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Elaboration de particules nanostructurées de nitrures et d'oxynitrures métalliques en milieu fluide supercritique. Etude et modélisation des mécanismes de croissance des particules

Abstract : Macroscopic and microscopic supercritical fluids properties can be easily tuned by weak variations of pressure and temperature near their critical point. So they represent an interesting alternative for nanomaterials synthesis. In this study we achieved an explorative research about thermal decomposition of metal precursors to allow a controlled synthesis of metal nitride nanoparticles in supercritical fluid. This decomposition, in supercritical conditions, permits to feed reactive media with metal atoms that react with supercritical ammonia to form nitride nanostructured particles. The aim is to couple within the material, intrinsic properties of nitrides with properties linked to nanoscopic scale. Firstly, we studied experimental parameters effect on material chemical composition and on material morphology in order to define the process potentialities. We showed that the limiting factor for this process is the oxygen presence in the experimental set-up which induces the formation of oxinitride. Next, we focus our researches on nickel nitride, Ni3N. Chemical and structural analysis revealed an insertion of oxygen atoms in the Ni3N structure. Nevertheless, we showed experimental conditions effect on morphology of synthesized material in supercritical ammonia. In addition, a preliminary study on magnetic properties of powders was performed. Finally, a numeric model to predict spherical nanostructured aggregates size evolution versus experimental parameters (residence time, precursor concentration, temperature ...) was developed.
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Submitted on : Thursday, October 21, 2004 - 6:49:07 PM
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Sophie Desmoulins-Krawiec. Elaboration de particules nanostructurées de nitrures et d'oxynitrures métalliques en milieu fluide supercritique. Etude et modélisation des mécanismes de croissance des particules. Matériaux. Université Sciences et Technologies - Bordeaux I, 2004. Français. ⟨NNT : 2004BOR12815⟩. ⟨tel-00007176⟩

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