A new technique for the silylation of pure-silica-zeolite MEL low-k films has been developed in which the spin-on films are calcined directly in trimethylchlorosilane or 1,1,1,3,3,3-hexamethyldisilazane (HMDS) in order to protect the films against corrosive wet etch chemicals and ambient moisture adsorption. In an alternative procedure, HMDS is also added to the zeolite suspension before film preparation. Fourier transform infrared spectroscopy, X-ray photoelectron spectroscopy, water-soak tests, and HF etch tests are performed to characterize the films. The dielectric constant is as low as 1.51, and the films resist HF attack up to 5.5 min. These properties are highly desirable by the semiconductor industry for next-generation microprocessors.