New Type Photocatalyst PbBiO2Cl: Materials Design and

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New Type Photocatalyst PbBiOCl: Materials Design and Experimental Validation Yanlong Yu, Yao Gu, Wenjun Zheng, Yihong Ding, and Yaan Cao J. Phys. Chem. C, Just Accepted Manuscript • DOI: 10.1021/acs.jpcc.5b09281 • Publication Date (Web): 17 Nov 2015 Downloaded from http://pubs.acs.org on November 28, 2015

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The Journal of Physical Chemistry

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New Type Photocatalyst PbBiO2Cl: Materials Design and Experimental Validation Yanlong Yu, a, b Yao Gu, a Wenjun Zheng, c Yihong Ding, d and Yaan Cao a* a

MOE Key Laboratory of Weak-Light Nonlinear Photonics, TEDA Applied Physics Institute

and School of Physics, Nankai University, Tianjin 300457, China. Tel: 86 22 66229419; E-mail: [email protected]. b

College of Materials Science & Engineering, Liaoning Technical University, Fuxin 123000,

China c

Department of Materials Chemistry, College of Chemistry, Nankai University, Tianjin, 300457,

China d

State Key Lab of Theoretical and Computational Chemistry, Jilin University, Changchun

120023, China

ACS Paragon Plus Environment


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Page 2 ABSTRACT: A new kind of nanostructured photocatalyst, PbBiO2Cl is synthesized by a simple hydrothermal method. The proposed formation mechanism of PbBiO2Cl is carried out by the analyzing the XRD patterns and SEM images of the products prepared under different conditions. The PbBiO2Cl nanostructure behaves as a truncated bipyramid, exposed with {002} and {103} facets. Moreover, theoretical calculation and absorption spectrum indicate the PbBiO2Cl shows strong absorption in visible region with a band gap of 2.53 eV. The obtained PbBiO2Cl nanostructures exhibit significantly enhanced photocatalytic activity on degradation of methyl orange (MO) and 4-chlorophonel (4-CP). This work may offer a paradigm on designing and synthesizing visible photocatalyst exposed with reactive facets, which can be applied in many fields.


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Page 3 INTRODUCTION Bismuth oxyhalides, especially BiOCl, has attracted lots of attention as one of most promising photocatalyst and exhibit significantly enhanced photocatalytic on degradation of organic pollutant1-11. It is noted that BiOCl is characterized as tetragonal crystal structure and consists of layered structure with [Bi2O2] slabs interleaved by double slabs of Cl atoms along the c-axis. Owing to the unique crystallite structure, the Bi-based photocatalyst usually behaves as nanosheet or nanoplate structure with exposed {001} facets and exhibit much better photocatalytic activity than TiO2 (P25) under UV light irradiation.5-10 However, the large band gap of BiOCl (3.4 eV) still limits the practical application, especially under solar light irradiation. PbBiO2Cl, a Bi-based oxychloride semiconductor with a narrow band gap of 2.45 eV, has been considered as a novel photocatalyst in recent years.12-13 Shan and his co-workers synthesized the RuO2 loaded PbBiO2Cl by solid state chemistry with enhanced photocatalytic activity.12 Füldner et al. used PbBiO2Cl as an efficient photocatalyst with selective reduction of nitrobenzene derivatives.13 However, these PbBiO2Cl products prepared by the solid state chemistry usually exhibit uncontrolled morphology, large particle size and require high reaction temperature as 800 °C or much time as long as several days. Moreover, the formation mechanism of the PbBiO2Cl is still unclear, which needs further investigation. Herein, we report a simple synthesis of PbBiO2Cl nanostructure by hydrothermal reaction without the use of any template or organic surfactant. The single crystalline PbBiO2Cl behaves as a truncated bipyramid nanostructure and exhibits significantly enhanced activity on degradation of organic pollutant under visible light irradiation. The formation mechanism and the band structure of PbBiO2Cl are also investigated in details.



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Page 4 MATERIALS AND METHODS Sample Preparation. The PbBiO2Cl nanostructure is prepared by a simple hydrothermal method. 1.577 g of BiCl3 was added into the mixture of 50 mL of deionized water and 2 mL of sodium hydroxide (10 mol/L) under vigorous stirring. After 30 minutes, 1.906 g of lead acetate was added. The mixture was stirred for another 30 minutes and then transferred into a 100 mL Teflon-lined stainless autoclave. The autoclave was heated at 160 °C in an oven for 20 hours and cooled down to the room temperature in the air. These obtained yellow participates are washed with deionized water for six times and dried at 60 °C. To investigate the formation mechanism of PbBiO2Cl, the PbBiO2Cl nanostructures were synthesized under different temperatures and pH values. Calculation. Theoretical calculation was carried out by a first-principle calculation software package CASTEP. Generalized gradient approximation (GGA) basede density functional theory (DFT) is applied to calculate the electric band structure and density of states (DOS) for PbBiO2Cl. The plane wave energy cutoffs are taken to be 380 eV and the k-point set is 2×2×2. The valence electronic configurations for Pb, Bi, O and Cl atoms are 5d10 6s2 6p2, 6s2 6p3, 2s2 2p4 and 3s2 3p5, respectively. Characterization. X-ray diffraction (XRD) patterns were acquired on a Rigaku D/max 2500 X-ray diffraction spectrometer (Cu Kα, λ=1.54056 Å). High-resolution transmission electron microscopy (HRTEM) images were obtained by a JEOL 3010, for which the samples were prepared by applying a drop of ethanol suspension onto an amorphous carbon-coated copper grid and dried naturally. The scanning electron microscopy images (SEM) were taken on a LEO 1530vp SEM. Diffuse reﬂectance UV–visible absorption spectra were collected on a UV–visible spectrometer (UV-1061PC, Shimadzu). All measurements were carried out at room temperature.


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Page 5 Evaluation of Photocatalytic Activity. The photocatalytic degradation of 4-chlorophenol (4-CP) was carried out in a 70 mL glass reactor with 10 mg amounts of catalysts suspended in 4chlorophenol solution (5 × 10−5 mol L−1 , 40 mL, pH =5.38). A sunlamp (Philips HPA 400/30S, Belgium) was used as the light source. The reactor was perpendicular to the light beam and located 15 cm away from the light source and a 420 nm cutoff filter is applied to remove the UV light. The 4-chlorophenol solution was continuously bubbled by O2 gas at a flux of 5 mL min −1 under magnetic stirring at 25 ± 2 °C. Before irradiation, the suspensions were stirred at room temperature in the dark for half an hour. The residual concentration of 4-chlorophenol was measured by a UV−visible spectrometer (UV-1061PC, SHIMADZU) by using 4aminoantipyrine as the chromogenic reagent.

RESULTS AND DISCUSSION In a typical synthesis, 5 mmol bismuth chloride (BiCl3) and 6 mmol lead acetate (Pb(CH3COO)2) was added into 50 mL 0.1M sodium hydroxide solution (NaOH). Then the mixture was hydrothermally heated at 160 °C in a 100 mL Teflon-lined stainless autoclave for 20 h. After washed with deionized water for several times and dried at 60 °C, the PbBiO2Cl nanostructure was obtained. For comparison, PbBiO2Cl particles were also prepared by solid states chemistry annealed at 800 °C. Figure 1a shows the XRD patterns of PbBiO2Cl particles and nanostructures, which is in good agreement with the diffraction peaks of PbBiO2Cl (JCPDS No. 39-0802). Moreover, two small diffraction peaks at about 11.8° and 25.9° are also found in Figure 1a, indicating existence of BiOCl. Furthermore, as shown in Figure 1b and inset of Figure 1b, the morphology of the PbBiO2Cl with an average diameter about 100-200 nm behaves as a truncated octahedral with well-defined facets. Some plate-like nanostructures are also observed in Figure



(206) (220)

(211) (116) (213)

(004)

(002)

(006) (200) (202)

(101)

a

(103) (110)

Page 6

Intensity(a.u.)

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PbBiO2Cl nanostructure PbBiO2Cl

10

20

30

40

2θ/

o

50

60

70

80

Figure 1. (a) XRD pattern, (b, d) TEM and (c, e) HR-TEM images of PbBiO2Cl nanostructures. The scale bar is 20 nm for TEM images. Inset of (e) shows the corresponding FFT of PbBiO2Cl.


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Page 7 1b, ascribed to BiOCl nanoplates. Figure 1c shows the side view of the HR-TEM image. The lattice fringe spacing is found to be about 0.63 nm (Figure 1c), corresponding to the (002) d spacing of PbBiO2Cl. This suggests the bottom and top surface side of the truncated octahedral are (002) planes of PbBiO2Cl. Moreover, it is found from Figure 1d that the PbBiO2Cl truncated bipyramid nanostructure is exposed with {002} and {103} facets. Furthermore, the fringe spacing shown in Figure 1e is determined to be 0.28 nm, corresponding to the (110) plane of PbBiO2Cl. The fast Fourier transform spectra (FFT; Inset of Figure 1e) also reveal the single crystal nature of PbBiO2Cl truncated octahedral bipyramid nanostructure. In addition, it is found that the PbBiO2Cl truncated bipyramid is composed of several PbBiO2Cl nanosheet layers stacked along the [001] direction. To investigate the formation mechanism of PbBiO2Cl, a series of PbBiO2Cl samples were prepared under different pH values and hydrothermal temperatures (Figure S2 and S3). Before the hydrothermal reaction, the BiOCl microspheres (Figure S4) are the only product and no PbBiO2Cl is detected. It is found that the increased pH value and hydrothermal temperature is in favor of the formation of PbBiO2Cl nanostructure. According to the synthesis procedures and obtained samples under different conditions, the possible formation mechanism of PbBiO2Cl can be summarized as two steps: Bi3+ + Cl- + 2 OH- =BiOCl↓ + H2O

(1)

Pb2+ + BiOCl + 2 OH- = PbBiO2Cl + H2O

(2)

At the beginning of the reaction, the pH value during the synthesis reaction is found to be at 3.07. The Bi3+ ions react with the Cl- and hydroxyl ions to form BiOCl immediately (BiOCl, Ksp=1.8 ×10-31)14. At the same time, the Pb2+ ions react with Cl- ions to form PbCl2 (PbCl2, Ksp=1.6×105 15

) which can be dissolved in the hot water, instead of Pb(OH)2 (Pb(OH)2, Ksp=1.43×10-15 )16.



Page 8 It is noted that BiOCl is a tetragonal PbFCl- type structure with a space group of P4/nmm and the lattice constants are a=b=3.890 Å , c=7.370 Å , α=β=γ=90 °.8 According to the crystal structure, BiOCl has a layered structure characterized by [Bi2O2] slabs interleaved by double slabs of Cl atoms along the c-axis.8 During the process of reaction, the Pb2+ ions is preferred to be adsorbed on the surface of BiOCl or weaved into the Cl atom layers, owing to the interaction between Pb and Cl. After the hydrothermal reaction, the Pb2+ ions would react with the BiOCl layers to from PbBiO2Cl layers. In addition, according to the minimum energy principle, the PbBiO2Cl layers would stack with each other form the truncated bipyramid nanostructure. That explains why both the BiOCl layers and PbBiO2Cl truncated bipyramid nanostructure are found in the TEM images.

Intensity(a.u.)

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PbBiO2Cl BiOCl

300

400

500

600

700

Wavelength(nm)

Figure 2. Diffuse Reflectance Absorption spectra of BiOCl and PbBiO2Cl. Diffuse reflectance absorption spectra of BiOCl and PbBiO2Cl nanostructures are plotted in Figure 2. Pure BiOCl exhibits a strong absorption in ultra-violet region, which is attributed to the band to band transition. The absorption edge is at 367 nm, hence the band gap is estimated to be 3.38 eV for BiOCl. In comparison with BiOCl, the PbBiO2Cl exhibit a strong absorption in visible region from 600 nm to 400 nm. The absorption edge is estimated to be 490 nm, corresponding to a band gap of 2.53 eV for PbBiO2Cl, which is close to the theory result, 1.985


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Page 9 eV. The strong absorption in visible region for photocatalyst usually implies an enhanced photocatalytic activity, as electrons and holes can be easily excited by the visible irradiation.

1.0 0.9

C/C0

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0.8 0.7

TiO2 N-TiO2

0.6

C3N4 PbBiO2Cl

0.5

0

120

240

360

480

Time(min)

Figure 3. Photocatalytic degradation of 4-CP for TiO2, N-TiO2, C3N4 and PbBiO2Cl under visible light irradiation (λ >420 nm). The photodegradation of 4-chlorophenol (4-CP) under visible irradiation (λ >420 nm) is applied to evaluate the photocatalytic performance of the PbBiO2Cl truncated octahedral bipyramid. A sunlamp (Philips HPA 400/30S, Belgium, λ ≥ 300 nm) was used as light source and a 420 nm cutoff filter is applied to remove the UV light. As shown in Figure 3, 4-CP can hardly be decomposed in the presence of pure TiO2. Nitrogen modified TiO2 (N-TiO2) and C3N4 exhibits limited photocatalytic activity. The PbBiO2Cl nanostructure exhibits a much better photocatalytic activity than pure C3N4 and self-made nitrogen doped TiO2(N-TiO2) samples17-18. About 45% of 4-CP is degraded for PbBiO2Cl, whose specific photocatalytic activity is about 5 times as that for N-TiO2 (8.7%). These results indicate that PbBiO2Cl truncated octahedral bipyramid is quite an effective photocatalyst with strong redox ability on degradation of organic pollutant.



Page 10 In addition, to remove the influence of BiOCl in the obtained products, a series of BiOCl/PbBiO2Cl composite samples are synthesized with the same procedure (Figure S1). It is found that the photocatalytic activity of the samples increases with the increase of the Pb content (Figure S5), indicating only PbBiO2Cl is responsible for the photocatalytic performance on degradation of organic pollutant under visible light irradiation. (A)

6

DOS(electrons/eV)

2

Eg= 2.018 eV

0 -2 -4 G Z

T Y

S

(B)

30

4 Energy(eV)

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X U

R

SUM O 2p Cl 2p Bi 6s Bi 6p Pb 6s Pb 6p

15

0

-4

-2

0 2 Energy(eV)

4

6

Figure 4. (a) Band structure (b) projected density of states for the PbBiO2Cl. For insight into the photocatalytic activity of PbBiO2Cl, the electric band structure and density of states are carried out by the DFT calculation. The top of valence band and bottom of the conduction band is located at G and S point, respectively (Figure 4a), indicating an indirect transition band gap for PbBiO2Cl. The band gap is calculated to be 2.018 eV, which is smaller than experiment result, 2.53 eV. The projected density of states for PbBiO2Cl is plotted in Figure 4b. The highly dispersive valence band and conduction band could also benefit for the transport of photogenerated electrons and holes by suppressing the recombination of photogenerated charge carriers, in favor of the photocatalytic activity. It is revealed that the top of the valence band is primarily dominated by O 2p and Cl 3p states, hybridized by Pb 6s, Pb 6p, Bi 6s and Bi 6p states. The bottom of conduction band is mainly composed of Pb 6p and Bi 6p states, as well as a small fraction of Pb 6s, Bi 6s, O 2p and Cl 3p states. It is found that PbO is a deep yellow


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Page 11 semiconductor with a narrow band gap. In this work, it seems like PbBiO2Cl combine the advantage of BiOCl and PbO, resulting in the enhanced photocatalytic activity under visible irradiation, compared with C3N4 and N-TiO2. Moreover, compared with PbBiO2Cl nanoparticles, the PbBiO2Cl truncated bipyramid exhibits remarkable enhanced photocatalytic activity (Figure S7), which can be attributed to the highly reactive surface structure, such as {103} and {200} facets. The high active photocatalytic activity of the surface facets may arise from their higher surface energy or superior hydrophilic ability. However, the detailed study about {103} and {200} facets still needs further investigation.

CONCLUSIONS In summary, PbBiO2Cl truncated octahedral bipyramid exposed with {002} and {103} facets is synthesized by a simple hydrothermal method. The PbBiO2Cl truncated octahedral consists of nanosheet stacked along the [001] direction. The PbBiO2Cl represents an indirect band gap of 2.53 eV and shows strong absorption in visible region. The nanostructure exhibits enhanced photocatalytic performance in comparison with C3N4 and N-TiO2 on degradation of organic pollutants. This work may offer a better understanding about the opti-electrical functional materials by controlling the nanostructure and adjusting the band structure.

ACKNOWLEDGEMENTS This work was supported by the National Natural Science Foundation of China (Nos 21173121 and 51372120).



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Page 12 Supporting information: XRD patterns, SEM images, DRS absorption spectra and photocatalytic activity of the PbBiO2Cl samples. This material is available free of charge via the Internet at http://pubs.acs.org.

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TOC IMAGE

The single crystalline PbBiO2Cl behaves as a truncated bipyramid nanostructure and exhibits significantly enhanced activity on degradation of organic pollutant under visible light irradiation.


New Type Photocatalyst PbBiO2Cl: Materials Design and

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