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首页> 外文期刊>Journal of surface investigation: x-ray, synchrotron and neutron techniques >Investigation of PdZn nanoparticle formation upon the thermal decomposition of acetate precursors by in situ XRD and XAFS
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Investigation of PdZn nanoparticle formation upon the thermal decomposition of acetate precursors by in situ XRD and XAFS

机译:原位XRD和XAFS对乙酸前体热分解后PdZn纳米颗粒形成的研究

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摘要

The formation of metal or metal-oxide nanoparticles from four different precursor systems, including palladium(II) acetate, zinc(II) acetate, their 1: 1 mechanical mixture and the palladium-zinc bimetallic acetate complex PdZn(OCOMe)_4 (H_2 O), upon heating in a He + 5% H_2 atmosphere is studied using the X-ray diffraction and EXAFS (Extended X-ray absorption fine structure) techniques in the in situ mode. X-ray diffraction is primarily used to monitor changes in the phase composition of the samples. At specific moments when qualitative changes in the composition occur, EXAFS spectra at the K-edges of Pd and Zn are also measured. Using a combination of these two techniques, a detailed sequence of the phase transformations in each of the four precursor systems is revealed. It is found that the bimetallic acetate complex and the mixture of two monometallic acetates undergo chemical reduction to form zerovalent palladium under milder conditions than zinc acetate. However, the formation of a PdZn alloy from the mixture of metal acetates proceeds with a significant diffusion barrier.
机译:由四种不同的前体系统形成金属或金属氧化物纳米颗粒,包括乙酸钯(II),乙酸锌(II),它们的1:1机械混合物以及钯-锌双金属乙酸盐络合物PdZn(OCOMe)_4(H_2 O ),在He + 5%H_2气氛中加热后,以原位模式使用X射线衍射和EXAFS(扩展X射线吸收精细结构)技术进行研究。 X射线衍射主要用于监测样品的相组成的变化。在组成发生质变的特定时刻,还测量了Pd和Zn的K边缘处的EXAFS光谱。使用这两种技术的组合,可以揭示四个前体系统中每个系统的详细相变顺序。发现双金属乙酸盐络合物和两种单金属乙酸盐的混合物在比乙酸锌温和的条件下经历化学还原以形成零价钯。但是,由金属乙酸盐的混合物形成PdZn合金会产生明显的扩散势垒。

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