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Synthesis and thermal decomposition study of dysprosium trifluoroacetate

机译:三氟乙酸镝的合成与热分解研究

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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 degrees 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 degrees C. With the temperature reaching 1300 degrees 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.
机译:介绍了流动氩气在流动氩气下的镝三氟乙酸镝水合物的热分解过程的研究。调查中采用了热重试验,差分热分析,进化气体分析和出原位X射线衍射技术。确定了三个主要阶段:从DYF3到DYFO的脱水,分解和相变。脱水发生在2个步骤中,分解也发生在两个阶段。观察到的残余物质证明了与DYF3形成的计算值差异。在分解步骤的温度下淬火样品和828摄氏度的淬火样品的观察显示了样品颜色的变化,在第一种情况下是暗的,并且在较高的淬火温度下,基于这一事实,我们得出结论,一些碳仍然存在在样品中高达800℃。随着达到1300℃的温度,在TG信号中观察到平台,该质量值与淬火粉末的前原位X射线数据验证的Dyfo的形成。在过程和TG数据期间,使用释放气体的FTIR和MS光谱,提出了分解方案。

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