| Citation: |
Qiang Zhang, Zhi-wen Jiang, Mo-zhen Wang, Xue-wu Ge. Gamma Ray Radiation Effect on Bi2WO6 Photocatalyst[J]. Chinese Journal of Chemical Physics , 2018, 31(5): 701-706. DOI: 10.1063/1674-0068/31/cjcp1805094
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Bi2WO6, the simplest Aurivillius-type oxide with a narrow band gap of about 2.8 eV [1, 2], is becoming more and more enthusiastic in view of their promising application in the photocatalytic degradation of organic pollutants [3-6]. However, the photocatalytic performance of Bi2WO6 remains to be improved due to its low light absorption efficiency and electron-hole separation efficiency [7-9]. Thus, many methods have been developed to improve the photocatalytic activity of Bi2WO6, including the regulation of morphology [10-13], doping [14-16], or the preparation of composite materials [17, 18]. For example, Zhou et al. [19] directly prepared three dimensional highly hierarchical flower-like Bi2WO6 microspheres which were formed by the self-aggregation of nanoplates in a hydrothermal way at low temperature. Zhu et al. [20] prepared F− substituted Bi2WO6 (Bi2WO6−xF2x) photocatalysts with high activity by a two-step process. Sun et al. [21] synthesized hollow sphere shaped Bi2WO6/reduced graphene oxide (RGO) composites by a facile and cost-effective route and evaluated their photocatalytic activities by the degradation of five different kinds of pollutants under natural sunlight irradiation.
On the other hand, researches show that the oxygen vacancies in the Bi2WO6 crystals can also improve their photocatalytic performance due to the reduction of the recombination of photo-generated carriers [22-25]. For example, Zhu et al. [24] reported Bi2WO6−x nanoplates with wide-range-visible photoresponse by introducing surface oxygen vacancies through the controllable hydrogen reduction method. Chai et al. [25] prepared Bi2WO6 with oxygen vacancies (Bi2WO6-OV) by simple assisted solvothermal method using ethylene glycol as the reducing agent. However, as far as we know, there are no reports about the creation of oxygen vacancies in Bi2WO6 under high energy radiation, although it is well-known that high energy radiation such as γ-ray can interact with semiconductors and generate defects [26-29], and be widely used for the synthesis of various inorganic or polymeric materials [30-34].
Herein, in this work, the γ-ray radiation effect on the crystal structure and light absorption characteristics of Bi2WO6 was studied by using 60Co as γ-ray source. The visible light photocatalytic degradation of MB in aqueous solution was also carried out to investigate the photocatalytic performance of the irradiated Bi2WO6. The results show that the oxygen vacancies can be created in Bi2WO6 nanocrystals under γ-ray radiation at a high absorbed dose, which improves the visible light photocatalytic performance of Bi2WO6.
All reagents used in this work including Bi(NO3)3⋅5H2O, Na2WO4⋅2H2O, hexadecyl trimethyl ammonium bromide (CTAB), and methylene blue (MB) were purchased from Sinopharm Chemical Reagents Co., Ltd. (Shanghai, China). The reagents were all analytical grade except that MB was BS grade. Deionized water was used in all experiments.
The synthesis of Bi2WO6 nanosheets was via a simple hydrothermal method [35]. In a typical procedure, 0.48 g of Bi(NO3)3⋅5H2O, 0.16 g of Na2WO4⋅2H2O, and 0.025 g of CTAB were dissolved in 40 mL of deionized water with magnetic stirring for 30 min. Next, the mixed solution was transferred into a 50 mL Teflon-lined stainless steel autoclave and stood for 24 h in an oven at 120 ℃. Then, the autoclave was cooled to room temperature naturally. The obtained product was collected by centrifugation, washed by water and absolute alcohol respectively for three times, and finally dried in an oven at 60 ℃ for 12 h. To remove the remaining surfactant CTAB, the dried sample was heated to 600 ℃ in air at a rate of 5 ℃/min in a muffle furnace and calcinated for 5 h.
The as-prepared powder of Bi2WO6 nanosheets (100 mg) was put in a 10 mL of plastic centrifuge tube and irradiated by 60Co γ-ray (1.37×1015 Bq, located in USTC, China) at a dose rate of 5.28 kGy/h for different total absorbed doses (127, 253, 380, and 507 kGy). The dose rate was calibrated using alanine/EPR standard dosimeter.
X-ray diffraction (XRD) spectra were obtained on a TTRIII diffractometer (Rigaku, Japan) using Cu Kα radiation source (λ=1.5418 Å) at a scanning rate of 8o/min in the range of 10o-70o. The field-emission scanning electron microscopy (FESEM, JEOL JSM-6700F, 5 kV) was used to observe the morphologies of Bi2WO6 nanosheets. UV-Vis diffuse-reflectance spectroscopy was performed on Shimadzu SOLID 3700 UV-Vis spectrophotometer. The X-ray photoelectron spectroscopy (XPS) was carried out with Thermo ESCALAB 250 using monochromatic Al Kα radiation. Photoluminescence spectra were obtained using steady-state transient fluorescence spectrometer (Horiba JY Fluorolog-3-tau) with the excitation laser irradiation of 250 nm.
The photocatalytic performance of the irradiated Bi2WO6 was evaluated using the decomposition of MB under the exposure of simulated visible light irradiation as the model reaction. A 300 W Xe lamp (Perfectlight PLS-SXE300/300UV) with a cut-off filter (λ
|
DMB=C0−CtC0×100/% |
where C0 is the concentration of MB at the adsorption-desorption equilibrium in dark environment, and Ct is the concentration of MB after being irradiated by light for a time period of t.
After the decomposition of MB, the irradiated Bi2WO6 nanosheets were recycled by centrifugation and washed by absolute alcohol to remove MB. After being dried at 60 ℃, the recycled Bi2WO6 nanosheets were used for the next cycle of photocatalytic experiment.
Disk-like Bi2WO6 nanosheets with a diameter of 400-800 nm and a thickness of about 100 nm can be facilely prepared by a solvothermal method [35], as shown in FIG. 1(a). After being irradiated by γ-ray, the morphology of these disk-like Bi2WO6 nanosheets has little change when observed by SEM even at an absorbed dose as high as 507 kGy, as exhibited in FIG. 1 (b)-(e). However, the color of Bi2WO6 powders obviously changes from light yellow to light blue after γ-ray radiation with an absorbed dose above 380 kGy, as shown in the insets of FIG. 1 (a)-(e), which means that there are some changes occurring in the physical structure of Bi2WO6 nanocrystals after high-dose γ-ray radiation although the morphology has not been destroyed.
FIG. 2 displays the XRD spectra of Bi2WO6 nanosheets after being irradiated at different absorbed doses, compared with that of the unirradiated sample. Basically, the distinct peaks at 2θ values of 28.3o (113), 32.9o (020), 47.2o (220), 55.8o (313), and 58.5o (226) (FIG. 2(a)), which are indexed to the orthorhombic phase of Bi2WO6 (JCPDS card No.73-1126), have been detected for both primary and the irradiated samples. It means that the unit cell of Bi2WO6 remains unchanged under γ-ray radiation. However, the corresponding magnified views of the peak at (113) of Bi2WO6 samples (FIG. 2(b)) show a regularly shift toward high angle with the increase of the absorbed dose. The similar shift has been reported in previous studies, which would be caused by shrinkage of the lattice spacing induced by the defects [23, 36].
In order to confirm the weak change in the crystal structure of Bi2WO6 nanosheets induced by γ-ray radiation, XPS spectra of the primary and irradiated Bi2WO6 nanosheets have been measured, as shown in FIG. 3. The peaks at 164.5 and 159.2 eV in FIG. 3(a) are ascribed to levels of Bi 4f5/2 and Bi 4f7/2 spin-orbit splitting photoelectrons in the Bi3+ chemical state of unirradiated Bi2WO6, respectively. However, these two peaks have a 0.1 eV shift to a higher binding energy, which can be contributed to the formation of neighbouring oxygen vacancies with higher electron attracting ability [25]. The similar change also occurs for the peaks at 35.45 and 37.6 eV which are assigned respectively to W 4f7/2 and W 4f5/2 spin-orbit doublets in the W6+ chemical state (FIG. 4(b)). There is a 0.15 eV shift to a higher binding energy for the irradiated Bi2WO6. Correspondingly, the binding energy of O 1s at 530.10 eV shifts to 530.25 eV after γ-ray irradiation, and splits into two peaks at 530.04 eV (Bi-O) and 530.66 eV (W-O) [24]. The decrease in the relative intensity of the peak for Bi-O to that for W-O reveals that oxygen vacancies are formed due to the removal of O atoms connected with Bi atoms.
The UV-Vis spectra of the primary and irradiated Bi2WO6 nanosheets are shown in FIG. 4. It is seen that both primary and irradiated Bi2WO6 nanosheets can absorb the light with a wavelength of between 300 and 450 nm. The corresponding band gaps (Eg) of the samples estimated according to the equation (αhν)2=A(hν-Eg) are 2.83 (primary), 2.83 eV (127 kGy), 2.82 eV (253 kGy), 2.77 eV (380 kGy), and 2.80 eV (507 kGy), showing a slight drop of the Eg of Bi2WO6 nanosheets with the increase of the absorbed dose, which means that the irradiated Bi2WO6 nanosheets theoretically have a better visible light absorption efficiency and photocatalytic performance than primary Bi2WO6.
It is known that the intensity of the steady-state photoluminescence (PL) spectrum can reflect the recombination rate of photogenerated carriers in semiconductor materials [37]. FIG. 5 displays the PL spectra of the primary and irradiated Bi2WO6 nanosheets under the excitation of 250 nm laser. All of the Bi2WO6 samples present broad-band emission spectra. The emission intensity of Bi2WO6 has no change until the absorbed dose reaches 380 kGy, but it drops significantly when the absorbed dose rises up to 507 kGy. The results indicate that the oxygen vacancy defects in Bi2WO6 generated under high-dose γ-ray radiation will make the charge carriers transfer fast and retard their recombination [38]. This manifests that Bi2WO6 nanosheets should have an improved photocatalytic performance after the exposure under high-dose γ-ray radiation.
The photocatalytic performances of Bi2WO6 nanosheets irradiated by γ-ray at different absorbed dose have been investigated using the decomposition of MB in aqueous solution under simulated visible light irradiation (λ
The cyclic photocatalytic activity of Bi2WO6 nanosheets irradiated at an absorbed dose of 507 kGy on the decomposition of MB is shown in FIG. 7. The catalytic performance of the recycled irradiated Bi2WO6 nanosheets seems to be little changed after three cycles, indicating a good stability of the oxygen vacancy defects existing in the irradiated Bi2WO6 nanosheets.
In this work, the effect of γ-ray radiation on the crystal structure of Bi2WO6 nanosheets was first studied. The color of Bi2WO6 nanosheets changed significantly after a high-dose γ-ray radiation up to 507 kGy. Although the morphologies of the irradiated Bi2WO6 nanosheets observed by SEM have no change, the XPS and XRD spectra confirm the generation of oxygen vacancy defects and the resulted shrinkage of the lattice spacing in the irradiated Bi2WO6 nanocrystals. The existence of oxygen vacancy defects lowered Eg and the peak intensity of photo-induced fluorescence, which favors to improve the photocatalytic activity of the irradiated Bi2WO6 nanosheets. The decomposition ratio of MB in aqueous solution at the presence of the Bi2WO6 nanosheets irradiated at an absorbed dose of 507 kGy can reach 99.2% under the exposure of visible-light for 150 min. The recycled irradiated Bi2WO6 nanosheets also can remain the excellent photocatalytic activity, indicating a good stability of the generated oxygen vacancy defects under γ-ray radiation. This work provides a new simple way to improve photocatalytic performance of Bi2WO6 through creating oxygen vacancy defects in the crystal structure by γ-ray radiation.
Supplementary materials: The photocatalytic performance of irradiated Bi2WO6 nanosheets with different absorbed doses and the working curve for the determination of MB concentration are given.
This work was supported by the National Natural Science Foundation of China (No.51473152, No.51573174, and No.51773189), Science Challenge Project (No.TZ2018004), and the Fundamental Research Funds for the Central Universities (WK3450000001 and WK3450000004).
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