Thermal decomposition of nickel acetate tetrahydrate:: an integrated study by TGA, QMS and XPS techniques
Thermal decomposition of nickel acetate tetrahydrate:: an integrated study by TGA, QMS and XPS techniques
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DOI：
10.1016/j.molcata.2004.09.065
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发表时间：
2005-03-16
影响因子：
--
通讯作者：
Puerta, T
中科院分区：
文献类型：
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作者：
De Jesus, JC;González, I;Puerta, T
羧酸镍的热分解是合成适用于催化目的的金属纳米粒子的可行途径。本工作的目的是表征四水合乙酸镍 Ni(CH3COO)(2)-4H(2)O 的热分解过程。在三种不同气氛（空气、C 氦气和氢气）中进行的热重 (TGA) 分解研究表明，母盐的脱水发生在 118 至 137 摄氏度之间。然而，无论选择何种气氛，此阶段记录的样品重量损失保持不变。表明形成了化学式为 0.86Ni(CH3COO)(2).0.14Ni(OH)(2) 的中间体碱性乙酸盐。脱水步骤在约100℃进行。随后在350℃下醋酸基发生一步主要分解，生成NiO和Ni。分别在空气和氢气的处理气氛中进行，但有一些迹象表明当热解在氦气中进行时需要额外的步骤。通过使用四极杆质谱 (QMS) 监测逸出气体，证实了热分析可能得出的结论。并提出了一系列与乙酸酯基团分解相关的反应来解释大多数检测到的气体产物。 X 射线光电子能谱 (XPS) 用于研究盐在 He 气氛中热分解过程中获得的固相。 (C) 2004 Elsevier B.V. 保留所有权利。
The thermal decomposition of nickel carboxylates is a feasible route to synthesize metal nanoparticles suitable for catalytic purposes. The aim of this work is the characterization of the thermal decomposition course of nickel acetate tetrahydrate, Ni(CH3COO)(2)-4H(2)O. A thermogravimetric (TGA) decomposition study carried out in three different atmospheres (air, C helium and hydrogen) showed that the dehydration of the parent salt occurs between 118 and 137 degreesC. However, irrespective of the chosen atmosphere, the sample weight loss registered in this stage remains invariable. suggesting the formation of a an intermediate basic acetate with the formula 0.86Ni(CH3COO)(2).0.14Ni(OH)(2). The dehydration step was followed at ca. 350 degreesC by the subsequent one-step major decomposition of the acetate group, producing NiO and Ni. in treatment atmospheres of air and hydrogen, respectively, but there was some indication of an additional step when the thermolysis was conducted in helium. The conclusions possible from thermal analysis were confirmed by monitoring evolved gases employing quadrupole mass spectrometry (QMS). and a set of reactions linked to the decomposition of the acetate group has been proposed to account for most of the gas products detected. X-ray photoelectron spectroscopy (XPS) was used to investigate the solid phases obtained during the thermal decomposition of the salt in He atmosphere. (C) 2004 Elsevier B.V. All rights reserved.