<p>This study investigates the effects of graphene incorporation and heat treatment on the corrosion resistance and structural integrity of Ni–B coatings. Ni–B coatings were produced using the electroless plating method, with the incorporation of 0.5 wt pct graphene, and evaluated after heat treatment at 400&#xa0;°C. The corrosion performance of the coatings was assessed using electrochemical potentiodynamic polarization tests and electrochemical impedance spectroscopy. The results demonstrate that the incorporation of graphene followed by heat treatment significantly increases the corrosion resistance. While the corrosion current density of the uncoated substrate was 3.82E−6 A/cm², this value decreased to 60.2E−9 A/cm² with the addition of graphene and subsequent heat treatment. Similarly, the polarization resistance was calculated as 17.4E+3 Ω·cm² for the substrate material, whereas it increased to 1.33E+7 Ω·cm² for the graphene-incorporated and heat-treated sample. These findings reveal that graphene incorporation and subsequent heat treatment constitute an effective enhancement strategy for Ni–B coatings.</p>