The effect of copper sulfate/thiourea on the diffusion and the dye exhaustion of two dyes, C. I. Acid Orange 7 and C. I. Food Yellow 3 in nylon 6 fiber has been studied. The results obtained from the experimetal are as follows : 1) Copper sulfate reacted with thiourea at constant temperature and then generated the colorless trasparent coordination compound, and then combinated end group of carboxyl of nylon 6 fiber. 2) The coordination compound [$Cu_{2}$($TU_{6}$)] ($(SO_{4})_2$) is conducted at pH 5-6 in solution intensity and repulsed the sulfonic acid group of dyes, and therefore the diffusion of dyes is restraint. 3) Dye uptake and diffusion coefficient were decreased in the order of untreated > copper sulfate/thiourea-treated > tannin-treated.