The purification in a mixture of concentrated acids was used to modify the surface of carbon nanotubes with hydroxyl groups and carboxyl groups, etc. Furthermore, the sensitizing treatment of the CNTs was made in the SnCl_2·2H₂O solution. After treatment the solution with stable homogeneous dispersions of CNTs and CuSO₄·5H₂O was prepared. Then, glucose and formol were used as reductant to reduce the Cu²⁺ and Cu⁺ in order. After deoxidation, The CNTs and superfine Cu compound powders were obtained. SEM and TEM results showed that CNTs dispersed homogeneously in the compound powder and combined firmly with superfine Cu.