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Solid-State Sodium Batteries Using Polymer Electrolytes and Sodium Intercalation Electrode Materials

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Solid-State Sodium Batteries Using Polymer Electrolytes and Sodium Intercalation Electrode Materials LBNL-39127 UC-404 ERNEST ORLANDO LAWRENCE IBERKELEY NATIONAL LABORATORY Solid-State Sodium Batteries Using Polymer Electrolytes and Sodium Intercalation Electrode Materials Y. Ma Materials Sciences Division August 1996 Ph.D. Thesis ·-- _,-_ ... .!, ·.- - '- l ,. •. ...;;. ~-:. '(. ' -~ .. , .., - ' - ·-. ,,_-; l zCD r- 0 1 0 w '0 10 '< ~ [\)..... DISCLAIMER This document was prepared as an account of work sponsored by the United States Government. While this document is believed to contain correct information, neither the United States Government nor any agency thereof, nor the Regents of the University of California, nor any of their employees, makes any warranty, express or implied, or assumes any legal responsibility for the accuracy, completeness, or usefulness of any information, apparatus, product, or process disclosed, or represents that its use would not infringe privately owned rights. Reference herein to any specific commercial product, process, or service by its trade name, trademark, manufacturer, or otherwise, does not necessarily constitute or imply its endorsement, recommendation, or favoring by the United States Government or any agency thereof, or the Regents of the University of California. The views and opinions of authors expressed herein do not necessarily state or reflect those of the United States Government or any agency thereof or the Regents of the University of California. LBNL--39127 Solid-State Sodium Batteries Using Polymer Electrolytes and Sodium Intercalation Electrode Materials YanpingMa (Ph.D. Thesis) Department ofMaterials Science and Mineral Engineering University of California, Berkeley and Materials Sciences Division Lawrence Berkeley National Laboratory University of California Berkeley, CA 94720-1760 Fall, 1996 Work supported by the Director, Office of Energy Research, Office of Basic Energy Sciences, Materials Sciences Division of the U.S. Department of Energy under Contract No. DE-AC03-76SF00098. Solid-State Sodium Batteries Using Polymer Electrolytes and Sodium Intercalation Electrode Materials By YanpingMa · B.E. (Tsinghua University) 1986 M.Eng. (Tsinghua University) 1989 DISSERTATION Submitted in partial satisfaction of the requirements for the degree of DOCTOR OF PIDLOSOPHY m ENGINEERING MATERIALS SCIENCE AND MINERAL ENGINEERING in the GRADUATE DIVISION of the UNIVERSITY of CALIFORNIA, BERKELEY Committee in Charge: Professor Lutgard C. De Jonghe Professor Alan W. Searcy Professor John Newman Fall, 1996 ABSTRACT Solid-State Sodium Batteries Using Polymer Electrolytes and Sodium Intercalation Electrode Materials By YanpingMa Doctor of Philosophy in Materials Science and Mineral Engineering University of California, Berkeley Professor Lutgard C. De Jonghe, Chair Solid-state sodium cells using polymer electrolytes (polyethylene oxide mixed with sodium trifluoromethanesulfonate: PEOnNaCF3S03) and sodium cobalt oxide positive electrodes are characterized in terms of discharge and charge characteristics~ rate / capability, cycle life, and energy and power densities. The experimental results are the best ever reported in the literature for sodium/polymer cells. The P2 phase NaxCo02 can reversibly intercalate sodium in the range of x = 0.3 to 0.9, giving a theoretical specific energy of 440 Whlkg and energy density of 1600 Wh/1. Over one hundred cycles to 60% depth of discharge have been obtained at 0.5 rnA/cm2 (C/lh). Experiments show that the electrolyte/Na interface is stable and is not the limiting factor to cell cycle life. Nao.1Co02 composite electrodes containing various amounts of carbon black additive are investigated. The electronic conductivity of these electrodes is found to be dominated by the volume fraction of carbon. The additive is also critical to cell cycle life. The transport properties of polymer electrolytes are the critical factors for performance. These properties (the ionic conductivity, salt diffusion coefficient, and ion 1 transference number) are measured for the PEOnNaCF3S03 system over a wide range of concentrations at 85°C. The ionic conductivity and the salt diffusion coefficient are measured using the ac-impedance technique and the restricted-diffusion method, respectively. A novel method to measure the ion transference number is developed and used in the present study. This method is based on de polarization experiments in combination with concentration cell measurements, and is theoretically rigorous for any I binary electrolyte and also experimentally simple. The thermodynamic factor (a factor that is related to the mean activity coefficient) of the electrolytes is determined, as well, using this method. All the three tran~port properties of the PEOnNaCF3S03 system are very salt-concentration dependent. The ionic conductivity exhibits a maximum at about n = 20. The transference number, diffusion coefficient, and thermodynamic factor all vary with salt concentration in a similar fashion, decreasing as the concentration increases, except for a local maximum. These results verify that polymer electrolytes cannot be treated as ideal solutions. The measured transport-property values are used to analyze and optimize the electrolytes by computer simulation and also cell testing. Salt precipitation is believed to be the rate limiting process for cells using highly concentrated solutions, as a result of lower values of these properties, while salt depletion is the limiting factor when a dilute solution is used. Moderately concentrated solutions (about n = 20) are found to have the optimum rate capability for the PEOnNaCF3S03 system. 2 TABLE OF CONTENTS CHAPTER 1 INTRODUCTION 1 PART I SOLID STATE RECHARGEABLE SODIUMPOLYMERBATTERIES 12 13 2. 1 Introduction 13 2.2 Experimental 15 2.3 Results and Discussion 17 2.3 .1 Charge and Discharge Characteristics 17 2.3 .2 Cycling Results 19 2.3.3. Four Probe DC Experiments 23 2.3.4 Power and Energy Density Calculations 26 2.3.5 Comparison with Other Sodium Systems 27 2.4 Conclusions 33 CHAPTER 3 Nao.1Co02 CO:MPOSITE ELECTRODES 34 3.1 Introduction 34 3.2 Experimental 35 3.3 Conductivity of the Nao.1Co02 Electrodes 37 3 .4 Charge and Discharge Characteristics 3 8 3.5 Conclusions 40 ( References for Part'I 42 Figure Captions for Part I 4 7 Figures for Part I 51 PART II SOLID STATEPOLYMERELECTROLYTES 73 ) CHAPTER4 TRANSPORT PROPERTIES OFPOLYMERELECTROLYTES 74 4.1 Introduction 74 lll 4.2 A Novel Method to Measure the Transference Number 77 v 4.3 Experimental 83 4.4 Results and Discussion 87 4.4.1 Ionic Conductivity 87 4.4.2 Salt Diffusion Coefficient 88 4.4.3 Ion Transference Number and Thermodynamic Factor 90 4.4.4 Comparison of the Novel Method to Other Methods 96 4.5 Speciation 101 4.6 Conclusions 105 List of Symbols 106 CHAPTER 5 ELECTROLYTE OPTIMIZATION 110 5.1 Introduction 110 5.2 Experimental Ill 5.3 Results and Discussion 112 5.4 Conclusions 118 References for Part II 120 Figure Captions for Part II 124 Figures for Part II 127 CHAPTER 6 CONCLUSIONS 144 IV To my parents, and my daughter Emily v Acknowledgments I wish to express my acknowledgment to Professor Lutgard C. De Jonghe for his ·valuable guidance. I also gratefully thank Dr. Marca M. Doeff for her valuable assistance, proofreading this thesis, and friendship. Special appreciation goes to Marc Doyle in the Department of Chemical Engineering at U.C. Berkeley for his major contribution in the development of transference number theory, computer simulations, and valuable discussion. Thanks also ·go to Professor John Newman for his contribution in the development of transference number theory. I gratefully acknowledge Professor Alan W. Searcy and Professor John Newman for reviewing this thesis and their valuable comments. I wish to express my appreciation to Dr. Carl M. Lampert for his financial support during the transition period to my Ph. D. program and his valued friendship. It is wish pleasure that I express my gratitude to all the friendly members of my research group. Special thanks go to Steve Visco, Mark Sixta, Marianna Niu, Mani Gopal, and Kazu Noda for the help they gave for this study. I am most grateful to my dear husband, Joe, for his constant love and support, and to my lovely daughter, Emily, for the wonderful time and joy with her. Vl Chapter 1 Introduction In recent years, consumer demand for electronic products such as portable computers, cellular phones, and video camcorders as well as environmental interests in promoting electric-powered vehicles have heralded the call for more advanced batteries. The criteria for superior batteries for these applications are high energy and/or high power density and long cycle lives. A great deal of attention has been given to lithium 1 batteries · because lithium has an extremely high charge capacity and very negative electrode potential. Alongside efforts to develop lithium batteries, there has also been exploration of similar systems that substitute lithium with other alkali metals or even divalent metals. Among the various proposed alternatives to lithium cells, the sodium battery is the most attractive. Sodium has a reasonably low equivalent weight and very negative electrode potential. More importantly, it is readily available and inexpensive. In addition, sodium ion conductors tend to have slightly higher ionic conductivity than their lithium analogues. Sodium, unlike lithium, does not form alloys with aluminum, making it feasible to use aluminum as current collectors in place of the heavier and more expensive nickel used in lithium cells. Though sodium has a lower charge capacity and less negative
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