This study reports on the solution combustion synthesis of two different ternary niobium oxides, namely, p-CuNb 2 O 6 and n-ZnNb 2 O 6. Such ternary oxides are attractive candidates in the "Holy Grail" search for efficient and stable semiconductors for solar energy conversion and environmental remediation. We demonstrate how this time-and energy-efficient method is capable of synthesizing high surface area and crystalline nanoparticles of the above compounds with enhanced optoelectronic properties. The synthesized crystalline samples were characterized by powder X-ray diffraction (with Rietveld refinement for phase purity), diffuse reflectance UV−visible and Raman spectroscopy, electron microscopy, and photoelectrochemical (PEC) techniques. The band structure of these oxides was probed by linear sweep voltammetry and by measuring their photoaction spectra (internal photon to electron conversion efficiency vs wavelength). The obtained bandgap energy values (1.9 and 3.2 eV for the Cu-and Zn-containing compounds, respectively) were in reasonable agreement with those obtained via electronic structure calculations (2.07 and 3.53 eV). Finally, p-CuNb 2 O 6 showed promising activity for the PEC reduction of CO 2 , while n-ZnNb 2 O 6 was active for sulfite and water photooxidation. HCOOH, CH 3 OH, etc., produced by the photochemical or PEC conversion of CO 2. 4,8,9 The most extensively studied n-type metal oxide semiconductor is TiO 2 , mostly because of its robustness, outstanding stability in aqueous media, coupled with nontoxicity and earth abundance of its constituent elements. 10,11 However, the wide bandgap (3.0−3.2 eV) of this material limits its application in solar energy utilization processes. A plethora of other n-type oxide semiconductors (binary or even ternary oxides) have been applied as photoanodes (e.g., ZnO, WO 3 , Nb 2 O 5 , SrTiO 3). 12 On the other hand, p-type semiconductors Special Issue: Kohei Uosaki Festschrift