A great necessity exists to reduce power consumption, cross-talk, and RC delay in ultralarge-scale integration (ULSI) devices to further improve their performance by replacing SiO 2 with a low dielectric constant material. Recently, much work has been focused on chemical vapor deposition (CVD) polymer thin films; however, they often suffer from poor resistance to metal diffusion and undesirable dielectric anisotropy. To overcome these limitations, a thermal CVD nanocomposite consisting of poly(chloro-p-xylylene) (PPXC) and SiO 2 was developed utilizing a recently developed near-room-temperature thermal CVD method to deposit SiO 2 . The composition of the nanocomposite thin films could be varied by increasing the vaporization temperature of the SiO 2 precursor, diacetoxy-di-tert-butoxysilane. Since the composition could be varied, both the index of refraction and the dielectric constant of the nanocomposites could potentially be varied, in situ, to deposit a graded film to eliminate the diffusion problem. The X-ray diffraction spectra show a reduction in the crystallinity of the nanocomposite with increasing weight fraction of SiO 2 compared to the PPXC homopolymer, thus reducing the dielectric anisotropy, resulting in a low in-plane capacitance desirable for ULSI devices. The thermal stability for the high polymer fraction (91%) nanocomposite was also better than that of the PPXC homopolymer at temperatures up to 415 °C after successive low-temperature postdeposition anneals in nitrogen. Microstructural analysis of a high weight fraction polymer nanocomposite, with transmission electron microscopy, revealed a continuous polymer phase with a largely interdispersed morphology on a ∼5-50-nm scale.