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Page 1 of 23 Environmental Science: Nano
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DOI: 10.1039/C6EN00597G
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3 The utilization of nanostructured photocatalysts is an efficient and cost effective
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5 approach for photocatalytic degradation of pollutants in water. Over the past years, SrTiO3 has
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Environmental Science: Nano Accepted Manuscript

7 been studied for the photocatalytic degradation of organic pollutants. But it only responds to
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9 ultraviolet light region and the inefficient use of visible light has restricted its practical
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11 application. So, modification is necessary to improve the potocatalytic performance of SrTiO3.
Published on 04 January 2017. Downloaded by Freie Universitaet Berlin on 10/01/2017 06:55:19.
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13 Here, SrTiO3 nanocubes decorated with Ag/AgCl nanoparticles were composed at ambient
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15 temperature by the method of the ultrasonic assisted precipitation-photoreduction reaction.
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17 The nano-photocatalysts exhibited excellent photocatalytic performance for the degradation
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of dyes, phenol and BPA. Besides, the composite photocatalysts with good stability could be
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20 fulfilled the demand for consecutive utilization of photocatalytic materials.
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Environmental Science: Nano Page 2 of 23
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3 1 SrTiO3 nanocubes decorated with Ag/AgCl nanoparticles as photocatalysts with
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5 2 enhanced visible-light photocatalytic activity towards the degradation of dyes, phenol
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7 3 and bisphenol A
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9 4 Shi-Feng Yanga, Cheng-Gang Niua,*, Da-Wei Huangb, Huan Zhanga, Chao Lianga,
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11 5 Guang-Ming Zenga, *
12 a
13 6 College of Environmental Science Engineering, Key Laboratory of Environmental Biology
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15 7 Pollution Control, Ministry of Education, Hunan University, Changsha 410082, China.
16 b
17 8 South China Institute of Environmental Sciences, Ministry of Environmental Protection of
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9 PRC, Guangzhou 510655, China.
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20 10 *Corresponding Author
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22 11 Cheng-Gang Niu, E-mail: cgniu@hnu.edu.cn; cgniu@hotmail.com; Tel: +86-731-88823820;
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24 12 Guang-Ming Zeng, E-mail: zgming@hnu.edu.cn
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26 13 Abstract
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28 14 Visible-light-sensitive photocatalysts Ag/AgCl/SrTiO3 have been successfully assembled
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30 15 through the precipitation reaction between AgNO3 and NaCl at ambient temperature, wherein
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32 16 Ag/AgCl nanoparticles were immobilized on the surface of SrTiO3. The composition,
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17 crystallinity, morphologies and optical properties of the as-perpared photocatalysts were
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18 sufficiently studied via various characterization techniques. In this paper, rhodamine B (RhB),
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37 19 methyl orange (MO), methylene blue (MB), phenol and bisphenol A (BPA) solution were
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39 20 photodegraded as target pollutants under visible light irradiation to evaluate the photocatalytic
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41 21 performances of the obtained products. By contrast with the pristine SrTiO3 and Ag/AgCl
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43 22 nanoparticles, the composite photocatalysts presented dramatically boosted visible-light
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45 23 photocatalytic performance in the matter of decomposing organic pollutants. It was observed
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47 24 that the Ag/AgCl/SrTiO3 (21.6%) composite possessed the best photocatalytic performance
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49 25 and kept favorable stability during consecutive cycling experiment. The improved
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26 photocatalytic performance of the catalysts resulted from the surface plasmon resonance
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52 27 effect of Ag/AgCl nanoparticles, as well as supernal separation efficiency of photogenerated
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54 28 electrons and holes. Meanwhile, a reasonable reaction mechanism on the composite
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56 29 photocatalysts of Ag/AgCl/SrTiO3 (21.6%) was brought up upon band energy analysis and
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58 30 trapping experiment.
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3 31 1. Introduction
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5 32 Semiconductor photocatalysts are a class of green materials and have been greatly
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7 33 investigated in the past few decades on account of their potential application in the renewable
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9 34 energy and environment fields . In photocatalysis technology, semiconductor materials are
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11 35 excited by light absorption to produce electron-hole pairs which are then separated and
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13 36 transferred to target object for redox reactions . Among them, strontium titanate (SrTiO3)
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15 37 has been widely known as an important perovskite semiconductor with photocatalytic activity.
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17 38 It draws extensive concern because of its anti-photochemical corrosion property, thermal
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39 stability, well heat resistance, corrosion resistance, and so on 9-13. However, SrTiO3 has a wide
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20 40 band gap of 3.2-3.4 eV and only responds to ultraviolet light region which occupies about 3-5%
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22 41 of the solar radiation spectrum 14, 15
. The inefficient use of visible light has restricted its
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24 42 practical application. So, modification is necessary to improve the potocatalytic performance
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26 43 of SrTiO3. In the previous literatures, the band gap of SrTiO3 could be narrowed via methods
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28 44 of fabricating heterojunction structure 16, ion doping 17, coupling plasmonic nanostructures 18,
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30 45 surface reconstruction 19, and etc. These surface modification methods of SrTiO3 have boosted
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32 46 the photocatalytic performance to a certain degree. But the enhancement is not obvious
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47 enough, so it is exigent to develop original visible-light-sensitive materials for making best of
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48 the solar energy.
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37 49 As demonstrated in previous literatures, integrating with the strategy of surface plasmon
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39 50 resonance (SPR) is broadly utilized to fabricate efficient visible-light-driven photocatalysts 20,
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41 51 . Due to the SPR structure, noble-metal nanopaiticles (NPs) have widened the absorption in
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43 52 the visible-light region and enhanced the performance of photocatalysts in the field of organic
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45 53 pollutants degradation 22. Among multifarious plasmonic photocatalytic systems, Ag/AgX (X
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47 54 = Cl, Br, I) have been widely concerned as a type of dopant to modify other photocatalysts. In
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49 55 the system, metallic Ag NPs can absorb visible light efficiently, and the highly dispersed AgX
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56 are able to expedite the decentralization of photocarriers . So far, a number of
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52 57 Ag/AgX-based plasmonic photocatalysts have been successfully composed, for instance,
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54 58 Ag/AgCl/BiVO4 24
, Ag/AgBr/TNF 25
, Ag/AgI/Bi2MoO6 26
, and so on. These hybrid
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56 59 photocatalysts showed superior photocatalytic performances. Therefore, incorporating with
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58 60 Ag and its halides is a useful means to form efficient visible-light-sensitive photocatalysts 27.
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3 61 Through the above analysis, the combination of SrTiO3 nanocubes and Ag/AgCl NPs which
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5 62 has not been reported stands a good chance of not only improving the utilization rate of solar
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7 63 energy but also enhancing the photocatalytic ability.
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9 64 Inspired by these work, a series of Ag/AgCl/SrTiO3 composites were composed at
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11 65 ambient temperature by the method of the ultrasonic assisted precipitation-photoreduction
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13 66 reaction. Herein, SrTiO3 was utilized as an applicable support to synthesize the hybrid
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15 67 composites. The photocatalytic performances of all obtained catalysts were assessed by the
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17 68 degradation of target pollutants under visible light irradiation. Results indicated that the
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69 photocatalytic performances of Ag/AgCl/SrTiO3 catalysts were superior for degrading target
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20 70 pollutants under visible light irradiation, which was much higher than those of pure SrTiO3
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22 71 and Ag/AgCl NPs. Besides, the reasonable mechanism for the enhanced photocatalytic
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24 72 performances of Ag/AgCl/SrTiO3 composites was also discussed detailedly in view of
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26 73 systematic experiments and analysis.
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28 74 2. Experimental
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30 75 2.1. Materials
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32 76 Potassium hydroxide (KOH), titanium sulfate (Ti(SO4)2), strontium nitrate (Sr(NO3)2),
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77 silver nitrate (AgNO3) and sodium chloride (NaCl) were purchased from Sinopharm
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78 Chemical Reagent Co., Ltd. Rhodamine B (RhB), methyl orange (MO), methylene blue (MB),
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37 79 phenol and bisphenol A (BPA) solution were adopted as target contaminants to assess the
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39 80 photocatalytic activities of the obtained catalysts. All reagents were analytical grade and
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41 81 utilized as received without further treatment. Deionized water was utilized as solvent in
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43 82 whole experimental process.
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45 83 2.2. Preparation of SrTiO3
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47 84 The SrTiO3 was synthesized through sonochemistry at ambient temperature . In a
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49 85 typical process, about 5 mmol of Ti(SO4)2 and 20 mmol of KOH were separately dissolved in
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86 50 mL of deionized water. Next, the KOH solution was added into the Ti(SO4)2 solution,
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52 87 followed by filtration. The formative white precipitate was rinsed three times with deionized
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54 88 water so that the adsorbed SO42– and K+ ions were removed completely. Then the above white
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56 89 precipitate along with 100 mmol of KOH was added into 50 mL of deionized water.
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58 90 Afterwards, the acquired suspension was added into the Sr(NO3)2 solution (50 mL, 0.10 mol
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3 91 L-1), followed by ultrasonication for 2 h. The products were collected through filtration,
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5 92 rinsing several times with deionized water, and drying at 60 ℃ for 8 h.
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7 93 2.3. Preparation of Ag/AgCl/SrTiO3 composites
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9 94 The Ag/AgCl/SrTiO3 composites were fabricated via the facile ultrasonic assisted
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11 95 precipitation-photoreduction means at ambient temperature. In a typical synthesis procedure,
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13 96 0.30 g of the acquired SrTiO3 suspended in deionized water (100 mL), and the resulting
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15 97 mixture was ultrasonicated for 20 min. Next 6.0 mL of 0.10 mol L–1 AgNO3 solution was
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17 98 added dropwise to the suspension under mechanical stirring. After stirring for a few minutes,
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99 the mixture was ultrasonicated for another 20 min. Then an overmuch amount of 0.10 mol L–1
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20 100 NaCl solution was dripped slowly to the above mixture. After stirring in darkness for 2 h, the
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22 101 resulting mixture was illuminated under a 300 W xenon lamp equipped with a UV cutoff filter
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24 102 (λ > 420 nm) for 30 min so that the particles Ag+ on the surface of AgCl/SrTiO3 were reduced
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26 103 to Ag0 NPs. The precipitate was filtered, rinsed with deionized water for several times to
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28 104 remove remanent ions and dried at 60 ℃ for 8 h. The final powder, in which the mass ratio
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30 105 of Ag to SrTiO3 was 21.6%, was denoted to be Ag/AgCl/SrTiO3 (21.6%). Samples
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32 106 Ag/AgCl/SrTiO3 (14.4%), Ag/AgCl/SrTiO3 (18.0%), and Ag/AgCl/SrTiO3 (25.2%) were
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107 fabricated homoplastically by altering the amount of AgNO3 to 4.0, 5.0, and 7.0 mL,
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108 respectively.
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37 109 2.4. Structure characterization
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39 110 X-ray diffraction (XRD) patterns were obtained on a Bruker D8-advance X-ray
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41 111 diffractometer with Cu Ka radiation (λ = 0.15406 nm) to investigate the crystalline phases of
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43 112 SrTiO3, Ag/AgCl, Ag/AgCl/SrTiO3 (21.6%) and the used Ag/AgCl/SrTiO3 (21.6%) samples.
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45 113 The morphologies of the fabricated photocatalysts were observed using a FESEM-4800 field
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47 114 emission scanning electron microscope (SEM, Hitachi) with 5.0 kV scanning voltages.
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49 115 Transmission electron microscopy (TEM) and high resolution TEM (HRTEM) images were
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116 obtained to elaborately analyze the microstructure of the Ag/AgCl/SrTiO3 (21.6%) sample
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52 117 using a transmission electron microscope (TEM, FEI Tecnai G20) with an accelerating
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54 118 voltage of 200 kV. The UV–vis diffuse reflectance spectra (DRS), which could reflect the
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56 119 optical properties of the samples, were recorded on a UV-vis spectrophotometer (Hitachi
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58 120 U-4100) in a wavelength range from 200 to 800 nm with BaSO4 as a reflectance sample. The
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3 121 X-ray photoelectron spectroscopy (XPS) spectra were performed on a Thermo ESCALAB
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5 122 250XI spectrometer with a focused monochromatized Al Ka radiation. Fourier transform
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7 123 infrared spectrometer (FTIR) spectra were collected on an IR Prestige-21 spectrometer
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9 124 (Shimadzu, Japan) at the room temperature by the standard KBr disk method. The
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11 125 photoluminescence (PL) spectra were acquired using a PerkinElmer LS-55 fluorescence
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13 126 spectrophotometer.
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15 127 2.5. Photocatalytic experiments
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17 128 Rhodamine B (RhB, 554 nm), methyl orange (MO, 464 nm), methylene blue (MB, 664
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129 nm), phenol (270 nm) and bisphenol A (BPA, 277 nm) were utilized as target contaminants to
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20 130 assess the photocatalytic activities. A 300 W Xe lamp equipped with a UV cutoff filter (λ >
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22 131 420 nm) was utilized as the light source. Briefly, 0.050 g photocatalysts suspended in target
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24 132 pollutants (100 mL, 10 mg L-1). Prior to irradiation, the suspension was magnetically stirred
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26 133 in the dark for 30 min to attain adsorption-desorption equilibrium. During visible light
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28 134 irradiation, 4 mL of the sample suspensions were taken out at certain time intervals and
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30 135 separated through centrifugation (8000 rpm, 5 min) to remove the residual particles. The
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32 136 supernatant was analyzed by recording variations of target pollutants at the characteristic
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137 absorption peak on a UV-vis spectrophotometer (Shimadzu 2550, Japan) with deionized water
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138 as the standard sample. Furthermore, the cycle experiments were performed under the same
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37 139 conditions to examine the stability and repeatability of the photocatalysts.
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39 140 3. Results and discussion
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41 141 3.1. Characterization
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43 142 3.1.1 XRD analysis
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45 143 The XRD patterns in Fig. 1 were applied to reveal the composition and crystallinity of
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47 144 the pure SrTiO3, Ag/AgCl and Ag/AgCl/SrTiO3 (21.6%) composite. Fig. 1a showed that all
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49 145 diffraction peaks of the pristine SrTiO3 (marked with “♣”) were in line with the perovskite
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146 SrTiO3 phase (JCPDS 35-0734). These significant intensity of peaks manifested that the pure
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52 147 SrTiO3 with good crystallinity had been successfully fabricated. For the Ag/AgCl sample (Fig.
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54 148 1b), the XRD pattern exhibited two kinds of diffraction peaks. Several peaks (marked with
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56 149 “♥”) were in accordance with the standard diffraction data of Ag (JCPDS 04-0783), and all
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58 150 another peaks (marked with “♦”) were well matched to the AgCl (JCPDS 31-1238). For the
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3 151 Ag/AgCl/SrTiO3 (21.6%) composite (Fig. 1c), the XRD pattern exhibited three kinds of
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5 152 diffraction peaks. The diffraction peaks were at 2θ = 27.83°, 54.83°, 74.47°, which were
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7 153 matched with (111), (311), (331) facets of AgCl (JCPDS 31-1238), respectively. Moreover,
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9 154 another two weak peaks at 2θ = 38.11°, 44.28° corresponded to (111), (200) facets of Ag
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11 155 (JCPDS 04-0783), respectively. Both of the two weak peaks were made via photoreducing
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13 156 AgCl/SrTiO3 under visible light irradiation. Besides, all characteristic diffraction peaks of
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15 157 SrTiO3 in the Ag/AgCl/SrTiO3 (21.6%) composite were quite same as those of the pristine
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17 158 SrTiO3. In addition, no other impurity phases were detected, indicating that the
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159 Ag/AgCl/SrTiO3 (21.6%) photocatalysts were three-phase hybrid. Thus, it was concluded that
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20 160 Ag/AgCl NPs should be simply anchored on the surface of the SrTiO3 rather than covalently
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22 161 embed in the crystal lattice of the SrTiO3.
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44 162
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163 Fig. 1 XRD patterns of (a) SrTiO3, (b) Ag/AgCl, (c) Ag/AgCl/SrTiO3 (21.6%), (d) used
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47 164 Ag/AgCl/SrTiO3 (21.6%) after five cycling runs.
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49 165 3.1.2 SEM analysis
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51 166 The specific morphologies of the pristine SrTiO3, also Ag/AgCl/SrTiO3 (21.6%)
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53 167 photocatalysts were revealed using SEM and illustrated in Fig. 2. Fig. 2a and b were the SEM
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55 168 images of the pure SrTiO3, which distinctly showed that the sample was made up of
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57 169 cubic-like nanoparticles with matte surface. And the length of SrTiO3 was approximately
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3 170 300-400 nm. As seen from Fig. 2c and d, a spot of Ag/AgCl NPs were attached on the surface
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5 171 of SrTiO3 nanocubes. By contrast with pristine SrTiO3, the morphology and size of SrTiO3 in
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7 172 the Ag/AgCl/SrTiO3 (21.6%) composite had no obvious changes, in line with the XRD
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9 173 results.
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33 174
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35 175 Fig. 2 SEM images of SrTiO3 (a and b) and Ag/AgCl/SrTiO3 (21.6%) (c and d).
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37 176 3.1.3. TEM and HRTEM analysis
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39 177 TEM as well as HRTEM measurements were performed to further investigate the
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178 microstructure of the Ag/AgCl/SrTiO3 (21.6%) composite. As shown in Fig. 3a and b, some
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42 179 particles which were deposited on the surface of SrTiO3 nanocubes could be regarded as
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44 180 Ag/AgCl NPs. Fig. 3c and d revealed the HRTEM images of Ag/AgCl/SrTiO3 (21.6%)
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46 181 composite. As shown in Fig. 3c, the distinct lattice fringes were 0.225 nm, 0.196 nm and
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48 182 0.236 nm, which were allocated to the facets of SrTiO3 (111) (JCPDS 35-0734), AgCl (220)
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50 183 (JCPDS 31-1238), and Ag (111) (JCPDS 04-0783), respectively. Another two interplanar
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52 184 spacing of 0.277 nm and 0.204 nm were also observed in Fig. 3d, which were severally
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54 185 assigned to the facets of AgCl (200) (JCPDS 31-1238) and Ag (200) (JCPDS 04-0783). The
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186 HRTEM results further demonstrated that the Ag/AgCl NPs were anchored on the surface of
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187 the SrTiO3. Such an Ag/AgCl/SrTiO3 (21.6%) structure could take advantage of the interfaces
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3 188 between Ag/AgCl NPs and SrTiO3 nanocubes, and avail to promoting the photocatalytic
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5 189 performance of SrTiO3 for organic contaminants degradation 24.
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32 191 Fig. 3 TEM (a and b) and HRTEM (c and d) images of the Ag/AgCl/SrTiO3 (21.6%).
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34 192 3.1.4. DRS analysis
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36 193 For any kind of semiconducting photocatalysts, the optical property plays a vital role in
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38 194 determining the photocatalytic performance. Fig. 4a showed DRS spectra of SrTiO3 and
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40 195 Ag/AgCl/SrTiO3 (21.6%). It was clearly that the pristine SrTiO3 exhibited distinct absorption
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42 196 band in the range of 200-370 nm. The sharp absorption edge at about 370 nm might be
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44 197 attributed to the electron transition from the valence band to the conduction band .
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198 Compared with the pristine SrTiO3, the Ag/AgCl/SrTiO3 (21.6%) photocatalysts showed a
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47 199 strong and broad absorbance in entire visible-light region (400-800 nm). The change mainly
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49 200 resulted from the SPR effect of metallic Ag formed in situ on the surface of AgCl/SrTiO3.
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51 201 Moreover, the absorption intensity of Ag/AgCl/SrTiO3 (21.6%) composite exhibited a
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53 202 remarkable improvement in visible-light region, which was mainly attributed to the existence
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55 203 of Ag/AgCl NPs 31.
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57 204 Furthermore, the band gap energy (Eg) of the pure SrTiO3 was computed from UV–vis
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3 205 DRS spectra using the following Eq. (1) 32 and illustrated in Fig. 4b:
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5 206
/ (1)
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7 207 where α, hν, Eg and A represent absorption index, light energy, band gap energy of
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9 208 semiconductor and constant value, respectively. The n is the index that characterizes the
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11 209 optical absorption process and is theoretically equal to 1 for allowed direct and 4 for allowed
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13 210 indirect . The Eg of SrTiO3 was determined by the related curve of (αhν)2 versus photon
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15 211 energy (hν) and shown in Fig. 4b. The results agreed fairly well with the literature results
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17 212 previously reported 14, 15.
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32 214 Fig. 4 (a) DRS spectra of pristine SrTiO3 and Ag/AgCl/SrTiO3 (21.6%) composite; (b) the
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34 215 band gap energy (E ) of pristine SrTiO3.
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36 216 3.1.5. XPS analysis
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38 217 Since it could provide information about chemical composition and oxidation state of the
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40 218 elements in the sample , XPS measurement was employed to characterize the
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42 219 Ag/AgCl/SrTiO3 (21.6%) composite. The XPS survey scan spectrum of the Ag/AgCl/SrTiO3
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44 220 (21.6%) sample was shown in Fig. 5a, which revealed the existence of Sr, Ti, O, Ag, and Cl
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221 elements in the composite. Whereas, the obtained binding energies of these elements from
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47 222 XPS analysis were calibrated by referencing the binding energy of 284.6 eV for C 1s. The
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49 223 binding energy of 458.6 and 464.35 eV (Fig. 5b) was the characteristic signal of the Ti 2p3/2
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51 224 and Ti 2p1/2, respectively, indicating its existence as the Ti4+ state 14. In the spectrum of Sr 3d
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53 225 (Fig. 5c), the peaks at 132.9 and 134.6 eV severally conformed to the binding energy of Sr
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55 226 3d5/2 and Sr 3d3/2, suggesting its existence as Sr2+ state 28
. In Fig. 5d, the peak located at
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57 227 binding energy of 198.5 eV was assigned to Cl 2p . Fig. 5e showed the spectra of Ag
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3 228 element and the peaks at 367.55 and 373.65 eV were consistent with the binding energy of Ag
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5 229 3d5/2 and Ag 3d3/2, respectively. These two peaks could be further divided into two peaks, at
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7 230 about 367.55/368.01 eV and 373.55/374.09 eV. The peaks at 367.55 and 373.55 eV were
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9 231 attributed to Ag+ of AgCl, and those at 368.01 and 374.09 eV belong to metallic Ag0 35. The
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11 232 XPS results manifested that metallic Ag0 existed in the Ag/AgCl/SrTiO3 (21.6%) composite,
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13 233 consistent with the above-discussed XRD analysis. In addition, the molar ratio of surface
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15 234 metallic Ag0 species to total Ag was semiquantitatively estimated to be 17.05% according to
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17 235 the XPS Ag 3d peak area analysis.
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3 237 Fig. 5 XPS spectra of Ag/AgCl/SrTiO3 (21.6%) sample: (a) the XPS survey spectrum, (b) Ti
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5 238 2p, (c) Sr 3d, (d) Cl 2p and (e) Ag 3d.
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7 239 3.1.6. FTIR spectroscopy analysis
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9 240 The FT-IR spectra of the SrTiO3 and Ag/AgCl/SrTiO3 (21.6%) photocatalysts were
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11 241 presented in Fig. 6. As shown in Fig. 6a, the spectrum of SrTiO3 was quite similar to SrTiO3
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13 242 reported previously 30. The bands at about 3440 and 1635 cm-1 were due to the O-H stretching
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15 243 vibration and deformation vibration of chemisorbed water molecules . The shoulder near
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17 244 1427 cm-1 was assigned to the bending vibration of CO32- 29, 36. The peaks at 625 and 855 cm-1
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245 were due to TiO6 stretching vibration and octahedron bending, respectively . As for
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20 246 Ag/AgCl/SrTiO3 (21.6%) composite, the similar absorption bands could also be discovered
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22 247 compared with the spectrum of SrTiO3. The above results illustrated that the addition of
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24 248 Ag/AgCl had no effect on the structure of SrTiO3, in accordance with XRD analysis.
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47 249
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49 250 Fig. 6 FTIR spectra of (a) the pure SrTiO3 and (b) Ag/AgCl/SrTiO3 (21.6%) sample.
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251 3.2. Photocatalytic activity
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52 252 3.2.1. Photodegradation of RhB
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54 253 The photocatalytic performances of all samples were assessed by monitoring the
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56 254 degradation of RhB aqueous solution under visible light irradiation. Fig. 7a showed that the
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58 255 direct photolysis of RhB from the blank experiment could almost be overlooked, also the
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3 256 pristine SrTiO3, Ag/AgCl, and Ag/SrTiO3 possessed poor photocatalytic ability. In addition,
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5 257 the photocatalytic activities of Ag/AgCl/SrTiO3 composites increased firstly and then
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7 258 decreased with the increase of Ag proportion. Among all proportion, Ag/AgCl/SrTiO3 (21.6%)
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9 259 showed the best photocatalytic efficiency and approximately 96% RhB (100 mL, 10 mg L-1)
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11 260 was degraded within 30 min. Fig. 7b displayed the UV-vis spectra in the degradation of RhB
12
13 261 solution under visible light irradiation over different periods of exposure. Based on the results,
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15 262 it could be confirmed that the Ag/AgCl/SrTiO3 photocatalysts system could dramatically
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17 263 improve the photocatalytic activity.
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264 To understand the reaction kinetics of the photodegradation process, the degradation
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20 265 rates were computed using the following pseudo-first-order kinetics Eq. (2) 37:
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22 266 / (2)
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24 267 where C0, Ct, and kapp stand for the initial concentration (mg L-1), the concentration at
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26 268 time t (mg L-1), and the apparent pseudo-first-order rate constant (min-1), respectively. Fig. 7c
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28 269 showed that the Ag/AgCl/SrTiO3 (21.6%) composite exhibited the topmost kapp (0.104 min-1),
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30 270 which was larger than the kapp value (0.002 min-1) of the pure SrTiO3.
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32 271 The photocatalytic degradation experiment of RhB was repeated five times of the
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34
272 Ag/AgCl/SrTiO3 (21.6%) sample for the purpose of testing the recyclability and stability of
35
273 photocatalysts. The sample was recycled via filtration and washed with deionized water
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37 274 afterwards. Besides, all other conditions stayed the same in the process of photodegradation.
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39 275 As shown in Fig. 7d, the photocatalytic activity decreased slightly after five cycling runs. The
40
41 276 decrease might be derived from the wastage of Ag/AgCl/SrTiO3 (21.6%) composite in the
42
43 277 cycling process. By contrast with the XRD pattern of fresh composite, that of used
44
45 278 Ag/AgCl/SrTiO3 (21.6%) (Fig. 1d) sample showed no obvious changes. Consequently, the
46
47 279 Ag/AgCl/SrTiO3 (21.6%) composite with good stability could be utilized to decompose
48
49 280 organic pollutants under visible light irradiation.
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30 282 Fig. 7 (a) Photocatalytic degradation of RhB of all samples under visible light irradiation; (b)
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32 283 absorption spectra of RhB over Ag/AgCl/SrTiO3 (21.6%); (c) -ln(Ct/C0) vs. t plot for
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34 284 photodegradation of RhB by different catalysts; (d) cycling degradation rate for RhB of
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285 Ag/AgCl/SrTiO3 (21.6%) under visible light irradiation.
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37 286 3.2.2. Photodegradation of MO and MB
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39 287 All photocatalysts were further used to degrade MO and MB under the same conditions
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41 288 to investigate the wide applications of the obtained samples. As seen from Fig. 8a and b, the
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43 289 photocatalytic performances of all Ag/AgCl/SrTiO3 composites exceeded the pristine SrTiO3
44
45 290 and Ag/AgCl NPs. Among all hybrid composites, the Ag/AgCl/SrTiO3 (21.6%) sample
46
47 291 exhibited the best photocatalytic ability in both aqueous solutions. Furthermore, about 93%
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49 292 MO (100 mL, 10 mg L-1) and 96% MB (100 mL, 10 mg L-1) were degraded within 40 min
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293 and 70 min, respectively. Fig. 8c and d displayed the UV-vis spectra in the degradation of MO
51
52 294 solution and MB solution under visible light irradiation over different periods of exposure,
53
54 295 respectively. It was obvious that the characteristic absorption peaks of MO and MB decreased
55
56 296 with reaction time going on. The results revealed that the Ag/AgCl/SrTiO3 (21.6%) composite
57
58 297 was efficient in catalyzing degradation of dyes under visible light irradiation.
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30 299 Fig. 8 Photocatalytic degradation of MO (a) and MB (b) by different photocatalysts under
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32 300 visible light irradiation；absorption spectra of MO (c) and MB (d) over Ag/AgCl/SrTiO3
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34 301 (21.6%) photocatalysts.
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302 3.2.3. Photodegradation of phenol and BPA
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37 303 With the purpose of avoiding dye self-sensitized in experiment, another two colorless
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39 304 persistent organic contaminants of phenol and BPA were employed herein to assess the
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41 305 photocatalytic activity of Ag/AgCl/SrTiO3 (21.6%) composite. UV-vis spectra were severally
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43 306 observed during degrading phenol solution and BPA solution under visible light irradiation.
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45 307 As shown in Fig. 9a and b, the characteristic absorption peaks of phenol and BPA decreased
46
47 308 as reaction time went on. It could be inferred that phenol and BPA were degraded in the
48
49 309 process of photodegradation. Besides, the degradation efficiencyies of phenol and BPA could
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310 reach to 70% and 83% in the degradation time of 4 h, respectively. The results disclosed that
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52 311 the Ag/AgCl/SrTiO3 (21.6%) composite possessed powerful photooxidating ability and could
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54 312 be utilized as photocatalysts for practical applications.
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15 313
16 314 Fig. 9 Absorption spectra of (a) phenol and (b) BPA over Ag/AgCl/SrTiO3 (21.6%) under
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18 315 visible light irradiation.
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20 316 3.3. Photocatalytic mechanism discussion
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22 317 Active species trapping measurements was utilized in the process of photodegrading
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318 RhB solution to disclose the photocatalytic mechanism of the Ag/AgCl/SrTiO3 (21.6%)
24
25 319 photocatalysts. In this work, iso-propyl alcohol (IPA, 10 mM) 38
, sodium oxalate (Na2C2O4,
26
27 320 10 mM) 39, and benzoquinone (BQ, 10 mM) 40
were applied to scavenge ·OH, h+ and ·O2–,
28
29 321 respectively. Fig. 10a showed the photodegradation curves of the Ag/AgCl/SrTiO3 (21.6%)
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31 322 composite in the RhB solution in the presence of different scavengers. It was found that no
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33 323 significant changes were observed in the presence of IPA, confirming that ·OH could not
34
35 324 make a difference in photodegrading process. Nevertheless, with the existence of Na2C2O4
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37 325 and BQ, the degradation efficiencies were 79.5% and 22.7%, respectively. In the light of
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39 326 trapping experimental results, it could be acquired that ·O2– was the main active species and
40
327 h+ played a secondary role in the photocatalytic degradation.
41
42 328 The photoluminescence (PL) spectra could afford the information of charge carrier
43
44 329 trapping, migration, and recombination process of photogenerated electrons (e–) and holes
45
46 330 (h+), so it was performed to further clarify the photocatalytic mechanism. The high PL
47
48 331 intensity manifested high electron–hole recombination rate and poor photocatalytic
49
50 332 performance 34. Fig. 10b presented the PL spectra of SrTiO3 and Ag/AgCl/SrTiO3 (21.6%) at
51
52 333 an excitation wavelength of 328 nm. It could be seen that the intensity of the pure SrTiO3 was
53
54 334 obviously stronger than that of Ag/AgCl/SrTiO3 (21.6%) composite. The results suggested
55
56
335 that the composition of Ag/AgCl/SrTiO3 (21.6%) was conducive to preventing the
57
336 recombination of electrons and holes, and enhancing the photocatalytic performance.
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17 338 Fig. 10 (a) Photodegradation curves of the Ag/AgCl/SrTiO3 (21.6%) composite in the RhB
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19 339 solution with the existence of different scavengers; (b) Photoluminescence spectra of pristine
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21 340 SrTiO3 and Ag/AgCl/SrTiO3 (21.6%) composite.
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23 341 In a hybrid composite, the band positions of each substance make a difference in the
24
25 342 processe of generation, transference and recombination of photogenerated electron-hole pairs.
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27 343 The band positions of Ag/AgCl and SrTiO3 were theoretically computed using the atom's
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344 Mulliken electronegativity definition Eqs. (3) and (4) 41, 42:
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30 345 0.5
(3)
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32 346
(4)
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34 347 where Evb is the valence band potential, Ecb is the conduction band potential, Ec is the
35
36 348 energy of free electrons on the hydrogen scale (ca. 4.5 eV), Eg is the band gap energy of the
37
38 349 semiconductor, and X is the absolute electronegativity of the semiconductor 18. Therefore, the
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40 350 Evb and Ecb of SrTiO3 were computed to be 2.46 eV and -0.86 eV, whereas the energies for
41
42 351 AgCl were about 3.19 eV and -0.06 eV 43.
43
44 352 In terms of the above-discussed results, a reasonable photocatalytic mechanism of
45
353 Ag/AgCl/SrTiO3 was brought up and illustrated in Fig. 11. Obviously, the Ag/AgCl/SrTiO3
46
47 354 photocatalysts exhibited high photocatalytic performance. However, neither SrTiO3 nor AgCl
48
49 355 could be stimulated under visible light irradiation, owing to their broad band gap. So the
50
51 356 photogenerated electrons and holes were simply produced by metallic Ag0 which was
52
53 357 sensitive to visible-light. Once upon the light absorption, the excited electrons of Ag NPs
54
44
55 358 possessed enough energy in the range of 1.0-4.0 eV so that they could transfer to the
56
57 359 conduction band (CB) of SrTiO3 and AgCl. Since the CB potential of SrTiO3 (-0.86 eV) and
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3 360 AgCl (-0.06 eV) were much more negative than the potential of O2/·O2– (-0.046 eV) 45, the
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5 361 oxygen O2 in the solution trapped the electrons on the surface of SrTiO3 and AgCl to
6

7 362 form ·O2–, then further oxidized the organic contaminants. Simultaneously, the
8
9 363 photogenerated holes were likely to immigrate to the AgCl surface to oxidize Cl– to ·Cl atoms
10
34, 46
11 364 . The ·Cl atoms were reactive radical species to oxidize organic contaminants and hence
12
13 365 reduced to Cl– again. And the left holes of metallic Ag could be directly used to oxidize
14
15 366 organic pollutants 47. Based on the above analysis, the detailed process could be described as
16
17 367 follows Eqs. (5) to (9):
18
368 Ag + hν → Ag (e– + h+) (5)
19
20 369 e− + O2 → ·O2– (6)
21
22 370 h+ + Cl– → ·Cl (7)
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24 371 ·Cl + organic pollutants → degradation products + Cl– (8)
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26 372 ·O2– + organic pollutants → degradation products (9)
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39
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41 373
42
43 374 Fig.11 Schematic drawing of the photocatalytic process in Ag/AgCl/SrTiO3 (21.6%).
44
45 375 4. Conclusion
46
47 376 In conclusion, the visible-light-sensitive Ag/AgCl/SrTiO3 composites have been
48
49 377 successfully fabricated via precipitation reaction followed by photoreduction. Compared with
50
378 the pristine SrTiO3 and Ag/AgCl NPs, the Ag/AgCl/SrTiO3 composites possessed higher
51
52 379 photocatalytic performance for the degradation of organic pollutants under visible light
53
54 380 irradiation. The enhanced photocatalytic efficiency might arise from the SPR with strong
55
56 381 visible light absorbance and efficient charge separation on the surface. The obtained
57
58 382 photocatalysts showed good stability and recyclability in the process of photodegradation.
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3 383 The composition of plasmonic Ag/AgCl/SrTiO3 photocatalysts in this paper could provide
4
5 384 insights into the design and development of other excellent ideal photocatalysts in
6

7 385 environment and energy issues.
8
9 386 Acknowledgement
10
11 387 This work was financially supported by the National Natural Science Foundation of China
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13 388 (51541801, 51521006 and 21507034), the Natural Science Foundation of Guangdong
14
15 389 Province, China (2016A030310022), and the Pearl River S&T Nova Program of Guangzhou.
16
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3 The Ag/AgCl/SrTiO3 composites were successfully fabricated and enhanced the
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Environmental Science: Nano Accepted Manuscript

Environmental Science: Nano Accepted Manuscript

Environmental Science: Nano Accepted Manuscript

Environmental Science: Nano Accepted Manuscript

Environmental Science: Nano Accepted Manuscript

Environmental Science: Nano Accepted Manuscript

Environmental Science: Nano Accepted Manuscript

Environmental Science: Nano Accepted Manuscript

Environmental Science: Nano Accepted Manuscript

Environmental Science: Nano Accepted Manuscript

Environmental Science: Nano Accepted Manuscript

Environmental Science: Nano Accepted Manuscript

Environmental Science: Nano Accepted Manuscript

Environmental Science: Nano Accepted Manuscript

Environmental Science: Nano Accepted Manuscript

Environmental Science: Nano Accepted Manuscript

Environmental Science: Nano Accepted Manuscript

Environmental Science: Nano Accepted Manuscript

Environmental Science: Nano Accepted Manuscript

Environmental Science: Nano Accepted Manuscript

Environmental Science: Nano Accepted Manuscript

Environmental Science: Nano Accepted Manuscript

Environmental Science: Nano Accepted Manuscript

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