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Separation and Purification Technology: Hong Liu, Zhitong Jin, Yun Su, Yong Wang
Separation and Purification Technology: Hong Liu, Zhitong Jin, Yun Su, Yong Wang
a r t i c l e i n f o a b s t r a c t
Article history: In this work, a novel Bi2Sn2O7/reduced graphene oxide (RGO) nanocomposite was synthesized by a one-
Received 27 August 2014 step hydrothermal method. The prepared composite was characterized by means of powder X-ray dif-
Received in revised form 26 December 2014 fraction (XRD), transmission electron microscopy (TEM), high resolution transmission electron micros-
Accepted 26 December 2014
copy (HRTEM), energy-dispersive X-ray spectrometry (EDS), Raman spectroscopy, X-ray photoelectron
Available online 8 January 2015
spectroscopy (XPS), UV–vis diffuse reflectance spectroscopy (DRS), photoluminescence (PL) emission
spectroscopy and electrochemical impedance spectroscopy (EIS). The photocatalytic activity of the Bi2-
Keywords:
Sn2O7/RGO composite was investigated by the degradation of rhodamine B (RhB) and phenol. An increase
Bi2Sn2O7
Graphene
in photocatalytic activity was observed for Bi2Sn2O7/RGO composite compared with pure Bi2Sn2O7 under
Photocatalysis visible light. The enhanced photocatalytic performance of the composite was mainly ascribed to the more
Visible light effective charge separations and the excellent adsorption capacity of RGO. The composite maintained its
Degradation ability to degrade pollutants efficiently, even after 4 cycles of photocatalysis. Further study proved that
both the holes and hydroxyl radicals were the active species in the degradation process.
Ó 2015 Elsevier B.V. All rights reserved.
http://dx.doi.org/10.1016/j.seppur.2014.12.027
1383-5866/Ó 2015 Elsevier B.V. All rights reserved.
26 H. Liu et al. / Separation and Purification Technology 142 (2015) 25–32
to high photocatalytic performance. However, to the best of our 2.3. Photocatalytic activity test
knowledge, there is no report on the design and fabrication of cou-
pled Bi2Sn2O7/graphene heterostructure so far. The photocatalytic activity of the as-prepared photocatalyst
In this paper, a novel Bi2Sn2O7/RGO composite has been synthe- was estimated by monitoring the degradation of RhB and phenol
sized by a one-step hydrothermal method for the first time. The pre- in an aqueous solution under visible light irradiation. The reaction
pared sample was characterized, and the photocatalytic activity was performed in a photochemical reactor (BL-GHX-V, Shanghai
under visible light irradiation (k > 420 nm) was evaluated by the Bilon Instruments Co., Ltd., China), equipped with a 500 W Xe lamp
degradation of RhB and phenol. The result revealed that the Bi2Sn2- combined with a 420 nm cut-off filter as a light source. All exper-
O7/RGO composite exhibited an enchenced photocatalytic activity iments were conducted at room temperature in air. In a typical
in comparison with bare Bi2Sn2O7. The obtained Bi2Sn2O7/RGO pho- photocatalytic experiment, 0.05 g of the photocatalyst was added
tocatalyst displayed good cycling stability under visible light. Fur- into 50 ml of 10 mg/L pollutant solution in a reaction cell with a
thermore, the mechanism of enhanced photocatalytic activity as Pyrex jacket. Prior to irradiation, the suspension was magnetically
well as the main active oxygen species in the photocatalytic reaction stirred in the dark for 1 h to reach an adsorption–desorption equi-
process was also investigated. librium. Then, the suspension was exposed to visible light irradia-
tion under magnetic stirring. At given time intervals, about 5 ml
suspensions were collected and centrifuged (12,000 rpm, 6 min)
2. Materials and methods to remove the photocatalyst particles. Then, the pollutant concen-
tration of the obtained solution was analyzed by a UV–vis spectro-
2.1. Preparation of Bi2Sn2O7/RGO composite photometer (Hitachi, U-3310) by checking the absorbance at
553 nm and 270 nm for RhB and phenol, respectively. To probe
All the chemicals were of analytical grade from the Sinopharm the oxidizing species in the photocatalytic process, the disodium
Chemical Reagent Co., Ltd. Graphene oxide (GO) was prepared by ethylenediamine tetraacetate (EDTA-2Na), tert-butyl alcohol (t-
a modified Hummers method [30]. The Bi2Sn2O7/RGO composite BuOH), or benzoquinone (BQ), was added in the solution. The con-
was prepared by a one-pot hydrothermal method. In a typical syn- centrations of the quenching chemicals were at 1 mM.
thesis, 0.73 g Bi(NO3)35H2O and 0.45 g K2SnO33H2O were added
into 50 mL of deionized water. Under vigorous stirring, the pH 3. Results and discussion
value of the mixture was adjusted to 12 by using NaOH solution.
Meanwhile, 0.1 g GO was dispersed in 20 mL ethanol by sonication 3.1. Structure and properties characterization
for 1 h to get a homogenous suspension of exfoliated graphene
oxide. Then, the obtained GO solution was added to the reacted- The XRD patterns of the pristine Bi2Sn2O7 and Bi2Sn2O7/RGO
mixture gradually. After stirring continuously for 2 h at room tem- composite are shown in Fig. 1. The XRD of Bi2Sn2O7 shows several
perature, the mixture was transferred into a Teflon-lined autoclave strong peaks at 2h = 28.8°, 33.4°, 47.9°, and 56.9°, which represent
with a volume of 100 mL. Then, the autoclave was sealed, heated the formation of a pure cubic phase of Bi2Sn2O7 (JCPDS No.
under autogenous pressure at 180 °C for 24 h, and then cooled 87-0284) [13,15]. It is found that the main diffraction peaks of
down to room temperature naturally. The resulting precipitate Bi2Sn2O7/RGO composite are similar to that of pristine Bi2Sn2O7,
was filtrated, washed thoroughly, and vacuum dried at 60 °C over- and no apparent peaks of RGO are observed in the Bi2Sn2O7/RGO
night. For comparison, pure Bi2Sn2O7 was prepared by using the composite, which might be due to the low amount of RGO
same method without the addition of GO. and relatively low diffraction intensity of RGO in the
composite. No apparent peaks of graphene oxide are observed in
the Bi2Sn2O7/RGO composite, indicating the successful reduction
2.2. Characterization
of GO to RGO through the hydrothermal process.
The morphologies of the pristine Bi2Sn2O7 and Bi2Sn2O7/RGO
The crystalline phases of prepared samples were identified by
composite were investigated by TEM as shown in Fig. 2. Fig. 2a
X-ray diffraction (XRD) on a D/MAX-2550 at 40 kV and 40 mA with
shows that pure Bi2Sn2O7 is comprised of many irregular nano-
Cu Ka radiation (k = 0.15418 nm). Structure and morphology of as
prepared samples were evaluated by TEM (200CX) and HRTEM
(JEM-2010F). Raman spectra were recorded on a microscopic con-
focal Raman spectrometer (Renishaw, INVIA) with an excitation of
514.5 nm laser light. UV–vis diffuse reflectance spectra (DRS) of the
samples were obtained on an UV–vis spectrophotometer (Hitachi
U-3010) using BaSO4 as a reference. The photoluminescence (PL) GO
spectra were measured using a Hitachi F-7000 fluorescence spec-
trophotometer at room temperature. Electrochemical impedance
Intensity (a. u.)
particles with diameters ranging from 5 to 15 nm. From Fig. 2b, it photoinduced charge separation rate during the photocatalytic pro-
can be clearly observed that the RGO sheets are decorated by cess [33]. In addition, the high-resolution spectra in Fig. 3d shows
irregular Bi2Sn2O7 nanoparticles, which confirmed the successful that the peak binding energies of 530.4 eV is assigned to O 1s [34].
attachment of Bi2Sn2O7 nanoparticles to RGO sheets. The HRTEM The XPS spectrum of C1s from GO (Fig. 3e) can be deconvoluted into
image shows the characteristic lattice fringes of Bi2Sn2O7 in the three smaller peaks, which are ascribed to the following functional
RGO nanosheets matrix (Fig. 2c). The lattice spacing is about groups: sp2 bonded carbon (CAC, 284.8 eV), epoxy/hydroxyls (CAO,
0.310 nm, which can be assigned to the (2 2 2) plane of cubic 286.8 eV), and carboxyl (OAC@O, 288.8 eV) [35], indicating the high
Bi2Sn2O7 [13]. Fig. 2c also reveals the intimate contact between percentage of oxygen-containing functional groups. In Fig. 3f,
Bi2Sn2O7 nanoparticles and RGO. This intimate contact is in although the three types of carbon species can still be seen in the
favour of the electronic interaction between Bi2Sn2O7 and Bi2Sn2O7/RGO composite, the XPS peaks corresponding to CAO
RGO and improves the charge separation and the photocatalytic and OAC@O are severely weakened in comparison to Fig. 3e, indi-
activity. The EDS spectrum of Bi2Sn2O7/RGO (Fig. 2d) exhibits cating that GO has been highly reduced during the hydrothermal
the presence of Bi, Sn, O and C elements. synthesis. Besides, no any peak corresponding to the BiAC bond
The X-ray photoelectron spectroscopy (XPS) was used to evalu- (at 281.2 eV in C 1s spectrum [36]) is observed, suggesting no car-
ate the surface elemental compositions of Bi2Sn2O7 and Bi2Sn2O7/ bon doping in the lattice of Bi2Sn2O7.
RGO. The survey XPS spectra (Fig. 3a) reveal that both Bi2Sn2O7 The Raman spectra of GO and Bi2Sn2O7/RGO are presented in
and Bi2Sn2O7/RGO are composed of Bi, Sn, O and C, which is in good Fig. 4. In Raman spectra, both samples exhibit two strong peaks,
agreement with the EDS results. The Bi 4f XPS spectra in Fig. 3b denoted as the disorder peak (D, centered at 1359 cm 1) and the
shows that the binding energies of Bi 4f7/2 and Bi 4f5/2 for Bi2Sn2O7 graphitic peak (G, at 1606 cm 1) [37,38]. Compared with GO,
occur at 158.8 and 164.2 eV, respectively, which are indicative of Bi2Sn2O7/RGO displays an increased D/G intensity ratio, indicating
Bi3+ in Bi2Sn2O7 [8,9,20]. The Sn 3d spectrum of Bi2Sn2O7 (Fig. 3c) the presence of localized sp3 defects within the sp2 carbon network
shows two peaks at 486.7 and 495.0 eV, indicating the presence of upon reduction of the exfoliated GO [39].
Sn4+ [31]. The peaks corresponding to Bi 4f and Sn 3d in the XPS The UV–vis diffuse reflectance spectra of the synthesized sam-
spectra of the as-prepared Bi2Sn2O7/RGO composite slightly shift ples are shown in Fig. 5a. Compared to pure Bi2Sn2O7, Bi2Sn2O7/
toward higher binding energies as compared to pure Bi2Sn2O7. This RGO composite shows an increased absorption in both UV and vis-
kind of shift in XPS measurement indicates that there is a strong ible range and an obvious red-shift in the absorption edge, which
interaction between Bi2Sn2O7 and RGO sheets in the nanohybrid can be attributed to the presence of carbon in the composites,
[32,33]. The intense interaction may result in the formation of elec- reducing reflection of light [22,40]. Similar phenomenon has been
tron transfer channel, which is beneficial to the improvement of noted in previous studies [3,9,20,27,40,41]. The band gap energy
(a) (b)
(c)
(d)
Cu
Itensity (a.u.)
C Bi
Sn
O Sn Cu Bi Bi
0 2 4 6 8 10 12 14
Energy (keV)
Fig. 2. TEM images of Bi2Sn2O7 (a) and Bi2Sn2O7/RGO (b), HRTEM image of Bi2Sn2O7/RGO (c) and EDS spectrum of Bi2Sn2O7/RGO (d).
28 H. Liu et al. / Separation and Purification Technology 142 (2015) 25–32
Sn 3d
(a) Survey (b) Bi 4f
Bi 4f7/2
Bi 4f
O 1s
Bi 4f5/2
Sn 3p
Sn 3p
Sn
Bi 4d
Sn 3s
Bi 4p
Bi 4d
O
C 1s
O 2s
Bi 5d
Bi2Sn2O7
Bi2Sn2O7
Bi2Sn2O7/RGO
Bi2Sn2O7/RGO
1000 800 600 400 200 0 168 166 164 162 160 158 156 154
Binding energy (eV) Binding energy (eV)
(c) Sn 3d (d) O 1s
Sn 3d5/2
Sn 3d3/2
Bi2Sn2O7
Bi2Sn2O
7
Bi2Sn2O7/RGO
Bi2Sn2O /RGO
7
500 498 496 494 492 490 488 486 484 482 540 538 536 534 532 530 528 526 524
Binding energy (eV) Binding energy (eV)
C-C
Intensity (a. u.)
C-C
O-C=O
O-C=O O-C
can be estimated by the following formula: a h m = A(h m–Eg)n/2, 3.2. Photocatalytic activity
where a, h, m, Eg, and A are the absorption coefficient, Planck con-
stant, the light frequency, the band gap, and a constant, respec- The photoactivity of the Bi2Sn2O7/RGO composite was evalu-
tively. And n is the electron transitions depending on the ated by photocatalytic degradation of RhB and phenol under visible
semiconductor characteristics (direct transition n = 1 and indirect light irradiation, and the results are shown in Fig. 6. It can be seen
transition n = 4). For Bi2Sn2O7, the value of n is 4 for the indirect that both RhB and phenol are very stable under visible light irradi-
transition [13]. Fig. 5b plots the relationship of (a h m)1/2 versus ation without the catalyst. Fig. 6a shows that the RhB removal rate
photon energy (h m), and shows that the bandgap energy of pure is about 95.8% after irradiation for 125 min in the presence of Bi2-
Bi2Sn2O7 is 2.48 eV, whereas this value is reduced to 1.85 eV by Sn2O7/RGO composite, while the value of pristine Bi2Sn2O7 is only
decorating with RGO. This phenomenon is possibly ascribed to 83.7%. Meanwhile, the degradation rate of phenol on Bi2Sn2O7/RGO
the interaction between Bi2Sn2O7 and RGO [3,20,22,29], which composite reaches 81.1% after irradiation for 200 min, whereas
has been evidenced by XPS analysis as described above. only 64.4% of phenol is removed by pristine Bi2Sn2O7 after same
H. Liu et al. / Separation and Purification Technology 142 (2015) 25–32 29
Table 1
Pseudo first-order rate constants of the photocatalytic decomposition of different
pollutants.
G Catalyst RhB Phenol
D
1
k (h ) R2 k (h 1
) R2
GO
Intensity (a. u.)
Bi2Sn2O7/RGO
concentration of pollutant is low [53]. The rate constants were
evaluated from the data plotted in Fig. 6a and b and summarized
ID/IG= 0.924 in Table 1. The rate constant for Bi2Sn2O7/RGO composite to
remove RhB is 1.54 h 1, which is 1.83 times as large as that of
pristine Bi2Sn2O7 (0.8382 h 1). This value for the composite is also
1.66 times larger than pristine Bi2Sn2O7 for the degradation of
phenol.
800 1200 1600 2000
In addition to photocatalytic activity, the stability of photocata-
Raman Shift (cm-1) lysts is another important issue for their practical applications. To
confirm the stability of the Bi2Sn2O7/RGO photocatalyst, the circu-
Fig. 4. Raman spectra of the Bi2Sn2O7/RGO composite and GO.
lating runs in the photocatalytic degradation of RhB and phenol in
the presence of Bi2Sn2O7/RGO under visible-light was checked. In
irradiation time (Fig. 6b). These results indicate clearly that the the work, Bi2Sn2O7/RGO was recycled for four times in the same
introduction of RGO can enhance the photocatalytic performance photocatalytic reactions. After each reuse cycle which lasted for
of Bi2Sn2O7. Notably, the photocatalytic activity of the obtained Bi2- 125 min (for degradation of RhB) or 200 min (for degradation of
Sn2O7/RGO composite on the degradation of organic pollutant RhB phenol), the photocatalyst was separated from the aqueous sus-
and phenol is higher than the Bi2Sn2O7-based materials reported pension by filtration, washed with deionized water and ethanol,
previously [42,43]. These photocatalytic properties are also better dried, and weighed for the next reuse cycle. It can be seen from
than various graphene-based composites [20,28,44–52]. For Fig. 7, after four recycles for the photodegradation of RhB and phe-
detailed analysis the photocatalysis kinetics of the pollutants deg- nol, the catalyst do not exhibit any significant loss of activity, indi-
radation, the pseudo-first order model was applied. This model is cating the good stability of the Bi2Sn2O7/RGO composite during
generally used for photocatalytic degradation process if the initial photocatalytic degradation of model pollutant.
(b) 3.0
(a) 1.6
2.5 Bi2Sn2O7/RGO
Adsorbance (a.u.)
1.2
2.0
(αhν)1/2
0.8 1.5
Bi2Sn2O7/RGO 1.0 Bi2Sn2O7
0.4 Bi2Sn2O7
0.5
0.0 0.0
200 300 400 500 600 700 800 1.5 2.0 2.5 3.0 3.5 4.0 4.5 5.0
Wavelength (nm) Photo energy (eV)
Fig. 5. (a) UV–vis spectra of Bi2Sn2O7 and Bi2Sn2O7/RGO composite and (b) plots of the (a h m)1/2 versus photon energy (h m) for as-synthesized samples.
C/C0
blank
0.4
0.4
0.2
0.2
0.0
0 25 50 75 100 125 0 40 80 120 160 200
Time (min) Time (min)
Fig. 6. Photocatalytic activities of as-prepared samples on the degradation of RhB (a) and phenol (b) under visible-light irradiation.
30 H. Liu et al. / Separation and Purification Technology 142 (2015) 25–32
0.92
0.4
C/C0
0.2 0.88
0.0
0 125 125 125 125
0.84
Time (min)
0 10 20 30 40 50 60
(b) 1.0
1 st run 2 nd run 3 rd run 4 th run Time (min)
0.8 Fig. 9. Absorption activities of Bi2Sn2O7 and Bi2Sn2O7/RGO.
0.6
C/C0
50
(a) (b)
Relative intensity (a. u.)
40 Bi2Sn2O7
Bi2Sn2O7/RGO
-Z''(ohm)
Bi2Sn2O7
30
20
Bi2Sn2O7/RGO 10
0
380 400 420 440 460 480 500 520 540 560 580 10 15 20 25 30 35 40 45 50
Wavelength (nm) Z'(ohm)
Fig. 8. (a) PL spectra and (b) Nyquist impedance plots of Bi2Sn2O7 and Bi2Sn2O7/RGO composite.
H. Liu et al. / Separation and Purification Technology 142 (2015) 25–32 31
C/C0
C/C0
+ BQ
0.4 0.4
Bi2Sn2O7/RGO
+ EDTA-2Na
0.2 0.2
+ t-BuOH
+ BQ
0.0 0.0
0 25 50 75 100 125 0 40 80 120 160 200
Time (min) Time (min)
Fig. 10. Photocatalytic degradation of RhB (a) and phenol (b) with the addition of hole and radical scavenger.
4. Conclusion
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