Transactions of Nonferrous Metals Society of China The Chinese Journal of Nonferrous Metals

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中国有色金属学报

ZHONGGUO YOUSEJINSHU XUEBAO

第17卷    第7期    总第100期    2007年7月

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文章编号:1004-0609(2007)07-1072-05
碳热还原合成Ti(C,N)晶须的相转变行为及生长机理
曹顺华,蔡志勇,谢 湛,邹仕民,李春香

(中南大学 粉末冶金国家重点实验室,长沙 410083)

摘 要:

以TiO2和碳黑为主要原料,NaCl为卤化剂,NiCl2作为晶须生长的添加剂,在N2气氛下采用碳热还原法,在不同温度下合成Ti(C,N)晶须。采用X射线衍射研究合成样品的相组成及合成过程中原料的相转变行为,采用扫描电镜观察合成样品的形貌,探讨晶须的生长机理并建立生长模型。结果表明:在1 200 ℃合成时,主要发生TiO2与碳黑、氮气之间的直接还原反应,形成TiN;在温度为1 250~1 400 ℃时,NaCl分解产生的Cl原子起卤化作用,从NiCl2中分解出的Ni起催化作用,合成出Ti(C,N)晶须,晶须长度在10~30 µm之间,直径大约1 µm;合成的晶须表面光滑,顶端残留有催化剂颗粒,具有典型的气−液−固晶须生长机制特征。

 

关键字: 碳氮化钛;碳热还原;晶须;气−液−固机制

Phase transformation behavior and growth mechanism of Ti(C, N)
whiskers synthesized through carbothermal reduction process
CAO Shun-hua, CAI Zhi-yong, XIE Zhan, ZOU Shi-min, LI Chun-xiang

State Key Laboratory of Powder Metallurgy, Central South University, Changsha 410083, China

Abstract:Ti(C, N) whiskers were fabricated through carbothermal reduction of TiO2 in nitrogen at different temperatures. The raw materials were TiO2, carbon black, NaCl and NiCl2, among which NaCl was added to form the chlorides of Ti and NiCl2 was used as catalyst for whisker growth. The phases of the synthesized samples and the corresponding phase-transformation behavior were analyzed by XRD, the micrographs of synthesized samples were characterized by scanning electron microscopy (SEM). Furthermore, the growth mechanism of Ti(C, N) whiskers was discussed. The results show that TiO2 directly reacts with carbon black and nitrogen to form TiN phase at 1 200℃. When the temperature is in the range of 1 250−1 400 ℃, NaCl is decomposed and functions as a halogenation reagent of TiO2 and NiCl2 acts as catalysts for the Ti(C, N) whisker formation. The whiskers obtained are 10−30 μm in length and about 1 μm in diameter. The phenomenon that whiskers with smooth surfaces are terminated by a droplet of catalyst indicates that the whiskers are grown by the “vapor-liquid-solid” mechanism.

 

Key words: Ti(C, N); carbothermal reduction process; whiskers; VLS mechanism

ISSN 1004-0609
CN 43-1238/TG
CODEN: ZYJXFK

ISSN 1003-6326
CN 43-1239/TG
CODEN: TNMCEW

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