The effect of nickel doping on the structure of Li2FeSiO4 is examined by X-ray diffraction, Mössbauer spectroscopy, Fourier transform infrared spectroscopy, scanning electron microscopy, energy dispersive spectrometer, and magnetization measurements. Both, the pristine and nickel doped Li2FeSiO4, crystallize in a monoclinic structure with (P21/n) symmetry. Their lattice parameters are similar, which suggests that Ni2+ doesn’t destroy the lattice structure. Some small amounts of Fe3+ impurity phases and unreacted Li2SiO3 are detected. Samples doped with more than 10 mol% contain some magnetic impurity of Fe-Ni alloy. Magnetic measurements indicated that Li2FeSiO4 is paramagnetic and becomes antiferromagnetic below 23 K. Nickel dopant does not modify the paramagnetic nature of this material.