実験報告書様式（一般利用課題・成果公開利用）（ ※本報告書は英語で記述してください。ただし、産業利用課題として採択されている方は日本語で記述していただいても結構です。 ）MLF Experimental Report

提出日 Date of Report2013.5.16

課題番号 Project No.

装置責任者 Name of responsible person

2012B0016

Kazuya Aizawa

実験課題名 Title of experiment

装置名 Name of Instrument/（BL No.）

Transformation of bonding and dynamics of magnesium hydroxide

TAKUMI (BL 19)

at high pressures

実施日 Date of Experiment

実験責任者名 Name of principal investigator2013.1.15-17

Takuo Okuchi

2013.3.10-13

所属 Affiliation
Okayama University
試料、実験方法、利用の結果得られた主なデータ、考察、結論等を、記述して下さい。（適宜、図表添付のこと）
Please report your samples, experimental method and results, discussion and conclusions. Please add figures andtables for better explanation.
1. 試料 Name of sample(s) and chemical formula, or compositions including physical form.

magnesium deuteroxide (Mg(OD)2)
deuterated magnesium-iron silicate (Mg,Fe)2SiO4: xD2O
grycerine-d8 (C3D5OD3)

2. 実験方法及び結果 （実験がうまくいかなかった場合、その理由を記述してください。）
Experimental method and results. If you failed to conduct experiment as planned, please describe reasons.

Powder Mg(OD)2 sample of appropriate grain size for neutron powder diffraction (ca. 5~10µm) was synthesized from MgO powder and D2O liquid in an autoclave kept at 240ºC and 40 MPafor five days. The sample was evaluated by powder x-ray diffraction and Raman spectroscopy
prior to the use for high pressure experiments. No contamination of additional phase and no OH
stretching peak were observed from the synthesized Mg(OD)2 powder.
We prepared several different types of compressed samples in compact opposed anvil cells,
those are with different volume and pressure. To compress these samples into desired pressures,
we used combinations of single crystal diamond, nano-polycrystalline diamond, and/or sinteredpolycrystalline diamond as two opposed anvils. We also prepared TiZr “null” alloy gaskets which
is not only very strong but also nearly transparent for neutron, so that is ideal material for opposedanvil cell compression experiments. Its heat-treatment procedure was optimized to accept
extensive deformation between these superhard anvils.
12. 実験方法及び結果（つづき） Experimental method and results (continued)

A photograph of typical opposed anvil cell used for the neutron diffraction measurement andrepresentative ruby fluorescence spectra indicating the pressure of the sample chamber are shownin the above figures. We have successfully obtained moderate-quality neutron diffraction patterns
up to 8 GPa pressures for ~4 mm3 volume of the sample and up to 17 GPa pressures for ~2 mm3volume of the sample. In most case, the sample powder was mixed with small amount of
deuterated glycerin to improve the hydrostacitity before compression.

Above figure shows lattice parameter change of the Mg(OD)2 sample with increasingpressure, preliminarily determined from the obtained neutron diffraction patterns. We are now
analyzing these patterns by Rietveld refinement method to find the structure parameters related tothe chemical bonding state of hydrogen, and to discuss the transportation of bonding and dynamics
of hydrogen at high pressures.

2以下は、ＭＬＦで内部資料として使用します。(日本語可)
The following sheet is for internal use only. Description in Japanese is acceptable.
○論文等による成果発表の予定 (Your publication plan)a) 発表形式(*1)
Publication style(*1)b) 発表先(誌名、講演先)(*2)
Publication/Meeting information(*2)(Name of journal/book or meeting)c)投稿/発表時期(*3)
Date of paper submission
or presentation(*3)

原著論文

Physics and Chemistry of Minerals

６ヶ月以内

その他口頭発表

鉱物科学会

２０１３年９月【記入要領】(Instructions)(*1)

原著論文、総説、プロシーディングス、単行本、特許、招待講演（国際会議）、その他口頭発表等、具体的な発表方法を示して下さい。

Please describe planned publication and/or presentation style; ex. refereed journal, review article, conference
proceedings, book, patent, invited talk, oral presentation etc.
(*2)

成果を発表する誌名、講演先を示して下さい。

Please describe the name of journal or book you are planning to submit, or name of meeting you will make apresentation.
(*3) およその発表予定時期を示して下さい。（３月以内、６月以内、１年以内、２年以内、２年以上先、等）Please describe the estimated date of paper submission or presentation; ex. within 3 months, within 6 months,
within 1 year, within 2 years, beyond 2 years, etc.

○成果になる予定が立たない場合の理由と今後の計画を記述してください。
In case you can not publish your results, please describe reasons and future plan.
（例：「論文になる十分な結果が得られなかった」、「複数回の実験が必要で次回の課題終了後に発表予定」、等）

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