· 480 ·
第41卷第4期 2013年4月
硅 酸 盐 学 报
2013年
Vol. 41，No. 4 April，2013
硅 酸 盐 学 报
JOURNAL OF THE CHINESE CERAMIC SOCIETY
DOI：10.7521/j.issn.0454–5648.2013.04.09
含复合晶核剂CaO–MgO–Al2O3–SiO2微晶玻璃析晶与性能
郭兴忠，杨 辉，杨广跃1，周 箭2 (1. 硅材料国家重点实验室，浙江大学材料科学与工程学系，杭州 310027；
2. 杭州师范大学材料与化学化工学院，杭州 310036)
摘 要：采用高温熔制法制备了含复合晶核剂的CaO–MgO–Al2O3–SiO2(CMAS)微晶玻璃，并借助差热分析、X射线衍射、扫描电子显微镜分析了复合晶核剂组成对CMAS微晶玻璃的析晶和性能的影响规律。结果表明：复合晶核剂CaF2+TiO2能使CMAS玻璃的析晶活化能E降至329.2 kJ/mol，且促进晶体快速生长；CaF2+P2O5可促进大量晶核生成，使晶体生长指数n增至2.87，从而实现CMAS玻璃整体析晶；CMAS微晶玻璃的主晶相为钙长石和透辉石，形状为长条状，TiO2和ZrO2的加入对主晶相种类和形状没有影响，但P2O5加入后玻璃不能析出透辉石晶相，而是辉石晶相，并产生许多细小晶粒；含复合晶核剂的微晶玻璃均具有较高Vicker硬度(7.0 GPa以上)，但引入CaF2+TiO2+P2O5时，微晶玻璃的Vicker硬度较低，这主要是晶粒排列不致密所致。
11
关键词：钙镁铝硅微晶玻璃；复合晶核剂；析晶；透辉石
中图分类号：TQ174 文献标志码：A 文章编号：0454–5648(2013)04–0480–06
网络出版时间：2013–03–02 9:39 网络出版地址：http://www.cnki.net/kcms/detail/11.2310.TQ.20130302.0939.007.html
Effect of Composite Nucleation Agents on Crystallization and Properties of CaO–MgO–Al2O3–SiO2
Glass Ceramics
GUO Xingzhong，YANG Hui，YANG Guangyue1，ZHOU Jian2
(1. State Key Laboratory of Silicon Materials, Department of Materials Science and Engineering, Zhejiang University, Hangzhou 310027,
China; 2. College of Materials, Chemistry and Chemical Engineering, Hangzhou Normal University, Hangzhou 310036, China)
Abstract: The CaO–MgO–Al2O3–SiO2 (CMAS) glass ceramics containing composite nucleation agents were prepared by a melting method. The effect of complex nucleation agents on the crystallization and properties of CMAS glass ceramics was investigated by means of differential thermal analysis, X-ray diffraction and scanning electron microscopy as well. The results show that the nuclea-tion agents of CaF2+TiO2 could reduce the activation energy of CMAS glass to 329.2 kJ/mol and accelerate the growth of crystalline phases. The CaF2+P2O5 could boost the formation of more crystal nucleus, and improve the Avrami index to 2.87, indicating the volumetric crystallization. The main crystallization phases of CMAS glass ceramic are diopside and anorthite with strip-like shape. The addition of TiO2 and ZrO2 had little effect on the compositions and shapes of main crystalline phases, while P2O5 resulted in the precipitation of pyroxene phase instead of diopside phase in the presence of more small crystals. The CMAS glass ceramics contain-ing composite nucleation agents had a higher Vicker hardness (i.e., > 7.0 GPa). However, the Vicker hardness decreased with the si-multaneous addition of CaF2+TiO2+P2O5, resulting from little tight arrangement of crystalline phases.
Key words: calcium–magnesium–alumium–silicate glass ceramics; composite nucleation agent; crystallization; diopside
1
1
CaO–MgO–Al2O3–SiO2(CMAS)是典型的微晶玻璃体系之一，由于可析出透辉石[CaMgSi2O6]、堇青石[Mg2Al4Si5O18]、钙长石[CaAl2Si2O8]等晶相，因而该微晶玻璃具有优良的机械强度、耐磨性、耐
收稿日期：2012–07–04。 修订日期：2012–12–10。
基金项目：国家支撑计划项目(2013BAE03B01)；硅材料国家重点实验室
开放资金(SKL2011-9)资助项目。
第一作者：郭兴忠(1974—)，男，副教授。 通信作者：杨 辉(1962—)，男，教授。
腐蚀性，可用作建筑装饰材料、工业防护材料等[1–5]。
但目前CMAS微晶玻璃主要采用烧结法制备，微晶玻璃的性能不高，且工艺复杂。整体析晶法是制备CMAS微晶玻璃的有效途径，但CMAS微晶玻璃的
Received date: 2012–07–04. Revised date: 2012–12–10. First author: GUO Xingzhong (1974–), male, Associate Professor. E-mail: gxzh_zju@163.com
Correspondent author: YANG Hui (1962–), male, Professor. E-mail: yanghui@zju.edu.cn
含复合晶核剂CaO_MgO_Al2O3_SiO2微晶玻璃析晶与性能
