Synthesis of ε-Keggin-Type Cobaltomolybdate-Based 3D Framework Material and Characterization Using Atomic-Scale HAADF-STEM and XANES.
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 CoO4tetrahedron 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 CoIIO4tetrahedron and 12 surrounding MoO6octahedra, are linked with CoIIto form 3D frameworks.
Department of Applied Chemistry, Graduate School of Engineering, Hiroshima University , 1-4-1 Kagamiyama, Higashi Hiroshima 739-8527, Japan.
Takumi
T
Igarashi
Faculty of Engineering, Kanagawa University , Rokkakubashi, Kanagawa-ku, Yokohama-shi, Kanagawa 221-8686, Japan.
Zhenxin
Z
Zhang
Department of Applied Chemistry, Graduate School of Engineering, Hiroshima University , 1-4-1 Kagamiyama, Higashi Hiroshima 739-8527, Japan.
Terufumi
T
Haioka
Department of Applied Chemistry, Graduate School of Engineering, Hiroshima University , 1-4-1 Kagamiyama, Higashi Hiroshima 739-8527, Japan.
Nao
N
Iseki
Research Institute for Chemical Process Technology, National Institute of Advanced Industrial Science and Technology (AIST) , 4-2-1 Nigatake, Miyagino, Sendai 983-8551, Japan.
Norihito
N
Hiyoshi
Faculty of Engineering, Hokkaido University , N-13, W-8, Sapporo 060-8626, Japan.
Norihito
N
Sakaguchi
Graduate School of Science & Center for Chiral Science, Hiroshima University , 1-3-1. Kagamiyama, 732-8526, Higashi-Hiroshima, Japan.
Chisato
C
Kato
Graduate School of Science & Center for Chiral Science, Hiroshima University , 1-3-1. Kagamiyama, 732-8526, Higashi-Hiroshima, Japan.|Institute for Advanced Materials Research, Hiroshima University & Natural Science Center for Basic Research and Development , 1-3-1, Kagamiyama, Higashi Hiroshima, Hiroshima 739-8526, Japan.
Sadafumi
S
Nishihara
Graduate School of Science & Center for Chiral Science, Hiroshima University , 1-3-1. Kagamiyama, 732-8526, Higashi-Hiroshima, Japan.|Institute for Advanced Materials Research, Hiroshima University & Natural Science Center for Basic Research and Development , 1-3-1, Kagamiyama, Higashi Hiroshima, Hiroshima 739-8526, Japan.
Katsuya
K
Inoue
Graduate School of Human and Environmental Studies, Kyoto University , Yoshida-nihonmatsu-cho, Sakyo-ku, Kyoto 606-8501, Japan.|Elements Strategy Initiative for Catalysts & Batteries (ESICB), Kyoto University , Kyotodaigaku Katsura, Nishikyo, Kyoto 615-8520, Japan.
Akira
http://orcid.org/0000-0002-1329-0807
A
Yamamoto
Graduate School of Human and Environmental Studies, Kyoto University , Yoshida-nihonmatsu-cho, Sakyo-ku, Kyoto 606-8501, Japan.|Elements Strategy Initiative for Catalysts & Batteries (ESICB), Kyoto University , Kyotodaigaku Katsura, Nishikyo, Kyoto 615-8520, Japan.
Hisao
H
Yoshida
Department of Applied Chemistry, Graduate School of Engineering, Hiroshima University , 1-4-1 Kagamiyama, Higashi Hiroshima 739-8527, Japan.
Nao
N
Tsunoji
Faculty of Engineering, Kanagawa University , Rokkakubashi, Kanagawa-ku, Yokohama-shi, Kanagawa 221-8686, Japan.
Wataru
W
Ueda
Department of Applied Chemistry, Graduate School of Engineering, Hiroshima University , 1-4-1 Kagamiyama, Higashi Hiroshima 739-8527, Japan.
Tsuneji
T
Sano
Department of Applied Chemistry, Graduate School of Engineering, Hiroshima University , 1-4-1 Kagamiyama, Higashi Hiroshima 739-8527, Japan.|JST, PRESTO , 4-1-8 Honcho, Kawaguchi, Saitama 332-0012, Japan.
Masahiro
http://orcid.org/0000-0001-7308-563X
M
Sadakane