高等学校化学学报 ›› 2017, Vol. 38 ›› Issue (3): 355.doi: 10.7503/cjcu20160572

• 研究论文: 无机化学 • 上一篇    下一篇

氨气还原氮化法制备有序介孔TiN粉体及其电化学性能

倪洁, 魏恒勇(), 卜景龙, 刘会兴, 崔燚, 吕东风, 魏颖娜, 张利芳   

  1. 华北理工大学材料科学与工程学院, 河北省无机非金属材料重点实验室, 唐山 063009
  • 收稿日期:2016-08-11 出版日期:2017-03-10 发布日期:2017-02-23
  • 作者简介:联系人简介: 魏恒勇, 男, 博士, 副教授, 主要从事氮化物材料合成研究. E-mail: why_why2000@163.com
  • 基金资助:
    国家自然科学基金(批准号: 51272066)、 河北省自然科学基金(批准号: E2013209183)和华北理工大学青年科学研究基金(批准号: Z201413)资助.

Synthesis of Ordered Mesoporous TiN Powder via Ammonia Reduction Nitridation Reaction and Its Electrochemical Performance

NI Jie, WEI Hengyong*(), BU Jinglong, LIU Huixing, CUI Yi, LÜ Dongfeng, WEI Yingna, ZHANG Lifang   

  1. College of Material Science and Engineering, Hebei Provincial Key Laboratory of Inorganic Nonmetallic Materials,North China University of Science and Technology, Tangshan 063009, China
  • Received:2016-08-11 Online:2017-03-10 Published:2017-02-23
  • Contact: WEI Hengyong E-mail:why_why2000@163.com
  • Supported by:
    † Supported by the National Natural Science Foundation of China(No.51272066), the Natural Science Foundation of Hebei Province, China(No.E2013209183) and the Youth Science Research Foundation of North China University of Science and Technology, China(No.Z201413).

摘要:

以四氯化钛为原料, 嵌段共聚物P123(PEO20-PPO70-PEO20)为模板剂, 氰胺为稳定剂, 采用非水解溶胶-凝胶法制备有序介孔TiO2粉体, 再经氨气还原氮化处理得到有序介孔TiN粉体. 利用广角/小角X 射线衍射、 电子显微镜和N2气吸-脱附等对TiN粉体的结构进行了表征, 并通过循环伏安和充放电测试表征了电化学性能. 结果显示, 该粉体为高纯立方TiN相, 呈球形颗粒状, 具有有序介孔结构, 比表面积高达97 m2/g. 在不同扫描速率下循环伏安曲线均呈类矩形, 根据电流密度为50 mA/g时的恒流充放电(GCD)曲线计算比电容为233 F/g, 且经2000次充放电循环后比容量仍保持90%以上, 在功率密度为0.1 kW/kg时能量密度高达65 W·h·kg-1.

关键词: 氮化钛粉体, 有序介孔, 非水解溶胶-凝胶法, 还原氮化, 电化学

Abstract:

The ordered mesoporous TiN powder was synthesized by reduction-nitridation method based on the nonhydrolytic sol-gel process using titanium tetrachloride as the raw material, P123 as the structure-directing agent and cyanamide as the stabilizer. The structural information of the composite powder was characterized by wide-angle/small-angle X-ray diffraction, scanning electronic microscopy, N2 adsorption-desorption analysis, and the electrochemical properties were characterized by cyclic voltammetry(CV) and galvanostatic charge-discharge(GCD) measurements. The results show that the synthesized TiN powder was highly pure cubic TiN phase and had ordered mesoporous structure, its specific surface area was 97 m2/g. The CV curves at different scan rates look like the rectangle. The specific capacitance was 233 F/g at current density of 50 mA/g, and remained 90% even after 2000 cycles. When the power density was 0.1 kW/kg, the energy density was as high as 65 W·h/kg.

Key words: Titanium nitride powder, Ordered mesopore, Nonhydrolytic sol-gel, Reduction-nitridation, Electrochemistry

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