One step convenient synthesis of crystalline β-Si3N4

Abstract

Well-crystallized β-Si3N4 was directly prepared at an initial reaction temperature of 150 °C through the reaction of SiCl4 and NaN3 in the presence of a small amount of CCl4. Characterization by X-ray diffraction, high-resolution electron microscopy, X-ray photoelectron spectroscopy and energy dispersive X-ray spectroscopy indicates that the product synthesized is crystalline β-Si3N4. The yield of β-Si3N4 is about 86% based on the amount of precursor SiCl4 used at the initial reaction temperature of 150 °C, and is more than 90% at the reaction temperature of 200 °C with the product β-Si3N4 in high crystallinity. The dominant morphology of the product is short rods with the growth axis along the [001] direction. The formation mechanism of crystalline β-Si3N4 was discussed briefly, and the role of CCl4 in the formation process of β-Si3N4 was analyzed.