THÔNG TIN TÀI LIỆU
HANOI UNIVERSITY OF SCIENCE AND TECHNOLOGY MASTER THESIS Synthesis of Ag/SrTiO3 nanocomposites and application in photocatalytic degradation of organic dye LE VAN TUYEN Tuyen.LVCA190124@sis.hust.edu.vn CHEMICAL ENGINEERING Supervisor: Assoc Prof Dr Pham Thanh Huyen School: Chemical Engineering Signature of supervisor Signature of supervisor Hanoi, 12/2021 TRƯỜNG ĐẠI HỌC BÁCH KHOA HÀ NỘI LUẬN VĂN THẠC SĨ Tổng hợp vật liệu nano Ag/SrTiO3 ứng dụng trình quang xúc tác phân hủy thuốc nhuộm hữu LÊ VĂN TUYẾN Tuyen.LVCA190124@sis.hust.edu.vn Ngành: Kỹ thuật Hóa học Giảng viên hướng dẫn: PGS TS Phạm Thanh Huyền Viện: Kỹ thuật Hóa học Chữ ký GVHD HÀ NỘI, 12/2021 ĐỀ TÀI LUẬN VĂN Tổng hợp vật liệu nano Ag/SrTiO3 ứng dụng trình quang xúc tác phân hủy thuốc nhuộm hữu Giáo viên hướng dẫn Ký ghi rõ họ tên PGS.TS Phạm Thanh Huyền TABLE OF CONTENTS LIST OF FIGURES .iii LIST OF TABLES vi LIST OF SYMBOLS AND ABBREVIATIONS vii ACKNOWLEDGEMENTS viii SUMMARY ix INTRODUCTION CHAPTER 1: LITERATURE REVIEW 1.1 Strontium titanate 1.1.1 Overview of strontium titanate 1.1.2 Synthesis methods of STO 1.1.3 Modification of STO by noble metal decorating a Localized surface plasmon b Incorporation of noble metal onto STO 10 1.2 Application of STO for photocatalysis 10 1.3 Photocatalytic oxidation of organic dye 17 CHAPTER EXPERIMENTAL 22 2.1 Synthesis of catalysts 22 2.1.1 Chemicals 22 2.1.2 Synthesis procedure 22 a Synthesis procedure of strontium titanate (STO) 22 b Synthesis of Ag/STO nanocomposites 23 2.2 Catalyst characterization method 24 2.2.1 X-ray diffraction (XRD) 24 2.2.2 Scanning Electron Microscopy (SEM) 26 2.2.3 Nitrogen adsorption-desorption method 27 2.2.4 X-ray Photoelectron Spectroscopy (XPS) 29 2.2.5 Transmission Electron Microscopy 30 2.2.6 Energy Dispersive X-ray Spectroscopy 32 2.3 Catalyst activity 33 2.4 Density functional calculations 33 CHAPTER 3: RESULTS AND DISCUSSION 3.1 35 Catalyst characterization 35 3.1.1 XRD results 35 i 3.1.2 Scanning electron micrographs 36 3.1.3 N2 adsorption and desorption analysis 38 3.1.4 X-ray Photoelectron Spectroscopy 40 3.1.5 Transmission electron micrographs 42 3.2 Photocatalytic activity of Ag/STO catalyst 43 3.2.1 The adsorption capacity of the catalysts 43 3.2.2 Activity of Ag/STO with different Ag loadings in RhB photodegradation 44 3.2.3 Effect of catalyst loading 46 3.2.4 Reusability 47 3.2.5 Proposal of RhB photodegradation mechanism 51 3.2.5.1 Trapping experiment 51 3.2.5.2 Adsorption and activation of oxidizing agents on the catalyst 52 CONCLUSIONS 57 REFERENCES 58 ii LIST OF FIGURES Figure 1.1 The lattice structure of STO [39] Figure 1.2 Number of publications using “strontium titanate” or “STO” as the topic keywords in the past 20 years [39] Figure 1.3 The energy band shifting of hydroxylation STO and pristine STO 13 Figure 1.4 Energy-level diagram shows the CB and VB edge positions of various semiconductors at pH=0 along with selected redox potentials The energy scales are referenced against both the vacuum level and the normal hydrogen electrode (NHE) [99] 19 Figure 1.5 Band gap diagram of (a) an insulator, (b) a semiconductor, and (c) a conductor 20 Figure 2.1 Synthesis procedure of STO by polymeric citrate precursor method 23 Figure 2.2 Synthesis procedure of Ag/STO nanocomposites 24 Figure 2.3 Constructive and destructive interferences when X-rays interact with crystals 25 Figure 2.4 Illustration for lattice plane in crystal 25 Figure 2.5 SEM layout and function 27 Figure 2.6 Classification of physisorption isotherms 27 Figure 2.7 Classification of hysteresis loops 28 Figure 2.8 Principle of XPS method 30 Figure 2.9 The working principle of TEM method 31 Figure 2.10 The interaction volume and signals generated from different regions in an SEM experiment 32 Figure 3.1 XRD patterns of pristine STO and Ag/STO photocatalysts 35 Figure 3.2 SEM images of STO (a), STO 1.0 (b) 37 Figure 3.3 EDX spectrums of STO 1.0 (a) 37 Figure 3.3 EDX spectrums of STO 1.0 (b) 38 Figure 3.4 Nitrogen adsorption-desorption isotherms of pristine STO and STO 1.0 38 Figure 3.5 Nitrogen adsorption-desorption isotherms of pristine STO (a) and STO 1.0 (b) 39 Figure 3.6 Survey XPS spectra of STO (a) and STO 1.0 (b) 40 iii Figure 3.7 High resolution XPS spectra of the Sr 3d peaks (a), Ti 2p peaks (b), O 1s peaks (c) and Ag 3d peaks (d) 41 Figure 3.8 (a) Low resolution TEM image of STO 1.0; (b) High resolution HRTEM image of STO 1.0, (c) histogram of the particle size distribution of metallic Ag 42 Figure 3.9 Slight EDX spectrums of STO 1.0 43 Figure 3.10 Dye adsorption ability of catalysts 44 Figure 3.11a Comparison of photocatalytic activity for the degradation of RhB in aqueous solution using solarium lamp over pure STO and Ag/STO photocatalysts RhB decomposition is also evaluated in the same reaction condition without catalyst Reaction condition: catalyst loading: 50 mg, RhB solution: 100ml, concentration: 10 ppm 44 Figure 3.11b Degradation rate of RhB in aqueous solution using solarium lamp over pure STO and Ag/STO composites after 60 minutes treatment Reaction condition: catalyst loading: 50 mg, RhB solution: 100 ml, concentration: 10 ppm 45 Figure 3.12 Time-dependent UV-vis spectra of photodegradation of RhB in solution in the presence of STO 1.0 Reaction condition: catalyst loading: 50 mg, RhB solution: 100 ml, concentration: 10 ppm The inset: Changes in solution colors over the course of photocatalytic 46 Figure 3.13 Effect of different amounts of photocatalyst (STO 1.0 was chosen for the test) on degradation efficiency 47 Figure 3.14.Reusability of STO 1.0 photocatalyst in four successive experimental runs for the photocatalytic degradation of RhB in aqueous solution using solarium lamp Reaction condition: Catalyst loading: 50 mg, RhB solution: 100 ml, concentration: 10 ppm 48 Figure 3.15 XRD patterns of fresh STO 1.0 before photocatalytic degradation of RhB and spent STO 1.0 after cycles of photocatalytic degradation of RhB 48 Figure 3.16 Optimized structures and charge density difference plot for (a) onelayer Ag/STO; (b) two-layers Ag/STO; (c) three-layers Ag/STO; (d) four-layers Ag/STO In the charge density difference plots, regions with depleted electron density (excess electron density) are shown in yellow (dark blue) Iso-surface levels are plotted from −0.002 to +0.002 e/bohr3 Ag, Sr, Ti and O are shown in light blue, green, grey, and red, respectively 49 Figure 3.17 Photocatalytic degradation results of RhB aqueous solution with STO nanocomposite in the presence of various scavengers with a iv concentration of mmol L-1 (a) No scavenger (b) t-BuOH (c) EDTA (d) BQ Reaction condition: catalyst loading: 50 mg, RhB solution: 100 ml, concentration: 10 ppm 52 Figure 3.18 (a) Binding energies of oxidizing agents (O2, H2O, OOH*, O* and OH*) at the interface of Ag and STO; on monolayer of Ag/STO; on clean STO(110) and on clean Ag(111) surface; (b) The Local Surface Plasmonic Resonance (LSPR) mediated charge transfer mechanism between Ag/STO Binding configurations and charge density difference plots for key reactive species including O2, OOH, and OH at the interface of Ag and STO 53 Figure 3.19 Activation of O2 (a) and H2O (b) and the formation of OOH (c) at the interface of Ag/STO IS, TS, and FS denote the initial state, transition state, and final state, respectively The activation barrier (in eV) for those reactions is presented in bold values, while the value in parentheses is activation barriers of the same reaction on pure Ag(111) surface (regular values)/clean STO(110) surface (italic values) 55 v LIST OF TABLES Table 1.1 Recent publications (2008-2018) of the preparation methods of STO nano-materials [39] Table 1.2 The list of photocatalysis applications for STO [39] 14 Table 1.3 Oxidation potential (Eox) of various oxidizing agents at pH = 0.106 20 Table 2.1 List of chemicals used in this work 22 Table 3.1 Lattice parameters of pristine STO and Ag/STO photocatalysts 36 Table 3.2 Elemental compositions of the sample STO and STO 1.0 (atomic percentages) 37 Table 3.3 Summary of the BET surface areas, pore volumes, and pore sizes of the photocatalysts 39 Table 3.4 Elemental compositions of the sample STO and STO 1.0 according to XPS measurement (atomic percentages) 42 Table 3.5 Adhesion energy and Bader charge of Ag atoms for Ag overlayer films on STO support 50 vi LIST OF SYMBOLS AND ABBREVIATIONS STO STO BOD biochemical oxygen demand COD chemical oxygen demand LSPR localized surface plasmon resonance h+ holes ·OH hydroxyl radicals ·O2− superoxide anion radicals t-BuOH tert-butyl alcohol EDTA ethylenediaminetetraacetic acid 1,4 BQ benzoquinone CB conduction band VB Valance band Eg Energy gap RhB Rhodamine B DFT Density Functional Theory vii that it might be an important oxidizing agent to facilitate the photo-degradation of RhB compound In contrast to the trend of O2 adsorption, water molecule is adsorbed weakly on all surfaces via the van der Waals interaction The binding energies of water with surfaces vary narrowly within the range from ~0.4 - 0.6 eV (Fig 3.18a) Therefore, water is unlikely a direct oxidizing agent However, other oxygenderivatives from water and O2, including O*, OH* and OOH* (* denotes the adsorbed state), all are adsorbed much stronger at the Ag/STO interface than on pure STO and clean Ag(111) surfaces (Fig 3.18a), demonstrating the crucial role of the interfacial sites in generating and stabilizing those high active oxygen species Indeed, the binding energies of O*, OH* and OOH* on Ag/STO interface are strengthened by 1.8 eV, 1.4 eV, and 1.0 eV compared to the Figure 3.18 (a) Binding energies of oxidizing agents (O2, H2O, OOH*, O* and OH*) at the interface of Ag and STO; on monolayer of Ag/STO; on clean STO(110) and on clean Ag(111) surface; (b) The Local Surface Plasmonic Resonance (LSPR) mediated charge transfer mechanism between Ag/STO Binding configurations and charge density difference plots for key reactive species including O2, OOH, and OH at the interface of Ag and STO 53 corresponding binding energies of those species on pure Ag(111) surface (Fig 3.18a), and those active oxygen species could feasibly participate in the oxidation of RhB compound at the interface of Ag/STO The widely proposed mechanism of the LSPR mediated charge transfer mechanism between Ag and STO and how the oxidizing agents are generated on this catalyst are presented in Fig 3.18b In this photocatalytic system, when Ag/STO nanocomposite is irradiated with light at the plasmon frequency of Ag nanoparticles, energetic electrons are produced and injected into the conduction band (CB) of STO by overcoming the Schottky barrier at the metal/semiconductor interface In addition, electrons could transfer from the dye in its singlet excited state to the CB of STO Part of these electrons is captured at interface Ag/STO sites and react with adsorbed oxygen to produce O2− species To maintain the electric neutrality, electrons on the valence band (VB) of STO are transferred to Ag nanoparticles, leaving behind holes that can further react with the adsorbed H2O molecules or surface hydroxyl group to produce •OH and •OOH radicals Subsequently, the generated highly active oxygen species •OH, •OOH and •O2radicals facilitate the degradation of RhB The structures of OH* and OOH* adsorbed at the interface of Ag/STO are shown as insets in Fig 3.18b Charge density difference plots for those structures also show the corporative role of the metal site and STO substrate site in stabilizing those oxygen species, similar to the adsorption of O2 at the interface The computed Bader charge indicates that upon adsorption at the interface of Ag/STO, the charge of adsorbed O2 is -1.13, consistent with the proposed active •O2- species in the photo-oxidation mechanism (Fig 3.18b) Finally, the activation barriers for the formation of those active oxygen species are computed on clean Ag(111), STO, and Ag/STO (Fig 3.19) On both Ag(111) and STO(110) surfaces, the direct activation of O2 generating atomic oxygen is difficult with extremely high barriers of 1.21 and 1.44 eV, respectively The activation of water forming hydroxy group is also not feasible with a high barrier of 1.97 and 1.11 eV on Ag(111) and STO(110) surfaces Those high barriers for both O2 and H2O activations on Ag(111) and STO(110) surfaces suggest that metallic Ag sites or STO sites separately are not active in generating those oxygen species which are crucial for the photo-oxidation reactions The computed barriers in this study are greatly consistent with low activity for Ag and STO towards O2 activation and H2O activation reported in the literature However, at the interface, the formations of those active oxygen species are much more feasible, except for the direct dissociation of O2 Although adsorbed strongly with the binding energy of -2.01 eV, breaking the O-O bond into two atomic oxygens at Ag/STO interface is still difficult with a high barrier of 1.25 54 eV (Fig 3.19a), rules out the contribution of O* as an oxidizing agent in the photo-oxidation reactions Water molecule is adsorbed slightly stronger at Ag/STO interfacial sites with a binding energy of -0.61 eV (vs -0.34 eV on Ag(111) surface), but it can be activated with a barrier of only 0.79 eV, producing OH* strongly adsorbed at the interface and H* adsorbed on metal Ag sites (Fig 3.19b) The kinetically feasible formation of OH* at the Ag/STO interface indicates that it might be an important oxidizing agent for Ag/STO and is consistent with the mechanism proposed in Fig 3.19b Figure 3.19 Activation of O2 (a) and H2O (b) and the formation of OOH (c) at the interface of Ag/STO IS, TS, and FS denote the initial state, transition state, and final state, respectively The activation barrier (in eV) for those reactions is presented in bold values, while the value in parentheses is activation barriers of the same reaction on pure Ag(111) surface (regular values)/clean STO(110) surface (italic values) Furthermore, H* generated from H2O activation can react with the adsorbed O2, forming adsorbed OOH* again strongly stabilized at the interface The activation barrier for OOH* formation is only 0.72 eV (Fig 3.19c) 55 From those kinetic data calculated and discussed and the experimental trapping results mentioned above, we could propose that O2, OH* and OOH* are likely the active oxidizing agents presented at Ag/STO interface to facilitate the photodegradation of RhB The obtained results also emphasize the important role of interfacial sites via the synergistic participation of both Ag site and STO sites in generating and stabilizing those active oxidizing agents, which are crucial for the oxidation-degradation reactions 56 CONCLUSIONS - Ag/STO composites with tunable Ag contents are synthesized via roomtemperature liquid-phase deposition of Ag nanoparticles on the surface of STO, which is pre-synthesized by a facile polymeric citrate precursor approach and subsequently annealed in air - Ag/STO catalysts enhance photocatalytic activity for the degradation of RhB under solarium irradiation in comparison with pristine STO The photocatalytic results reveal that the valence state of Ag plays an important role via LSPR mechanism which improves photocatalytic activity of Ag/STO composites In addition, the trapping experiments confirm that photogenerated •OH and •O2− radicals are the major reactive species responsible for the photodegradation of RhB in the Ag/STO system - Atomic scale simulations are performed with DFT to understand electronic properties and interaction, understand the activity of interfacial sites A quantitative analysis of how the Ag/STO interfacial perturbation varies with proximity to the interface has been conducted The interaction between Ag and STO (via charge transfer) is majorly confined to the first Ag atomic layer, with small residual charges existing in the second layer Ag atoms at layer and above are not chemically modified by STO and have 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TÀI LUẬN VĂN Tổng hợp vật liệu nano Ag/SrTiO3 ứng dụng trình quang xúc tác phân hủy thuốc nhuộm hữu Giáo viên hướng dẫn Ký ghi rõ họ tên PGS.TS Phạm Thanh Huyền TABLE OF CONTENTS LIST OF FIGURES...TRƯỜNG ĐẠI HỌC BÁCH KHOA HÀ NỘI LUẬN VĂN THẠC SĨ Tổng hợp vật liệu nano Ag/SrTiO3 ứng dụng trình quang xúc tác phân hủy thuốc nhuộm hữu LÊ VĂN TUYẾN Tuyen.LVCA190124@sis.hust.edu.vn Ngành:... xanthene dyes, namely rose bengal (RB) are extensively used in printing, insecticides, and in dying industries [78] It is considered one of the new emerging pollutants in surface and probably drinking
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