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(Sofc) Fuel Electrodes University of Pennsylvania ScholarlyCommons Publicly Accessible Penn Dissertations 2013 Approaches to Mitigate Metal Catalyst Deactivation in Solid Oxide Fuel Cell (SofC) Fuel Electrodes Lawrence Adijanto University of Pennsylvania, [email protected] Follow this and additional works at: https://repository.upenn.edu/edissertations Part of the Chemical Engineering Commons, Nanoscience and Nanotechnology Commons, and the Oil, Gas, and Energy Commons Recommended Citation Adijanto, Lawrence, "Approaches to Mitigate Metal Catalyst Deactivation in Solid Oxide Fuel Cell (SofC) Fuel Electrodes" (2013). Publicly Accessible Penn Dissertations. 728. https://repository.upenn.edu/edissertations/728 This paper is posted at ScholarlyCommons. https://repository.upenn.edu/edissertations/728 For more information, please contact [email protected]. Approaches to Mitigate Metal Catalyst Deactivation in Solid Oxide Fuel Cell (SofC) Fuel Electrodes Abstract While Ni/YSZ cermets have been used successfully in SOFCs, they also have several limitations, thus motivating the use of highly conductive ceramics to replace the Ni components in SOFC anodes. Ceramic electrodes are promising for use in SOFC anodes because they are expected to be less susceptible to sintering and coking, be redox stable, and be more tolerant of impurities like sulfur. In this thesis, for catalytic studies, the infiltration procedure has been used to form composites which have greatly simplified the search for the best ceramics for anode applications. In the development of ceramic fuel electrodes for SOFC, high performance can only be achieved when a transition metal catalyst is added. Because of the high operating temperatures, deactivation of the metal catalyst by sintering and/or coking is a severe problem. In this thesis, two approaches aimed at mitigating metal catalyst deactivation which was achieved by: 1) designing a catalyst that is resistant to coking and sintering and 2) developing a new method for catalyst deposition, will be presented. The first approach involved synthesizing a self-regenerating, "smart" catalyst, in which Co, Cu, or Ni were inserted into the B-site of a perovskite oxide under oxidizing conditions and then brought back to the surface under reducing conditions. This restores lost surface area of sintered metal particles through an oxidation/reduction cycle. Results will be shown for each of the metals, as well as for Cu-Co mixed metal systems, which are found to exhibit good tolerance to carbon deposition and interesting catalytic properties. The second strategy involves depositing novel Pd@CeO2 core-shell nanostructure catalysts onto a substrate surface which had been chemically modified ot anchor the nanoparticles. The catalyst deposited onto the chemically modified, hydrophobic surface is shown to be uniform and well dispersed, and exhibit excellent thermal stability to temperatures as high as 1373 K. Similar metal catalyst deposition method was also employed to access their suitability for use in SOFC anodes. Degree Type Dissertation Degree Name Doctor of Philosophy (PhD) Graduate Group Chemical and Biomolecular Engineering First Advisor Raymond J. Gorte Second Advisor John M. Vohs Keywords catalyst, ceramic anode, core-shell nanostructures, intelligent catalyst, solid oxide fuel cells, vanadates Subject Categories Chemical Engineering | Nanoscience and Nanotechnology | Oil, Gas, and Energy This dissertation is available at ScholarlyCommons: https://repository.upenn.edu/edissertations/728 APPROACHES TO MITIGATE METAL CATALYST DEACTIVATION IN SOLID OXIDE FUEL CELL (SOFC) FUEL ELECTRODES Lawrence Adijanto A DISSERTATION in Chemical and Biomolecular Engineering Presented to the Faculties of the University of Pennsylvania in Partial Fulfillment of the Requirements for the Degree of Doctor of Philosophy 2013 Supervisor of Dissertation Co-Supervisor of Dissertation ___________________________ ____________________________ Raymond J. Gorte, Professor, CBE John M. Vohs, Professor,CBE Graduate Group Chairperson ____________________________ Raymond J. Gorte, Professor, Chemical and Biomolecular Engineering Dissertation Committee Warren D. Seider, Professor, Chemical and Biomolecular Engineering Paulo E. Arratia, Associate Professor, Mechanical Engineering and Applied Mechanics This work is dedicated to my Family With Thanks to Professor Ray Gorte and Professor John Vohs ii Acknowledgements First and foremost, I would like to express my sincere appreciation to my thesis advisors, Professor Ray Gorte and Professor John Vohs, for their unconditional support, guidance, patience, and encouragement throughout my research work. I would also like to thank all the students that I have worked with during the past four years, particularly, Venu Balaji Padmanabhan. Moreover, I want to give thanks to my committee, Professor Warren Seider and Professor Paulo Arratia for their support and guidance. My appreciation likewise extends to my colleagues and friends as they are the sources of laughter, joy, and support. My life at Penn would not have been the same without them. I particularly wish to offer my special thanks to: Dr. Rainer Küngas, who has been an inspiring, supportive, and patient role model to me, for always entertaining even my trivial questions. Dr. Matteo Cargnello for always being there for discussion, tennis and meals at Han Dynasty. Lu Yao and Kwadwo Tettey for your time and support during my job search. Ami Tiyaboonchai for always providing great support in all my struggles and frustrations in my life and studies. In addition, I wish to thank the financial support for this project, which was provided by the Office of Naval Research (N00014-11-1-0229), and the U.S. Department of Energy, Office of Basic Energy Sciences (DE-FG02-13ER16380). Finally, my deepest gratitude goes to my family for their love and support throughout my life. Without whom I could not have made it here. iii ABSTRACT APPROACHES TO MITIGATE METAL CATALYST DEACTIVATION IN SOLID OXIDE FUEL CELL (SOFC) FUEL ELECTRODES Lawrence Adijanto Raymond J. Gorte John M. Vohs While Ni/YSZ cermets have been used successfully in SOFCs, they also have several limitations, thus motivating the use of highly conductive ceramics to replace the Ni components in SOFC anodes. Ceramic electrodes are promising for use in SOFC anodes because they are expected to be less susceptible to sintering and coking, be redox stable, and be more tolerant of impurities like sulfur. In this thesis, for catalytic studies, the infiltration procedure has been used to form composites which have greatly simplified the search for the best ceramics for anode applications. In the development of ceramic fuel electrodes for SOFC, high performance can only be achieved when a transition metal catalyst is added. Because of the high operating temperatures, deactivation of the metal catalyst by sintering and/or coking is a severe problem. In this thesis, two approaches aimed at mitigating metal catalyst deactivation iv which was achieved by: 1) designing a catalyst that is resistant to coking and sintering and 2) developing a new method for catalyst deposition, will be presented. The first approach involved synthesizing a self-regenerating, “smart” catalyst, in which Co, Cu, or Ni were inserted into the B-site of a perovskite oxide under oxidizing conditions and then brought back to the surface under reducing conditions. This restores lost surface area of sintered metal particles through an oxidation/reduction cycle. Results will be shown for each of the metals, as well as for Cu-Co mixed metal systems, which are found to exhibit good tolerance to carbon deposition and interesting catalytic properties. The second strategy involves depositing novel Pd@CeO2 core-shell nanostructure catalysts onto a substrate surface which had been chemically modified to anchor the nanoparticles. The catalyst deposited onto the chemically modified, hydrophobic surface is shown to be uniform and well dispersed, and exhibit excellent thermal stability to temperatures as high as 1373 K. Similar metal catalyst deposition method was also employed to access their suitability for use in SOFC anodes. v Table of Contents Chapter 1. Introduction 1 1.1 Motivation 1 1.2 Solid Oxide Fuel Cells (SOFCs) 2 1.2.1 SOFC Operating Principles 2 1.2.2 Three-Phase Boundary (TPB) 5 1.3 Materials for SOFC 5 1.3.1 Perovskite Materials 6 1.3.2 Cathode (air electrode) 7 1.3.3 Electrolyte 9 1.3.4 Interconnect 10 1.3.5 Anode (fuel electrode) 11 1.4 Ceramic Electrodes as Alternative Anode Materials 12 1.5 Approaches to Mitigate Metal Catalyst Deactivation 13 1.6 References 15 Chapter 2. Experimental Techniques 26 2.1 Materials Synthesis 26 2.1.1 Mixed Oxides 26 2.1.2 Pd@CeO2 Core-Shell Nanostructures 26 2.2 Fuel Cell Preparation 27 2.2.1 Tape Casting 28 2.2.2 Cell Assembly Sintering 30 vi 2.2.3 Cathode Preparation 30 2.2.4 Anode Preparation 31 2.2.5 Preparation for Testing 31 2.2.6 Advantages of the Infiltration Method over Traditional 31 Method 2.3 Cell Performance Measurements 33 2.3.1 V-i Polarization Curves 33 2.3.2 Electrochemical Impedance Spectroscopy 34 2.4 Composite Slabs 36 2.5 Surface Chemical Modification of Metal Oxide Powders or Planar 36 Supports 2.5.1 Liquid Silanization 36 2.5.2 Gas Silanization 37 2.5.3 Liquid Phosphonation 37 2.6 Materials Characterization Techniques 38 2.6.1 Electrical Conductivity Measurements (4 Point DC-Probe) 38 2.6.2 X-Ray Diffraction (XRD) 38 2.6.3 Scanning Electron Microscopy (SEM) 39 2.6.4 BET Surface Area Measurements
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