X-ray powder diffraction analysis of a silicon carbide-based ceramic

Abstract Accurate X-ray powder diffraction (XRD) analysis of SiC-based ceramics is a difficult task due to the significant overlap of the Bragg reflections from the different SiC polytypes. For this reason, results obtained by traditional XRD methods are, in general, unsatisfactory. Here, we have applied the Rietveld and two line-broadening (variance and integral breadth) methods to analyze a liquid phase-sintered SiC sample. The Rietveld method was used to carry out the quantitative phase-composition analysis and to resolve (as a first step) the overlapped SiC Bragg reflections. Starting from the Rietveld results, the different SiC peaks were then unambiguously obtained by a Levenberg–Marquardt non-linear least-squares fit. Subsequently, the variance and integral breadth methods were used to perform the microstructural analysis. It is shown not only that the procedure is especially useful, but also that both line-broadening methods lead to similar crystallite sizes. The co-existence of β (3C) and α (4H and 6H) SiC polytypes and the nanometric diffraction domain sizes for the SiC polytypes were also found. Finally, these results are discussed in the light of the β to α partial transformation that took place during the sintering.