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Silicon nitride and oxynitride films of very low hydrogen content have been deposited on silicon at low temperatures (150–200 °C) using ion‐beam sputtering. A dual‐ion‐beam sputtering technique, making simultaneous use of an energetic argon‐ion beam to sputter silicon nitride from a target and a low‐energy oxygen or nitrogen ion beam to react with the sputtered films on the substrate, has been employed to control the composition of the films. A precise control of film composition independent of deposition rate has been achieved through the control of oxygen/nitrogen ion‐beam parameters and gas flow ratios. The films have been characterized by the measurement and study of refractive index, chemical etch rate, infrared absorption, and x‐ray photoelectron spectra. A direct correlation between film properties with oxygen content has been obtained for silicon oxynitride films. The electrical properties have been studied by the measurement of the characteristics of metal‐insulator‐semiconductor capacitors fabricated using the deposited films. In situ ion‐beam oxidation of silicon prior to the oxynitride deposition has resulted in a film with a low insulator charge number density (3.5×1011 cm-2) and interface trap density (4×1011 cm-2 eV-1), which is suitable for device applications.