Small quantities of amorphous content can have a profound influence on the properties of a material, however their instability means that quantifying amorphous content over time is important for proving the stability of a drug. Quantifying amorphous content in α-lactose monohydrate by solid state 13C CP MAS NMR, has been carried out by use of proton saturation recovery relaxation and differentiating between spectra by partial least squares (PLS), however these techniques have not proved sensitive on their own, this work investigates their sensitivity in combination. Crystalline α-lactose monohydrate and a rapidly quenched melt were combined to create a set of calibration mixes, whose spectra were recorded using proton saturation recovery relaxations ranging from 2 to 60 seconds. This technique showed a limit of detection of 0.17% (LOD = intercept + 3xSy/x), with a relaxation delay of 15 s and was able to recognise amorphous materials generated by spray and freeze drying. The atmospheric effects on the proton saturation recovery relaxation times of different amorphous lactose preparations were investigated. This found that an oxygen atmosphere reduced the relaxation times, of amorphous lactose that was prepared from a rapidly quenched melt. The loss of moisture from spray dried and freeze dried samples to less than 1% removed the significance of this effect. Lactose is an important excipient in pharmaceuticals and a key ingredient of confectionary, very little research has been carried out in to the quantification of the isomers of different preparations of amorphous lactose. This work quantifies the isomer content by Gas Chromatography with Flame Ionisation Detection (GC-FID) using a DB-17 15m 0.53mm 1.00 μm column and derivatisation with N- (trimethylsilyl)imidazole.

The perovskite family of materials is extremely large and provides a template for designing materials for different purposes. Among them, hybrid organic-inorganic perovskites (HOIPs) are very interesting and have been recently identified as possible next generation light harvesting materials because they combine low manufacturing cost and relatively high power conversion efficiencies (PCEs). In addition, some other applications like light emitting devices are also highly studied. This thesis starts with an introduction to the solar cell technologies that could use HOIPs. In Chapter 2, previously published results on the structural, electronic, optical and mechanical properties of HOIPs are reviewed in order to understand the background and latest developments in this field. Chapter 3 discusses the computational and experimental methods used in the following chapters. Then Chapter 4 describes the discovery of several hybrid double perovskites, with the formula (MA)$_2$M$^I$M$^{III}$X$_6$ (MA = methylammonium, CH$_3$NH$_3$, M$^I$ = K, Ag and Tl, M$^{III}$ = Bi, Y and Gd, X = Cl and Br). Chapter 5 presents studies on the variable presure and temperature response of formamidinium lead halides FAPbBr$_3$ (FA = formamidinium, CH(NH$_2$)$_2$) as well as the mechanical properties of FAPbBr$_3$ and FAPbI$_3$, followed by a computational study connecting the mechanical properties of halide perovskites ABX$_3$ (A = K, Rb, Cs, Fr and MA, X = Cl, Br and I) to their electronic transport properties. Chapter 6 describes a study on the phase stability, transformation and electronic properties of low-dimensional hybrid perovskites containing the guanidinium cation Gua$_x$PbI$_{x+2}$ (x = 1, 2 and 3, Gua = guanidinium, C(NH$_2$)$_3$). The conclusions and possible future work are summarized in Chapter 7. These results provide theoreticians and experimentalists with insight into the design and synthesis of novel, highly efficient, stable and environmentally friendly materials for solar cell applications as well as for other purposes in the future.

O resíduo estudado neste trabalho é originado do processo de obtenção de alumínio metálico, de grande interesse no Brasil pelo fato do país ser detentor de algumas das maiores reservas do mineral bauxita no mundo, utilizado como fonte de alumínio. Tendo como estratégia a geração de resíduo zero, colaborando para as tecnologias ambientalmente amigáveis, este trabalho estuda a incorporação de um resíduo resultante da recuperação de alumínio presente na escória gerada durante o processo de produção primária do alumínio metálico, por plasma térmico. Utilizando-se o diagrama de equilíbrio de fases do sistema Al2O3-CaO-SiO2, fez-se a adequação das composições visando a incorporação de resíduo no produto cerâmico sem alterar as características de processamento do material. A obtenção de vidros e de fritas vitrocerâmicas com o resíduo borra branca foi realizada fazendo-se a fusão das composições calculadas e, para os vitrocerâmicos, tratamento térmico posterior de devitrificação. Os produtos obtidos foram caracterizados utilizando-se técnicas de análise tais como difração de raios X (DRX), microscopia eletrônica de varredura (MEV) e espectroscopia do infravermelho (FTIR). Foi possível obter material vitrocerâmico com até 30% de resíduo de alumínio, após a fusão a 1300°C e devitrificação a 900°C. Em adição, o resíduo demonstrou ser um promissor material auxiliar na formação de fases cristalinas em baixos tempos de tratamento térmico. / This work studies the residue obtained from the process of aluminum metal extraction activities, a great interest process, because of Brazil own some of the biggest bauxite mineral reserves in all the world. As a useful choice for no residue generation, and a support for environmentally friendly technologies, this work studies the white dross residue (WDR), from the process of aluminum metal reduction by thermal plasma. The phase equilibrium diagram of Al2O3-Ca O-SiO2 system was used to calculate the compositions. The WDR were incorporated in a ceramic product without modifying its principal characteristics. The fusion and devitrification treatments were studied. XRD (X-ray diffractometry), SEM (scanning electron microscopy) and FTIR (transformed Fourier infrared) were used to investigate the glass and glassceramic samples. These techniques showed that is possible to get glassceramic with up to 30 mass% of WDR after molten at 1300 deg C and annealed at 900 deg C. In addition, the WDR showed to be a promising material in attainment of crystalline phases in less times of heat treatment for annealing.

Materiais cerâmicos, como a alumina e a zircônia têm sido explorados ao longo dos anos na aplicação como biomateriais. Sua natureza bioinerte, tem estimulado o desenvolvimento de novas alternativas, como tratamentos químicos para tornar o desempenho biológico destas cerâmicas mais adequadas. O recobrimento biomimético de cerâmicas bioinertes a partir de soluções com concentrações iguais às do plasma sanguíneo humano, SBF, pemiite o crescimento de uma camada bioativa na superfície dos implantes. A bioatividade do material está relacionada com a formação de uma camada constituída por cristais de hidroxiapatita carbonatada de baixa cristalinidade, similar à apatita biológica. A biocompatibilidade associada às propriedades estruturais da alumina e da zircônia tem estimulado o uso clínico destes materiais, inclusive em regiões de maiores solicitações mecânicas. Neste trabalho foram produzidas amostras de alumina, zircônia dopada com ítria (3% mol) e compósitos de alumina e zircônia dopada com ítria (3% mol) preparadas pelo método de co-precipitação, calcinadas, sinterizadas, tratadas quimicamente com soluções de ácido fosfórico e hidróxido de sódio e imersas em 1,0M e 1,5M SBF. Os pós calcinados foram analisados por difração de raios x (DRX), microscopia eletrônica de varredura (MEV), análise de área de superfície específica (BET) e análise de distribuição granulométrica (CILAS). Os resuhados por DRX indicam que as amostras possuem baixa cristalinidade. Observou-se que por BET as amostras apresentam alta área de superfície específica. Os resultados de CILAS e MEV mostraram que os pós encontram-se na forma de aglomerados. As amostras sinterizadas, foram analisadas por difração de raios x (DRX), microscopia eletrônica de varredura (MEV) e fluorescência de raios x (FRX), apresentando 96% da densidade teórica e as fases analisadas pelo método de Rietveld foram identificadas e quantificadas como: cúbica, tetragonal e monoclínica da zircônia, além da fase alfa da alumina. O tratamento químico com ácido fosfórico não apresentou uma tendência de maior formação de apatita em relação às amostras não tratada quimicamente. O tratamento com hidróxido de sódio provocou transformação acentuada da fase cúbica para tetragonal e da fase tetragonal para a fase monoclínica da zircônia. Os ensaios biomiméticos proporcionaram a formação de apatita sobre as superfícies das amostras, identificadas por DRX, e sua espessura foi medida por FRX. / Ceramic materials, as akimina and zirconia have been explored along the years as biomateriais application. The bioinert nature has been stimulating the development of new alternatives, as chemical treatments to improve the biological application of these ceramics. The biomimetic process of bioinerts ceramics for coating apatite is based on soaking the implant in a simulated body fluid, SBF, with ion concentrations nearly equal to those of human blood plasma. The bioactivity of the material is related with the formation of a layer constituted of hidroxiapatite low crystalline, similar to the biological apatite. The biocompatibility associated to the structural properties of the alumina and zirconia has been stimulating the clinical use of these materials, mainly in areas of larger mechanical requests, places not recommended for bioactive hidroxiapatite, for instance. In this work samples of alumina, zirconia doped with yttria (3% mol) and composites of alumina and zirconia doped with yttria (3% mol) were prepared by co-precipitation method, calcinated, sintered, chemically treated with solutions of acid phosphoric and sodium hydroxide and them immersed in l.OM and 1.5M SBF. The calcinated powders were analyzed by X-ray diffraction (XRD), scanning electron microscopy (SEM), gas adsorption (BET) and laser diffraction. The XRD resuhs indicate that the samples are low crystalline. It was observed for BET that the samples present high specific surface area. The resuhs of laser diffraction and SEM showed that the powders are agglomerates. The sintered samples were analyzed by XRD, SEM and X-ray fluorescence (XRF). The phases quantified by Rietveld method were: cubic, tetragonal and monoclinic of the zirconia, besides the phase alpha of the alumina. The chemical treatment with phosphoric acid didn\'t present a tendency of larger apatite formation in relation to the samples no chemically treated. The treatment with sodium hydroxide provoked accentuated transformation of the cubic phase for tetragonal phase and of tetragonal phase for the monoclinic phase of the zirconia. The immersion of samples in SBF provided apatite coating formation on the surfaces of the samples, identified by XRD, and the coating thiclmess was measured by XRF.

O presente trabalho tem como dupla finalidade a determinação de algumas estruturas moleculares inéditas e o desenvolvimento de dois sistemas computacionais de uso em cristalografia. Primeiramente, determinamos quatro estruturas moleculares de complexos de ácido piridinacarboxílico ligados a íons metálicos (Co, Ni, Cu e Zn), os quais apresentam interesse farmacológico e se enquadram em uma das linhas de pesquisa do grupo de Cristalografia de São Carlos. Nesta Dissertação, a ênfase dada a esta parte do trabalho é a aprendizagem das técnicas relativamente complexas para a resolução e refinamento de estruturas moleculares obtidas através de difração de raios X, como uma motivação preliminar para o subseqüente trabalho computacional. Com relação ao desenvolvimento de sistemas computacionais, são apresentados dois programas que representam importantes ferramentas cristalográficas. O Xandrix realiza todos os cálculos matriciais necessários em transformações cristalográficas, tanto no espaço real como no recíproco, envolvendo tensores de até segunda ordem. O WinKabsch é uma implementação do algoritmo de Kabsch que melhor sobrepõe, utilizando mínimos quadrados, dois conjuntos de vetores e é usado para comparar moléculas inteiras ou fragmentos. Ambos foram desenvolvidos para ambiente Windows, oferecendo uma interface visual poderosa e amigável. O WinKabsch permite que o usuário gire, visualmente, duas moléculas dadas de maneira que elas se posicionem em orientações similares, para então selecionar, com o mouse, alguns átomos homólogos a partir dos quais é obtida uma primeira matriz de transformação. A seguir, o programa reconhece todos os outros pares de átomos homólogos para os cálculos finais. A transformação pode ser forçada a ser uma rotação própria quando as moléculas comparadas são suspeitas de possuir a mesma quiralidade. / This work has the two-fold purpose of determining a few novel crystal structures and to develop two computational systems for crystallographic use. First, we determined four molecular structures of complexes of a derivative of the pyridinacarboxilic acid with a metal ion (Co, Ni, Cu and Zn), which are of pharmacological interest and belong to one of the research lines of the group. In the present contribution the emphasis of these studies is in mastering the somewhat involved techniques for solving and refining molecular structures by X-ray diffraction, as a preliminary motivation for the subsequent computational work. Second, two programs which turn out to be useful tools for crystallographic work were developed. Xandrix, permits all matrix calculations necessary in crystallography transformations, both in real and reciprocal space, involving tensors up to the second rank. WinKabsch is an implementation of the Kabsch algorithm for the best least squares superposition of two sets of vectors and is used to compare molecules or molecular fragments. Both programs were developed to run in a Windows environment with a powerful and friendly visual interface. WinKabsch allows the user to visually rotate two given molecules to achieve similar orientations to perform later a mouse selection of a few homologous atoms from which a first orthogonal transformation matrix is obtained, after which the program recognizes all other pairs of homologous atoms for the final calculation. The transformation may be forced to be a proper rotation when the compared molecules are known to be of the same chirality.

Tendo como vantagem a elevada resistência ao choque térmico da zircônia:magnésia e a alta condutividade iônica da zircônia:ítria, compósitos dessas cerâmicas foram preparados por meio da mistura, em diferentes concentrações, de eletrólitos sólidos de ZrO2: 8,6 mol% MgO e de ZrO2: 3 mol% Y2O3, compactação e sinterização. A caracterização microestrutural foi feita por meio de difração de raios X e microscopia eletrônica de varredura. A análise do comportamento térmico foi feita por dilatometria. As propriedades elétricas foram estudadas por meio de espectroscopia de impedância. Foi feita uma montagem experimental para monitorar a resposta elétrica gerada em função do teor de oxigênio a altas temperaturas. Os principais resultados mostram que os compósitos cerâmicos são parcialmente estabilizados nas fases monoclínica, cúbica e tetragonal, e apresentam comportamento térmico similar ao apresentado por eletrólitos sólidos de zircônia:magnésia de dispositivos sensores de oxigênio. Além disso, os resultados de análise de espectroscopia de impedância mostram que a adição da zircônia:ítria melhora o comportamento elétrico da zircônia:magnésia, e que resposta elétrica gerada é dependente do teor de oxigênio a 1000 °C, mostrando ser possível construir sensores de oxigênio utilizando compósitos cerâmicos. / Taking advantage of the high thermal shock resistance of zirconia-magnesia ceramics and the high oxide ion conductivity of zirconia-yttria ceramics, composites of these ceramics were prepared by mixing, pressing and sintering different relative concentrations of ZrO2: 8.6 mol% MgO and ZrO2: 3mol% Y2O3 solid electrolytes. Microstructural analysis of the composites was carried out by X-ray diffraction and scanning electron microscopy analyses. The thermal behavior was studied by dilatometric analysis. The electrical behavior was evaluated by the impedance spectroscopy technique. An experimental setup was designed for measurement the electrical signal generated as a function of the amount of oxygen at high temperatures. The main results show that these composites are partially stabilized (monoclinic, cubic and tetragonal) and the thermal behavior is similar to that of ZrO2: 8.6 mol% MgO materials used in disposable high temperature oxygen sensors. Moreover, the results of analysis of impedance spectroscopy show that the electrical conductivity of zirconia:magnesia is improved with zirconia-yttria addition and that the electrical signal depends on the amount of oxygen at 1000 °C, showing that the ceramic composites can be used in oxygen sensors.

O NbAl3 e algumas ligas intermetálicas do sistema Nb-Ni-AI foram sintetizadas por combustão a partir dos pós de seus elementos constituintes. O efeito de variáveis de processo, como o tamanho de partícula dos pós, a composição química, a pressão de compactação, o tratamento de desgaseificação e a taxa de aquecimento, foram investigados na síntese do NbAl3 na forma de pastilhas cilíndricas. A síntese de ligas do sistema Nb-Ni-AI foi realizada a partir de misturas com as composições Nb10Ni70AI, Nb20Ni65AI e Nb30Ni60AI. A microestrutura das amostras reagidas foi caracterizada por microscopia óptica, microscopia eletrônica de varredura, EDS e difração de raios-X (método de Rietveld). Foram obtidas pastilhas de NbAl3 com 98,5 % da densidade teórica, superior ao valor encontrado na literatura (95%), mediante o controle de variáveis de processo. Nas pastilhas contendo níquel, a combustão ocorreu nas pastilhas de todas as composições. Fases metaestáveis, presentes na microestrutura das pastilhas baitas de reação, foram transformadas após tratamento térmico, originando ligas trifásicas com diferentes concentrações de fases (NbAl3, NiAI e NbNiAI), conforme a composição inicial do compactado. Algumas propriedades mecânicas de amostras brutas de reação e tratadas termicamente foram determinadas pela técnica da impressão (microdureza e tenacidade). Os resultados obtidos são comparáveis aos da literatura, salvo algumas discrepâncias atribuídas a processos de fabricação distintos. As etapas de reação da síntese do NbAl3 e de ligas Nb-Ni-AI foram posteriormente investigadas mediante interrupção da reação durante sua propagação ao longo de barras paralelepipédicas compactadas. Verificou-se que a síntese do NbAl3 ocorre pela dissolução de nióbio no alumínio fundido, seguida da precipitação do NbAl3. Nas amostras contendo níquel, a síntese ocorre em dois estágios: no primeiro estágio formam-se o Ni2Al3 ou o NiAl3, em quantidades relativas dependentes da composição geral. As reações deste primeiro estágio podem disparar as reações do segundo estágio, referentes à síntese do NbAl3. / NbAl3 and Nb-Ni-AI intermetallic alloys have been obtained by pressureless combustion synthesis from elemental powders. The effects of process variables as powder particle size, composition, compaction pressure (green density), degassing treatment and heating rate on the combustion (thermal explosion mode) of NbAl3 cylindrical pellets were studied. Combustion synthesis of Nb-Ni-AI alloys was performed on powder mixtures with nominal compositions Nb10Ni70AI, Nb20Ni65AI and Nb30NI60AI. The microstructure of reacted samples was characterized by optical microscopy, scanning electron microscopy, EDS and X-ray diffraction (Rietveld method). It was shown that careful control of the processing conditions allowed near full (98,5%) dense pellets of NbAl3. In the nickel containing pellets, reaction occurred for all the compositions investigated. Metastable phases were seen to be present in the as reacted pellets, which were transformed after a heat treatment, producing a three phase alloy (NbAl3, NiAI and NbNiAI) with different phase concentrations, depending on the initial compact composition. Some mechanical properties, like microhardness and tenacity were measured by microidentation technique on the as reacted and heat-treated samples. The results are comparable with the literature, excepted for some discrepancies caused by different fabrication processes. The reaction sequence for both cases (NbAl3 and Nb-Ni-AI alloys) was further investigated by DSC analysis and also by interrupting the reaction during its propagation along compacted parallelopipedal bars. It was found that the NbAl3 synthesis occurs through niobium dissolution in molten aluminum and precipitation of NbAl3. In the nickel containing samples, synthesis occurs as two-stage reaction: Ni2Al3 or NiAl3 are formed in the first stage, with relative amounts depending on the general composition. This first stage reaction can trigger the second one, related to the formation of NbAl3.

Cette thèse présents plusieurs techniques de caractérisation appliqués à diverses matières organiques dans le but de démêler leur structure-propriétés relation once encapsulés comme matériaux actifs dans les dispositifs de OFET. Un soin particulier est alors dédié aux méthodes de caractérisation structurale (2D-GIXRD, XRR et XRD) à la fois de source de laboratoire classique et de rayonnement de synchrotron. Divers matériaux polymères organiques, compris de p- et n-type de petites molécules et polymères en solution ou déposés par sublimation sous vide sont étudiées. En particulier, l'étude de OFET basée sur deux fonctionnalisés isomères péryléne ne différant que par la forme des alkyle côté chaînes démontre comment la nature ramifié et asymétrique des chaînes peut conduire à une amélioration de la performance électrique avec un simple traitement thermique post-dépôt, tandis que la fabrication de dispositifs ambipolaire polymères au moyen de la technique Langmuir-Schaefer souligne l'importance de la méthode de dépôt sur l'agencement de la matière sur la surface du substrat. Une approche inhabituelle, nommé enquête structurelle in_situ et en temps réel, est aussi présenté pour évaluer les modifications structurelles dans les films minces organiques subissent un processus particulier. Plus précisément, la réponse de la structure des films minces de pentacene à l’application de VSG et VSD au OFET et des films minces dérivés de TTF à la variation d’humidité ont été étudiés. / This thesis presents multiple characterization techniques applied to various organic materials with the ultimate goal of unraveling their structure-properties relationship once encapsulated as active materials in OFETs devices. Particular care is then dedicated to the structural characterization methods (2D-GIXRD, XRR and XRD) both from classical laboratory source and from synchrotron radiation. Various organic materials, comprising p- and n-type small molecules and polymers deposited from solution or by vacuum sublimation are investigated. In particular, the study on OFETs based two functionalized perylene isomers differing only in the shape of the alkyl side-chians demonstrates how the branched and asymmetric nature of the chains can lead to an improvement of the electrical performance with a simple post-deposition thermal treatment, while the fabrication of ambipolar polymeric devices by means of Langmir-Schaefer technique highligts the importance of the deposition method on the arrangement of the material on the substrate surface. A more unusual approach, named in-situ and real-time structural investigation, is also presented to evaluate structural modifications in organic thin films undergoing a particular process. Specifically, the structural responce of pentacene thin films to the application of VSG and VSD to the OFET and of TTF derivatives thin films to the variation of humidty were investigated.

Cette thèse porte sur les propriétés magnétiques et structurales de MnAs/GaAs(001) et sur la dynamique photo-induite du système hétéroépitaxial Fe/MnAs/GaAs(001). MnAs présente une séquence inhabituelle de transitions de phases magnéto-structurales. En volume, α-MnAs est hexagonal et ferromagnétique (FM). A 313 K, il transite (1er ordre) vers β-MnAs, perd son ordre FM et devient orthorhombique. A 400 K, il transite (2nd ordre) vers γ-MnAs, hexagonale et paramagnétique. En couche mince épitaxiée sur GaAs(001), α- et β-MnAs coexistent entre 283 et 313K sous la forme de bandes auto-organisées avec alternance des phases ce qui permet l’émergence d’un champ magnétique dipolaire de surface. Ce champ permet de manipuler via la température, et sans champ magnétique appliqué, l’aimantation de Fe, ou encore localement via une impulsion laser femtoseconde. Des mesures ont été réalisées sur ce système par effet Kerr magnéto-optique (MOKE) et par diffusion résonante des rayons X (XRMS). La XRMS donne accès à l’évolution en température des bandes et à l’aimantation de chacune des couches (aux seuils L3 de Fe et de Mn). Il est montré que les cycles de chaque couche peuvent être obtenus aussi bien par MOKE que par XRMS grâce à la linéarité de la réponse MOKE. La dynamique structurale photo-induite de MnAs/GaAs(001) a aussi été étudiée par diffraction des rayons X résolue en temps sur des temps allant de la picoseconde à la microseconde. Ces résultats mettent en évidence l’excitation de phonons cohérents, la génération d’une onde de déformation, la nucléation de la phase γ et enfin la formation transitoire de bandes auto-organisées pendant la phase de refroidissement. Ces résultats ont été corrélés aux résultats sur le renversement de l’aimantation du fer dans Fe/MnAs et un mécanisme est proposé. / The subject of this thesis is the study of the magnetic and structural properties of MnAs/GaAs(001) and of the photoinduced phase transition dynamics in MnAs/GaAs(001). MnAs exhibits a peculiar sequence of magneto-structural phase transitions. In the bulk, α-MnAs is hexagonal and ferromagnetic (FM). At 313K, it transits (1st order) towards β-MnAs becoming orthorhombic and FM order is lost. At 400K, it transits (2nd order) towards γ-MnAs becoming paramagnetic and hexagonal. When MnAs is grown epitaxially on GaAs(001), α and β phases coexist in the form of self-organized stripes with alternating phases, which permits the appearance of a dipolar magnetic field close to the surface. This field allows the manipulation of the Fe magnetization via the temperature, without applying magnetic field, or locally via a femtosecond laser pulse. Measurements were made using magneto-optical Kerr effect (MOKE) and X-ray resonant scattering (XRMS). The XRMS gives access to the evolution of the stripes with the temperature and to the magnetization of each layer (at the L3 edge of Fe and Mn). Hysteresis cycles of magnetic layers can be obtained by XRMS and also by MOKE thanks to the linearity of the response. The photo-induced structural dynamics of MnAs/GaAs(001) was also studied by time-resolved X-ray diffraction from the picosecond to the microsecond timescales. The results evidence the excitation of coherent phonons, the generation of a strain wave, the nucleation of the γ phase, and finally the transient formation of self-organized stripes during the cooling phase. These results provide insight into the Fe magnetization reversal process in Fe/MnAs/GaAs(001) and a mechanism is proposed.

The purpose of this study was to evaluate four different measuring methods as potentialquality control tests for Tungsten Carbide (WC) raw material used in the hard metalmanufacturing at Seco Tools Fagersta. This was warranted as the current quality testcalled the HcK test, is very time consuming and the results provided that are used formilling time calculations cannot be relied on. The four measuring methods chosen wasLaser diffraction, X-Ray diffraction, Brunauer Emmett Teller analysis and Fisher Sub-Sieve Sizer measurement. These measuring techniques were chosen by Seco ToolsThe project followed the general structure of the project cycle modified to fit the projectand involving the steps project planning, present state analysis, goals and requirementdetermination, evaluation elimination of options and final of choice of option. Thealternative methods were evaluated using an evaluation matrix containing therequirements determined to be the most relevant for the quality control process. Therequirements were measurement precision, operator influence, ease of use, time requiredand operator time required. The ability of the measurement method to distinguishbetween all of the different WC powders used a Seco Tools was put as a must requirementas the new method is meant to serve as a verification test as well as a quality test.The analysis methods were evaluated practically through experiments and therefore atesting strategy was established. Initial test on two powder types was performed so thatan early evaluation could be done. During this stage both the Laser diffraction and the XRaydiffraction were eliminated due to poor results. The BET analysis and the Fisher Sub-Sieve Sizer performed better and was therefore tested further. Randomized testing wasthe method chosen when testing with all powders to minimize the environmental impacton the testing as this could affect the results of the study.The testing showed that only the Fisher SSS was able to distinguish between all thedifferent powders making it the only viable option as a new quality test. This was onlypossible when measuring on agglomerated material and the values extracted couldtherefore not be used further in the production. The Fisher SSS also performed the bestwhen ranked against the rest of the requirements, showing a high precision whenmeasuring on deagglomerated material and a combination of the two tests was thereforeconsidered.When compared to the HcK test the Fisher SSS showed a significant reduction in lead timebut also a reduction in information gathered and eventual defects controlled. The FisherSSS provides only an average particle size measurement and since no correlation has yetbeen established between the measured particle size and the required milling times it wasrecommended that the HcK test remains.It was recommended that a study is started aimed at establishing a correlation betweenthe measured particle size and the required milling time is started to investigate if this ispossible.