TiO2微波碳热合成纳米TiC及其转化过程研

doi:10.15541/jim20160642

无机材料学报 ›› 2017, Vol. 32 ›› Issue (9): 991-996.DOI: 10.15541/jim20160642 CSTR: 32189.14.10.15541/jim20160642

TiO₂微波碳热合成纳米TiC及其转化过程研

袁振侠¹, 陆有军^{1, 2}, 陈炜晔¹, 吴澜尔^{1, 2}

(北方民族大学 1. 材料科学与工程学院; 2. 粉体材料与特种陶瓷省部共建重点实验室, 银川750021)

收稿日期:2016-11-25 修回日期:2016-01-05 出版日期:2017-09-30 网络出版日期:2017-08-29
作者简介:袁振侠(1992-), 男, 硕士研究生. E-mail: 2394053570@qq.com
基金资助:
国家自然科学基金(51662002);国家民委科研项目(14BFZ006);2015年宁夏回族自治区科技创新领军人才项目

Preparation of TiC Nano-particles and Transformation of TiO₂ via Microwave Carbothermic Reduction Rout

YUAN Zhen-Xia¹, LU You-Jun^{1, 2}, CHEN Wei-Ye¹, WU Lan-Er^{1, 2}

(1. School of Material Science and Engineering, Beifang University of Nationalities, Yinchuan 750021, China 2. Key Laboratory of Powder Materials & Special Ceramics, Beifang University of Nationalities, Yinchuan 750021, China)

Received:2016-11-25 Revised:2016-01-05 Published:2017-09-30 Online:2017-08-29
About author:YUAN Zhen-Xia. E-mail: 2394053570@qq.com
Supported by:
National Natural Science Foundation of China (51662002);Project of State Ethnic Affairs Commission (14BFZ006);Innovative Talents of Ningxia

摘要/Abstract

摘要：

以TiO₂和纳米炭黑为原料, 机械干法混合后, 在Ar气氛下微波碳热合成纳米TiC。合成产物通过XRD和SEM进行表征, 研究了TiO₂粒径、反应温度、保温时间对微波碳热合成纳米TiC物相、显微形貌和TiO₂自身转化率的影响。实验结果表明, 微波碳热还原合成纳米TiC经1300℃保温40 min和1400℃保温30 min可使TiO₂充分反应, 且粒径为40 nm的TiO₂的转化率可达到98.2%, 合成的TiC粒度分布均匀, 平均粒径约小于100 nm。此外, 根据固相扩散机制对不同反应温度下两种粒径TiO₂转化率随时间的变化进行了Avrami方程拟合, 并绘制了两种粒径TiO₂的转化曲线, 为TiO₂与纳米炭黑微波合成纳米TiC提供理论参考。

关键词: 纳米TiC, 微波合成, 物相分析, 扩散机制

Abstract:

TiC powders were prepared via microwave carbothermic reduction in Ar with TiO₂ and nano-carbon black as starting materials. Effects of TiO₂ particle sizes, temperature and holding time on phase compositions, particle morphologies and TiC yields in the reaction products were investigated by means of X-ray diffraction (XRD) and scanning electron microscopy (SEM). Avrami equation was fitted to the change of TiO₂ conversion with time at different temperatures. Results show that TiO₂ powders with average diameters ranging from 40 to 400 nm were fully reduced at 1300-1400℃ for 30-40 min with TiC yield as high as 98.2%. TiC powder with uniform particle size less than 100 nm was obtained in case of reaction at 1400℃ for 30 min by using 40 nm TiO₂ as starting material. Transformation curves of TiO₂ were prepared for the synthesis of nano-TiC by microwave carbothermic reduction.

Key words: nano-TiC, microwave synthesis, phase analysis, diffusion mechanism

中图分类号:

TQ174

袁振侠, 陆有军, 陈炜晔, 吴澜尔. TiO₂微波碳热合成纳米TiC及其转化过程研[J]. 无机材料学报, 2017, 32(9): 991-996.

YUAN Zhen-Xia, LU You-Jun, CHEN Wei-Ye, WU Lan-Er. Preparation of TiC Nano-particles and Transformation of TiO₂ via Microwave Carbothermic Reduction Rout[J]. Journal of Inorganic Materials, 2017, 32(9): 991-996.

图/表 7

图1 40 nm的TiO2在不同温度反应30 min产物的XRD图谱

Fig. 1 XRD patterns of the products synthesized at different temperatures for 30 min by using 40 nm TiO2 powders

图2 40 nm(a)和400 nm(b)的TiO2在1300℃合成产物的XRD图谱

Fig. 2 XRD patterns of products synthesized at 1300℃ using 40 nm (a) and 400 nm (b) TiO2 powders as raw material

图3 不同粒径TiO2 1300℃-40min合成产物的XRD图谱

Fig. 3 XRD patterns of products synthesized at 1300℃ for 40 min using TiO2 powders with different particle sizes as raw material

图4 合成TiC颗粒的EDS能谱图

Fig. 4 EDS spectrum of the synthesized TiC grain

图5 不同条件下合成TiC的SEM照片

Fig. 5 SEM images of TiC powder prepared under different conditions (a) 40 nm TiO2, 1400℃-30 min; (b) 400 nm TiO2, 1400℃-30 min; (c) 40 nm TiO2, 1300℃-40 min; (d) 400 nm TiO2, 1300℃-40 min

图6 40 nm(a)和400 nm(b) 的TiO2不同温度Avrami方程拟合图及其温度-时间-转化曲线

Fig. 6 Fitting curves of Avrami equation at different temperature and the Temperature-Time-Conversion graph using 40 nm (a) and 400 nm (b) TiO2 powders as raw material

表1 40 nm和400 nm TiO2不同温度下反应的扩散系数

Table 1 Diffusion coefficient of the reaction system at different temperature using 40 nm TiO2 and 400 nm TiO2 powders as raw material

d₅₀/nm	Temperature/℃	D	Standard error
40	1200	0.02063	0.00255
	1300	0.07091	0.00353
	1400	0.15901	0.01508
400	1200	0.01677	0.00288
	1300	0.05615	0.00221
	1400	0.11888	0.00899

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TiO₂微波碳热合成纳米TiC及其转化过程研

Preparation of TiC Nano-particles and Transformation of TiO₂ via Microwave Carbothermic Reduction Rout

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