For the nano-ZrO2 powders, it is difficult to disperse the particles in a highly concentrated electrolyte. Polymer MZN with composite structure was employed as a dispersant in this work. On the basis of having obtained the optimum quantity of dispersant MZN, the effects of process conditions on stability of Ni-ZrO2 composite electroplating bath were investigated via sedimentation experiments and SEM micrograph. The results showed that the charging sequence have a significant influence on the stability of composite electroplating bath, and the optimum process conditions is that the stable aqueous suspension of 2.5g nano-powders in 100 ml water should be prepared at first by milling for 3 hours, and then the electrolytes were added in it. The well-dispersed composite electroplating bath was obtained, which made sure that the nano-ZrO2 smaller than 30nm was found in the Ni matrix.