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Synthesis and Thermal decomposition study of Dysprosium Trifluoroacetate
Journal of Analytical and Applied Pyrolysis ( IF 6 ) Pub Date : 2018-06-01 , DOI: 10.1016/j.jaap.2018.03.018
Y.A. Opata , J.-C. Grivel

Abstract A study of the thermal decomposition process of dysprosium trifluoroacetate hydrate under flowing argon is presented. Thermogravimetry, differential thermal analysis, evolved gas analysis and ex-situ x-ray diffraction techniques have been employed in the investigation. Three main stages were identified: dehydration, decomposition and phase transformation from DyF3 to DyFO. The dehydration takes place in 2 steps and the decomposition also occurs in two stages. The observed residual mass demonstrated a discrepancy with the calculated value for DyF3 formation. Observations on quenched samples at temperatures just above the decomposition step and at 828 °C showed a variation in the sample color, being dark in the first case and rather bright at the higher quenching temperature. Based on this fact, we concluded that some carbon remains in the sample up to 800 °C. With the temperature reaching 1300 °C, a plateau is observed in the TG signal, which mass value agrees with the formation of DyFO as verified by the ex-situ x-ray data of quenched powder. Using the FTIR and MS spectra of released gases during the process and the TG data, a decomposition scheme is suggested.

中文翻译:

三氟乙酸镝的合成及热分解研究

摘要 研究了流动氩气下三氟乙酸镝水合物的热分解过程。热重分析、差热分析、逸出气体分析和非原位 X 射线衍射技术已用于研究。确定了三个主要阶段:脱水、分解和从 DyF3 到 DyFO 的相变。脱水分两步进行,分解也分两步进行。观察到的残余质量与 DyF3 形成的计算值存在差异。在刚好高于分解步骤和 828 °C 的温度下对淬火样品的观察显示样品颜色发生变化,在第一种情况下变暗,而在更高的淬火温度下则相当亮。基于这个事实,我们得出结论,在高达 800 °C 的温度下,样品中仍会残留一些碳。随着温度达到 1300 °C,在 TG 信号中观察到一个平台,该质量值与 DyFO 的形成一致,如淬火粉末的非原位 X 射线数据所证实的。使用过程中释放气体的 FTIR 和 MS 光谱以及 TG 数据,建议分解方案。
更新日期:2018-06-01
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