Photo-active nanomaterials are extensively used in the degradation of organic pollutants and in splitting water to produce energy. Current methods to produce photo-active nanomaterials generate toxic waste and require large amounts of energy to synthesize. The advent of green, facile, and benign methods of producing these nanomaterials is necessary to comply with modern environmental concerns. Important aspects for such green methods is low temperature, fast reaction rate, and reduced toxic agents. This chapter highlights new techniques to produce photo-active nanomaterials in order to minimize the use and generation of hazardous substances during the manufacturing process. Methods include hydrothermal methods, along with the polymer-gel technique, chemical precipitation technique, the solvothermal method, ultrasound sonication, and hybrid synthesis methods. Characterization techniques used to verify the successful synthesis of these photo-active nanomaterials and demonstrate improvement of their photoactivity will also be introduced.