Journal
JOURNAL OF PHYSICAL CHEMISTRY C
Volume 119, Issue 24, Pages 13472-13480Publisher
AMER CHEMICAL SOC
DOI: 10.1021/acs.jpcc.5b03273
Keywords
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Funding
- Research and Development Innovative for Scientific Innovation of New Generation Battery (RISING) Project from New Energy and Industrial Technology Development Organization (NEDO), Japan
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Delithiation and lithiation behaviors of ordered spinel LiNi0.5Mn1.5O4 and disordered spinel LiNi0.4Mn1.6O4 were investigated by using in situ (in operando) Li-7 NMR and ex situ Li-6 MAS NMR spectroscopy. The in situ Li-7 monitoring of the ordered spinel revealed. a clear appearance and subsequent disappearance of a new signal from the well-defined phase Li0.5Ni0.5Mn1.5O4, suggesting the two-phase reaction processes among Li1.0Ni0.5Mn1.5O4, Li0.5Ni0.5Mn1.5O4, and Li0.0Ni0.5Mn1.5O4. Also:, for the disordered spinel, Li0.5Ni0.4Mn1.6O4 was identified with a broad distribution in Li environment. High-resolution Li-6 MAS NMR spectra were also acquired for the delithiated and lithiated samples to understand the detailed local structure around Li ions. We suggested that the nominal Li-free phase Li0.0Ni0.5Mn1.5O4 can accommodate a small amount of Li ions in its structure. The tetragonal phases Li2.0Ni0.5Mn1.5O4 and Li2.0Ni0.4Mn1.6O4, which occurred when the cell was discharged down to 2.0 V, were very different in the Li environment from each other It is found that Li-6,Li-7 NMR is highly sensitive not only to the Ni/Mn ordering in LiNi0.5Mn1.5O4 but also to the valence changes of Ni and Mn on charge-discharge process.
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