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热处理条件对纳米锌铝尖晶石颗粒尺寸的影响
作者:文钰斌 刘新红 陈晓雨 杨林 马腾 
单位:郑州大学 河南省高温功能材料重点实验室 郑州 450052 
关键词:溶胶–凝胶法 纳米锌铝尖晶石 气氛 纳米颗粒 
分类号:TB35
出版年,卷(期):页码:2017,45(6):880-886
DOI:
摘要:

 以硝酸铝、硝酸锌和柠檬酸为原料,采用溶胶–凝胶法制备纳米锌铝尖晶石粉体,研究了热处理条件(温度和气氛)对纳米锌铝尖晶石颗粒尺寸的影响。结果表明:在空气气氛下,600 ℃热处理后即可制备出纳米锌铝尖晶石颗粒,纳米颗粒团聚严重,其颗粒尺寸在20~30 nm之间;随热处理温度升高,纳米锌铝尖晶石颗粒尺寸快速增加,1 000 ℃开始出现微米尺寸颗粒,1 400 ℃大部分颗粒尺寸在微米级别,且呈烧结状。在还原性气氛下,柠檬酸分解残留部分碳,碳分布在锌铝尖晶石颗粒间,可阻碍纳米锌铝尖晶石团聚和烧结,进而抑制高温下纳米锌铝尖晶石颗粒长大,1 000 ℃热处理后,纳米尖晶石颗粒尺寸较小(约10 nm)。然而,在还原性气氛下,当热处理温度≥1 200 ℃时,锌铝尖晶石与CO或柠檬酸分解残留的碳反应,使锌以气态的形式逸出,只有α-Al2O3晶相。

 

 ZnAl2O4 nano-powder was prepared by a sol–gel method with aluminum nitrate, zinc nitrate and citric acid as starting materials. Effect of heat treatment condition (i.e., temperature and atmosphere) on the size of ZnAl2O4 nano-particles was investigated. The results show that ZnAl2O4 nano-powder can be prepared in air at 600 ℃, and the nano-particles with the sizes of 20–30 nm are seriously agglomerated. The size of ZnAl2O4 nano-particles increases greatly with increasing temperature, some micron-sized particles appear after heat treatment at 1 000 ℃, most of ZnAl2O4 nano-particles grow into micron-sized particles after they are sintered at 1 400 ℃. In a reductive atmosphere, there is residual carbon from citric acid decomposition. The carbon inclusions are well distributed in the boundaries of ZnAl2O4 particles, which can restrict the particle growth and/or lower the mobility of pores attached to particle boundaries, creating a retard effect on the growth and sintering behavior of ZnAl2O4 particles. The nano-particle size is approximately 10nm even after heat treatment at 1 000 ℃. However, in a reductive atmosphere, ZnAl2O4 reacts with CO or C (from citric acid decomposition) to form volatile Zn (g), and there is only single crystal phase of α-Al2O3 when the temperature increases to 1 200 ℃.

 
基金项目:
国家自然科学基金面上项目(51672253);河南省重点科技攻关项目(152102410014);河南省科技厅基础研究项目(162300410044)资助。
作者简介:
文钰斌(1992—),男,硕士研究生。
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