This report discusses the efficiency of photo‐recovery of orthophosphate anions in water under visible irradiation using materials containing amorphous carbon, ceria and gold‐ceria species. Catalysts were obtained by the exchange of Amberlite‐732 polymeric‐resin with isolated Ce(III) and co‐mixing of Ce(III)‐Au(III) cations. Syntheses were developed for molar ratios Ce(III)/3H+=100 and Au(III)‐Ce(III)/3H+=0.01. Solids were treated at 800 °C under Air or Ar atmosphere then characterized by: X‐ray diffraction (XRD), Raman spectroscopy, scanning electron microscopy coupled to energy‐dispersive X‐ray spectroscopy (EDS), X‐ray photoemission spectroscopy (XPS) and UV‐visible spectroscopy. By XRD, non‐stoichiometric Ce2.658S4 sulfide and particles of metallic gold are identified in Ce‐Au‐Amb‐Ar and in the case of Ce‐Au‐Amb‐Air, mixture of CeO2 and Au0 is clearly observed. Moreover, XPS study of Ce3d emission spectra showed well resolved electronic states of the spin‐orbit Ce3d5/2 and Ce3d3/2 levels in the Ce4+ and Ce3+ oxidation states confirming coexistence of Ce(IV)/Ce(III). On the surfaces of both Ce‐Au‐Amb‐Air and Ce‐Au‐Amb‐Ar, XPS revealed metallic Au species. A certain amount of carbon, identified by EDS and XPS, corresponds to poorly ordered carbon formed by the resin decomposition during thermal treatments under Air and Ar. The UV‐vis spectroscopy was valuable to quantify the remaining PO43− anions in solution (at each moment of reaction) using “Molybdenum Blue” method. Photo‐recovery of orthophosphates under visible irradiation yields optimal trapping of ∼75 % of PO43− on Ce‐Au‐Amb‐Ar, attributed to a catalyst surface enrichment with Ce3+ species, which promoted structural oxygen vacancies.
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