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Daf25thesispdf.Pdf (3.166Mb) Borohydride, a Next-Generation Material for Energy Storage and Conversion, and the First Description of a Borohydride / Dichromate Fuel Cell A Dissertation Presented to the Faculty of the Graduate School of Cornell University In Partial Fulfillment of the Requirements for the Degree of Doctor of Philosophy by David Alan Finkelstein August 2011 © 2011 David Alan Finkelstein Borohydride, a Next-Generation Material for Energy Storage and Conversion, and the First Description of a Borohydride / Dichromate Fuel Cell David Alan Finkelstein, Ph. D. Cornell University 2011 – Borohydride (BH 4 ), a promising new fuel for fuel cell applications, is rigorously analyzed and explored in the context of a membraneless, microfluidic fuel cell. Though MeOH – – and H 2 have been studied much more thoroughly than BH 4 , BH 4 possesses important – advantages relative to these more common fuels. Due to a faster reaction rate, BH 4 offers over 200 times the current density per mole achievable with MeOH. With a room temperature – solubility 90 times higher than H 2 at 3000 psi, BH 4 has a theoretical maximum current density – 170 times that of pressurized H2. BH 4 's main drawback is a hydrolytic decomposition to H2, which occurs in bulk solution and at Pt surfaces. We describe a low-potential (high voltage), hydrolysis-free oxidation mechanism at Pt, while hydrolysis-prone, low-voltage oxidation is – described for Au, in direct contrast to prevailing opinions in the literature. BH 4 oxidation is described for the first time, for modern literature, in nonaqueous solvents, where bulk hydrolysis – is eliminated, but oxidative activity detrimentally affected. To balance BH 4 's tremendous current, common oxidants alternative to O 2 are examined, and none found to be suitable. The high-voltage, side-reaction free reduction of cerium ammonium nitrate (CAN) is employed to develop a fuel cell with the highest Pt utilization yet recorded for a non-H2 fuel cell, and which exceeds the Pt utilization of a typical H 2 fuel cell by 50%. This is achieved at room temperature – with a fuel concentration of 0.15 M, which represents only 1% of BH 4 's solubility in aqueous 2– solution. From an array of unconventional fuel cell oxidants, dichromate (Cr 2O7 ) is characterized, and found to deliver an order of magnitude more current than CAN at a small cost – 2– to fuel cell voltage. Preliminary results indicate that a BH 4 / Cr 2O7 fuel cell may deliver five – times the power density of the BH 4 / CAN system. For the first time, poisoning mechanisms for – BH 4 at Pt and Au catalysts are described, and an in-situ cleaning method developed, which is – 2– demonstrated to operate in a BH 4 / Cr 2O7 fuel cell for >7 hours. Finally, oxidative activity for – 2– BH 4 and reductive activity for Cr 2O7 are demonstrated at catalysts of significantly lower cost – than Pt or Au, including Pd, Ag, and Ni, providing an important cost flexibility for the BH 4 / 2– Cr 2O7 fuel cell that is often unachievable for conventional H 2 / O 2 and MeOH fuel cells. Biographical Sketch David Finkelstein has worked and studied in the areas of alternative energy and environmental engineering for over 10 years. He received his B.S. in Biological and Environmental Engineering Technology and Biology from Cornell in 2002. For his undergraduate research, he designed a microbial biofilter for methane-producing, plug-flow digesters with Dr. Norman Scott and Dr. Jean Hunter. He also implemented a project in fluvial geomorphology for streambank restoration with Dr. Jose Lozano of the City of Ithaca Environmental Laboratories. His interests turned to energy exclusively, and he pursued microbial fuel cells for his first M.S. (Professional) in Industrial Microbiology at Michigan State with Dr. J. Gregory Zeikus, collaborating with Dr. Leonard Tender of the Naval Research Lab. He later worked in solar energy for his second M.S. in Biophysics by designing artificial proteins for Pt-free H 2 production, studying at the University of Pennsylvania with Dr. P. Leslie Dutton. Finally, desiring to work on nearer-term technologies, he joined the Cornell Fuel Cell Institute (CFCI), now the Energy Materials Center at Cornell (emc 2), to pursue membraneless, microfluidic fuel cells with Dr. Héctor Abruña in the Department of Chemistry, collaborating with Dr. Abraham Stroock of the Department of Chemical Engineering. In addition to his interests in alternative energy, David maintains a hobby of political awareness, for without the right governmental climate, energy technology becomes trivialized, rather than cultivated, and never effects the change intended by its designers. iii Dedication This Thesis is dedicated to Dr. Leonard Tender of the Naval Research Laboratory, known as "Lenny" not only to his friends, but to essentially everyone he's ever met. Lenny provides a kind and supportive environment to his research team, assisting those in need with what limited time he has, and treating everyone with the same respect he gives to the Congressional lawyers and military brass that provide much of his funding. He expects the best from his staff, but that's because he gives them his best every day, genuinely listening to their concerns and taking their suggestions, while dispensing expert advice in a stress-free atmosphere. Lenny is driven by a passion to do quality research that has an impact on society, and he insists, in his characteristic nonaggressive way, that his team members enjoy their time in the process. I am personally indebted to Lenny for promoting both my career as an energy scientist and my first paper, on which he served as a co-principal investigator. He helped to inspire my interest for electrochemistry and set a standard for how to treat the people that one depends on, which has been enormously helpful in working with the six undergraduate students that I have mentored during my Ph.D. program. iv Acknowledgments This work was supported by the Office of Basic Energy Sciences, Division of Materials Sciences, U.S. Department of Energy, under Grant DE-FG02-05ER46250. This work was additionally supported by the Cornell Center for Materials Research (CCMR) with funding from the Materials Research Science and Engineering Center program of the National Science Foundation (NSF) (cooperative agreement DMR 0520404). The NSF Research Education for Undergraduates program, administered through the CCMR, provided funding for Kenneth Hernandez-Burgos, David Jones, Claudia Rodriguez, Lori Sandberg, and David Watts, who each made significant contribution to the work presented. The research presented was performed in the laboratory of Prof. Héctor Abruña, with Prof. Abraham Stroock serving as a collaborator. Dr. Jamie Cohen, Dr. Nicolas Da Mota, Dr. Joseph Kirtland, and Corey Letcher provided key support and contribution, as noted in the relevant chapters. I would like to thank Prof. Abruña for providing an excellent research atmosphere. He regularly attracts top talent, and personalities, from around the world. At a time when I was disenchanted with research science, having completed two graduate programs with few publications to show for the effort, Prof. Abruña took a chance on me, and gave me the green light for my third endeavor in energy research. He has allowed me exceptional independence in steering my project, and with his guidance, I have learned a great deal about science management, from the art of grant writing to the politics of peer review. Should I continue my career in electrochemistry, I will owe much of its foundation to him. v Prof. Stroock has also played a critical role in my graduate studies. He provided endless support and enthusiasm for the project, acting on team concerns to continually improve the quality of our research, and translated industry goals into specific research objectives. Through his expertise in materials transport, he legitimized our efforts to develop a functional fuel cell. Though Prof. DiSalvo is one of the busiest professors in the Department of Chemistry and Chemical Biology, he has always made time to meet with students. He has provided me with a kind sounding board for new ideas, and encouraged me to consider the underlying chemical properties behind electrocatalysis. Through his efforts as a co-leader of intergroup meetings for the Cornell Fuel Cell Institute and its successor, the Energy Materials Center at Cornell, I have had the opportunity to meet with many of the leading experts in fuel cell and battery technology. I would also like to thank the many people at the Abruña lab who created a friendly and supportive atmosphere, which made each day at work that much more enjoyable and relaxing. Various lab members, such as Dr. Nicolas Da Mota and Dr. Yasuyuki Kiya, also taught me some of the advanced electrochemistry that later became integral to understanding and establishing unique fuel cell chemistries. I greatly appreciate the work put in by my many undergraduate students over the years, as their work at the bench freed my time to publish our findings and maintain our funding. vi Table of Contents Autobiography iii Dedication iv Acknowledgments v – Chapter 1: Introduction to BH 4 and Membraneless 1 (Laminar-Flow) Fuel Cells 1.1 Membraneless Fuel Cells 1 – 1.2 Employment of BH 4 in Fuel Cells 3 1.3 Summary of Chapter Contents 6 1.4 References 8 Chapter 2: Electroanalytical Methodology 9 2.1 Electrochemical Setup 9 2.2 Electrode Cleaning 11 2.3 Electrochemical Equations 13 2.4 References 20 Chapter 3: Rotating disk electrode (RDE) Investigation of 21 – – BH 4 and
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