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Catalytic partial oxidation of methane (CPO) to synthesis gas was performed over differently prepared CeO₂ supported nickel catalysts with 6 wt% Ni content. The samples were synthesized by microwave assisted procedures and by hydrothermal deposition procedure. Differences in the catalyst structural properties of the prepared catalysts were detected by XRD, TPR and XPS measurement. When tested at atmospheric pressure with feed gas mixture containing methane and oxygen in molecular ratio CH₄/O₂ = 2, all the samples reached 98% conversion with CO selectivity values >95% in the 700–800 °C temperature range. The samples exhibited different behavior towards carbon formation during the tests. Moreover, according to XRD, XPS and TGA results, when the carbon was formed it did not cause catalyst deactivation. TPR profiles confirmed different degree of chemical interaction between NiO and CeO₂ …