This work presents investigations on preparation of 20 wt. % Pt0.5Pd0.5/C nanoelectrocatalysts by electroless and their electrocatalytic properties. The 20 wt. % Pt0.5Pd0.5/C nanoelectrocatalysts were prepared by electroless successfully. The optimum experimental conditions of the main effect factors in preparing the PtPd nanoelectrocatalysts are [Pt2+ or Pd2+] =2-10g/L, [HCHO] =10-20g/L, temperature: 40-60°C, the dosage of protection reagent: 1-3 % of the platinum and palladium content, the agitation rate 400-500r/min. The characterization of 20 wt. % Pt0.5Pd0.5/C was performed with cyclic voltammetry (CV) and transmission electron microscope (TEM), respectively. Particles of PtPd are distributed symmetrically on C by TEM, of which are very small and the average granularity is less than 3nm. The nanoelectrocatalysts have high stabilization and lots of catalysis nuclei through CV.