A practical technique to prepare transmission electron microscopy (TEM) thin foil containing powder particle was described and the data for the codeposition of two type particles with copper in the electroplating were presented. By depositing the particles which were distributed in CuSO4 electrolyte on cathode together with Cu2+ in electrodeposition bath, composite coating with suitable thickness could be formed. The thin coating was separated from the substrate and cut into a disc with diameter of 3mm for electropolishing. When the Cu matrix was thinned during electropolishing, the particles contained in the coating plate were also thinned to meet the suitable thickness for TEM observation. Various experimental results revealed that during electrodepositing the current density, pH-value of electrolyte and stirring mode all have significant effects on the distribution of particles in composite coating and the surface quality of the composite coating. The proper parameters used during electrodepositing to prepare TEM thin foil containing powder particle were discussed.