Solvothermal Synthesis of Si₃N₄ Nanomaterials at a Low Temperature

Abstract

Silicon nitride nanowires or nanorods have been synthesized from SiCl 4 , NaN 3 , and metallic Mg at temperatures ranging from 2001 to 3001C. X-ray powder diffraction patterns indicated that the as-obtained products were mainly b-Si 3 N 4 . Scanning electron microscope and high-resolution transmission electronic microscopy showed that the samples mostly consisted of Si 3 N 4 nanowires or nanorods. As metallic iron powder was used, a-Si 3 N 4 was mainly formed at 2501C.

Orthogonal Design‐Assisted Solvothermal Strategy for Preparing Silicon Nitride Nanodendrites on a Large Scale

“…Here, the dose of NaN 3 in all the experiments is an invariable 2 g as a limited reactant. The orthogonal experiments were carried out according to the process reported by Guo et al 19 …”

“…18 In this study, we brought forward an orthogonal strategy based on a convenient method using NaN 3 and SiCl 4 in the range of 200-3501C to synthesize a mixture of aand b-Si 3 N 4 nanocrystals. 19 Orthogonal experiments were designed to obtain the optimized conditions for the synthesis of Si 3 N 4 in a 20 mL autoclave, and then magnified experiments were carried out in a 1 L autoclave with a conversion ratio exceeding 50%. (Warning: these procedures should be done carefully, because NaN 3 can cause an explosion if treated incorrectly.…”

Growth and Mechanism of Network‐Like Branched Si3N4 Nanostructures

“…Many groups fabricated various Si 3 N 4 nanostructures via different routes such as chemical vapor deposition, 3 thermal decomposition/nitridation, 5 solvothermal synthesis, 6 carbothermal reduction and nitridation of Si–C xerogels, 7 and catalyst‐assisted pyrolysis of polymer precursors 8 . The prepared Si 3 N 4 nanostructures included nanowires, 9 nanobelts, 10 nanorods, 11 nanodendrites, 12 and nanotubes 13 .…”

Additive‐Assisted Nitridation to Synthesize Si3N4 Nanomaterials at a Low Temperature

“…However, this reaction was difficult to repeat. If Mg powder was added to the reaction system of SiCl 4 and NaN 3 , β‐Si 3 N 4 nanowires or nanorods were prepared at 200°–300°C 17 …”

“…If Mg powder was added to the reaction system of SiCl 4 and NaN 3 , b-Si 3 N 4 nanowires or nanorods were prepared at 2001-3001C. 17 Si 3 N 4 nanomaterial was also synthesized at a low temperature through solid-state reactions in autoclaves. a-Si 3 N 4 nanorods were synthesized through reduction-nitridation of silica using NaNH 2 at 7001C.…”