Аннотация:Electrochemical properties of nickel-containing polyanionic cathode materials for metal-ion batteries crystallized in three structure types (olivine, NASICON, and α-CrPO4) are studied. The subjects of the research are: LiFe0.5Ni0.5PO4 (olivine), Na1 + 2xNixZr2 – x(PO4)3 (NASICON), as well as Na2Ni2Cr(PO4)3 and Na2Ni2Al(PO4)3 (α-CrPO4). The samples are prepared by different synthetic methods; their phase composition, crystal structure, and morphology are studied. The LiFe0.5Ni0.5PO4- and Na1 + 2xNixZr2 – x(PO4)3-based materials are shown undergoing irreversible structure changes during the first charge with significant irreversible electrochemical capacity (~70−100 mA h g–1). During the cycling of Na2Ni2Cr(PO4)3 and Na2Ni2Al(PO4)3 in sodium half-cell, only Cr3+/Cr4+-redox-couple demonstrated electrochemical activity. The correlation of structure features and electrochemical properties of the studied materials is discussed.