The Ti-containing metal organic framework (MOF) MIL-125 has been used as sacrificial precursor to obtain TiO2 materials through the MOF-mediated synthesis route. In this study, Fe 3+ was deposited on the surface of MIL-125 after its hydrothermal synthesis. Targeted Fe-doped titania photocatalysts were prepared through the direct calcination in air of Fe/MIL-125 crystals and/or by using a two-step method, including carbonization in inert atmosphere followed by calcination in air. The relationship between the synthesis conditions and the properties of the Fe-doped titania nanopowders, such as Fe content, porosity, phase composition and particle size was investigated.From elemental mapping, X-ray photoelectron spectroscopy, X-ray absorption spectroscopy, UV-Vis absorption spectroscopy and photoluminescence emission spectra, the presence of highly dispersed Fe 3+ ions incorporated into the TiO2 crystal lattice was confirmed, which led to a significant red shift of photoresponse towards visible light and reduced the recombination rate of electron-hole pairs at low iron content. By varying the pre-carbonization temperature, both crystal size and phase composition in the final materials were modulated. The performance of Fe-doped titania materials in photocatalytic water-splitting was tested for hydrogen evolution. Optimal photocatalytic performance was found at 0.15 and 0.5 wt. % iron concentration and exceeded those of non-doped titania and commercial anatase both under visible and UV light irradiation, respectively, and among the highest reported in literature for these systems.

Optimized TiO2/CuxO/C nanocomposites derived from bi-MOF NH2-MIL-125(Ti/Cu) with in situ formed p–n heterojunctions exhibited superior photocatalytic HER performance without noble metals.

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