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

Etsuo Akiba1, Hiroshi Hayakawa1, Shigenobu Hayashi1, Ritsuro Miyawaki2, †, Shinji Tomura2, Yasuo Shibasaki2, Fujio Izumi3, Hajime Asano4 and Takashi Kamiyama4
1 National Institute of Materials and Chemical Research, 1-1 Higashi, Tsukuba, Ibaraki, 305 Japan
2 National Industrial Research Institute of Nagoya, 1-1 Hirate-cho, Kita-ku, Nagoya, 462 Japan
3 National Institute for Research in Inorganic Materials, 1-1 Namiki, Tsukuba, Ibaraki, 305 Japan
4 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, C1 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 P1(C1), a = 5.169(1) Å, b = 8.960(2) Å, c = 7.410(2) Å, α = 91.26(2)°, β = 104.99(2)°, γ = 89.93(1)°, Rwp = 3.17%, RI = 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.

Key Words: Crystal Structure • Kaolinite • Neutron Powder Diffraction • Rietveld Refinement • Synthetic Kaolinite

Clays and Clay Minerals; December 1997 v. 45; no. 6; p. 781-788; DOI: 10.1346/CCMN.1997.0450602
© 1997, The Clay Minerals Society
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