Abstract: Hot-filament chemical vapor deposition has been used to deposit copolymer thin films consisting of fluorocarbon and siloxane groups. The presence of covalent bonds between the fluorocarbon and organosilicon moieties in the thin film has been confirmed by Infrared, X-ray Photoelectron (XPS) and solid-state 29Si, 19F, and 13C Nuclear Magnetic Resonance (NMR) spectroscopy. The film structure consists of chains with linear and cyclic siloxane groups and CF2 groups as repeat units.