Abstract
Structural characterization of Li2–xMP2O7 (M = Fe, Co) was carried out using neutron diffraction (ND) and X-ray diffraction (XRD) analyses to elucidate structural information and structural changes during an electrochemical reaction. The crystal system and space group were determined to be monoclinic P21/c for both materials with a = 11.0192 (4) A, b = 9.7488 (3) A, c = 9.8057 (4) A, and β = 101.569 (3)° for Li2–xFeP2O7 and a = 10.9574 (3), b = 9.6921 (3), c = 9.7611 (3), and β = 101.776 (2)° for Li2–xCoP2O7. XRD analysis revealed partial occupancy of iron and cobalt in the structures of Li2–xFeP2O7 and Li2–xCoP2O7, respectively. Also, ND identified lithium positions and partial occupancies in five different Li sites of Li2–xMP2O7 (M = Fe, Co). Further ex situ XRD showed that the charging/discharging of Li2–xFeP2O7 occurred primarily via a two-phase reaction with a slight solid solution behavior. We also demonstrated for the first time that Li2–xCoP2O7 electrodes are electrochemically active, with a redox...
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