One-dimensional Si3N4 nanostructures are desirable for constructing nanoscale electric and optoelectronic devices due to their peculiar morphologies. Herein, a facile and environmentally friendly catalyst-free method is proposed to synthesize ultra-long single crystal α-Si3N4 nanobelts via carbothermal nitridation of carbon nanotubes at 1750 °C. The obtained α-Si3N4 nanobelts with a flat surface (thickness of ∼150 nm, length of several millimeters) exhibited an extremely high aspect ratio, perfect crystal structure, and high specific surface area of 7.34–10.09 m2 g−1. In addition, the width was increased from approximately 80 nm to 8 μm by increasing the holding time from 1 to 3 h. The nanobelt formation was governed by the vapor–solid (VS) reaction between SiO vapor, N2 and carbon nanotubes, and the vapor–vapor reaction between SiO, CO and N2. The former was responsible for the initial nucleation and successive base-growth of α-Si3N4 nanotubes. The latter additionally contributed to the nanorod and subsequent proto-nanobelt formation and to the growth of the nanobelts. During high-temperature annealing at 1750 °C, the original Si3N4 nanotubes gradually transformed into nanorods, and, finally, nanobelts with stable shapes as a result of surface energy minimization.
In this study, zirconium nitride nanopowders with a high specific surface area were synthesized by carbothermal nitridation with fructose as a double-function additive. The precursor was prepared by an internal gelation process. The first function of fructose was to act as an organic carbon source for the nitridation reaction to decrease the apparent activation energy . The second function of fructose was to act as a microstructural controller of products to obtain a high specific surface area of 315.7 m 2 /g. The effects of temperature on the phase composition, chemical elements, morphology and specific surface area were investigated. The microstructure development upon heating was illustrated and the relationship between the structure evolution and variation in the specific surface area was elucidated. This method with fructose as a water-soluble organic additive could be expanded to prepare transition metal nitrides with a high specific surface area.
Zirconium compounds has been widely attention over the last decades due to its excellent physical and chemical properties. Zirconium nitride nanopowders were synthesized via a simple direct carbothermic nitridation process of internal gel derived zirconia in the presence of nano-sized carbon black. The effects of reaction temperature, dwell time and molar ratio of carbon black to Zr (C/Zr) on the phase composition, grain size and crystal parameters of products were studied. Based upon the analysis of crystallite phase evolution and microstructure characterization, it was found that zirconium oxynitride is intermediate product and then O atoms in oxynitride were extracted by oxygen getter, carbon black. Anion sites were directly replaced by N atoms to form rock-salt type nitride in carbothermic nitridation process.
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