In this research, we studied an easy method to prepare pure cerium oxide nano particle (CeONP), pure zinc oxide nano particle (ZnONP) and Ce/Zn nano composite (Ce/ZnONP) coupled oxide by one pot reaction of cerium and zinc nitrate as precursors in aqueous solution using a Teflon-lined stainless autoclave at 120 °C for 12 h. Model water pollutant Acid Black 4BN as a di-azo textile dye was used to compare the photo-catalytic activity of (CeONP), (ZnONP) and (CeZnONP) deposited on flat-glass surface to overcome the problem of nano catalyst separation from suspension. Thermal, structural and spectral characterization of nano-structures were studied by thermo-gravimetric analysis, X-ray diffraction method, field emission scanning electron microscopy, Fourier transform infrared spectroscopy, energy dispersive X-ray spectroscopy. The elemental analysis using energy dispersive X-ray spectroscopy proved the existence of cerium and zinc in immobilized nano-structures Ce/Zn oxides. The X-ray diffraction result of the composite showed high crystalline cubic cerium oxide and hexagonal wurtzite zinc oxide. The photo-catalytic activity of Ce/Zn nano composite oxide coated on flat-glass surface for degradation dia-azo dye was enhanced compared to their single oxide counterparts. This heterogeneous photo-catalytic degradation of dia-azo dye can be applied as an alternative to suspended oxide powders and over-come drawbacks of filtration of photo-catalysts. This study for the first time showed the potential application of Ce/Zn nano composite for removal of organic pollutant from water.