Fe 3 O 4 @ZrO 2 @TiO 2 (Y@ DS FZT) nanospheres were synthesized based on the calcination and solvothermal process parameters. The architectural ternary nanocatalyst was characterized by Xray diffraction (XRD), energy-dispersive X-ray spectroscopy (EDS), field emission scanning electron microscopy (FESEM), transmission electron microscopy (TEM), Brunauer−Emmett−Teller (BET), Fourier transform infrared (FTIR) spectroscopy, Raman spectroscopy, X-ray photoelectron spectroscopy (XPS), thermogravimetric analysis (TGA), photoluminescence (PL), and VSM analyses. The architectural nanostructured samples Y@DS FZT, prepared by a hybrid synthesis method of solvothermal, sol−gel, selective etching, and calcination, showed significant differences in band gap energy, optical properties, and crystal phase under different synthesis conditions. The effect of the parameters of the solvothermal and calcination processes on the band gap energy of nanoreactors with Y@DS FZT architecture was investigated, and the optimal conditions for these parameters were determined based on the designed Box−Behnken model. The photocatalytic activity of ZrO 2 and TiO 2 with a high band gap energy is investigated in the UV region, while the architectural structure of Y@DS FZT was studied based on the decrease of band gap energy in the visible light region. In addition, the influence of crystal size and specific surface area (SSA) on the band gap energy of Y@DS FZT samples was investigated. For the photocatalytic conversion of CO 2 to fuel, the best developed sample Y@DS FZT was used as the selected photocatalyst in this reaction, achieving a methanol production efficiency of 301.29 μmol/g cat •h. The photocatalytic conversion performance of the CO 2 reduction depends on the band gap energy of the nanophotocatalysts, the architectural structure of the Y@ DS FZT nanoreactor, and the presence of structural defects on the deposited shells that were studied.