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Structure Refinement of Synthetic Deuterated Kaolinite by Rietveld Analysis Using Time-of-flight Neutron Powder Diffraction Data

Published online by Cambridge University Press:  28 February 2024

Etsuo Akiba
Affiliation:
National Institute of Materials and Chemical Research, 1-1 Higashi, Tsukuba, Ibaraki, 305 Japan
Hiroshi Hayakawa
Affiliation:
National Institute of Materials and Chemical Research, 1-1 Higashi, Tsukuba, Ibaraki, 305 Japan
Shigenobu Hayashi
Affiliation:
National Institute of Materials and Chemical Research, 1-1 Higashi, Tsukuba, Ibaraki, 305 Japan
Ritsuro Miyawaki*
Affiliation:
National Industrial Research Institute of Nagoya, 1-1 Hirate-cho, Kita-ku, Nagoya, 462 Japan
Shinji Tomura
Affiliation:
National Industrial Research Institute of Nagoya, 1-1 Hirate-cho, Kita-ku, Nagoya, 462 Japan
Yasuo Shibasaki
Affiliation:
National Industrial Research Institute of Nagoya, 1-1 Hirate-cho, Kita-ku, Nagoya, 462 Japan
Fujio Izumi
Affiliation:
National Institute for Research in Inorganic Materials, 1-1 Namiki, Tsukuba, Ibaraki, 305 Japan
Hajime Asano
Affiliation:
Institute for Materials Science, University of Tsukuba, Tenoudai, Tsukuba, Ibaraki, 305 Japan
Takashi Kamiyama
Affiliation:
Institute for Materials Science, University of Tsukuba, Tenoudai, Tsukuba, Ibaraki, 305 Japan
*
Current address: Department of Geology, National Science Museum, 3-23-1, Hyakunin-cho, Shinjuku, Tokyo, 169 Japan.

Abstract

The crystal structure of synthetic deuterated kaolinite was refined by Rietveld analysis using time-of-flight (TOF) neutron powder diffraction data. For non-hydrogen atoms, Cl symmetry was assumed. Starting models were tested in which only the direction of O-D vectors was varied. The constraints were introduced to all Al-O, Si-O and O-D bonds. The refinement adopting the former gives Pl(C1), a = 5.169(1) Å, b = 8.960(2) Å, c = 7.410(2) Å, α = 91.26(2)°, ß = 104.99(2)°, γ = 89.93(1)°, Rwp = 3.17%, R1 = 5.78% and S = 1.34 with constraints of l(Al-O)= 1.93 ± 0.05 Å, l(Si-O)= 1.62 ± 0.03 Å and l(D-O) = 0.95 ± 0.15 Å. The inner O-D vector points toward the tetrahedral sheet. All inner-surface O-D groups form H bonding with basal O atoms in the next kaolinite layers. The results agreed with those obtained from natural kaolinite.

Type
Research Article
Copyright
Copyright © 1997, The Clay Minerals Society

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