成果報告書詳細
管理番号20110000001408
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 7
公開日2012/6/27
報告書年度2010 - 2010
委託先名国立大学法人東北大学
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. 研究開発の内容及び成果等 a. 超高磁場(14T 以上)のNMR・MRI システムの開発 核磁気共鳴(NMR)はリチウム電池中の7Li 核をはじめ、電解質中の1H 核(プロトン)、F-19 核などの様々な原子核スピンをプローブとして、電池材料の構造変化やイオン移動に関する情報を得ることができる。平成21 年度に京都大学に設置した蓄電池材料用の高磁場NMR システムの特性評価と安定化について京都大学と連携して行った。東北大付属のNMR 装置を用いて、既存物質のNMR?MAS スペクトル(正極物質LiCoO2 等)を計測し、京都大学設置のNMR 装置の特性評価・性能比較が可能な資料を提供した。
b.高磁場(9.4T)NMR/MRI システムの開発(東北大担当)
モデルリチウムイオン電池の充放電時における活物質・電解液の構造変化を観測するために、東北大学既設の超伝導磁石を用いたNMR 施設を用いてNMR/MRI システムの開発を行った。平成21年度に行った測定技術検証を基に、東北大ではAvance 400 (9.4T)のマイクロMRI システムを稼動させ、チューニング・マッチング・磁場強度の調整などを行い、1H,7Li 核のNMR マイクロイメージング画像を取得できるシステムの調整を完了した。
英文要約Title : Research & Development Initiative for Scientific Innovation of New Generation Batteries (FY2009-FY2011) FY2010 Annual Report
a. Development of ultra high-field NMR system: Facilities of ultra high-magnetic field NMR system were installed in Kyoto University, which is specialized for analysis of new generation rechargeable batteries. We have measured MAS spectrum of typical cathode materials by existing NMR instrument in Tohoku university to evaluate characteristics and performances of new NMR devices in Kyoto University.
b. Development of high-field NMR system (in Tohoku University):  We have developed NMR/MRI system for particular application of rechargeable batteries by using existing superconducting magnet NMR instrument in Tohoku University. We made model lithium ion battery specialized for MRI measurement which was composed by glass and PTFE. It was a purpose of transmission of radio-frequency wave and magnetic gradients applied by a gradient probe. MRI results elucidate that it can detect spatial distribution of relaxation time (T2) in liquid electrolyte. This value is related to mobility of solvent and lithium ion in electrolyte, it is quite important factor of high performance lithium ion battery. We concluded that this characteristic feature has a potentiality of deterioration diagnosis of lithium ion battery.
d.Development of high-magnetic NMR system for multinuclear diffusion measurement:
We have installed high-gradient magnetic prove (diff60) on NMR instrument in Tohoku university. The maximum gradient is 3000G/cm, low temperature limit is -60℃, observable diffusion coefficient in lower limit is 10-10cm2/s. Using the above-mentioned probe, the diffusion coefficient of lithium ion (7Li) and proton (1H) has been measured for typical electrolytes for lithium ion battery, LiClO4+Propylene carbonate (PC), LiPF6 +Ethylene carbonate + dimethyl carbonate (DMC) etc. From the ratio of diffusion coefficient between lithium ion and solvent, we have discussed effective radius of solvent and ions, and concluded that in the entire systems lithium ion is associated with solvent strongly.
e.Development of high-magnetic MRI system for rechargeable battery:
 We detected 1H NMR images of lithium ion battery which composes LiMn2O4 / LiClO4+Propylene Carbonate (PC) / Li-metal during charging and discharging process. 1H NMR images of electrolyte near cathode material (LiMn2O4) shows anomalous intensity distribution, which is quite inhomogeneous. From NMR images as a function of repetition time (TR), We conclude it is not due to reduction effect of relaxation time but an indirect (spatial) magnetization effect from cathode material. The para-magnetization induced by high magnetic field distorts linearity of magnetic gradient field, it produces apparent intensity variance. This functional image is an easy diagnostic measurement for magnetization of cathode material, which has possibility to check a uniformity of cathode material and change of magnetizations under electrochemical process.
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