化工学报 ›› 2020, Vol. 71 ›› Issue (6): 2743-2751.DOI: 10.11949/0438-1157.20200077

• 材料化学工程与纳米技术 • 上一篇    下一篇

流化床化学气相沉积法制备近化学计量比的TiN粉体

桑元1,2(),向茂乔1,宋淼1,2,朱庆山1,2()   

  1. 1.中国科学院过程工程研究所,北京 100190
    2.中国科学院大学化学工程学院,北京 100049
  • 收稿日期:2020-01-19 修回日期:2020-03-22 出版日期:2020-06-05 发布日期:2020-06-05
  • 通讯作者: 朱庆山
  • 作者简介:桑元(1994—),男,硕士研究生,ysang@ipe.ac.cn
  • 基金资助:
    国家自然科学基金青年基金项目(11805227);中国科学院基础前沿科学研究项目(ZDBS-LY-JSC041)

Preparation of nearly-stoichiometric TiN powder by chemical vapor deposition in fluidized-bed

Yuan SANG1,2(),Maoqiao XIANG1,Miao SONG1,2,Qingshan ZHU1,2()   

  1. 1.Institute of Process Engineering, Chinese Academy of Sciences, Beijing 100190, China
    2.School of Chemical Engineering, University of Chinese Academy of Sciences, Beijing 100049, China
  • Received:2020-01-19 Revised:2020-03-22 Online:2020-06-05 Published:2020-06-05
  • Contact: Qingshan ZHU

摘要:

传统气-固反应工艺制备TiN粉体存在难以逾越的内扩散控制过程,导致制备高纯、正化学计量比的TiN粉体至今存在巨大困难。提出了流态化化学气相沉积工艺(FBCVD)制备高质量TiN粉体,即基于TiCl4-N2-H2体系,在往复运动的TiN种子粉体上沉积新生高质量TiN粉体的新方法。实验发现,当TiN种子粉体粒径大于52.95 μm时,即使在1000℃沉积2 h也不会失流,同时在TiN种子粉体上获得了亚微米级的结节状新生TiN颗粒。通过氧氮分析仪和XRD分析发现,新方法显著提升了粉体的氮含量,获得了近化学计量比的TiN0.96,且氧含量下降了约40%。此外,流化床中气相沉积TiN的生长模式为岛状生长模式,为工业中制备高质量TiN粉体提供了一种新的方法。

关键词: 流化床化学气相沉积, 氮化钛, 粉体, 化学计量比

Abstract:

The traditional gas-solid reaction process for preparing TiN powder has an insurmountable internal diffusion control process, which has caused great difficulties in preparing high-purity, positive stoichiometric ratio TiN powder. Herein, to address the issue, a fluidized bed chemical vapor deposition (FBCVD) process was developed to fabricate high quality TiN powders based on TiCl4-N2-H2 system. The results showed that when the average particle size of TiN seeds was larger than 52.95 μm, they can realize long-term stable fluidization at 1000℃ even for 2 h and the obtained powders was nearly stoichiometric ratio TiN0.96. In addition, the oxygen content of obtained TiN powders decreased about 40% compared with raw TiN seeds. Moreover, the growth of TiN was controlled by the Volmer-Weber growth mode, which provides a new horizon for preparing high quality TiN powder in industry.

Key words: fluidized-bed chemical vapor deposition, titanium nitride, powder, stoichiometric

中图分类号: