Facile Synthesis, Characterization of Flower-Like Vanadium Pentoxide Powders and Their Photocatalytic Behavior

doi:10.1007/s40195-017-0611-6

Abstract

Abstract:

In this paper, V₂O₅ sol was firstly prepared using vanadyl sulfate as a vanadium source by modified sol-gel method at room temperature. Then flower-like V₂O₅ powders were prepared by coagulating as-prepared sol with anhydrous ethanol and subsequent annealing crystallization. The X-ray diffraction analysis indicated that V₂O₅ powders exhibited orthorhombic crystal structure after annealing at 450 °C. The experimental data obtained from both field emission scanning electron microscopy and high-resolution transmission electron microscopy identified that V₂O₅ powders were approximately flower-like in shape and about 5 μm in size. Besides, the Brunauer-Emmett-Teller specific surface area of flower-like V₂O₅ powders was 24.25 m²/g. According to Uv-Vis spectroscopy, the degradation rate of toluidine blue O (TBO) on as-prepared flower-like V₂O₅ powders during 10 h of visible light irradiation with an intensity of 15.4 mW/m² was 88%, which was faster than those over P25 (46%) as a comparison. In addition, the mineralization process of TBO was investigated, which primarily consisted of demethylation and ring-opening oxidation processes, and confirmed by liquid chromatograph-mass spectrometry. The precipitation-oxidation-peptization, coagulation, and crystallization processes were proposed as the formation mechanism for the preparation of flower-like V₂O₅.

Key words: Vanadium pentoxide, Photocatalyst, Toluidine Blue O, Mechanism, Demethylation

Yao Li, Jian-Lei Kuang, Yi Lu, Wen-Bin Cao. Facile Synthesis, Characterization of Flower-Like Vanadium Pentoxide Powders and Their Photocatalytic Behavior[J]. Acta Metallurgica Sinica (English Letters), 2017, 30(10): 1017-1026.

Figures/Tables 12

Fig. 1 Schematic illustration of the proposed synthesis of V2O5 powders

Fig. 2 XRD patterns of a as-synthesized sample from a sol prepared at room temperature, coagulated, dried at 60 °C for 6 h, and subjected to heat treatments at 450 °C for 3 h; b compared nanoparticles from a solution dried at 80 °C and subjected to heat treatments at 500 °C for 2 h according to previous report [27]

Fig. 3 XPS spectra of sol dried at 60 °C for 6 h a survey scan, b V2p and O1s core-level spectra, and V2O5 sample annealed at 450 °C, c fully scanned spectrum, d V2p and O1s core-level spectra. Inset is molar ratio of vanadium and oxygen in xerogel

Fig. 4 Typical FESEM and TEM images of the as-prepared samples. a, b FESEM images of xerogel at 60 °C for 6 h, and, c-e FESEM images of V2O5 powders at 450 °C for 3 h. f TEM, g HRTEM images of the V2O5 powders

Fig. 5 Proposed formation mechanism of V2O5 sol at room temperature in air

Fig. 6 Schematic illustration of evolution process from sol to flower-like V2O5

Fig. 7 a Diffuse reflectance UV-Vis spectrum of flower-like V2O5 powders thermally treated at 450 °C; b Tauc’s plot of (αhυ)2 versus hυ for band gap energy

Fig. 8 a Comparison of photocatalytic performance of the samples by testing the degradation of TBO under visible light irradiation. b Graphical evaluation of the rate constants for mineralization of TBO in the presence of flower-like V2O5 powders under visible light irradiation. c Percentage of TOC removal over flower-like V2O5 powders

Fig. 9 Reusability study of flower-like V2O5 powders for TBO degradation under visible light irradiation

Fig. 10 LC-MS spectra of the observed products under visible light for 0-10 h with flower-like V2O5: a the peak at m/z=270 due to compound A; b the peak at m/z=256 attributed to compound B; c the peak at m/z=242 attributed to compound C; d the peaks at m/z=242, 243, 229, 170, and 161 attributed to compounds C, detected C +H, detected D +H, F, and G, respectively; e the peaks at m/z=149 and 116 attributed to compounds H, K, respectively; f the peaks at m/z=149, 133, and 116 attributed to compounds H, J, and K, respectively

Fig. 11 Proposed degradation pathway of TBO dye under visible light irradiation followed by the identification of several intermediates by LC-MS spectral techniques

Fig. 12 LC-MS spectra of the observed products under visible light for 6 h with flower-like V2O5: a the peak at m/z=261 assigned to the ring-opened sulfoxide oxidation product; b the peak at m/z=277 attributed to the sulfone

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