熔盐法合成高结晶相纯亚metastate钙

I.A. Disher Al-Hydary, S.J. Edress Al-Mohana, M.M. Hussein Al-Marzooqee
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引用次数: 1

摘要

以KCl-LiCl为反应介质,等量的SnO2和CaCO3为前驱体,采用熔盐法在低温下合成了具有正交晶系的钙转移酸CaSnO3。考察了反应温度、盐的种类、盐与前驱物的质量比等工艺参数。使用X'Pert HighScore Plus软件对X射线粉末衍射图进行Rietveld细化,以计算所获得的粉末中存在的每个相的相百分比。根据这些计算结果,选择反应温度最低的盐体系,以产生最高的casno3%。利用x射线衍射(XRD)、能量色散x射线光谱(EDX)、傅里叶变换红外光谱(FTIR)和场发射扫描电镜(FE-SEM)等技术对所制备的化合物进行了表征。实验结果表明,在1000℃下,短时间内可以制备出高结晶相的纯CaSnO3层流板,且无其他可检测到的二次相。
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Synthesis of highly crystalline phase pure calcium metastannate by molten salt method

Calcium metastannate CaSnO3 with orthorhombic crystal system has been synthesized at low temperature by molten salt method using KCl-LiCl as a reaction medium and equimolar of SnO2 and CaCO3 as precursors. The process parameters including the reaction temperature, salt type, and salt to precursor weight ratio were investigated. Rietveld refinements on X-ray powder diffraction patterns were performed using X'Pert HighScore Plus software to calculate phase percent of each phase present in the obtained powder. The results of these calculations were followed in order to choose the salt system that requires the least reaction temperature to produce the highest CaSnO3 percent. The as-prepared compound was characterized by various techniques such as X-Ray diffraction (XRD), energy dispersive X-Ray spectrometry (EDX), Fourier transform infrared spectrometry (FTIR), and field emission scanning electron microscope (FE-SEM). The experimental results showed that highly crystalline phase pure CaSnO3 laminar plates could be prepared at 1000 °C for short period of time without any other detectable secondary phases.

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