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In Situ Powder Diffraction Study of the Hydrothermal Synthesis of ZnO Nanoparticles

机译:水热合成ZnO纳米粒子的原位粉末衍射研究

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ZnO is one of the most widely applied nanomaterials, and the vast majority of ZnO nanoparticles are synthesized from aqueous solutions of inexpensive salts. Here we present the first in situ powder X-ray diffraction(PXRD) study of the formation of ZnO nanoparticles under hydrothermal conditions. An aqueous Zn(NO_3)_2 and NaOH precursor gel was studied at three different temperatures (150, 200, and 250 °C) by in situ PXRD, and Rietveld refinements of the data were used to extract crystal structure and nanostructural information. Interesting trends in the evolution of crystallite size and twin faulting with temperature were established. The morphology of the synthesized crystallites depends on temperature and reaction time; at high temperatures and long reaction times almost isotropic crystallites are formed, while the anisotropy increases with shorter synthesis times and lower temperatures. Furthermore, the twin fault probability decreases with reaction time and increasing reaction temperature. Under the present synthesis conditions, a minimum ZnO crystallite size of around 14 nm in the a-direction and 22 nm in the c-direction is observed.
机译:ZnO是应用最广泛的纳米材料之一,并且绝大多数ZnO纳米颗粒都是由廉价盐的水溶液合成的。在这里,我们介绍了在水热条件下形成ZnO纳米粒子的第一个原位粉末X射线衍射(PXRD)研究。 Zn(NO_3)_2和NaOH水溶液前体凝胶在三种不同温度(150、200和250°C)下通过原位PXRD研究,并利用Rietveld数据精炼方法提取晶体结构和纳米结构信息。建立了微晶尺寸和温度双晶断层演化的有趣趋势。合成微晶的形态取决于温度和反应时间。在高温和长反应时间下,几乎形成各向同性的微晶,而各向异性随着合成时间的缩短和温度的降低而增加。此外,孪生故障概率随着反应时间和反应温度的升高而降低。在当前的合成条件下,观察到最小的ZnO微晶尺寸在a方向上约为14nm,在c方向上约为22nm。

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