The effect of heat-treatment on the grain-size of nanodisperse plasmathermal silicon nitride powder

Nanodisperse silicon nitride has been synthesized by vapor phase reaction of silicon tetrachloride and ammonia in a thermal plasma reactor and crystallized at temperatures 1250, 1350, 1450 and 1500 degrees C. The average grain-size and the dislocation density of the samples were determined by the recently developed modified Williamson-Hall and Warren-Averbach procedures from X-ray diffraction profiles. A new numerical method provided log-normal grain-size distributions from the size parameters derived from X-ray diffraction profiles. It has been shown that the average grain-size in the amorphous phase is lower than that observed in the crystalline fraction. On the other hand, the average grain-size in the crystalline fraction decreases up to 1450 degrees C while it increases during heat-treatment at 1500 degrees C. The size distribution and the area-weighted average grain-size obtained by X-rays were in good agreement with those determined by TEM and from the specific surface area, respectively. The dislocation density was found to be of the order of 10(14) and 10(15) m(-2). (C) 2000 Kluwer Academic Publishers.