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Novel silver encapsulated nanocomposite zinc oxide/iron tetra-poly-vanadate (Ag-ZnO/Fe2V4O13) was synthesized with various wt% of silver (1.0–2.5 wt% of Ag) by cost-effective photo-deposition method under the irradiation of ultraviolet-A (UV-A) light. The nanostructure of the Ag-ZnO/Fe2V4O13 was explored by various characterization techniques. The surface functionalities were confirmed by Fourier transform infrared spectra and the crystalline nature of the material was revealed by X-ray diffraction patterns. Furthermore, the surface morphology and the optical properties of the composites were analyzed by scanning electron microscopy, energy dispersive X-ray–elemental color mapping (ECM), high-resolution transmission electron microscopy (HRTEM), ultraviolet–visible diffuse reflectance spectroscopy and photoluminescence. The crystallite size of Ag-ZnO/Fe2V4O13 was 28.5 nm which was consistent with HRTEM analysis. The photocatalytic activity was tested against aqueous methyl orange degradation under UV-A light irradiation. In all five runs, the stability of the catalyst was confirmed by reusability measurements and almost 98% of degradation was achieved. A suitable degradation pathway was proposed based on intermediates obtained during the degradation analyzed by gas chromatography–mass spectrometry. Trapping experiments confirmed that the superoxide radical anion (O2•−) was considered as the most active species for this degradation process. Complete mineralization was confirmed by the measurements of chemical oxygen demand. [ABSTRACT FROM AUTHOR]