LiNiPO4 belongs to a family of olivine type compounds, with members LiMPO4 where M =Fe, Mn, Co or Ni are transition metals. The lithium nickel phosphate was prepared and characterized in order to evaluate a new potential cathode material for our ongoing research in aqueous rechargeable batteries. Annealing the final product is critical in obtaining the stoichiometric LiNiPO4 pure phase; conventional cooling to a room temperature leads to an indication of Li3PO4 and NiO secondary phases as impurities. The synchrotron infrared radiation (SR-IR) as a source for IR spectroscopy pins down the differences in the chemical bonding for annealed and conventional cooled LiNiPO4 samples. The cyclic voltammetric and galvanostatic studies showed annealed LiNiPO4 is electrochemically active from which lithium ions can be de-intercalated during oxidation process leading to an amorphous NiPO4 and a minor product of nickel(II) hydroxide (β-NiOOH). During subsequent reduction, lithium ions are not fully intercalated, however, the structure is reversible and adequate for multiple cycles. The high potential in LiNiPO4 looks to be very attractive in terms of high energy density, given the efficiency is improved.