Structural studies of high voltage cathode materials are necessary to understand their chemistry to improve the electrochemical performance for applications in lithium ion batteries. LiNiPO 4 nanorods and nanoplates are synthesized via a one pot synthesis using supercritical fluid process at 450 o C for 10min. The X-ray diffraction (XRD) analysis confirmed that LiNiPO 4 phase is well crystallized, phase purity supported by energy dispersive spectroscopy (EDS) and elemental mapping by scanning electron transmission electron microscopy (STEM). For the first time, we have carried out direct visualization of atom-by-atom structural observation of LiNiPO 4 nanomaterials using high-angle annular dark-field (HAADF) and annular bright-field (ABF) scanning transmission electron microscopy (STEM) analysis. The Rietveld refinement analysis was performed to find out the percentage of antisite defects presents in LiNiPO 4 nanoplates and about 11% of antisite defects were found. Here, we provide the direct evidence for the presence of Ni atoms in Li sites and Li in Ni sites as an antisite defects are provided for understanding of electrochemical behavior of high voltage Li ion battery cathode materials.
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