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Structural study of Li2MnO3 by electron microscopy

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Abstract

Detailed crystallographic data on high-quality Li2MnO3 material has been obtained using a combination of X-ray diffraction (XRD), selected-area electron diffraction (SAED), high-resolution electron microscopy (HREM), and 0.1 nm probe high-angle annular dark-field imaging (HAADF) in a scanning transmission electron microscope. A high-purity Li2MnO3 powder was annealed at 950 °C for 3 days to obtain predominantly defect-free grains which average size was 3.0 ± 1.5 μm. Rietveld refinement indicated that the C2/m spacegroup provided the best fit for the XRD data. Electron diffraction patterns obtained along various zone axes, on defect-free oxide particles, could be uniquely indexed to the monoclinic structure. HREM and HAADF images of defect-free grains were consistent with a Li–Mn–Mn– arrangement, i.e., lithium ordering in the transition metal planes. Low-magnification TEM images occasionally revealed stacking defects within oxide particles. HREM images of sample areas containing defects revealed a low density of stacking faults within the monoclinic sequence, resulting in a trigonal P3 1 12 local arrangement.

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Acknowledgements

We acknowledge D. Howell at the U.S. Department of Energy (DOE), Office of Vehicle Technologies, for supporting this research. We acknowledge the use of the Center for Microanalysis of Materials (CMM) at the Frederick Sietz Materials Research Laboratory, University of Illinois at Urbana-Champaign (UIUC), which is partially supported by the U.S. Department of Energy under grant DEFG02-91ER45439. Argonne National Laboratory is a U.S. Department of Energy Office of Science laboratory operated by UChicago Argonne LLC under contract DE-AC02-06CH11357.

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Correspondence to D. P. Abraham.

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Lei, C.H., Wen, J.G., Sardela, M. et al. Structural study of Li2MnO3 by electron microscopy. J Mater Sci 44, 5579–5587 (2009). https://doi.org/10.1007/s10853-009-3784-1

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