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[en] TANTALUM PENTOXIDE CHLORINATION WITH TETRACHLORETHYLENE / [pt] CLORAÇÃO DO PENTÓXIDO DE TÂNTALO COM TETRACLOROETILENOTAIANE FRACALOSSI ZOCATELLI 18 February 2019 (has links)
[pt] Processos de ustulação cloretante podem ser realizados de forma direta, utilizando o Cl2 como agente cloretante, ou através de agentes cloretantes alternativos. Neste contexto, compostos organoclorados são promissores, pois além de serem facilmente volatizados, já apresentam na mesma molécula o agente cloretante e redutor. O presente estudo teve como principal objetivo a avaliação quantitativa da cinética de cloração do pentóxido de tântalo com tetracloroetileno através dos modelos do núcleo não reagido (SC) e auto catalítico (AC). Tanto o material inicial, quanto o mesmo após o processo, bem como o produto sólido depositado na saída do reator foram caracterizados via DRX e MEV/EDS. Através de simulações termodinâmicas foi possível verificar a viabilidade de cloração de amostras puras de Ta2O5 com C2Cl4 diluído em atmosfera de N2 na faixa de temperatura entre 800 a 950 graus Celsius, sendo os principais cloretos gasosos formados, TaOCl3 e TaCl5. Verificou-se ainda a possível decomposição térmica do agente cloretante no caminho entre a entrada do reator e a amostra. Os resultados provenientes das caracterizações comprovaram as tendências apontadas pelas simulações termodinâmicas, comprovando a formação exclusiva de cloretos voláteis. No que diz respeito à modelagem cinética ambos os modelos permitiram o ajuste dos dados em nível quantitativo, sendo os valores de energia de ativação global iguais a 93,8 kJ/mol (SC) e 32 kJ/mol (AC). A comparação dos valores obtidos com dados da literatura sugere que o controle é de natureza química, sendo a decomposição do C2Cl4 na superfície das nanopartículas de Ta2O5, possivelmente, a etapa controladora. / [en] Chlorination roasting can be carried out directly, using Cl2 as a chlorinating agent, or through alternative reagents. In this context, organochlorine compounds are promising, since besides being easily volatilized, they already present in the same molecule the chlorinating and reducing agents. The present study had as main objective the quantitative evaluation of the chlorination kinetics of tantalum pentoxide with tetrachlorethylene through the shrinking core (SC) and auto catalytic (AC) models. The initial material, as well as post-processed materials, and also the solid product deposited at the reactor s exit were characterized through DRX and MEV/EDS. By means of thermodynamic simulations, it was possible to verify the viability of pure Ta2O5 samples chlorination with C2Cl4 diluted in N2 in the temperature range of interest (800 - 950 Celsius Degree), thereby producing only gaseous chlorides, TaOCl3 and TaCl5. The possible C2Cl4 thermal decomposition in the path between the reactor inlet and sample was also identified. The characterization results were in accordance with the tendencies indicated by the thermodynamic simulations, proving the exclusive formation of volatile chlorides. With regard to the kinetic study, both tested models allowed quantitative adjustment of the conversion data, with overall activation energies equal to 93.8 kJ/mol (SC) and 32 kJ/mol (AC). The comparison of the values obtained with literature data suggests that the control is of chemical nature, the decomposition of C2Cl4 on the surface of the Ta2O5 nanoparticles being, possibly, the main control reaction step.
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Revêtement de Phosphate de calcium sur dioxyde de titane pour des implants métalliques pour des applications médicales / Compound coatings of Ca-phosphates and/ titanate on metallic implants for medical applicationsMohamed, Ibrahim 10 September 2013 (has links)
Pour combiner les bonnes propriétés mécaniques des matériaux métalliques et obtenir des surfaces bioactives, des revêtements de phosphate de calcium (Ca-P) ont été développés. Le but est d’améliorer la biocompatibilité et la bioactivité du système et créer une barrière contre l’éventuelle libération d’ions toxiques du substrat métallique. Notre démarche a été de développer une nouvelle voie de synthèse. Après un polissage mécanique et décapage chimique du substrat de Titane ou Ti–6Al–4V une couche intermédiaire en titanate de sodium a été obtenue par un prétraitement alcalin sur les substrats. Elle a été ensuite soumise à un traitement thermique afin de créer une couche alvéolaire nanométrique. Celle-ci facilite la croissance une couche de phosphate de calcium par voie autocatalytique d'une manière similaire au procédé de formation de l'os naturel. La caractérisation et l’étude des revêtements des Ca-P obtenus par les trois bains (acides, alcalins et oxydant) sur les substrats métalliques ont été réalisés. Les dépôts ont été étudiés d’un point de vue structural et morphologique. La stabilité des couches de Ca-P a été mesurée dans le fluide corporel (SBF) pour des périodes différentes utilisant des analyses biochimiques. En conclusion, cette méthode est une solution peu coûteuse, fiable, et utilisable à l'échelle industrielle. La couche de Ca-P aussi bien que le titanate de sodium obtenus peuvent permettre d’être imprégnés par des agents actifs comme un ou plusieurs agents antibactériens. / To combine the good mechanical properties of metallic substrate with the bioactivity of some ceramics, to obtain bioactive surface, a calcium phosphate (Ca-P) coating has been developed. The goal is to improve the biocompatibility and bioactivity of metallic implant and create a barrier against the possible release of toxic ions from the metallic substrate. Our approach has been to develop a new synthetic route. After mechanical polishing and chemical etching of the titanium or Ti-6Al-4V substrates, an interlayer of sodium titanate was obtained by an alkaline pretreatment of the substrates. Then, it was subjected to a heat treatment to create a nanometeric layer. The latter facilitates the growth of a layer of Ca-P by means of an electroless manner similar to the forming process of the natural bone. Characterization and study of Ca-P coatings obtained by the three baths (acids, alkalis and oxidizing) on metallic substrates have been made. The deposits were studied from a structural and morphological point of view. The stability of Ca-P layers was measured in simulated body fluid (SBF) for different periods using biochemical analyzes. In conclusion, this method is a cheap and reliable solution that can be used on an industrial scale. The Ca-P as well as the sodium titanate layers can afford to be impregnated with active agents such as one or more antibacterial agents.
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