<p>The development of high-performance and sustainable electrode materials is essential for next-generation supercapacitors. Here, we report a CeO₂/N-doped carbon (CeO₂/NC) hybrid synthesized by integrating hydrothermally prepared CeO₂ nanoparticles with nitrogen-doped carbon derived from a Na-MOF precursor. Structural and morphological analyses confirm a mesoporous hybrid with strong CeO₂–carbon interfacial coupling. Among the various weight-percentage CeO₂/NC composites synthesized, CeO₂/NC-20 exhibits the highest surface area (186.7 m²&#xa0;g⁻¹) and uniform nanoparticle dispersion. Electrochemically, the CeO₂/NC-20 electrode delivers 1452 F g⁻¹ at 1 A g⁻¹ in a three-electrode system, superior rate performance, and dominant surface-controlled charge storage. The fabricated symmetric device achieves 215 F g⁻¹, 29.8 Wh kg⁻¹, and 92% retention over 5000 cycles, with low charge-transfer resistance and stable ion diffusion. The successful lighting of an LED demonstrates its practical potential. This work highlights the promise of Na-MOF-derived N-doped carbon/metal oxide hybrids for scalable, high-energy supercapacitor applications.</p>