Sol–gel synthesis of iron titanates for the photocatalytic degradation of cyanide

• Published in: Journal of materials science 2024-08, Vol.59 (30), p.13772-13787
• Main Authors: Córdoba-Miranda, Stefanny, Ortiz-Rojas, Ingrid C., Cañas-Martínez, Diana M., Vazquez-Samperio, Juvencio, Pedraza-Avella, Julio A.
• Format: Article
• Language: English
• Subjects: Anatase; Catalytic activity; Characterization and Evaluation of Materials; Chelating agents; Chelation; Chemical Routes to Materials; Chemistry and Materials Science; Classical Mechanics; Crystallography and Scattering Methods; Diffraction patterns; Diffuse reflectance spectroscopy; Fourier transforms; Hematite; Ilmenite; Infrared spectroscopy; Iron; Light irradiation; Materials Science; Metal oxides; Oxidation; Photocatalysis; Photodegradation; Polymer Sciences; Precursors; Reagents; Sol-gel processes; Solid Mechanics; Spectroscopic analysis; Spectrum analysis; Synthesis; Titanates; Titanium; Titanium dioxide
• ISSN: 0022-2461; 1573-4803
• DOI: 10.1007/s10853-024-09940-7

Iron titanate mixed metal oxides were synthesized by the sol–gel method through four different routes. The effect of (i) the solvent of iron precursor, (ii) the addition of the chelating agent to the titanium or iron solution and (iii) the molar ratio between the chelating agent and the titanium or iron precursor over the overall percentage of obtained iron titanates was evaluated. Fourier-transform infrared spectroscopy (FTIR) and UV–Vis spectroscopy (UV–Vis) performed on the reaction medium evidenced the formation of acetate complexes of titanium (IV) or iron (III) during the different routes. X-ray diffraction (XRD) patterns of the obtained materials showed the formation of ilmenite (FeTiO 3 ), pseudorutile (Fe 2 Ti 3 O 9 ) and pseudobrookite (Fe 2 TiO 5 ) in different proportions, as well as hematite (Fe 2 O 3 ), rutile [TiO 2 (R)] and anatase [TiO 2 (A)]. The materials with the highest content of iron titanates obtained in each route were characterized and evaluated in the photocatalytic degradation of cyanide using visible light irradiation. UV–Vis Diffuse Reflectance Spectroscopy (UV–Vis DRS) showed that the samples exhibited energy bandgap values between 2.31 and 2.90 eV, which agrees with the values reported for iron titanates and evidence the possible activation of the materials under visible light. Scanning electron microscopy (SEM) and nitrogen physisorption results showed that the synthesized materials exhibited nanometric particle size and lower surface area (36.7 ± 4.8 m 2 ·g -1 ) than TiO 2 Degussa P-25 (72–155 m 2 ·g -1 ). The photocatalytic performance of the synthesized materials toward oxidation of CN − exceeded by 56% the activity of pure TiO 2 . The content of iron titanates in the synthesized materials was found to be the variable with the greatest influence on the photodegradation of cyanide. In addition, an inversely proportional relationship between the pseudorutile content of the materials and their photocatalytic activity was observed.