摘要
以ZrOCl2·8H2O为锆源,CO(NH2)2为沉淀剂,去离子水为溶剂,通过水热法合成单斜晶型的纳米ZrO2。讨论水热温度和水热时间对纳米二氧化锆晶粒尺寸的影响,并利用场发射扫描电镜(SEM)和XRD衍射仪表征手段,对产品形貌及物相进行了表征分析。实验结果表明,水热温度是影响ZrO2粉体晶化的主要因素,在140℃水热温度下,ZrOCl2·8H2O和CO(NH2)2反应生成Zr(OH)4胶体。随着水热温度升高到160℃,大部分的Zr(OH)4胶体分解生成ZrO2并结晶。当水热温度继续升高至180℃时,Zr(OH)4全部分解生成ZrO2。水热时间的增加并不改变ZrO2的晶型,且对ZrO2的晶粒尺寸影响不大,随着水热时间由3 h增加到18 h,其粒径分别为51.2、46.1、45.6 nm和54.3 nm,且样品具有良好的分散性。
In this essay,with ZrOCl2·8H2O,CO(NH2)2 and deionized water as zirconium source,precipitant and solvent respectively,monoclinic nanocrystalline ZrO2 powder was synthesized through hydrothermal method.The impact of hydrothermal temperature and hydrothermal time on the grain size of nano-ZrO2 was investigated.Scanning electron microscopy(SEM)and X-ray diffraction(XRD)were used to characterize the morphology and phase compositions of products.The results showed that hydrothermal temperature was the main influencing factor in crystallization of ZrO2 powder.At the hydrothermal temperature of 140℃,ZrOCl2·8H2O reacted with CO(NH2)2 to form Zr(OH)4 colloid.When the temperature rose to 160℃,most of Zr(OH)4 colloid decomposed and crystallized into ZrO2.At the hydrothermal temperature of 180℃,all Zr(OH)4 decomposed into ZrO2.The increase of hydrothermal time did not change the crystal structure of ZrO2,and had little effect on the grain size of ZrO2.For products with the hydrothermal time of 3,6,12 h and 18 h,the grain size was 51.2,46.1,45.6 nm and 54.3 nm respectively,and the obtained powder had good dispersibility.
作者
王敬飞
张国华
周国治
WANG Jingfei;ZHANG Guohua;ZHOU Guozhi(State Key Laboratory of Advanced Metallurgy,University of Science and Technology Beijing,Beijing 100083,China)
出处
《江西冶金》
2020年第3期1-5,共5页
Jiangxi Metallurgy
关键词
水热法
纳米二氧化锆
粒度
hydrothermal method
nano-ZrO2 powder
grain size
