The invention discloses a process for preparing nanometer composite material of poly thiofuran metal-oxide. The process for preparation is as follows: charging nanometer composite material into solution, and then charging sodium polystyrene sulfonate solution to agitate at high speed or scatter though supersonic, under the obtained solution is agitated, charging thiofuran monomer, oxidant and accelerant respectively, which the mol ratio between the oxidant and the monomer is 0.1-5 and the mol ratio between the accelerant and the monomer is 0.001-0.01, dropping hydrochloric acid to regulate the pH level between 2 and 5 and agitating at high speed for 24-48 hours, drying the obtained miscible liquids at 60-120 DEG C for 3-12 hours, and milling the solid to obtain the nanometer composite material of poly thiofuran metal-oxide. The invention solves the problems effectively of easily agglomerate metal-oxide nanometer particle, bad stability of chemical stability, the composite material has the advantages of simple preparing process, low the cost of the preparing and better property of light, electricity and magnetism and the like.