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Although nickel-based alloys are widely used in industries due to their oxidation and corrosion resistance, the pursuit of better performance in harsh environments is still a great challenge. In this work, we developed a sol–gel method to synthesize Ni₃Al coating on a nickel alloy, assisted by a post-annealing process, and investigated the oxidation-resistant performance. The coating thickness can be controlled by designing the deposition times, which keep the pure Ni₃Al phase stable. In addition, the surface morphologies indicate that the coating is compact without obvious voids or cracks. Furthermore, the oxidation-resistant property of the coating was investigated by carrying out a supercritical water oxidation experiment. The crystalline structure and surface morphology of the samples before and after 72-h oxidation demonstrated the superior oxidation resistance of the coating. This work provides a convenient method to fabricate an oxidation-resistant coating on a nickel-based alloy, which would be significant for prolonging the service life of vessels under oxidation conditions, especially for supercritical water reactions.