In this study, nickel oxide–Y2O3-doped ZrO2 (NiO-YSZ) composite powder as an anode material was synthesized using a cost-effective combustion method for high-temperature solid oxide fuel cell (SOFC). Further, the effects of sintering temperatures (1200, 1300, and 1400 °C) were studied for its properties in relation to the SOFC performance. The prepared and sintered NiO-YSZ materials were characterized for their surface morphology, composition, structure, and conductivity. The cubic crystalline nature of NiO and YSZ was sufficed by X-ray diffraction, and SEM images revealed an increase in the densification of microstructure by an increase in the sintering temperature. EDX spectrum confirmed the presence of nickel, yttrium, and zirconia without any impurity. Conductivity measurements, under a hydrogen environment, revealed that NiO-YSZ, sintered at 1400 °C, exhibits better conductivity compared to the samples sintered at lower temperatures. Electrochemical performance of button-cells was also evaluated and peak power density of 0.62 Wcm−2 is observed at 800 °C. The citrate combustion method provided peak performance for cells containing anode sintered at 1200 °C, which was previously reported at higher sintering temperatures. Therefore, the citrate combustion method is found to be a suitable route to synthesize NiO-YSZ at low sintering temperature.