Micro slide glass surfaces was coated by the self-assembled technique with a monolayer of hydrocarbon/fluorocarbon(HC/FC) compounds, such as CH₃(CH₂)_nC₂H₄-Si(CH₃)₂Cl (n=3,5,7,9) and CF₃(CF₂)_nC₂H₄Si(CH₃)₂Cl(n=3,5,7,9). These materials was synthesised by the hydrosilation reaction. These monomers was characterized using nuclear magnetic resonance(NMR). The effect of concentration of HC/FC on coating quantity was investigated. Sessile drop measurement was used for quantitative characterization of formation for the monolayer. An increase of concentration of HC/FC raised contact angle of water and methylene iodide. Contact angle of water and methylene iodide was increased according to an increment of alkyl chain length.