We have utilized the Langmuir-Blodgett (L-B) technique to develop the generic technology that can prepare nonsymmetrical microspheres. The dispersion of the microspheres in butanol was spread on a water surface and compressed by a L-B apparatus to obtain a microsphere monolayer. Then, an amphiphilic and reactive polymer was prepared by terpolymerization of N-octadecyl acrylamide,p-nitrophenyl acrylate, and 2,2,2,-trifluoroethyl methacrylate. A stable polymer monolayer was transferred onto the microsphere monolayer by the L-B technique. It was found from contact angle measurement that the surface became hydrophobic with deposit of the terpolymer. X-ray photoelectron spectroscopy data demonstrated that only the top side of modified microspheres was covered with the terpolymer.