Preparation of titanium nitride powders by citrate complex precursor method

doi:10.3969/j.issn.1001-1935.2021.03.004

Abstract

Abstract:

Citric acid complex precursor was prepared by the sol-gel method with citric acid as the complexing agent and tetrabutyl titanate as the titanium source.Then TiN powder was prepared after the heat treatment of the precursor in nitrogen atmosphere.The effects of the reaction temperature (800-1 300 ℃) and the molar ratio of tetrabutyl titanate to citric acid (3:1,2:1,1.7:1) on the proportion of TiN by carbothermal nitridation reduction were studied.The results show that ammonium titanium citrate complex can be prepared by the precursor xerogel;higher citric acid addition is beneficial to the carbothermal reduction reaction;higher heat treatment temperature accelerates the nucleation of TiN;when the molar ratio of tetrabutyl titanate to citric acid is 2:1,equiaxed TiN powder with an average particle size of ~60 nm was prepared after the precursor xerogel was heat treated at 1 200 ℃ in flowing N₂ atmosphere.

Key words: titanium nitrate powder, ammonium titanium citrate, carbothermal reduction nitridation, sol-gel method

摘要：

以一水合柠檬酸为络合剂,钛酸四丁酯为钛源,采用溶胶-凝胶法制备了柠檬酸盐络合物前驱体,然后在氮气气氛中对前驱体进行热处理制备TiN粉体,研究了反应温度(800~1 300 ℃)、原料配比(n(钛酸四丁酯):n(柠檬酸)分别为3:1、2:1、1.7:1)对碳热还原氮化反应制备TiN粉体的影响。结果表明:前驱体干凝胶为柠檬酸钛铵络合物;柠檬酸用量的增加有利于碳热还原反应的进行,热处理温度的升高促进了TiN成核。n(钛酸四丁酯):n(柠檬酸)为2:1时,前驱体干凝胶在流动N₂气氛下经1 200 ℃热处理后制得了平均粒径约60 nm的等轴状的TiN粉体。

关键词: TiN粉体, 柠檬酸钛铵, 碳热还原氮化, 溶胶-凝胶法

CLC Number:

TQ134

Qin Xing, Zhang Jinhua, Wang Jingran, Ni Yue’e, Ke Changming. Preparation of titanium nitride powders by citrate complex precursor method[J]. Refractories, 2021, 55(3): 198-202.

覃星, 张锦化, 王景然, 倪月娥, 柯昌明. 柠檬酸盐络合物前驱体法制备TiN粉体[J]. 耐火材料, 2021, 55(3): 198-202.

Figures/Tables 6

Fig.1 FT-IR spectra of precursor xerogels

Fig.2 XRD spectra of xerogels obtained by heat treatment at different temperatures in N2 atmosphere

Fig.3 TG analysis curve of xerogel

Table 1 Average grain size of TiN

试样编号	平均晶粒尺寸/nm
试样编号	1 100 ℃	1 200 ℃	1 300 ℃
试样T1	48	58	107
试样T2	47	54	51
试样T3	33	42	32

Fig.4 XPS spectra of products obtained after 1 200 ℃ heat treatment of T2 sample

Fig.5 TEM diagram of TiN powder obtained after 1 200 ℃ heat treatment of T2 sample

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