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Journal Articles

Characterization of electrode/electrolyte interface for lithium batteries using ${it in situ}$ synchrotron X-ray reflectometry; A New experimental technique for LiCoO$$_{2}$$ model electrode

Hirayama, Masaaki*; Sonoyama, Noriyuki*; Abe, Takashi*; Minoura, Machiko*; Ito, Masumi*; Mori, Daisuke*; Yamada, Atsuo*; Kanno, Ryoji*; Terashima, Takahito*; Takano, Mikio*; et al.

Journal of Power Sources, 168(2), p.493 - 500, 2007/06

 Times Cited Count:89 Percentile:90.34(Chemistry, Physical)

A new experimental technique was developed for detecting structure changes at electrode/electrolyte interface of lithium cell using X-ray reflectometry and two-dimensional model electrodes with a restricted lattice-plane. The electrodes were constructed with an epitaxial film of LiCoO$$_{2}$$ synthesized by pulsed laser deposition method. The anisotropic properties were confirmed by electrochemical measurements. ${it Ex situ}$ X-ray reflectivity measurements indicated that the impurity layer existed on the as-grown LiCoO$$_{2}$$ was dissolved and a new SEI layer with lower density was formed after soaking into the electrolyte. ${it In situ}$ X-ray reflectivity measurements indicated that the surface roughness of the intercalation (1 1 0) plane increased with applying voltages, while no significant changes in surface morphology were observed for the intercalation non-active (0 0 3) plane during the pristine stage of the charge-discharge process.

Journal Articles

Characterization of electrode/electrolyte interface with X-ray reflectometry and epitaxial-film LiMn$$_{2}$$O$$_{4}$$ electrode

Hirayama, Masaaki*; Sonoyama, Noriyuki*; Ito, Masumi*; Minoura, Machiko*; Mori, Daisuke*; Yamada, Atsuo*; Tamura, Kazuhisa; Mizuki, Junichiro; Kanno, Ryoji*

Journal of the Electrochemical Society, 154(11), p.A1065 - A1072, 2007/00

 Times Cited Count:96 Percentile:95.4(Electrochemistry)

Structural changes at electrode/electrolyte interface of a lithium cell were studied by X-ray reflectometry and two-dimensional model electrodes with a restricted lattice plane of LiMn$$_{2}$$O$$_{4}$$. The ex situ reflectometry indicated that a thin impurity layer covered the lattice plane of the as-grown film. The impurity layer was dissolved and a solid-electrolyte-interface-like phase appeared after the electrode was soaked into the electrolyte. The in situ observation clarified that the surface reactivity depended on the lattice planes of the spinel; the defect layer at the (111) plane was stable during the electrochemical reaction, whereas a slight decrease in the film thickness was observed for the (110) plane. Our surface characterization of the intercalation electrode indicated that the surface structure changes during the pristine stage of the change-discharge processes and these changes are dependent on the lattice orientation of LiMn$$_{2}$$O$$_{4}$$.

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