The aim of this study was to provide an experimental investigation on the novel method for recycling chips of duplex stainless steel, with the addition of vanadium carbide, in order to produce metal/carbide composites from a high-energy mechanical milling process. Powders of duplex stainless steel with the addition of vanadium carbide were prepared by high-energy mechanical ball milling utilizing a planetary ball mill. For this proposal, experiments following a full factorial design with two replicates were planned, performed, and then analyzed. The four factors investigated in this study were rotation speed, milling time, powder to ball weight ratio and carbide percentage. For each factor, the experiments were conducted into two levels so that the internal behavior among them could be statistically estimated: 250 to 350 rpm for rotation speed, 10 to 50 h for milling time, 10:1 to 22:1 for powder to ball weight ratio, and 0 to 3% carbide percentage. In order to measure and characterize particle size, we utilized the analysis of particle size and a scanning electron microscopy. The results showed with the addition of carbide in the milling process cause an average of reduction in particle size when compared with the material without carbide added. All the four factors investigated in this study presented significant influence on the milling process of duplex stainless steel chips and the reduction of particle size. The statistical analysis showed that the addition of carbide in the process is the most influential factor, followed by the milling time, rotation speed and powder to ball weight ratio. Significant interaction effects among these factors were also identified.