Abstract
The crystal structure and defect chemistry of hydrothermally synthesized LiFe1-xMnxPO4 (x = 0, 0.25, and 0.50) particles have been characterized by simultaneous neutron and X-ray Rietveld refinement as well as X-ray and neutron pair distribution function (PDF) analysis, crystallinity determination, Mossbauer spectroscopy, ion coupled plasma (ICP) studies, and scanning electron microscopy (SEM). The very detailed structural refinements show that fast hydrothermal synthesis causes partial Fe-occupancy and vacancies on the Li (M1) site, while the Fe (M2) site is always fully occupied by iron. Thus, the defect is not merely a Li/Fe antisite defect, and excessive amounts of Fe are the origin of the disorder in the structure. Neutron and X-ray total scattering with PDF analysis show that after fast hydrothermal synthesis, the crystalline, defective LixFeyPO4 coexists with amorphous Li/Fe-PO4 structures having just short-range order. Iron excess is only seen in the crystalline part of the particles, and as the c...
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