The influence of concentration of complexant, dispersing agent and stable agent on the weight rate of electroless nickel plating on diamond powder was investigated by means of orthogonal experiment method. The results show that the influence order of factors on weight is as follows: ammonia> citric acid> sodium citrate> thiourea> dodecyl benzene sulfonate. Considering the weight gain rate, electroless plating leakage and crystals stock, the optimal recipe of electroless nickel plating on diamond powder is nickel sulfate 25 g/L, sodium hypophosphite 33 g/L, ammonia 10-15 mL/L, citric acid 15-20 g/L, sodium citrate 10-15 g/L, thiourea 1.3-2.1 mg/L, dodecyl benzene sulfonate 1.6-2.4 g/L。