The purpose of this work was to prepare electrodes from nickel-manganese-cobalt oxide and lithium ferrophosphate and test them as positive electrodes in lithium-ion galvanic cells. The electrodes were obtained by applying the paste to the aluminum foil current collector. The paste consists of active material, binders and additives. Lithium-ion galvanic cells were prepared in a commercial El-Cell cell. Electrochemical measurements were carried out in a two-electrode and three-electrode system using the cell charging/discharging method and cyclic voltammetry and electrochemical impedance spectroscopy in a two-electrode system. Dynamic light scattering was used to determine particle size, while FTIR was used to detect possible contaminants. Cyclic voltammetry points to a two-phase intercalation reaction in LFP materials and a stepwise electrochemical reaction in NMC materials. NMC material potentially achieves higher power due to reactions at higher potentials. The cyclic voltammogram of LFP shows one electroactive redox (Fe2+/Fe3+), while NMC indicates two couples with different degrees of oxidation (Ni2+/Ni4+ and Co3+/Co4+). The voltage profile of the LFP positive electrode is a plateau characteristic of a twophase (de)intercalation reaction, while the voltage profile of the NMC electrode is in constant decline. NMC achieves higher specific charge and discharge capacities but has weaker capacity retention at higher charge/discharge currents than the LFP positive electrode. Both materials show a loss of capacity in the first charging cycle due to the SEI layer formation, but it is more pronounced in NMC. Electrochemical impedance spectroscopy indicates better electronic and ionic conductivity of NMC material. Dynamic light scattering shows better uniformity and optimal particle size for NMC materials. The FTIR spectra show a weak signal of the possible content of water molecules on the NMC powder.