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Synthèse de films minces de CNx et de SiCN par dépôt chimique en phase vapeur assisté par plasma micro-onde et par dépôt physique en phase vapeur assisté par pulvérisation magnétron réactive

Abstract : This thesis contributes to the study of the synthesis of CNx and SiCN thin films by Microwave Plasma Assisted Chemical Vapour Deposition (MPACVD) and by reactive magnetron sputtering assisted Physical Vapour Deposition (PVD). The study on this subject has begun since the prediction of the existence of a material, particularly the [bêta]-C3N4 phase that could have properties close to those of diamond. The main object of this thesis is to study the growth mechanisms of these thin films in order to optimize their synthesis. The work was divided into 5 chapters. A state of the art made on these types of materials enabled us to show that they have many potential applications. An in-situ study of the microwave discharge in the gas mixture N2/CH4 was systematically carried out according to the experimental parameters, namely, the microwave power, the gas pressure, the total flow rate, the gas percentage, by Optical Emission Spectroscopy (OES). It permits us to observe a maximum reactivity of the discharge at 4% CH4. The films were also realised according to the experimental parameters. This study permits us to show that the methane percentage should be less or equal to 4 % in order to avoid the formation of carbon balls on the surface of obtained films. The micrographs obtained by scanning and transmission electron microscopy show that films are made of nanocristallites with size varying between 20 and 70 nm. A structural study carried out by X-Ray Diffraction, coupled with Electronic Diffraction has shown that the films are probably made of a mixture of [bêta]-C3N4, c-C3N4 and c-SiCN phases. We then studied the microwave discharge in pulsed mode according to the pulse parameters namely, the duty cycle, the frequency and the post-discharge duration. We found more important etching of the film beyond a frequency of 700 Hz. In the fourth chapter, we proposed growth mechanisms of the films and found the role of the silicon in deposition process. This study has enabled us to clearly understand that the silicon in the films comes from the etching of the silicon by the plasma species. The silicon acts as a catalyst and promotes the incorporation of nitrogen in the films. It also helps to stabilize the C3N4 phases. Finally, amorphous SiCN thin films depositing by PVD with silicon and carbon target have been studied. Unlike metallic target, the sputtering of carbon target is easier when it is nitride. The SiCN film deposition rate increases with the nitrogen flow rate without substrate polarization while it decreases very quickly when the substrate is biased because of the re-sputtering of the deposited film as a result of ion bombardment. The substrate biasing promotes formation of strong C=N types bonds observed by Fourier Transformed Infrared Spectroscopy (FTIR). Nanoscratch tests realised on films deposited on different kinds of under-layers have shown that the SiNx under-layer is most appropriate to get a better SiCN film adhesion on the WC-Co substrate.
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Ahoutou Paul Kouakou. Synthèse de films minces de CNx et de SiCN par dépôt chimique en phase vapeur assisté par plasma micro-onde et par dépôt physique en phase vapeur assisté par pulvérisation magnétron réactive. Autre [cond-mat.other]. Université Henri Poincaré - Nancy 1, 2008. Français. ⟨NNT : 2008NAN10018⟩. ⟨tel-01748326⟩

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