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In our recent papers, it was shown that the thermal nanocrystallization of glassy analogs of selected cathode materials led to a substantial increase in electrical conductivity. The advantage of this technique is the lack of carbon additive during synthesis. In this paper, the electrochemical performance of nanocrystalline LiFePO₄ (LFP) and LiFe_0.88V_0.08PO₄ (LFVP) cathode materials was studied and compared with commercially purchased high-performance LiFePO₄ (C-LFP). The structure of the nanocrystalline materials was confirmed using X-ray diffractometry. The laboratory cells were tested at a wide variety of loads ranging from 0.1 to 3 C-rate. Their performance is discussed with reference to their microstructure and electrical conductivity. LFP exhibited a modest electrochemical performance, while the gravimetric capacity of LFVP reached ca. 100 mAh/g. This value is lower than the theoretical capacity, probably due to the residual glassy matrix in which the nanocrystallites are embedded, and thus does not play a significant role in the electrochemistry of the material. The relative capacity fade at high loads was, however, comparable to that of the commercially purchased high-performance LFP. Further optimization of the crystallites-to-matrix ratio could possibly result in further improvement of the electrochemical performance of nanocrystallized LFVP glasses.