We report the preparation and characterization of pure polyaniline nanoparticles (PANI_NPs), zinc oxide nanoparticles (ZnO_NPs), and ZnO_NPs/PANI hybrid inorganic/organic nanocomposites (HION) dispersed in aqueous sodium dodecyl sulfate solutions. We have characterized the HION, which were prepared by the polymerization of aniline in presence of sodium dodecyl sulfate and ZnO_NPs, by dynamic light scattering, zeta potential, Fourier transform infrared (FTIR), X-ray diffraction (XRD), and scanning electron microscope (SEM). We have obtained ZnO_NPs, PANI_NPs, and ZnO_NPs/ PANI with negative values of zeta potential and average diameters of 4.6 nm, 3.6 nm and 8.1 nm, respectively. XRD results reveal that the polymer exhibits a well-defined crystalline phase, as well as the presence of ZnO in a hex-agonal phase. The observed changes in the FTIR spectra of the HION are associated to the formation of hydrogen bonding between the ZnO_NPs and the NAH groups present in the PANI chains. Heterogeneous structures with fibrous characteristics are identified in the SEM images. Electrical measurements indicate that the ZnO_NPs/PANI HION exhibit a noticeable light-sensitive ohmic behavior. We suggest that the preparation method here described offers an easy route of synthesis for the development of water-soluble ZnO/PANI-based nanostructures with high colloidal stability and varied functionality. V C 2011 Wiley Periodicals, Inc. J Appl Polym Sci 125: E141-E147, 2012