Li2NixFe1−xSiO4 (x = 0, 0.2, 0.4, 0.6, 0.8, and 1) samples were prepared by sol–gel process. The crystal structure of prepared samples of Li2NixFe1−xSiO4 was characterized by XRD. The different crystallographic parameters such as crystallite size and lattice cell parameters have been calculated. Scanning electron microscope (SEM) and Fourier transform infrared spectroscopy (FTIR) investigations were carried out explaining the morphology and function groups of the synthesized samples. Furthermore, electrochemical impedance spectra (EIS) measurements are applied. The obtained results indicated that the highest conductivity is achieved for Li2Ni0.4Fe0.6SiO4 electrode compound. It was observed that Li/Li2Ni0.4Fe0.6SiO4 battery has initial discharge capacity of 164 mAh g−1 at 0.1 C rate. The cycle life performance of all Li2NixFe1−xSiO4 batteries was ranged between 100 and 156 mAh g−1 with coulombic efficiency range between 70.9% and 93.9%.

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