成果報告書詳細
管理番号20110000001410
タイトル*平成22年度中間年報 革新型蓄電池先端科学基礎研究事業 革新型蓄電池先端科学基礎研究開発 3
公開日2012/6/27
報告書年度2010 - 2010
委託先名学校法人立命館
プロジェクト番号P09012
部署名スマートコミュニティ部
和文要約和文要約等以下本編抜粋:1. 共同研究の内容及び成果等 立命館大学SRセンターでは、SPring-8と相補的な軟X線領域のX線吸収分光(XAFS)、光電子分光(PES)を用いた手法の高度化を行っている。その目的のため、センターの3つの既存ビームライン、超軟X線分光(BL-2)、軟X線分光(BL-10)、硬X線分光(BL-3)ビームラインを蓄電池材料研究に特化し、研究環境を整備し、これまで不可能であった実験実施に向けての高度化を目的としている。平成22年度における研究の内容と成果は以下のとおりである。
(1) 超軟X線分光ビームラインの高度化と電池材料物質のXAFSスペクトルデータベースの構築 超軟X線分光ビームライン(BL-2)は3種類の不等間隔溝回折格子により、40?550 eVの単色光を供給していたが、蓄電池材料研究に必要な3d遷移元素のL吸収端XAFS測定用に、1000 eVまでの単色光が供給できる新規回折格子を平成21年度に設計製作した。平成22年度は新規回折格子の性能評価と、これを含めたすべての回折格子を用いて、40 ?1000 eVの範囲で蓄電池材料に関連した標準物質のLi, C, O, F K-XAFS, Mn, Fe, Co, Ni L-XAFS測定を行い、データベースを作成した。
英文要約Title:[NEDO1]Development of innovative analytical methods using soft X-ray synchrotron radiation(FY2009-2011)FY2010 Annual Report[NEDO2]
(1) Improvement of the ultra-soft X-ray spectroscopy beamline (BL-2) and implementation of the database of the standard materials for secondary batteries
By using four different plane gratings, including a newly designed and fabricated grating for high energy (500 - 1000 eV), BL-2 provides photons in the wide energy range from 40 eV to 1000 eV. This covers K- and L-edges of essential elements for batteries, such as Li, C, O, and Mn, Co, Ni. Database for the XAFS spectra of the standard compounds have been integrated and will be used for the future characterization of real secondary batteries.
(2) XAFS characterization of real electrodes with a transfer vessel
By using a simple and portable vessel, which was developed in the last fiscal year, we measured soft X-ray spectra of several cathode samples, prepared in a glove box, transferred in the SR center and introduced in the XAFS chambers without exposing to air. This system enables us to study the deterioration processes of real cathodes in the discharging and charging cycles without worrying about the effects of water and oxygen.
(3) Performance test of a newly-built PES-XAFS apparatus
The performance of the apparatus for PES and XAFS measurements was tested at BL-2. It revealed that the tuning of the photon energy is effective to enhance the photoelectron peaks of specific elements. Although further adjustment is necessary to get the full performance, preliminary tests demonstrate the effectiveness of a combined use of XAFS and PES.
(4) Surface and bulk XAFS with the total electron yield and total fluorescence yield
We found it very powerful to measure XAFS spectra simultaneously with the leak current mode and the total fluorescence mode using a micro-channel plate (MCP). The former probes the surface region, while the latter probes the bulk. This method is especially useful to discriminate the structural information of SEI from that of active materials in the batteries. We have successfully applied this method for characterization of real electrodes, but also found it necessary to develop a high sensitive X-ray fluorescence detector to improve the S/B ratio of XAFS spectra.
(5) Development of an imaging XAFS system in the hard X-ray beamline (BL-3)
Since real electrodes are, in general, inhomogeneous, structure determination of a local area is very promising. In the hard X-ray beamlines (BL-3 and 4), an imaging XAFS system was developed, where a photodiode array with 1024 pixels is adopted for 1-D imaging and a CMOS detector for 2-D imaging. With several demonstrative experiments, we found it possible to get the chemical species mapping with the spatial resolution of 0.1x 0.05 mm2. This resolution is comparable with those of NMR and neutron imaging.
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