Synthesis of ε-Keggin-Type Cobaltomolybdate-Based 3D Framework Material and Characterization Using Atomic-Scale HAADF-STEM and XANES.
Synthesis of ε-Keggin-Type Cobaltomolybdate-Based 3D Framework Material and Characterization Using Atomic-Scale HAADF-STEM and XANES.
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DOI：
10.1021/acs.inorgchem.6b02748
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发表时间：
2017-02
影响因子：
4.6
通讯作者：
Takumi Igarashi;Zhenxin Zhang;Terufumi Haioka;N. Iseki;N. Hiyoshi;N. Sakaguchi;C. Kato;S. Nishihara;K. Inoue;A. Yamamoto;H. Yoshida;Nao Tsunoji;W. Ueda;T. Sano;M. Sadakane
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文献类型：
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作者：
Takumi Igarashi;Zhenxin Zhang;Terufumi Haioka;N. Iseki;N. Hiyoshi;N. Sakaguchi;C. Kato;S. Nishihara;K. Inoue;A. Yamamoto;H. Yoshida;Nao Tsunoji;W. Ueda;T. Sano;M. Sadakane
我们描述了具有钠阳离子NaH 9 [ε-CoIIMoV 8 MoVI 4 O 40 CoII 2]的ε-Keggin型钴钼酸盐基3D框架的制备，以及通过高分辨率高角度环形暗场扫描透射电子显微镜（HAADF-STEM）和X射线吸收精细结构（XAFS）光谱对其进行表征。首次获得了ε-Keggin化合物的原子级HAADF-STEM图像，确定了Mo和Co的位置。此外，通过X射线吸收近边结构（XANES）分析获得了CoO 4四面体存在的明确证据。它们的表征清楚地表明，ε-Keggin型钴钼酸盐单元，[ε-CoMo 12 O 40]n-，由一个中心CoIIO 4四面体和12个周围的MoO 6八面体构成，与CoII连接形成3D框架。
We describe the preparation of ε-Keggin-type cobaltomolybdate-based 3D frameworks with sodium cations, NaH9[ε-CoIIMoV8MoVI4O40CoII2], and their characterization by high-resolution high-angle annular dark-field scanning transmission electron microscopy (HAADF-STEM) and X-ray absorption fine structure (XAFS) spectroscopy. Atomic-scale HAADF-STEM images of ε-Keggin compounds were obtained for the first time, and positions of Mo and Co were confirmed. Furthermore, clear evidence of the presence of a CoO4 tetrahedron was obtained by X-ray absorption near-edge structure (XANES) analysis. Their characterization clearly revealed that ε-Keggin-type cobaltomolybdate units, [ε-CoMo12O40]n-, constructed by a central CoIIO4 tetrahedron and 12 surrounding MoO6 octahedra, are linked with CoII to form 3D frameworks.