Particle size distribution and dislocation density determined by high resolution X-ray diffraction in nanocrystalline silicon nitride powders

Two silicon nitride powders were investigated by high resolution X-ray diffraction. The first sample was crystallized from the powder prepared by the vapour phase reaction of silicon tetrachloride and ammonia while the second was a commercial powder produced by the direct nitridation of silicon. Their particle size and dislocation density were obtained by the recently developed modified Williamson–Hall and Warren–Averbach procedures from X-ray diffraction profiles. Assuming that the particle size distribution is log-normal the size distribution function was calculated from the size parameters derived from X-ray diffraction profiles. The size distributions determined from TEM micrographs were in good correlation with the X-ray results. The area-weighted average particle size calculated from nitrogen adsorption isotherms was in good agreement with that obtained from X-rays. The powder produced by silicon nitridation has a wider size distribution with a smaller average size than the powder prepared by vapour phase reaction. The dislocation densities were found to be between about 1014 and 1015 m−2.