Hydrothermal Synthesis and Photocatalytic Prореrties of Iron-Doped Tungsten Oxide

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Abstract

Substitutional solid solutions of the general formula h-W1–xFexO3, where 0.01 ≤ x ≤ 0.06, crystallizing in the hexagonal system based on h-WO3, were obtained using the hydrothermal synthesis method. It was shown that the crystal lattice of the synthesized compounds h-W1–xFexO3 is stabilized by NH4+ cations in hexagonal channels. Using quantum chemical calculations, it has been proven that doping with iron is realized by replacing cations in the tungsten sublattice, and not by intercalation into lattice channels. In this case, the dopant is not an independent participant in reactions involving h-W1–xFexO3, causing only the reorganization of the near-Fermi states of the h-WO3 matrix. It has been established that the region of solid solution homogeneity with respect to the dopant ion is determined by the pH of the working solution. The largest specific surface area, equal to 108 m2/g, has h-W0.94Fe0.06O3, synthesized at pH 2.3. Its photoactivity when applied to 1,2,4-trichlorobenzene is several times higher than that of m-W0.94Fe0.06O3.

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About the authors

G. S. Zakharova

Institute of Solid State Chemistry of the Ural Branch of the Russian Academy of Sciences

Author for correspondence.
Email: volkov@ihim.uran.ru
Russian Federation, Ekaterinburg

N. V. Podvalnaya

Institute of Solid State Chemistry of the Ural Branch of the Russian Academy of Sciences

Email: volkov@ihim.uran.ru
Russian Federation, Ekaterinburg

T. l. Gorbunova

Postovsky Institute of Organic Synthesis of the Ural Branch of the Russian Academy of Sciences

Email: volkov@ihim.uran.ru
Russian Federation, Ekaterinburg

M. G. Реrvоva

Postovsky Institute of Organic Synthesis of the Ural Branch of the Russian Academy of Sciences

Email: volkov@ihim.uran.ru
Russian Federation, Ekaterinburg

A. N. Enyashin

Institute of Solid State Chemistry of the Ural Branch of the Russian Academy of Sciences

Email: volkov@ihim.uran.ru
Russian Federation, Ekaterinburg

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Supplementary files

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2. Fig. 1. Diffractograms of tungsten oxide powders doped with iron(III), composition h-W1–xFexO3, synthesized at pH 1.7(a) and x = 0.01 (1), 0.03 (2), 0.05 (3), at pH 2.3 (b) and x = 0.01 (1), 0.03 (2), 0.06 (3). Calculated diffractograms and difference curves are additionally presented for samples with the maximum content of the dopant ion. The vertical lines indicate the positions of reflexes

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3. Fig. 2. Concentration dependences of unit cell parameters a(a), c(b), V(c) for WO3 doped with iron(III) synthesized at pH 1.7 (1) and 2.3 (2)

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4. Fig. 3. SEM images of h-W0.95Fe0.05O3 (a) and h-W0.94Fe0.06O3 (b) synthesized at pH 1.7 and 2.3. X-ray energy dispersion microanalysis spectrum for sample h-W0.94Fe0.06O3 (c). An additional peak from carbon is caused by the substrate, used to fix the sample

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5. Fig. 4. IR (a) and Raman spectra (b) of h-WO3 (1), h-W0.95Fe0.05O3 (2) and h-W0.94Fe0.06O3 (3) synthesized at pH 1.7 and 2.3, respectively. Vaseline oil strips are marked with an asterisk

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6. Fig. 5. TG, DSC, and MS curves for h-W0.95Fe0.05O3 (a) and h-W0.94Fe0.06O3 (b) synthesized at pH 1.7 and 2.3, respectively

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7. Fig. 6. Electronic state densities (ED) calculated by the DFT method for h-WO3 and h-W1–xFexO3 with model compositions (NH4)0.33WO3 · 0.33H2O(a) and (NH4)0.50W0.95Fe0.05O3 · 0.33H2O (b) respectively

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8. Fig. 7. Sorption isotherms (1 — adsorption, 2 — desorption) and pore size distribution curves (inserts) h-W0.95Fe0.05O3 (a) and h-W0.94Fe0.06O3 (b) obtained at pH 1.7 and 2.3, respectively

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9. Fig. 8. Absorption spectra in the UV and visible ranges (a), dependences (ahv)1/2 on the photon energy (E) in the region of the absorption edge (b) for h-WO3 (1), h-W0.99Fe0.01O3 (2), h-W0.97Fe0.03O3 (3) and h-W0.94Fe0.06O3 (4) synthesized at pH 2.3

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