The study has explored the physical and chemical properties of nickel‐boron/nano‐diamond composite coatings upon pre/post heat treatment. The nano‐composite coatings were produced by electroless plating. In fact, the effects of using the nano‐diamond additives (0 g l−1, 0.1 g l−1, 0.3 g l−1, 0.5 g l−1, 0.7 g l−1) were investigated in pre/post heat treatment. According to the results, the micro‐hardness of the nickel‐boron/nano‐diamond composite coating produced in the bath containing 0.5 g l−1 nano‐diamond additive reached to 1005 HV 0.05 upon post‐heat treatment. Also, the corrosion resistance of the nickel‐boron/nano‐diamond composite coatings was modified by using the nano‐additive or heat treatment. But, adding nano‐diamond particles reduced the ductility and wear resistance of the nickel‐boron coatings. We also found, modification of the properties (ductility and wear resistance) of the composite coatings was achieved by using the heat treatment.