Heterogeneous photocatalysis has demonstrated efficacy for the removal of toxic organic pollutants using semiconductor oxides. Microwave-assisted synthesis is a very attractive method for the fabrication of photocatalysts since microwave irradiation interacts directly with the solvent molecules due to its dielectric properties, and a uniform and rapid heating can be achieved. IIn this work, BiVO₄, ZnO, and BiVO₄/ZnO heterojunctions with different BiVO₄ loadings (20BVZO, 50BVZO, and 80BVZO, corresponding to 20%, 50%, and 80% BiVO₄, respectively) were synthesized via a microwave-assisted method without any subsequent high-temperature calcination. It was confirmed by X-ray diffraction (XRD) analysis that the crystal structures obtained were monoclinic scheelite for BiVO4 and hexagonal wurtzite for ZnO. Ultraviolet–visible spectroscopy technique was performed to determine the bandgap of the materials: 2.29–3.16 eV. Surface area analysis of the samples was performed to determine the surface measurements of the materials. The specific surface area of the ZnO, BiVO4, 20BVZO, 50BVZO, and 80BVZO samples was found to be 8.53, 0.72, 7.99, 5.91, and 3.59 m2/g, respectively. To complement the structural information, a Raman spectroscopy analysis was performed. The morphological analysis was carried out to determine the particle size and the distribution of particles. The photocatalytic activity of BiVO4/ZnO compounds in comparison with bare BiVO4 and pristine ZnO was tested for the degradation of methylene blue (MB), tetracycline hydrochloride (TC), and ciprofloxacin (CIP). The 20BVZO sample revealed enhanced photocatalytic performance (64.43%) among other compounds for tetracycline hydrochloride (TC) photodegradation with a photocatalyst dosage of 0.3 g/L.