Etude du procédé de croissance de films de diamant nanocristallin par dépôt chimique en phase vapeur assisté par plasma micro-onde distribué, à basse température et basse pression

Abstract : This PhD thesis focuses on the understanding and the control of the nanocrystalline diamond (NCD) film growth process by distributed antenna array microwave plasma-assisted chemical vapor deposition. Two approaches were followed to reach these objectives: a « material » study aiming at studying the nucleation and growth mechanisms and the characteristics of the synthesized NCD films; a « plasma » study focusing on the diagnostics of H₂/CH₄/CO₂ low-pressure discharges used for NCD growth.Concerning the first part of this work, ex situ characterization techniques, such as scanning and high resolution transmission electron microscopy, atomic force microscopy, Raman spectroscopy, X-ray diffraction, UV-visible reflectometry, and in situ, such as laser reflectance interferometry, were used to study the nucleation density, morphology, topography, microstructure, purity, and growth rate of NCD films. The influence of some process parameters, such as chamber pressure, substrate position, gas composition, surface temperature, microwave power and ex situ substrate pretreatment, has been studied for silicon. The synthesis of NCD down to a substrate temperature as low as 130 °C has been thus investigated. The feasibility of NCD growth at this temperature on a polymeric material such as polytetrafluoroethylene (PTFE) has been demonstrated. The growth of NCD films on other kinds of substrates such as silicon nitride and stainless steel was also examined.Concerning the second part of this work, the diagnostics of the deposition plasma was carried out by optical emission spectroscopy and infrared absorption spectroscopy using wavelength-tunable laser diodes and external cavity quantum cascade lasers as radiation sources. The influence of the experimental conditions, in particular of the microwave power and the pressure in the chamber, on the concentration of the methyl radical CH₃, the diamond growth precursor, and of five stable molecules (CH₄, CO₂, CO, C₂H₂, C₂H₆), as well as on the degree of dissociation of H₂ and the kinetic, vibrational and rotational temperatures of the species, was studied. The high degree of dissociation of gas precursors, for a relatively low gas temperature of a few hundred degrees, indicates that the plasma chemistry is mainly governed by electronic processes. The considered distributed microwave plasma system nevertheless allows to produce some growth and etching species in amount comparable to conventional NCD growth processes, while permitting low temperature synthesis process.
Keywords : In situ diagnostic
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Benoit Baudrillart. Etude du procédé de croissance de films de diamant nanocristallin par dépôt chimique en phase vapeur assisté par plasma micro-onde distribué, à basse température et basse pression. Génie des procédés. Université Sorbonne Paris Cité, 2017. Français. ⟨NNT : 2017USPCD051⟩. ⟨tel-02186838⟩

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