This paper reports a surface process technology that simultaneously enables the formation of a hydrogel and its fixation on the surface of gold substrates. The technology utilizes two different chemical reactions of thiols : oxidation-induced disulfide bond formation and chemisorption on gold. Thiol-derivatized poly (vinyl alcohol)s (SH-PVAs), which were synthesized by radical copolymerization of vinylbenzyl N,N-diethyldithiocarbamate and vinyl acetate, followed by alkaline hydrolysis, were coated on gold surfaces and then air-dried at room temperature. X-ray photoelectron spectroscopy (XPS) analyses and water contact angle measurements of a gold surface before and after treatment with SH-PVA provided evidence that a hydrogel was formed and fixed on the gold surface. Atomic force microscopic (AFM) observations showed that the gel was tightly fixed even after thorough washing with hot water. Surfaces with regional hydrogelation, which were prepared on a gold-deposited micropatterned polymer, were visualized by cellular patterning under a phase-contrast microscope and by fluorescein-labeled protein immobilization under a fluorescent microscope.