Cuprous oxide and zinc oxide nanoparticles were prepared at room temperature by inorganic polycondensation. X-ray diffraction (XRD) analyses show that the oxide phases formed are pure and well crystallized. The spark plasma sintering (SPS) technique was successfully used to prepare dense nanoceramics with superimposed layers of Cu 2 O and ZnO nanopowders. Sintering conditions were optimized to densify the ceramics without phase transformation or diffusion. These ceramics were also characterized by XRD and scanning electron microscopy (SEM), as well as X-ray computed tomography (XCT). SEM and XCT showed that nanograins are preserved after SPS throughout both oxide materials, while a smaller layer (*20 lm) of pure oxide phase with larger grains is formed in between Cu 2 O and ZnO during the sintering process. The SPS technique results in high material density, with the absence of porosity and cracks, homogenous distribution, and a good phase separation. This is the first time that such as-prepared dense oxide-based heterojunction exhibits a photovoltaic effect under illumination opening a new route for preparing solar cells.