Herein, Fe-doped C₃N₄ high-performance photocatalysts, synthesized by a facile and cost effective heat stirring method, were investigated systematically using powder X-ray diffraction (XRD), Fourier transform infrared (FTIR), scanning electron microscopy (SEM) and Brunauer-Emmett-Teller (BET) surface area measurement, X-ray photoelectron (XPS), UV-Vis diffusion reflectance (DRS) and photoluminescence (PL) spectroscopy. The results showed that Fe ions incorporated into a g-C₃N₄ nanosheet in both +3 and +2 oxidation states and in interstitial configuration. Absorption edge shifted slightly toward the red light along with an increase of absorbance in the wavelength range of 430-570 nm. Specific surface area increased with the incorporation of Fe into g-C₃N₄ lattice, reaching the highest value at the sample doped with 7 mol% Fe (FeCN7). A sharp decrease in PL intensity with increasing Fe content is an indirect evidence showing that electron-hole pair recombination rate decreased. Interestingly, Fe-doped g-C₃N₄ nanosheets present a superior photocatalytic activity compared to pure g-C₃N₄ in decomposing RhB solution. FeCN7 sample exhibits the highest photocatalytic efficiency, decomposing almost completely RhB 10 ppm solution after 30 min of xenon lamp illumination with a reaction rate approximately ten times greater than that of pure g-C₃N₄ nanosheet. This is in an agreement with the BET measurement and photoluminescence result which shows that FeCN7 possesses the largest specific surface area and low electron-hole recombination rate. The mechanism of photocatalytic enhancement is mainly explained through the charge transfer processes related to Fe²⁺/Fe³⁺ impurity in g-C₃N₄ crystal lattice.

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