Abstract. A1-and Co-substituted lithium nickel oxide of the nominal composition Li(Ni0.75Alo.17Co0,08)O2 was synthesised by a coprecipitation technique and by several solid state routes. Rietveld analysis of XRD profiles and galvanostatic cycling in glass cells were performed for structural and electrochemical characterisation. Depending on the reactivity of the respective precursor, there is in each case a minimal synthesis temperature, at which a single phase of the R 3m layered structure could be obtained. The coprecipitation technique and solid state routes using pre-substituted nickel hydroxide are suitable for the synthesis of single phase A1-and Co-substituted lithium nickel oxide, even at rather low synthesis temperatures. The electrochemical performance of lithium nickel oxide Li(Nio.75Alo.17Coo.08)O 2 synthesised in air is poor due to an enhanced lithium nickel disorder. Synthesis in oxygen atmosphere seems to be required.
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