Abstract: Pure monoclinic ZrO₂, tetragonal ZrO₂ and the mixed phases of monoclinic and tetragonal ZrO₂, were prepared by hydrothermal method using Zr(NO₃)₄ as precursor. The influences of the precursor concentration, crystallization temperature, and crystallization time on the particle size and crystalline phase of ZrO₂nanoparticles were studied by XRD, Raman spectroscopy and TEM. It is found that all the above synthesis conditions have influences on the particle size of ZrO₂. Among those above experimental conditions, the particle size of ZrO₂ is more related to the crystallization temperature while the crystallization temperature has little influence on the morphology of ZrO₂. Furthermore, it is show that the monoclinic ZrO₂ is easily formed for the longer crystallization time, and the crystallization degree of ZrO₂ is increased when longer crystallization time is used. This paper provides a strategy to synthesize the monoclinic ZrO₂ using low precursor concentration, high crystallization temperature and the long crystallization time.

Key words: Hydrothermal,    ,  ZrO_2,    ,  Crystal phase

摘要： 以硝酸锆为前驱物, 用水热法分别合成了纯单斜相、四方相以及四方和单斜混合相的氧化锆纳米粒子。应用XRD、拉曼光谱和TEM探讨了水热过程中前驱体浓度、晶化温度和晶化时间对ZrO₂晶粒尺寸和相变的影响。结果表明，水热制备过程中上述合成条件均影响ZrO₂晶粒尺寸，其中晶化温度对其影响最大，但是晶化温度对ZrO₂的形貌影响不大。延长晶化时间有利于单斜晶相的形成，而且随着晶化时间延长，ZrO₂的晶化程度增加。在水热合成过程中采用较低的前驱体浓度、较高晶化温度及延长晶化时间有利于控制合成单斜相ZrO₂。

关键词: 水热 , 氧化锆 , 晶相