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肼溶胶-凝胶法制备高比表面积纳米氮化钛粉体的研究

刘美英, 由万胜, 雷志斌, 宗旭, 应品良, 李灿   

  1. 中国科学院大连化学物理研究所催化基础国家重点实验室, 大连 116023
  • 收稿日期:2005-10-21 修回日期:1900-01-01 出版日期:2006-08-10 发布日期:2006-08-10
  • 通讯作者: 李灿

Synthesis of TiN Nanocrystals with High Specific Surface Area by Hydrazide Sol-gel Method

LIU Mei-Ying, YOU Wan-Sheng, LEI Zhi-Bin, ZONG Xu, YING Pin-Liang, LI Can   

  1. State Key Laboratory of Catalysis Basis, Dalian Institute of Chemical Physics, Chinese Academy of Sciences, Dalian 116023, China
  • Received:2005-10-21 Revised:1900-01-01 Online:2006-08-10 Published:2006-08-10
  • Contact: LI Can

摘要: 以无水肼作氮源, 采用肼溶胶-凝胶技术(HSG)成功地制备了TiN粉体, 研究了不同钛源、处理气氛及焙烧温度对TiN粉体晶化过程的影响, 并对其形成机理进行了讨论. 与氨气氮化法相比, 该方法所需温度低、TiN的粒径小、比表面积大, 并且分散均匀.

关键词: 肼, 溶胶-凝胶, 低温, 大比表面积, 纳米TiN

Abstract: Nanocrystalline TiN with a high specific surface area was successfully prepared by the hydrazide sol-gel method with N2H4 as the nitrogen source. The effects of Ti sources, heat-treatment atmospheres, and temperature on the crystallization of TiN powder were studied and the crystallization mechanism of TiN nanocrystals was also discussed. TiCl3 is superior to TiCl4 and isopropoxide in the formation of well-crystallized TiN nanocrystals. NH3 has the advantage over N2 and Ar in the complete removal of residual carbon in TiN powder. In comparison with the traditional temperature-programmed reduction under flowing NH3 atmosphere, the hydrazide sol-gel route requires a relatively low temperature on the one hand(600 ℃) and TiN powder prepared by this synthetic approach exhibits a small particle size(10 nm) and an exceedingly high specific surface area(>135 m2/g) and disperses uniformly on the other hand. We expect that this methodology will provide a novel low-temperature route to synthesize nanocrystalline transition metal nitrides through choosing hydrazine as N-source precursor.

Key words: Hydrazine, Sol-gel, Low temperature, High specific surface area, Nano TiN

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