Lithium nickelate was synthesized by self-propagating high-temperature comb
ustion. The electrochemical behaviour of the product was studied by cyclic
voltammetry of microparticles immobilized on the surface of graphite electr
odes. Whereas numerous previous studies have dealt with non-aqueous electro
lyte solutions, here the behaviour of lithium nickelate in contact with aqu
eous electrolyte solutions was investigated. It could be shown that protons
are intercalating upon reduction of the Ni(III) to Ni(II) and deintercalat
ing upon oxidation. This insertion electrochemistry is chemically reversibl
e. Within 1600 oxidation-reduction cycles, the response diminished only by
about 10%. Scanning electron microscopy reveals a considerable recrystalliz
ation during the electrochemical cycles. Energy dispersive X-ray detection
proved that no metal cations are intercalating. The electrochemical system
is accessible only in very alkaline solutions as it shifts to more positive
values with decreasing pH.