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Synthesis of Dysprosium Oxychloride (DyOCl)
Journal of Chemical Crystallography ( IF 0.4 ) Pub Date : 2021-09-24 , DOI: 10.1007/s10870-021-00904-2
Saehwa Chong 1 , Brian J. Riley 1 , José Marcial 1 , Charmayne E. Lonergan 1 , Derek A. Cutforth 1
Affiliation  

Dysprosium oxychloride, DyOCl, was synthesized using a simple hydrolysis method with DyCl3·6H2O. X-ray powder diffraction (XRD) data was used to determine the crystal structure. The DyOCl compound is isostructural to the matlockite (PbFCl) crystal structure and crystallizes in the tetragonal P4/nmm (#129) space group. The crystal structure contains the alternating cationic layers of (DyO)n and anionic layers of nCl along the c-axis. The structural data including unit cell, volume, and density of DyOCl were compared to other rare-earth oxychloride data from the Inorganic Crystal Structure Database (ICSD) and our previous study on TbOCl. Fourier-transform infrared spectroscopy was performed on DyOCl and peaks observed at 543 and 744 cm−1 were attributed to Dy–O and Dy–Cl. Scanning electron microscopy analysis showed irregularly shaped crystals. Hot-stage XRD, thermogravimetry, as well as differential scanning calorimetry coupled to a gas chromatograph and a mass spectrometer (evolved gas analysis) were performed on DyCl3·6H2O to understand the phase transformation to DyOCl (and Dy2O3) as a function of temperature and time at temperature.

Graphic Abstract

DyOCl compound with the tetragonal P4/nmm space group is composed of the alternating layers of (DyO)n and nCl along the c-axis.



中文翻译:

氧氯化镝 (DyOCl) 的合成

使用简单的水解方法与 DyCl 3 ·6H 2 O合成了氧氯化镝 DyOCl。X射线粉末衍射 (XRD) 数据用于确定晶体结构。DyOCl 化合物与 matlockite (PbFCl) 晶体结构同构,并在四方P 4/ nmm (#129) 空间群中结晶。晶体结构包含交替的 (DyO) n阳离子层和n Cl -阴离子层沿c-轴。将 DyOCl 的晶胞、体积和密度等结构数据与无机晶体结构数据库 (ICSD) 中的其他稀土氯氧化物数据和我们之前对 TbOCl 的研究进行了比较。对 DyOCl 进行傅里叶变换红外光谱,在 543 和 744 cm -1处观察到的峰 归因于 Dy-O 和 Dy-Cl。扫描电子显微镜分析显示不规则形状的晶体。对 DyCl 3 ·6H 2 O 进行了热台 XRD、热重分析以及差示扫描量热法与气相色谱仪和质谱仪联用(逸出气体分析),以了解向 DyOCl(和 Dy 2 O 3) 作为温度和时间的函数。

图形摘要

具有四方 P4/nmm 空间群的 DyOCl 化合物由 (DyO) nn Cl -沿c轴的交替层组成。

更新日期:2021-09-24
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