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Hybrid thin films containing nano-sized inorganic domains were synthesized from UV-curable acrylate-modified waterborne polyurethane (WPU-AC) and monodispersed colloidal silica with coupling agent. The coupling agent, 3-(trimethoxysilyl)propyl methacrylate (MSMA), was bonded onto colloidal silica first, and then mixed with WPU-AC to form a precursor solution. This precursor was spin coated, dried and UV-cured to generate the hybrid films. The silica content in the hybrid thin films was varied from 0 to 30 wt%. Experimental results showed the aggregation of silica particles in the hybrid films. Thus, the silica domain in the hybrid films was varied from 30 to 50 nm by the different ratios of MSMAsilica to WPU-AC. The prepared hybrid films from the crosslinked WPU-AC/MSMA-silica showed much better thermal stability and mechanical properties than pure WPU-AC.