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Non-Precious Metal Catalysts for Oxygen Reduction Reaction in Alkaline Solutions Zhewen Yin University of South Florida, [email protected]

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Non-Precious Metal Catalysts for Oxygen Reduction Reaction in Alkaline Solutions Zhewen Yin University of South Florida, Yzw994@Gmail.Com University of South Florida Scholar Commons Graduate Theses and Dissertations Graduate School March 2018 Non-precious Metal Catalysts for Oxygen Reduction Reaction in Alkaline Solutions Zhewen Yin University of South Florida, [email protected] Follow this and additional works at: http://scholarcommons.usf.edu/etd Part of the Materials Science and Engineering Commons Scholar Commons Citation Yin, Zhewen, "Non-precious Metal Catalysts for Oxygen Reduction Reaction in Alkaline Solutions" (2018). Graduate Theses and Dissertations. http://scholarcommons.usf.edu/etd/7250 This Thesis is brought to you for free and open access by the Graduate School at Scholar Commons. It has been accepted for inclusion in Graduate Theses and Dissertations by an authorized administrator of Scholar Commons. For more information, please contact [email protected]. Non-precious Metal Catalysts for Oxygen Reduction Reaction in Alkaline Solutions by Zhewen Yin A thesis submitted in partial fulfillment of the requirements for the degree of Master of Science in Materials Science and Engineering Department of Chemical and Biomedical Engineering College of Engineering University of South Florida Co-Major Professor: Venkat R. Bhethanabotla, Ph.D. Co-Major Professor: John N. Kuhn, Ph.D. Scott Campbell, Ph.D. Date of Approval: March 19, 2018 Keywords: Tungsten oxide, Sol-gel processing, Mesoporous, Fuel cells, Electrochemistry Copyright © 2018, Zhewen Yin DEDICATION This work is dedicated to my parents, Mrs. Mei Chen and Mr. Bin Yin, who despite all the sufferings and prolonged separation love me, trust me and have supported me every step of the way. Without their sacrifices and encouragement I could never have walked this far. ACKNOWLEDGMENTS I owe my greatest debt of gratitude to my advisors, Dr. Venkat R. Bhethanabotla and Dr. John N. Kuhn, who encouraged me to undertake this challenging work and offered me invaluable advice and informative suggestions. My thanks go to all the teachers who have taught me in these two years, who have helped me enrich and broaden my knowledge. My Special thanks to Swetha Ramani, who is always kind and patient in giving me her constant guide and help. My sincere thanks to Dr. Xianhui Zhao, Dr. Debtanu Maiti and Dr. Shuangming Li for their help in my experimental work. Finally, my thanks to USF Nanotechnology Research and Education Center (NREC) for their assistance in characterization techniques. TABLE OF CONTENTS LIST OF TABLES ........................................................................................................................................ ii LIST OF FIGURES ..................................................................................................................................... iii ABSTRACT ................................................................................................................................................. iv CHAPTER 1: INTRODUCTION ................................................................................................................. 1 CHAPTER 2: EXPERIMENTAL METHODS ............................................................................................ 4 2.1 Materials ........................................................................................................................................... 4 2.2 Synthesis of Samples ........................................................................................................................ 5 2.2.1 Synthesis of Mesoporous WO3 .................................................................................. 5 2.2.2 Synthesis of Modified WO3 ....................................................................................... 6 2.3 Electrochemical Measurement ......................................................................................................... 6 2.3.1 Work Station Set Up .................................................................................................. 7 2.3.2 Electrochemical Sample Preparation ......................................................................... 7 2.3.3 Testing Process .......................................................................................................... 8 2.3.4 Calculation of Scan Range ......................................................................................... 8 2.4 Characterization ................................................................................................................................ 8 2.4.1 X-ray Diffraction (XRD) ........................................................................................... 8 2.4.2 Transmission Electron Microscopy (TEM) ............................................................... 9 2.4.3 N2 Adsorption-Desorption Analysis .......................................................................... 9 CHAPTER 3: RESULTS AND DISCUSSION .......................................................................................... 10 3.1 Selection of Heating Temperature ................................................................................................. 10 3.2 Comparison of Three Kinds of Modifications............................................................................... 14 3.3 Effect of Vulcan Carbon Powder ................................................................................................... 16 3.4 Characterization of La/WO3 Catalysts ........................................................................................... 16 3.5 Stability of La/WO3 Catalysts ........................................................................................................ 21 CHAPTER 4: CONCLUSIONS ................................................................................................................. 22 REFERENCES ........................................................................................................................................... 23 APPENDIX A: COPYRIGHT PERMISSIONS ......................................................................................... 25 A.1 Permission for the Use of Figure 1 in Chapter 1 .......................................................................... 25 A.2 Permission for the Use of Figure 3 in Chapter 2 .......................................................................... 25 APPENDIX B: CALCULATIONS ............................................................................................................ 26 B.1 Calculations for Chapter 3 ............................................................................................................. 26 i LIST OF TABLES Table 1A Properties of reagents ................................................................................................................. 4 Table 2A Mean crystallite sizes and lattice parameters calculated for the WO3 and La/WO3 ................. 18 Table 3A Onset, half-wave potential and limiting current for the studied La/WO3 catalysts .................. 20 Table B1 Calculations of mean crystallite size ........................................................................................ 26 ii LIST OF FIGURES Figure 1 Structure diagram of proton exchange membrane fuel cells ..................................................... 2 Figure 2 Mesoporous WO3 synthesis stages ............................................................................................ 5 Figure 3 The schematic of rotating disk electrode system ....................................................................... 7 Figure 4 X-ray diffraction of WO3 calcined at different temperatures................................................... 11 Figure 5 N2 adsorption-desorption isotherms ........................................................................................ 11 Figure 6 TEM images of mesoporous WO3 ........................................................................................... 13 Figure 7 V-A diagram of WO3 samples calcined at different temperatures ........................................... 14 Figure 8 XRD images and ORR polarization curves of modified WO3 catalysts. ................................. 15 Figure 9 ORR polarization curves with/without Vulcan carbon powder ............................................... 16 Figure 10 XRD of pure mesoporous WO3 and La/WO3 catalysts ........................................................... 17 Figure 11 TEM images of La/WO3 1:10 .................................................................................................. 19 Figure 12 Electrochemical measurement curves...................................................................................... 20 Figure 13 ORR polarization curves of La/WO3 catalysts ........................................................................ 21 iii ABSTRACT Mesoporous WO3 powders were prepared via sol-gel processing synthesis using nonionic surfactant Pluronic (P-123) as the template. The influences of heating temperature on the pore structure and properties of WO3 powders were investigated. Three kinds of modifications were compared and evaluated after finding out the best heating condition. Different amount of lanthanum was doped into mesoporous WO3 to improve its Oxygen Reduction Reaction (ORR) activity. Several factors contributing to the increase of catalytic performance were discussed. Vulcan carbon powder was also used as a support to increase the catalysts’ electrical conductivity as well as dispersity. The component, microstructure and specific surface area of samples were
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