Single crystals of intercalation compounds CuxTiS2 were prepared by the electrochemical method with an alternating current (voltage) applied. Structural characteristics of the compounds were investigated by x-ray diffraction method. The concentration of Cu atoms, x, is proportional to the time that the voltage is applied and the maximal value of x was estimated to be 0.7. Mosaic spreads of the intercalation compounds parallel to the c axis have almost the same value (similar-to 0.5 degrees) as that of pure TiS2, using estimates of the full width at half maximum (FWHM) of the (004) x-ray Bragg reflection. The diffraction patterns for all intercalation compounds are the same in that only the stage 1 structure exists. The c-axis lattice constant increases gradually with increase of x and is about 3% larger at x = 0.61 compared with that for pure TiS2.