The utilisation of methane (CH4) to produce syngas (H2, CO) via partial oxidation of methane (POM) is an attractive technique, as syngas is a very valuable entity to produce liquid fuels and fuel cell applications. This work presents the hydrothermal growth of ZnO nanoprisms (ZnO-NPr) in a dual solvent for a controlled structure. The Co-Ni loaded ZnO-NPr catalysts were obtained in an aqueous solution by wetness impregnation method and tested for POM for the first time. The synthesized catalysts were characterized by employing XRD, SEM-EDX, TGA and RAMAN spectroscopy for structural and morphological analysis. The catalysts were analyzed for POM at 850 °C and demonstrated high catalytic activity. It was observed that the catalytic activity of Co loaded ZnO-NPr, and Ni-Co loaded ZnO-NPr was more and demonstrated the stable behaviour for CH4 conversion in comparison to Ni loaded catalysts. The Co-Ni loaded ZnO-NPr has shown a high CH4 conversion (XCH4) (98%), and excellent stability over 56 h on stream. The average value of H2/CO for Co-Ni loaded ZnO-NPr was 2.11, above the theoretical value for POM. It is attributed to the better performance of catalyst towards the selectivity of H2 in reaction pathways.