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Formation mechanisms of Ni_2P nanocrystals using XANES and EXAFS spectroscopy

机译：XANES和EXAFS光谱分析Ni_2P纳米晶的形成机理

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摘要

Ni_2P nanocrystals have been synthesized by a ligand stabilization method with adopting nickel acetylacetonate (Ni(acac)2) as a nickel precursor and trioctylphosphine (TOP) as a phosphorous precursor in the presence of trioctylphosphine oxide (TOPO) as a coordinating solvent. In order to better understand the formation of Ni_2P nanocrystals, various synthetic routes were employed with varying the mixing order of TOP or TOPO with Ni(acac)2 in the complexation and nucleation steps, and the phosphidation temperatures of Ni-TOP solution in TOPO. In all cases the formation of Ni_2 P nanocrystals having an average size in range of 5-11 nm was achieved, but with slightly larger particle distribution of ca. 11 nm being observed for the case where the TOP was injected after a nucleation of Ni-TOPO was formed. In particular, XAFS techniques of EXAXS and XANES which are effective to characterize either amorphous or crystalline materials were applied to examine the structural and electrical properties of the precursor, intermediate and final materials. This led to elucidate the role and the effect of TOP and TOPO on the formation of Ni_2P nanocrystals. It is concluded that the formation of Ni_2P nanocrystals proceeds through three consecutive steps of complexation, nucleation and phosphidation. In phosphidation, TOP works as a reducing agent on the Ni precursor as well as a phosphorous source through the cleavage of P-C bonds.
机译：Ni_2P纳米晶体已经通过配体稳定化方法合成，采用乙酰丙酮镍（Ni（acac）2）作为镍前体，三辛基膦（TOP）作为磷前体，在三辛基氧化膦（TOPO）作为配位溶剂的情况下。为了更好地理解Ni_2P纳米晶体的形成，在络合和成核步骤中采用了多种合成途径，改变了TOP或TOPO与Ni（acac）2的混合顺序，以及TOPO中Ni-TOP溶液的磷化温度。在所有情况下，均能形成平均粒径在5-11 nm范围内的Ni_2 P纳米晶体，但其粒径分布略大。在Ni-TOPO成核后注入TOP的情况下观察到11nm。特别地，将有效表征非晶或结晶材料的EXAXS和XANES的XAFS技术应用于检查前体，中间材料和最终材料的结构和电性能。这阐明了TOP和TOPO在Ni_2P纳米晶体形成中的作用和作用。可以得出结论，Ni_2P纳米晶体的形成是通过三个连续的络合，成核和磷酸化步骤进行的。在磷化过程中，TOP充当Ni前体的还原剂以及通过P-C键断裂的磷源。

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  • 来源
    《Materials Science and Engineering》 |2011年第2期|p.132-140|共9页
  • 作者

    Hye-Ryun Seo; Kye-Sung Cho; Yong-Kul Lee;

  • 作者单位

    Laboratory of Advanced Catalysis for Energy and Environments, Department of Chemical Engineering, Dankook University, 126 Jukjeondong, Yongin 448-701, Republic of Korea;

    Laboratory of Advanced Catalysis for Energy and Environments, Department of Chemical Engineering, Dankook University, 126 Jukjeondong, Yongin 448-701, Republic of Korea;

    Laboratory of Advanced Catalysis for Energy and Environments, Department of Chemical Engineering, Dankook University, 126 Jukjeondong, Yongin 448-701, Republic of Korea;

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  • 正文语种 eng
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  • 关键词

    ni_2p nanocrystals formation mechanism exafs xanes;

    机译：ni_2p纳米晶形成机理消除了烷;

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