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研究生： TRAN THUY TUYET MAI
TRAN THUY TUYET MAI
論文名稱： Influences of MOISTURE on ROOM TEMPERATURE CO OXIDATION over Au/BN catalysts
Influences of MOISTURE on ROOM TEMPERATURE CO OXIDATION over Au/BN catalysts
指導教授： 林昇佃
Shawn D. Lin
口試委員: 林昇佃
Shawn D. Lin
江志強
Jyh-Chiang Jiang
劉端祺
Tuan-Chi Liu
萬本儒
Ben-Zu Wan
鄭淑芬
Soofin Cheng
葉君棣
Chuin-Tih Yeh
學位類別： 博士
Doctor
系所名稱： 工程學院 - 化學工程系
Department of Chemical Engineering
論文出版年： 2017
畢業學年度： 105
語文別： 英文
論文頁數： 120
中文關鍵詞： Au/BN catalyst 、*OOH species 、*CO(H2O)n species 、water co-catalyst
外文關鍵詞： Au/BN catalyst, *OOH species, *CO(H2O)n species, water co-catalyst
相關次數： 點閱：211  下載：0 
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    • Metal oxide supported gold catalysts readily catalyze CO oxidation at sub-ambient temperature, wherein moisture can influence the activity typically with a volcano-shape dependence. The abundant OH density on metal oxide surface hinders the study of how moisture may influence the CO oxidation over Au catalysts. In this work, we use hexagonal Boron Nitride (h-BN), a hydrophobic material, as the support for gold catalyst to study room temperature CO oxidation with various partial pressure of water (PH2O). A deposition method was conducted for preparing 1wt%Au/BN. Two commercial h-BN supports are compared and the effect of pretreatment conditions is examined for understanding the observed moisture-enhanced catalytic activity.
    The first strategy of this work is using spectroscopic methods to explore roles of water co-catalyst with Au/BN in RT CO oxidation. Au/BN catalyst shows a quick increasing CO oxidation with increase of moisture concentration upto 100% relative humidity (RH). How water can enhance RT CO oxidation over Au/BN is found related to intermediate species of hydroperoxyl (*OOH) and CO(H2O)2 complex upon O2-H2O and CO-H2O cofeedings, respectively. Injection of isotope labeled H218O demonstrates that OH from H2O takes part in the process of CO2 formation and proton transfer to oxygen leading production of CO2.
    The second focus in this work is the effect of calcination conditions on water adsorption behaviors and catalyst activity in RT CO oxidation over Au/BN. Ex situ XPS analysis demonstrates only metallic gold (Au0) dominated on Au/BN1 and Au/BN2 after calcination at temperatures from 300 to 600oC, with the exception of Au/BN1-300 and Au/BN2-600. The existence of Au+ (plus charged gold) on Au/BN1-300 and Au/BN2-600 presents less active CO oxidation in nominal dry and wet conditions. Increasing calcination temperature results in increase of both physisorption and chemisorption of water on Au/BN1 and Au/BN2, which can be described by Henry’s model and non-dissociative Langmuir model, respectively. This suggests that H2O adsorbs probably at the interface between Au and BN and that COad on Au surface may interact with the adsorbed H2O to form CO-(H2O)n and *OOH species. That also regards to the significant enhancement of moistened RT CO oxidation over Au/BN at elevated calcination temperature. Experimental evidences in this section indicates the interfacial perimeter of Au/BN is involved in the activation of CO and O2.
    The third achievement of this work examines the nature of active site on Au/BN catalyst. We examined how an additional H2 treatment at 300oC influence Au/BN1-600, Au/BN2-450 and Au/BN2-600. Only Au0 governed on Au/BN1 and Au/BN2 as proven by in situ DRIFTS of dry CO adsorption. Only a slight increase in nominal dry CO oxidation activity was found over Au/BN after the additional H2 treatment. The catalytic activity of wet RT CO oxidation is almost the same over Au/BN1-600 with/without the additional H2 treatment. However, a noticeable increase in wet CO oxidation rate over Au/BN2-600 was found after H2 treatment. This suggests that Au0 is more likely the active phase than Au+ in water co-feed RT CO oxidation over Au/BN.
    Another contribution of this work is to propose a possible mechanism that is consistent with the spectroscopic data and the kinetic data. The kinetic study was performed by varying space velocity and concentration of CO, O2 and H2O and then the kinetic data was reported. The reaction order on CO, O2 and H2O was found as 0.5 - 0.9, 0.5 – 0.5, and 0.6 – 1.5, respectively, which are not much influenced by catalyst pretreatment and type of BN (exception of H2O reaction order of 0.3 and 1.04 for Au/BN2-600 and Au/BN2-600-H2, respectively). A mechanism with good species balance is proposed which may explain how water acts as a co-catalyst in RT CO oxidation over Au/BN. Au0 is the surface site for COad and O2ad while the interface of Au-BN involved the sites for molecular H2Oad. CO(H2O)n complex is formed from the interaction between COad and H2Oad and the rate-determining step is the reaction between CO(H2O)n and O2ad.

    Metal oxide supported gold catalysts readily catalyze CO oxidation at sub-ambient temperature, wherein moisture can influence the activity typically with a volcano-shape dependence. The abundant OH density on metal oxide surface hinders the study of how moisture may influence the CO oxidation over Au catalysts. In this work, we use hexagonal Boron Nitride (h-BN), a hydrophobic material, as the support for gold catalyst to study room temperature CO oxidation with various partial pressure of water (PH2O). A deposition method was conducted for preparing 1wt%Au/BN. Two commercial h-BN supports are compared and the effect of pretreatment conditions is examined for understanding the observed moisture-enhanced catalytic activity.
    The first strategy of this work is using spectroscopic methods to explore roles of water co-catalyst with Au/BN in RT CO oxidation. Au/BN catalyst shows a quick increasing CO oxidation with increase of moisture concentration upto 100% relative humidity (RH). How water can enhance RT CO oxidation over Au/BN is found related to intermediate species of hydroperoxyl (*OOH) and CO(H2O)2 complex upon O2-H2O and CO-H2O cofeedings, respectively. Injection of isotope labeled H218O demonstrates that OH from H2O takes part in the process of CO2 formation and proton transfer to oxygen leading production of CO2.
    The second focus in this work is the effect of calcination conditions on water adsorption behaviors and catalyst activity in RT CO oxidation over Au/BN. Ex situ XPS analysis demonstrates only metallic gold (Au0) dominated on Au/BN1 and Au/BN2 after calcination at temperatures from 300 to 600oC, with the exception of Au/BN1-300 and Au/BN2-600. The existence of Au+ (plus charged gold) on Au/BN1-300 and Au/BN2-600 presents less active CO oxidation in nominal dry and wet conditions. Increasing calcination temperature results in increase of both physisorption and chemisorption of water on Au/BN1 and Au/BN2, which can be described by Henry’s model and non-dissociative Langmuir model, respectively. This suggests that H2O adsorbs probably at the interface between Au and BN and that COad on Au surface may interact with the adsorbed H2O to form CO-(H2O)n and *OOH species. That also regards to the significant enhancement of moistened RT CO oxidation over Au/BN at elevated calcination temperature. Experimental evidences in this section indicates the interfacial perimeter of Au/BN is involved in the activation of CO and O2.
    The third achievement of this work examines the nature of active site on Au/BN catalyst. We examined how an additional H2 treatment at 300oC influence Au/BN1-600, Au/BN2-450 and Au/BN2-600. Only Au0 governed on Au/BN1 and Au/BN2 as proven by in situ DRIFTS of dry CO adsorption. Only a slight increase in nominal dry CO oxidation activity was found over Au/BN after the additional H2 treatment. The catalytic activity of wet RT CO oxidation is almost the same over Au/BN1-600 with/without the additional H2 treatment. However, a noticeable increase in wet CO oxidation rate over Au/BN2-600 was found after H2 treatment. This suggests that Au0 is more likely the active phase than Au+ in water co-feed RT CO oxidation over Au/BN.
    Another contribution of this work is to propose a possible mechanism that is consistent with the spectroscopic data and the kinetic data. The kinetic study was performed by varying space velocity and concentration of CO, O2 and H2O and then the kinetic data was reported. The reaction order on CO, O2 and H2O was found as 0.5 - 0.9, 0.5 – 0.5, and 0.6 – 1.5, respectively, which are not much influenced by catalyst pretreatment and type of BN (exception of H2O reaction order of 0.3 and 1.04 for Au/BN2-600 and Au/BN2-600-H2, respectively). A mechanism with good species balance is proposed which may explain how water acts as a co-catalyst in RT CO oxidation over Au/BN. Au0 is the surface site for COad and O2ad while the interface of Au-BN involved the sites for molecular H2Oad. CO(H2O)n complex is formed from the interaction between COad and H2Oad and the rate-determining step is the reaction between CO(H2O)n and O2ad.

    Abstract i Acknowledgements iii Table of Contents v List of Abbreviations viii List of Tables xiv List of Schemes xv Chapter 1. Literature Review 1 1. 1. Gold catalysts for CO oxidation 1 1. 1. 1. The important role of Au valence state in CO oxidation 1 1. 1. 2. Water enhance co oxidation at low temperature over au/metal oxide catalysts 4 1. 1. 3. Mechanism of CO oxidation over gold catalysts 7 1. 2. Carbon monoxide (CO) - the silent killer 12 1. 2. 1. Impact to human 12 1. 2. 2. Impact to climate modification 13 1. 3. Boron Nitride (BN) 13 1. 4. Motivation and goal 15 Chapter 2. Experimental Section 16 2. 1. Catalyst preparation 16 2. 1. 1. Methods for preparation of gold catalysts 16 2.1.1.1. Incipient wetness (wet impregnation – IMP) method80 16 2.1.1.2. Deposition – precipitation (DP) method 16 2. 1. 2. Deposition method for synthesis of 1wt% Au/BN 17 2. 2. Characterization 18 2. 2. 1. ICP-AES measurement 18 2. 2. 2. X-ray powder diffraction (XRD) 18 2. 2. 3. Scanning Electron Microscope (SEM) 18 2. 2. 4. High Resolution Transmission Electron Microscopy (HRTEM) Analysis 18 2. 2. 5. Adsorption-desorption isotherms 19 2. 2. 6. XPS analysis 19 2. 3. CO oxidation tests 19 2. 4. In-situ DRIFTS 21 2. 5. In situ UV-Vis-DRS 22 Chapter 3. Spectroscopic Studies of How Moisture Enhances CO Oxidation over Au/BN at Ambient Temperature 23 3. 1. Motivation 23 3. 2. Results 25 3. 2. 1. Effect of H2O on CO oxidation over Au/BN 25 3. 2. 2. In situ DRIFTS 27 3. 2. 3. In situ UV-Vis-DRS 31 3. 3. Discussion 34 3. 4. Summary 37 Chapter 4. Effect of Calcination Temperature on Water Adsorption Behavior and Au/BN Catalytic Activity in Moistened RT CO Oxidation 38 4. 1. Motivation 38 4. 2. Results 39 4. 2. 1. Effect of PH2O on moistened CO oxidation on Au/BN with various calcination 39 4. 2. 2. In situ DRIFTS of CO and CO-H2O feeding on Au/BN with various calcination 41 4. 2. 3. Effect of calcination temperature on water adsorption behaviors 42 4. 2. 4. Catalyst Characterization 44 4. 2. 5. XPS analysis 47 4. 3. Discussion 53 4. 4. Summary 56 Chapter 5. Kinetic and Mechanism Study of H2O co-catalyst with Au/BN in Room Temperature CO Oxidation 57 5. 1. Motivation 57 5. 2. Results 58 5. 2. 1. Effect of H2 treatment on dry and wet CO oxidations 58 5. 2. 2. Evidences from in situ DRIFTS 59 5. 2. 3. Proposed mechanism of H2O co-catalyst with Au/BN in RT CO oxidation 62 5. 2. 3. 1. Model 1: CO, O2, H2O adsorbed on the same site of Au 62 5. 2. 3. 2. Model 2: H2Oad on interfacial perimeter () and CO, O2 adsorbed on the same site of Au (*): 64 5. 3. Discussion 66 5. 4. Summary 69 Chapter 6. Concluding Remarks 71 Chapter 7. Recommendations for Future Research 73 References 74 Appendix A 85 Appendix B 90 Appendix C 96 Curriculum Vitae of Author 101 Publications 103 Conferences 103

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