This work explored the effects of Zn doping on the structural, micrographic, optical and photocatalytic behaviour of gallium oxide (β-Ga2O3) microrods. The X-ray diffractogram (XRD) and Raman spectral analyses confirmed the monoclinic structure of β-Ga2O3, with a shift to lower angles in the XRD pattern indicating Zn incorporation into the Ga2O3 lattice. The Scanning electron microscopy (SEM) images revealed a rod-like shape, with the diameter decreasing from 604 nm to 573 nm with Zn doping. Further analysis using TEM, HR-TEM, SAED, EDX, and elemental mapping confirmed the shape, crystallinity, crystal structure, and elemental distribution. The interplanar spacings were measured as 0.4 and 0.2 nm, corresponding to the (002) and (−311) planes of β-Ga2O3. UV–Vis diffuse reflectance spectroscopy (UV–Vis DRS) showed a slight shift in the absorption edge, while photoluminescence (PL) analysis demonstrated strong UV and weak visible light emission. Photocatalytic results revealed a high efficiency of dye degradation,(i.e) 98 % (20 ppm) and 89 % (30 ppm) against methyl orange (MO) dye aqueous solution over 150 min, with a rate constant of 0.02/min and 0.01/min, respectively for 1.5 wt% Zn doping. This suggests that the Zn-doped material holds promise as a photocatalyst for wastewater treatment applications.