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
2018/3/22

課題番号 Project No.

装置責任者 Name of responsible person

2017A0130

Toshiya Otomo

実験課題名 Title of experiment

装置名 Name of Instrument/（BL No.）

Pair distribution function analysis on lithium-rich transition-metal

NOVA/BL21

oxide after delithiation

実施日 Date of Experiment

実験責任者名 Name of principal investigator

2017/5/19 - 2017/5/21

Yasushi Idemoto

2017/10/29 - 2017/10/30

所属 Affiliation
Tokyo University of 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.

Compositions: Li1.2-xMn0.54Ni0.13Co0.13O2
Physical form: 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.

Experimental method
By means of a coprecipitation method, lithium-rich transition-metal oxides with a layered structure, suchas Li1.2Mn0.54Ni0.13Co0.13O2, were synthesized. Phases of the samples were identified preliminarily by laboratorial
X-ray diffraction measurements, and the metal compositions are determined by the inductively-coupled plasma(ICP) spectroscopy. Samples with different Li contents were also prepared.
For these samples, neutron total scattering data were measured with NOVA installed at J-PARC. Powderof each sample was loaded in a V-Ni alloy container with 6 mm diameter and its total scattering pattern wasmeasured for 12 h under ambient condition. Additional data for calibration (background, empty container and Vrod) were also collected. By using the data, the obtained spectra of the samples were normalized into structure
factors S(Q) and then converted to reduced pair distribution functions G(r). The G(r) were analyzed by the PDF
fitting (PDFgui).

12. 実験方法及び結果（つづき） Experimental method and results (continued)
Results
From the Rietveld analysis using Bragg profiles, it was found that the synthesized samples had a single
phase of a layered structure with a space group of C2/m. It was also confirmed that the samples could deliver
higher discharge capacities than 200 mAh/g at room temperature.
For a sample with a composition of Li0.85Mn0.51Ni0.13Co0.12O2, a neutron total scattering pattern wasmeasured. Figure 1 (a) shows S(Q) derived from the pattern recorded at 45 o bank. As shown in the figure, S(Q)
could be normalized successfully. Figure 1 (b) shows G(r) obtained by the Fourier transform of S(Q) with the Q
range from 0.4 to 22 Å-1. The Q range was determined by considering data quality at high Q region. Although theQ range was a little bit narrow, clear atomic correlations could be observed in G(r) spectrum. A peak around 1.6
Å-1 seems to reflect C-C correlation in binder and/or conductive material which were used in a delithiation
process, and large negative peaks around 2.0 Å-1 could be attributed to Li-O and Mn-O. PDF fitting withsynchrotron X-ray PDF in addition to the neutron PDF is in progress.
(a)

(b)

Fig. 1 (a) structure factor S(Q) and (b) reduced pair distribution function G(r) of Li0.85Mn0.51Ni0.13Co0.12O2.

2