Comparing the results from substrate curvature measurement, XRD, XANES, and IR spectroscopy possible mechanisms of stress relaxation are discussed. Concluding the results, it can be stated that using simultaneous ion implantation for stress relaxation during the deposition it is possible to produce BN films with a high amount of the cubic phase and with very low residual stress.

Основными технологическими и трудно определяемыми примесями в h-BN выступают углерод и кислород. На производстве возникает необходимость в контроле качества с высоким пространственным разрешением как отдельных нанослоев h-BN, так и готовых гетероструктур на его основе. Целью работы является разработка способа неразрушающего контроля дефектности и примесного состава тонких слоев h-BN методами комбинационного рассеяния света и катодолюминесцентной спектрометрии. Выполнен литературный обзор особенностей материала гексагонального нитрида бора и его люминесцентных свойств. Проведены измерения исследуемых образцов при помощи рамановского спектрометра, сканирующего электронного микроскопа с катодолюминесцентной приставкой и электронно-зондового микроанализатора. Выполнен анализ полученных результатов. / The main technological and difficult-to-determine impurities in h-BN are carbon and oxygen. In production, there is a need for quality control with high spatial resolution of both individual h-BN nanolayers and heterostructures based on it. The aim of the work is to develop a method for non-destructive testing of the defects and impurity composition of h-BN thin layers by Raman scattering and cathodoluminescence spectrometry. A literature review of the features of the material of hexagonal boron nitride and its luminescent properties is performed. The samples were measured using a Raman spectrometer, a scanning electron microscope with a cathodoluminescent attachment, and an electron probe microanalyzer. The analysis of the obtained results is performed. Areas of application: diagnostics and quality control.

Thesis (M.Sc. (Physics)) -- University of Limpopo, 2022 / The gas sensing performance of two-dimensional (2D) hexagonal boron nitride nanosheets (h-BNNSs) has being studied by means of computational and experimental methods. The structural, stability and vacancies properties of both defect free and defected 2D h-BNNSs were studied using the classical molecular dynamics (MD) approach. The calculations were performed in the NVT Evans and NPT hoover ensembles using the Tersoff potentials with the Verlet leapfrog algorithm to obtain reliable structural properties and energies for defect free, boron (B) and nitrogen (N) vacancies. B and N defect energies were calculated relative to the bulk defect free total energies, and the results suggest that N vacancy is the most stable vacancy as compared to the B vacancy. The radial distribution functions and structure factors were used to predict the most probable structural form. Mean square displacements suggests the mobility of B and N atoms in the system is increasing with an increase in the surface area of the nanosheets. Results obtained are compared with the bulk defect free h-BNNSs. Experimentally, 2D h-BNNSs were synthesised using the wet chemical reaction method through chemical vapour deposition (CVD) catalyst free approach. The X-Ray Diffraction (XRD), Transmission Electron Microscopy (TEM), Fourier Transform Infrared Spectroscopy (FTIR), Raman Spectroscopy (RM), UV-visible Spectroscopy (UV-VIS), dynamic light scattering (DLS), Energy Dispersion Spectroscopy (EDS) and Brunauer-Emmett Teller (BET) were adopted to attain the structural properties of the nanosheets. Each spectroscopic technique affirmed unique features about the surface morphology of h BNNSs. The crystallinity of the nanosheets with the stacking of the B and N vii honeycomb lattice was validated by the XRD, while the TEM disclosed the specimen orientations and chemical compositions of phases with the number of layers of a planar honeycomb BN sheet, the EDS express the atoms present in the samples and BET validated the surface area of the materials. The FTIR, RM, DLS and the UV-vis expressed the formation of the in-plane, out-of-plane h-BN vibrations and, the nature of the surface with the thickness, particles stability together with the optical properties of the nanosheets. From TEM, FTIR, RS and BET the material fabricated at 800°C showed different morphologies, large number of disordering together with high surface area, which enhances the sensing properties of the nanosheets. However, with an increase in temperature the sensitivity of the nanosheets was found to decrease. Additionally, the UV-vis results, confirmed a lower energy band gap of 4.79, 4.55 and 4.70 eV for materials fabricated at 800, 900 and 1000 °C, that improved the semiconducting properties of the materials, which in return enhanced the sensing properties of the nanosheets. The gas sensing properties of the 2D h BNNSs were also investigated on hydrogen sulphide (H2S) and carbon monoxide (CO). The fabricated sensor based on 800 – 900 °C h-BNNSs showed good sensitivity towards ppm of H2S at 250 °C. The excellent gas sensing properties could be attributed to high surface area, small crystallite size, defect/disordering of h BNNSs. Overall, the h-BNNSs were found to be more sensitive to H2S over CO. / University of Limpopo (UL) Mintek Council for Scientific and Industrial Research (CSIR) Center for High Performance Computing (CHPC)

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Friction stir welding (FSW) of steel is often performed with an insert made of polycrystalline cubic boron nitride (PCBN). Specifically, MS80 is a grade of PCBN made by Smith MegaDiamond that has been optimized for the FSW process. The PCBN insert is attached to a tungsten carbide (WC) shank by a compression fitting. However, FSW tools manufactured by this method inevitably fail by fracture in the PCBN. Permanently bonding PCBN to WC would likely solve the fracturing problem and increase the life of PCBN FSW tools to be economically viable. Partial transient liquid phase (PTLP) bonding, a process used to join ceramics with thin metallic interlayers, was proposed as a method to permanently bond PCBN to WC. PTLP bonding is often performed using three layers of pure elements. On heating, the two thin outer interlayers melt and bond to the ceramics. Concurrently, these liquid layers diffuse into the thicker refractory core until solidification has occurred isothermally. A procedure was developed to reduce the number of possible three-layer PTLP bonding setups to a small set of ideal setups using logical filters. Steps in this filtering method include a database of all existing binary systems, sessile drop testing of 20 elements, and a routine that calculates maximum interlayer thicknesses. Results of sessile drop testing showed that the PCBN grade required for this research could only be bonded with an alloy of Ti, Cu, Mg, and Sb. Two PTLP bond setups were tested using this special coating on the PCBN, but a successful bond could not be achieved. However, a PTLP bond of WC to WC was successful and proved the usefulness of the filtering procedure for determining PTLP bond setups. This filtering procedure is then set forth in generalized terms that can be used to PTLP bond any material. Also, recommendations for future research to bond this grade of PCBN, or some other grade, to WC are presented.

This thesis aims to investigate the coefficient of friction between steel on steel contacts with the addition of solid lubricants such as h-BN, WS2, MoS2 in powder form, in dry conditions and wet conditions. More specifically, the purpose is to enhance the sliding between the piston rings and cylinder block in a modern high temperature steam engine developed by RANOTOR. The friction test was carried out as a linear sliding test with determined loads and sliding speed. Hertzian contact theory was deployed to calculate contact pressure and shear stresses to make sure the contact was elastic, alternatively plastic. It was found that WS2 and  MoS2 lowered the coefficient of friction quite heavily in dry conditions, acting as a thin protective-lubricating film. h-BN performed rather poorly, increasing the coefficient of friction. In a water slurry, none of the powders managed to decrease the COF due to the particles not interacting with the surfaces.The solid lubricants tested should be further tested as coatings since they acted like it in dry conditions. / Denna rapport syftar till att undersöka friktionskoefficienten i stålkontakter med tillsats av fasta smörjmedel som  h-BN, WS2, MoS2 i pulverform, under torra och våta förhållanden. Mer specifikt är syftet att förbättra glidningen mellan kolvringarna och insidan av cylindern i en modern högtemperatur-ångmotor utvecklad av RANOTOR. Friktionstestet genomfördes som ett linjärt glidtest med bestämda belastningar och glidhastighet. Hertzian-kontaktteorin användes för att beräkna kontakttryck och skjuvspänningar för att säkerställa att kontakten var elastisk alternativt plastisk. Det visade sig att WS2och MoS2 kraftigt sänkte friktionskoefficienten under torra förhållanden genom att agera som en tunn skyddande-smörjfilm. h-BN presterade dåligt och ökade friktionskoefficienten. I vattenblandning lyckades inget av pulverna minska friktionskoefficienten eftersom partiklarna inte interagerade med ytorna. De testade fasta smörjmedlen bör vidare testas som beläggningar eftersom de fungerade som dessa under torra förhållanden.

Объекты разработки и исследования: канал лазерной стимуляции для измерения электрофизических параметров структуры Ti/TiO2-НТ/Au и канал оптической стимуляции для исследования люминесцентных свойств нанопорошка гексагонального нитрида бора. Цель работы – разработать измерительные каналы лазерной стимуляции исследуемых образцов на основе контроля и управления параметрами излучения в различных режимах в ходе экспериментальных исследований оптически стимулированных и родственных процессов в широкозонных наноструктурированных материалах. В результате работы разработан канал лазерной стимуляции для существующего комплекса по измерению вольт-амперных характеристик на базе микрозондовой станции Cascade Microtech MPS 150, а также модернизирован канал оптической стимуляции на базе люминесцентного спектрометра Perkin Elmer LS 55 со встроенной высокотемпературной приставкой. Реализованные программно-аппаратные измерительные комплексы позволили успешно применить на практике методики исследования широкозонных наноструктур посредством оптически стимулированных процессов. Полученные в ходе работы данные, как для образцов Ti/TiO2-НТ/Au, так и для наноструктурированного порошка h-BN, отлично согласуются с результатами различных исследовательских работ из независимых научных источников. / Objects of development and research: a laser stimulation channel for measuring the electrophysical parameters of the Ti/TiO2-HT/Au structure and an optical stimulation channel for studying the luminescent properties of a hexagonal boron nitride nanopowder. The aim of the work is to develop measuring channels of laser stimulation of the studied samples based on the control and operating of radiation parameters in various modes during experimental studies of optically stimulated and related processes in wide-gap nanostructured materials. As a result of the work, a laser stimulation channel was developed for the existing complex for measuring current-voltage characteristics based on the Cascade Microtech MPS 150 microprobe station, and the optical stimulation channel was modernized on the basis of a Perkin Elmer LS 55 luminescence spectrometer with a built-in high-temperature attachment. The implemented software and hardware measuring systems made it possible to successfully apply in practice the methods of studying wide-gap nanostructures by means of optically stimulated processes. The data obtained during the work, both for the Ti / TiO2-NT / Au samples and for the nanostructured h-BN powder, are in excellent agreement with the results of various research works from independent scientific sources.