ZnO 2 nanoparticles (NPs) have been studied, which, due to their semiconducting and oxidizing properties, are promising for the development of new materials for optoelectronics, photocatalysis, sensorics, biomedicine, and theranostics. The synthesis of ZnO 2 NPs in dispersed systems based on lipophilic surfactants has been tested. The possibility of simple synthesis of ZnO 2 NPs ~5 nm in size by the reaction of Zn (CH 3 COO) 2 and H 2 O 2 in reverse micelles and emulsions of surfactants Brij 30, Span 80, and AOT has been shown. It has been found that the type of dispersed system and the nature of surfactants of the studied series have no strong effect on the size of NPs. The powder of ZnO 2 NPs exhibits photoluminescence with an emission maximum at 520 nm; upon heating, it decomposes to ZnO with the release of oxygen and an exotherm with a maximum at 213°C. Using organosols of ZnO 2 NPs and their mixtures with Au NPs, films were obtained on glass and polyethylene terephthalate substrates, as well as ZnO films by heating the ZnO 2 films. The ZnO 2 and ZnO films have a granular morphology, the composite ZnO 2 and Au films have an island morphology based on spheroidal agglomerates of Au NPs with inclusions of ZnO 2 nanocrystals.