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 Report

課題番号 Project No.

装置責任者 Name of responsible person

2016B0049

Takanori Hattori

実験課題名 Title of experiment

装置名 Name of Instrument/（BL No.）

Pressure response of deuterated boehmite (AlOOD) to observe

PLANET (BL 11)

hydrogen bond symmetrization

実施日 Date of Experiment

実験責任者名 Name of principal investigator

2016/11/28-2016/11/30

Kazuki Komatsu
所属 Affiliation
Gradutate School of Science, The University of Tokyo
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.
deuterated boehmite, AlOOD

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.
Deuterated sample of boehmite was synthesized by hydrothermal treatment for the hydrogenated boehmitewith D2O. Powder of Al(OH)3 (99.99%, High Purity chemical. inc.) with 10 ml mill-Q water was inserted into aPTFE-lined autoclave, and kept at temperature of 513 K for 48 h. The same treatment was conducted withdeuterated water twice. In-situ neutron diffraction measurements of deuterated boehmite under pressure werealso performed on the PLANET beamline. The synthesized deuterated samples and deuterated
methanol-ethanol 4:1 mixture were loaded into a pair of encapsulating TiZr gaskets fitted with a tapered
aluminum ring, sandwiched with WC anvils (MF10, Fujilloy) and compressed by using the Paris-Edinburgh press(type V4). Sample pressures were estimated from the equation-of-state (EoS) obtained from the in-situ x-ray
diffraction separately conducted at PF-18C, KEK.

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2. 実験方法及び結果（つづき） Experimental method and results (continued)
The hydrogen bonding geometric parameters, O-D, D…O and O…O distances, obtained from the Rietveld
refinements for neutron diffraction patterns up to 9.48 GPa, are shown in Figure 1. Typical compression behavior
for hydrogen bond is found; O…O and D…O distances linearly decreases with increasing pressure, whereas O-D
distance linearly increases, i.e., O-D and D…O distances approach each other and their linear extrapolation will
merge at around 26 GPa (Fig. 2).

1.0

1.0

0.22 GPa 1.0

Iobs
Icalc
Ibkg
Iobs-Icalc
Boehmite

0.8

9.48 GPa 1.0

0.8

0.5

Intensity / a.u.

Intensity / a.u.

0.5
0.6

0.0

0.4

2

3

4

5

6

0.6

2
0.2

0.0

0.0
2

4

68

1012

0.0

0.4

0.2

(a)

Iobs
Icalc
Ibkg
Iobs-Icalc
Boehmite142(b)

Q (Å-1)46384

10512614Q (Å-1)

Fig. 1. Results of Rietveld refinements for neutron diffraction patterns acquired at (a) 0.22 GPa and (b) 9.48 GPa.
Insets show the enlarged plot for low-Q region. Broad scattering particularly seen in low-Q is derived from theAtomic distance (Å)

methanol-ethanol mixture used as pressure transmitting medium.

2.8
2.6
2.4
2.2
2.0
1.8
1.6
1.4
1.2
1.005 10 15 20 25 30 35 40

P (GPa)Fig. 2 Selective atomic distances, d(O-D), d(D…O) and d(O…O) in O-D…O H-bond, with increasing pressure.
Lines describe linear extrapolations for respective distances. Errors are within the size of symbols.

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