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。 ）Experimental Report

承認日 Date of Approval 2014/9/1
承認者 Approver Takanori HATTORI
2014/9/1
提出日 Date of Report

課題番号 Project No.

装置責任者 Name of Instrument scientist

2014A0110

Takanori Hattori

実験課題名 Title of experiment

装置名 Name of Instrument/（BL No.）

Structural analysis of the condensed phase of lithium borohydride

PLANET (BL11)

using high-pressure neutron diffraction

実施日 Date of Experiment

実験責任者名 Name of principal investigator

2014.5.8-5.13

Satoshi Nakano
所属 Affiliation
National Institution for Materials Science
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.
(1) Lithium borodeuteride (LiBD4), powder(2) Deuterated ammonia borane (ND3BD3), powder

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.

Low-Z hydrides are attractive as novel hydrogen-storage materials for their high hydrogen density, andnovel superionic conductors or superconductors. In the present work, we investigated the densification
behavior of two kinds of high hydrogen-density low-Z hydride, lithium borodeuteride (LiBD4) and deuterated
ammonia borane (ND3 BD3) using neutron diffraction under high-pressure for studies on novel materials.
The samples are loaded into an encapsulating gasket of a Ti-Zr alloy as a sample capsule in an inert
atmosphere of an Ar glove box. The capsule was clamped with toroid-type high-pressure anvils and set into
Paris-Edinburgh (PE) high-pressure cell. Since the sample is small, a focusing mirror and hBN collimator of theincident beam and a radial collimator are used. Usual 90-degree neutron diffraction measurement is performedin the duration of 8 hours. Pressure value was estimated from lattice parameters of the sample which has beenobtained using x-ray diffraction measurement.

2. 実験方法及び結果（つづき） Experimental method and results (continued)(1) Lithium borodeuteride (LiBD4)
In the experiment for LiBD4, a diffraction pattern obtained was quite weak. Absorption by boron in the sample
could be considered as a cause. Therefore, the sample was diluted with fluorinert as a pressure medium andthe similar measurement was carried out. The diffraction intensity was obtained from the diluted sample, but it
was not enough for structural analysis. For a future experiment, we will carry out an isotopic substitution ofboron in LiBD4 and try the similar measurement.
(2) Deuterated ammonia borane (ND3BD3)
The sample ND3 BD3 transforms to the first high-pressure phase (HP1) at 1.1 GPa and the second
high-pressure phase (HP2) at about 10 GPa. We have performed a neutron diffraction experiment for the firsttransformation last year. In the present work, we examined the similar experiment for the second
transformation. Diffraction data was obtained at 7.2, 9.8, and 14.1 GPa as shown in Figure 1. The diffraction
intensity obtained was enough to analyze the structure. Also, measurements of vanadium and empty cell werecarried out at the same conditions for an absorption correction of the diffraction profiles. Using the present
data, the crystal structures of HP1 and HP2 will be analyzed in detail and a pressure dependence of theirdehydration bond length will be calculated.

Figure 1. Neutron diffraction patterns of two kinds of high-pressure
phase of ND3BD3 (before an absorption correction).