碳热还原氮化工艺制备AlON透明陶瓷
收稿日期: 2009-10-19
修回日期: 2010-01-19
网络出版日期: 2010-06-10
基金资助
国家自然科学基金(50672113, 50802106)
Fabrication of Aluminum Oxynitride Transparent Ceramics by Carbothermal Reduction Nitridation Processing
Received date: 2009-10-19
Revised date: 2010-01-19
Online published: 2010-06-10
以g-Al2O3为原料, 炭黑(C)为还原剂, 通过碳热还原氮化(carbothermal reduction and nitridation, CTRN)工艺合成了氮氧化铝(AlON)粉体, 并通过气压烧结工艺制备了AlON透明陶瓷. 借助X射线衍射分析研究了反应温度、保温时间及碳用量对CTRN反应产物相组成的影响, 借助电子探针研究了AlON透明陶瓷的微观结构. 研究结果表明: 该反应主要受热力学控制, 动力学因素也具有重要作用, 反应温度和保温时间对AlON粉体的合成均具有重要影响. 在1300℃时, 开始发生CTRN反应; 随着反应温度的升高, AlN的生成量逐渐增加; 在1650℃时, 开始形成AlON; 在1700℃时, AlON的CTRN合成反应基本完成, 产物中除含有极少量的AlN外, 其余均为AlON相; 进一步提高反应温度至1750℃, 产物中残余AlN的量有所减少, 但不能完全消除. 采用CTRN工艺制备的粉体为原料, 经1950℃高温气氛反应6h可制备出AlON透明陶瓷, 材料微观结构致密、均匀, 平均晶粒尺寸约50mm.
关键词: 氮氧化铝(AlON); 粉体; 透明陶瓷; 碳热还原氮化反应
刘学建, 袁贤阳, 张 芳, 黄政仁, 王士维 . 碳热还原氮化工艺制备AlON透明陶瓷[J]. 无机材料学报, 2010 , 25(7) : 678 -682 . DOI: 10.3724/SP.J.1077.2010.00678
Aluminum oxynitride (AlON) powders were firstly prepared by carbothermal reduction and nitridation processing with g-Al2O3 as starting material and carbon black (C) as a reducing agent and then AlON transparent ceramics were fabricated by gas-pressure sintering technique under nitrogen atmosphere. The effects of reactive temperature, holding time, and C content on the resultant phase compositions were investigated systematically by XRD. The microstructure of AlON transparent ceramics was observed by EPMA. The experimental results indicate that the CTRN processing for AlON formation is thermodynamically controlled and both reactive temperature and holding time are crucial to the reactive progress. The CTRN reaction begins at 1300℃ and finishes at 1700℃ with most of AlON and a trace of AlN. The AlN content further decreases with increasing reactive temperature while AlN phase can not disappear even at 1750℃ for 4h. With the as-prepared AlON powders as starting materials, AlON transparent ceramics can be fabricated by gas-pressure sintering technique at 1950℃ for 6h. The fabricated AlON transparent ceramics presents uniform microstructure with an average grains size of 50 mm.
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