Caractérisation par infrarouge à transformée de Fourier des réactions chimiques entre post-décharges et précurseurs organosiliciés : cas du 3-aminopropyltriethoxysilane (APTES)

Abstract : The present work deals with the characterization by Fourier transform infrared spectroscopy (FTIR) and by optical emission spectroscopy of chemical reactions between a post-discharge and an organosilicon precursor: the 3-aminopropyltriethoxysilane (APTES). The aim is to keep the highest retention of amine functions -NH2 in coatings or in the synthesized nanoparticles. First, a state of the art of Ar-N2 and Ar-O2 post-discharges and their applications is presented as well as the kinetics of the interaction of APTES in these post-discharges, highlighting the role plasma gases on the decomposition of the precursor and the nature of the deposited films. Then, the study of the decomposition of APTES in an Ar-N2 post-discharge is carried out. Analysis by optical emission spectroscopy (OES) and in situ FTIR show the role of the nitrogen atoms N in the formation of various main by-products, namely HCN, CO and C=O. The synthesized nanoparticles contain few primary amines, and have a significant concentration of nitrogen in the form of secondary amide. In the case of interaction APTES with pulsed Ar-O2 afterglow, there is one main trend: the nanoparticles synthesized in the gas phase when the duty cycle increases have a composition that decreases in nitrogen and carbon but increases in oxygen. The -NH2 groups are efficiently converted into amide groups. The nanoparticles synthesized with high duty cycle exhibit compositions that are different from those of thin films deposited on the walls, the latter being close to silica because of the etching by atomic oxygen, which affects them more. The specific behavior of oxygen and nitrogen atoms in post-discharge makes difficult the retention of a high level of amines in plasma polymers. Finally, we finished with a study of the hydrodynamics in the case of the interaction of acetylene with an Ar-O2 post-discharge and proved the key role of the flow for any approach aiming at getting time-resolved FTIR measurements
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Magamou Gueye. Caractérisation par infrarouge à transformée de Fourier des réactions chimiques entre post-décharges et précurseurs organosiliciés : cas du 3-aminopropyltriethoxysilane (APTES). Autre. Université de Lorraine, 2016. Français. ⟨NNT : 2016LORR0020⟩. ⟨tel-01754637⟩

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