A convenient procedure to synthesize highly dispersed Ni1-xPdx alloys has been developed. The procedure is based on thermal decomposition in the reducing atmosphere of specially synthesized multicomponent precursor. The formation of single-phase solid solutions in the entire range of palladium concentrations was confirmed by powder XRD. The alloys have a porous structure composed of grains whose size depends on the synthesis temperature. The study of the catalytic properties of Ni1-xPdx alloys (5 wt% Pd) showed their high activity in the 1,2-dichloroethane decomposition process. After 5 h of catalytic experiment the yield of carbon material was 160 gС/gcat for Ni1-хPdх. This is more than 3 times higher than the yield of reference samples (porous Ni, Ni–Co, Ni–Cu). The carbon material formed has a segmented fibrous structure. It is characterized by high morphological uniformity. The specific surface area of the obtained carbon material is 580 m2/g.