This paper investigates the adsorption behavior of triblock copolymer Poly (propylene oxide)-poly (ethylene oxide)-poly (propylene oxide), PPO-PEO-PPO on silicon and iron surfaces by using the contact angle goniometer, spectroscopic ellipsometer and atomic force microscopy (AFM). After adsorption, the decrease of water contact angle was observed on each surface; and a larger reduction of water contact angle occurred on the surface covered by the copolymer film with longer and higher weight percent of hydrophilic PEO block. This means that the PEO block may be on the top of the adsorbed copolymer film. The film thickness measurement shows that the copolymer with longer and higher weight percent of PPO block forms a thicker film on the hydrophobic surface, which suggests that the hydrophobic PPO block of the copolymer in the aqueous solution plays the main role during the adsorption of PPO-PEO-PPO onto the hydrophobic surface. It has been found from the AFM results that the roughness of the surface decreased after adsorption and the smoother topography was observed on the surface adsorbed by a thicker adsorbed film.