Composition, bonding state, and electrical properties of CNx films formed by electro-chemical deposition using liquid acrylonitrile were studied. X-ray photoelectron spectra reveal that C, N, and O are major components of the deposited films. From analysis of C 1s and N 1s spectra, the major bonding state in the CNx film is attributed to a mixture of C≡N and partially hydrogenated C=N bond. Metal-insulator-semiconductor capacitors incorporating the CNx insulating layers are fabricated to evaluate the electrical properties of the deposited films. The lowest dielectric constant k of the CNx film is determined to be 2.6 from the accumulation capacitance and the thickness of the film. It is demonstrated that the CNx film formed by electrochemical deposition is a promising low-k material for use in ultralarge-scale integration multilevel interconnections.