Transmission electron microscopy study of low-temperature silicon epitaxy by plasma enhanced chemical vapor deposition

Abstract : This thesis focuses on low temperature (LT, ~200°C) epitaxial growth of silicon thin films by plasma enhanced chemical vapor deposition (PECVD) for solar cell applications. Our starting goal was to acquire a better understanding of epitaxial growth, by using transmission electron microscopy (TEM) as the main experimental tool. First, we investigated the initial stages of epitaxial growth using SiF4/H2/Ar chemistry by performing a series of short depositions – from few tens to few hundred of seconds – on different types of substrates. We made a correlation between cross-sectional and plan-view TEM images and in-situ ellipsometry measurements. We discussed the growth mechanisms under the hypotheses of the traditional growth mediated by atoms, radicals and ions and the relatively new approach based on the melting of plasma generated nanoparticles upon impact with the substrate. Additionally, in order to understand how epitaxy by LT-PECVD is sustained, we studied how it is lost or how it breaks down. For that, experiments of intentional breakdown of epitaxy were performed by either increasing the RF power or the hydrogen flow rate using the same SiF4/H2/Ar chemistry. In both cases, the breakdown mechanism was based on the development of twins and stacking faults thus disrupting epitaxial configuration; this was accommodated with surface roughening. Thanks to this new understanding of epitaxy breakdown, we can propose some ways to sustain epitaxy for higher thicknesses. Moreover, we fascinatingly observed a quasi-fivefold symmetry in the diffraction patterns for these layers and for layers deposited using SiH4/H2/HMDSO/B2H6/Ar plasma chemistry as well. We attributed such symmetry to the breakdown of epitaxy through multiple twinning. We developed a quantitative analysis method to discriminate twin positions from random microcrystalline ones in the diffraction patterns and to estimate the number of twin operations. We also discussed some probable reasons for the occurrence of twinning and multiple twinning in a fivefold symmetry fashion. Finally, one important achievement to the TEM world is the optimization, during this doctoral work, of the traditional TEM sample preparation (tripod polishing), transforming it from a long and boring method to a fast method that is competitive with the relatively expensive focus ion beam (FIB) technique.
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Farah Haddad. Transmission electron microscopy study of low-temperature silicon epitaxy by plasma enhanced chemical vapor deposition. Materials Science [cond-mat.mtrl-sci]. Université Paris-Saclay, 2016. English. ⟨NNT : 2016SACLX107⟩. ⟨tel-01508918⟩

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