以炭黑为还原剂制备硅酸锆晶须的研究

doi:10.15541/jim20130618

无机材料学报 ›› 2014, Vol. 29 ›› Issue (8): 835-838.DOI: 10.15541/jim20130618

以炭黑为还原剂制备硅酸锆晶须的研究

王三海¹, 江伟辉^1,2, 冯果¹, 刘健敏¹, 苗立锋¹, 王洪达¹

(1. 景德镇陶瓷学院材料科学与工程学院, 景德镇 333000; 2. 江西省先进陶瓷材料重点实验室, 景德镇 333001)

收稿日期:2013-11-26 修回日期:2014-01-08 出版日期:2014-08-20 网络出版日期:2014-07-15
作者简介:王三海(1986–), 男, 硕士研究生. E-mail:wangsanhai0@sina.com
基金资助:
国家自然科学基金(51162013, 51362014);江西省主要学科学术和技术带头人培养计划(20113BCB22009)

Preparation of Zircon Whisker Using Carbon Black as Reducing Agent

WANG San-Hai¹, JIANG Wei-Hui^1,2, FENG Guo¹, LIU Jian-Min¹, MIAO Li-Feng¹, WANG Hong-Da¹

(1. School of Material Science and Engineering, Jingdezhen Ceramic Institute, Jingdezhen 333000, China; 2. Jiangxi Key Laboratory of Advanced Ceramic Materials, Jingdezhen 333001, China)

Received:2013-11-26 Revised:2014-01-08 Published:2014-08-20 Online:2014-07-15
About author:WANG San-Hai. E-mail:wangsanhai0@sina.com
Supported by:
National Natural Science Foundation of China(51162013, 51362014);Major Discipline Academic and Technical Leader Training Plan Project of Jiangxi Province(20113BCB22009)

摘要/Abstract

摘要：

以无水四氯化锆为锆源, 正硅酸乙酯(TEOS)为硅源, 氟化锂为矿化剂, 乙醇为溶剂, 炭黑为还原剂, 采用非水解溶胶-凝胶法在700 ℃制备得到硅酸锆晶须, 借助TG-DTA、XRD和TEM等测试手段研究了炭黑加入方式及用量对硅酸锆合成与形貌的影响。结果表明: 炭黑以悬浮液形式加入有助于硅酸锆的一维择优生长; 炭黑用量为6wt%时能获得直径为30~90 nm, 长径比为6~15, 沿[001]方向择优生长的硅酸锆晶须。炭黑与氧反应形成二氧化碳和一氧化碳, 炭黑加入方式及用量能够调控反应体系的氧分压。降低氧分压有利于形成更多的气相SiF₄, 这是促进ZrSiO₄一维定向生长的基础, 但氧分压过低又妨碍ZrSiO₄晶体的合成。因此, 适当氧分压有利于ZrSiO₄晶须的生长。

关键词: 非水解溶胶-凝胶法, 炭黑, 硅酸锆, 晶须

Abstract:

Zircon whisker was synthesized at 700 ℃ via non-hydrolytic Sol-Gel method using anhydrous zirconium tetrachloride (ZrCl₄) as zirconium source, tetraethylorthosilicate (TEOS) as silicon source, lithium fluoride (LiF) as mineralizer, ethanol as solvent and carbon black as reducing agent. Thermogravimetric analysis and differential thermal analysis (TG-DTA), X-ray diffraction analysis (XRD) and transmission electron microscope (TEM) were employed to characterize the influences of adding ways and amount of carbon black on the synthesis and morphology of zircon whisker. The results show that the carbon black added in form of suspension is favorable to the one-dimension growth of zircon. When 6wt% carbon black is added, optimized zircon whiskers are achieved along the growth direction of [001], which diameter and aspect ratio are in the range of 30-90 nm and 6-15, respectively. Because of carbon black reacting with oxygen to form carbon dioxide and monoxide, the adding way and amount of carbon black efficiently regulate the oxygen partial pressure in the reaction system. Reducing oxygen partial pressure can form more SiF₄gas, which is the basis of one-dimensional direction growth of zircon. However, excessively low oxygen partial pressure is against the ZrSiO₄ formation. Therefore, appropriate oxygen partial pressure can promote the growth of zircon whisker.

Key words: zircon, whisker, non-hydrolytic Sol-Gel method, carbon black

中图分类号:

TQ174

王三海, 江伟辉, 冯果, 刘健敏, 苗立锋, 王洪达. 以炭黑为还原剂制备硅酸锆晶须的研究[J]. 无机材料学报, 2014, 29(8): 835-838.

WANG San-Hai, JIANG Wei-Hui, FENG Guo, LIU Jian-Min, MIAO Li-Feng, WANG Hong-Da. Preparation of Zircon Whisker Using Carbon Black as Reducing Agent[J]. Journal of Inorganic Materials, 2014, 29(8): 835-838.

图/表 5

图1 添加炭黑所制干凝胶的DTA-TG曲线

Fig. 1 DTA-TG curves of xerogel prepared by adding carbon black

图2 不同热处理温度所制样品的XRD图谱

Fig. 2 XRD patterns of the samples annealed at different temperatures

图3 不同炭黑添加方式所得样品的TEM照片

Fig. 3 TEM images of samples prepared by adding carbon black with different ways

图4 不同炭黑含量制备样品的TEM照片

Fig. 4 TEM photographs of samples prepared at different carbon black contents (a) 0; (b) 3wt%; (c) 6wt%; (d) 9wt%

图5 硅酸锆晶须的(a)TEM和(b) HRTEM照片

Fig. 5 TEM (a) and HRTEM (b) images of zircon whisker Inset in Fig. 5 (a) is the corresponding SAED pattern

参考文献 15

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以炭黑为还原剂制备硅酸锆晶须的研究

Preparation of Zircon Whisker Using Carbon Black as Reducing Agent

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