Polymer microspheres were prepared by dispersion copolymerization of styrene with poly(oxyethylene) (peo) macromonomer. A dispersion terpolymerization of styrene, PEO macromonomer and acrylic acid was also conducted to prepare polymer microspheres with both surface carboxyl groups and PEO polymer chains. The microspheres thus obtained were characterized with TEM, IR, and X-ray photoelectron spectroscopy analyses. Palladium nanoparticles were then formed on the surface of these copolymer microspheres forming polymer/metal nanocomposites which were then studied by TEM and X-ray diffraction.