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Front Matter Template Copyright by Preethi Mathew 2013 The Dissertation Committee for Preethi Mathew Certifies that this is the approved version of the following dissertation: CATHODE CATALYSTS FOR LOW-TEMPERATURE FUEL CELLS: ANALYSIS OF SURFACE PHENOMENA Committee: Arumugam Manthiram, Supervisor John B Goodenough, Co-Supervisor Allen J Bard Charles B Mullins Guihua Yu CATHODE CATALYSTS FOR LOW-TEMPERATURE FUEL CELLS: ANALYSIS OF SURFACE PHENOMENA by Preethi Mathew, B.Tech., M.Tech. Dissertation Presented to the Faculty of the Graduate School of The University of Texas at Austin in Partial Fulfillment of the Requirements for the Degree of Doctor of Philosophy The University of Texas at Austin December 2013 Dedication To my beloved Lord (Papa) and To my beloved parents Acknowledgement I wish to place on record my profound gratitude to my dissertation advisors, Professors John B. Goodenough and Arumugam Manthiram for their invaluable guidance, constant encouragement and inspiring discussions as well as the opportunity to continue my Doctoral degree. I am forever indebted to both of them for the freedom given to pursue my research interests. I express my gratefulness to Professors Allen J. Bard, Charles B. Mullins and Guihua Yu for serving on my dissertation committee and for their helpful suggestions and ideas. I also wish to thank Dr. Jeremy P. Meyers for his guidance and support. My sincere thanks are due to Dr. Thomas Cochell and Dr. Wei Li for stimulated discussions and their assistance on a variety of topics. I wish to thank Dr. Nathan Miller, Dr. Wei Li, Dr. Hugo Celio, Craig Milroy, and Zachary Moorhead-Rosenberg for ICP- MS, TEM, UVPES, XPS, and magnetic measurements, respectively. I thank Dr. Xiaole Chen and CEC for assistance with QCM-D measurements. I also thank past and current members of my research groups for their assistance and support. I wish to thank the staff of the Texas Materials Institute and the Materials Science and Engineering Graduate program for their support. Financial support by Norman Hackerman Advanced Research Program, Argonne National Laboratories–DOE project, Office of Naval Research (MURI), and Robert A. Welch Foundation is gratefully acknowledged. I humbly thank my parents and my siblings for their unconditional love and support over the years. I also thank my friends for their encouragement during this journey. I thank my Lord and Savior Jesus Christ for loving me just as I am, restoring me, and meeting all my needs according to His riches in glory. v CATHODE CATALYSTS FOR LOW-TEMPERATURE FUEL CELLS: ANALYSIS OF SURFACE PHENOMENA Preethi Mathew, Ph.D. The University of Texas at Austin, 2013 Supervisors: Arumugam Manthiram, John B Goodenough The electrochemical oxygen reduction reaction (ORR) steps on a noble metal catalyst in an acidic aqueous electrolyte depend on the nature of the catalytic surface with which the O2 molecule interacts. It has been assumed that the O2 molecules interact directly with a bare noble-metal surface. By studying the nature of chemisorbed species on the surface of a metal catalyst as a function of the voltage on the anodic and cathodic sweeps, it is shown here that the O2 reacts with a surface covered with oxide species extracted from the aqueous electrolyte and not from the O2 molecules; the ORR is more active when the surface species are OH rather than O. Moreover, the strength of the chemical bond of the adsorbed species was shown to depend on the relative strengths of the metal-metal versus metal-oxide bonds. The Pt-Pt bonds are stronger than the Pd-Pd bonds, and the relative Pd-O bonds are stronger than the relative Pt-O bonds. As a result, the chemisorbed O species is stable to lower anodic potentials on Pd. CO oxidation to CO2 occurs at a higher potential on Pd than on Pt, which is why Pd (not Pt) is tolerant to methanol. Experiments with alloys show the following: (1) methanol tolerance decreases with the increase of Pt in the Pd-Pt alloys with Pd3Pt/C showing an initial tolerance that decreases with cycling; (2) OH is formed on Pt3Co/C and core-shell Pt-Cu/C, which results in a higher activity and durability for the ORR on these catalysts; (3) a 300 oC vi anneal is needed to stabilize the Pd3Au/C catalyst that forms an O adsorbate; and (4) OH is formed on Pd3Co/C and Pd3CoNi/C. These studies provide a perspective on possible pathways of the ORR on oxide-coated noble-metal alloy catalysts. vii Table of Contents List of Tables ................................................................................................... xiv List of Figures ................................................................................................. xvii 1. Introduction .................................................................................................... 1 1.1. Polymer electrolyte fuel cells (PEFCs) ............................................... 2 1.2. Direct methanol fuel cells (DMFCs) ................................................... 6 1.3. Cathode catalysts ............................................................................... 7 1.4. Description of the research problem ................................................... 9 1.5. Scope and objectives ........................................................................ 11 1.6. Methodology .................................................................................... 15 2. Experimental techniques ............................................................................... 17 2.1. Synthesis of carbon-supported palladium-based catalysts ................. 17 2.2. Structural and chemical characterization .......................................... 19 2.2.1. X-Ray diffraction (XRD) measurement........................... 19 2.2.2. Energy dispersive X-Ray spectroscopy (EDS) measurement................................................................... 20 2.2.3. Thermogravimetric analysis (TGA) ................................ 22 2.2.4. Transmission electron microscopy (TEM) measurement . 23 2.2.5. Inductively coupled plasma (ICP) spectroscopy measurement................................................................... 24 2.2.6. X-ray photoelectron spectroscopy (XPS) measurement ... 25 2.3. Electrochemical characterization ...................................................... 26 2.3.1. Preparation of catalyst ink and thin-film electrode .......... 27 2.3.2. Rotating (ring) disk electrode (R(R)DE) setup ................ 28 2.3.3. Electrochemical quartz crystal nanobalance (EQCN) measurement setup ......................................................... 30 2.3.3.1. Factors affecting EQCN response ............................. 33 2.3.3.2. Establishing the use of EQCN measurement with catalyst loaded sensor ...................................... 34 viii 2.3.4. Interfacial mass change ................................................... 36 2.3.5. Measurement of electrochemical active surface area (ECSA) by HUPD method ......................................... 37 2.3.6. Carbon monoxide (CO) stripping voltammetry ............... 38 2.3.7. Activity measurement for oxygen reduction reaction (ORR) ............................................................... 40 2.3.8. Determination of hydrogen peroxide (H2O2) intermediates ....................................................... 43 2.3.9. Electrochemical durability measurement ......................... 45 PLATINUM-BASED CATALYSTS ........................................................................... 47 3. Surface oxide growth on polycrystalline platinum electrodes by EQCN analysis.............................................................................................. 48 3.1. Introduction ..................................................................................... 48 3.2. Experimental methods ...................................................................... 49 3.2.1. Electrochemical characterization ..................................... 49 3.3. Results and discussion...................................................................... 51 3.3.1. Electrochemical characterization ..................................... 51 3.3.1.1. Effect of upper potential and the adsorbing ions ....... 51 3.3.1.2. Effect of double-layer capacitance ............................ 54 3.3.1.3. Influence of O2-saturated solution ............................ 56 3.3.1.4. Effect of the pH of the solution ................................. 58 3.4. Conclusions ..................................................................................... 62 4. Analysis of surface oxidation and the extent of surface oxide growth on the durability of carbon-supported platinum and platinum binary-alloy catalysts ........................................................................................................ 63 4.1. Introduction ..................................................................................... 63 4.2. Experimental methods ...................................................................... 64 4.2.1. Structural/chemical characterization ............................... 64 ix 4.2.2. Electrochemical characterization ..................................... 64 4.2.2.1. Preparation of catalyst ink and electrode ................... 64 4.2.2.2. Cyclic voltammetry (CV) ......................................... 64 4.2.2.3. Electrochemical quartz crystal nanobalance measurements (EQCN) ............................................ 65 4.2.2.4. Accelerated degradation tests ................................... 65 4.2.2.5. Determination of H2O2 intermediates.......................
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