Novel alumina modified zinc oxide materials were prepared by co-precipitation method in the presence of different amounts of cetyltrimethylammonium bromide (CTAB) surfactant. X-ray diffraction, Al-27 magic-angle spinning Nuclear Magnetic Resonance Spectroscopy, and transmission electron microscopy studies evidenced formation of 10-15 nm zinc oxide nanoparticles in the presence of the small amounts of surfactant. Amorphous alumina and zinc aluminate phases of different coordination environment of Al sites were identified. An increase of surfactant concentration led to the elongation of nanoparticles and changes of the nature of hydroxyl groups. Precipitation in the high CTAB concentration conditions facilitated formation of mesoporous materials of high specific surface area. The materials were composed of very small (2-3 nm) zinc aluminate spinel nanoparticles. High concentration of CTAB induced widening of band gap energy. (C) 2016 Elsevier Ltd. All rights reserved.