This work is to develop an easy method of plasma treatment and graft polymerization to prepare thermosensitive gold nanoparticles. Gold nanoparticles (Nano-Au) were reduced by trisodium citrate combined with hydrogen tetrachloroaurate(III) tetrahydrate (chloroauric acid) and modified with 11-mercaptoundecanoic acid (MUA) by the self-assembly monolayers (SAM). The surface graft polymerization of N-isopropylacrylamide (NIPAAm) was carried out by two steps, using O(2) plasma pretreatment of the surface on MUA SAM modified Nano-Au to form the peroxide groups on Nano-Au(MUA), and then subsequently using UV light to induce grafting with thermosensitive polymer. Transmission electron microscopy (TEM) and scanning electron microscopy (SEM) were used to direct investigation of the particle size and morphology in situ. The diameters of the gold nanoparticles measured from the TEM images are in good agreement with data measured at room temperature which is about 15 nm. The thermosensitive gold nanoparticles were characterized by chemical structure of surface (ESCA) and Fourier-transform infrared spectroscopy (FUR). ESCA result suggests that plasma treatments can be employed to generate peroxides on the Nano-Au(MUA) for the subsequent UV graft polymerization of PNIPAAm. (C) 2010 Elsevier B.V. All rights reserved.