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DEVELOPMENT of BATTERIES for IMPLANTABLE APPLICATIONS By DEVELOPMENT OF BATTERIES FOR IMPLANTABLE APPLICATIONS by BUSHAN KUMAR PURUSHOTHAMAN Submitted in partial fulfillment of the requirements For the degree of Doctor of Philosophy Dissertation Advisor: Prof. Jesse S. Wainright Department of Chemical Engineering CASE WESTERN RESERVE UNIVERSITY August, 2006 CASE WESTERN RESERVE UNIVERSITY SCHOOL OF GRADUATE STUDIES We hereby approve the dissertation of ______________________________________________________ candidate for the Ph.D. degree *. (signed)_______________________________________________ (chair of the committee) ________________________________________________ ________________________________________________ ________________________________________________ ________________________________________________ ________________________________________________ (date) _______________________ *We also certify that written approval has been obtained for any proprietary material contained therein. I dedicate the dissertation to my family members for their love and steadfast support to me at all times. I am grateful for their many sacrifices to make my life successful. iii TABLE OF CONTENTS Page Number List of Tables x List of Figures xiii Acknowledgements xxvi List of Symbols xxvii Abstract xxviii 1.0 Introduction 1 1.1 Background of Networked Neuroprosthetic System 1 1.2 Existing Rechargeable Battery Technologies 2 1.3 Overview of High Pressure Nickel-Hydrogen Batteries 4 1.3.1 Introduction 4 1.3.2 Cell Components and Electrochemistry involved 5 1.3.3 Nickel-Hydrogen Cell Construction 8 1.4 Proposed Research 12 1.5 Prior Work 12 1.6 Objective and Overview of this work 12 1.6.1 Primary Objective 13 1.3.3 Secondary Objective 14 Works Cited 14 2.0 Cycle Life Tests on Lithium Ion Batteries for Implantable Applications 16 2.1 Overview of Lithium Ion Batteries 16 2.2 Description of Li Ion Cell 17 2.3 Implantable Li Ion Batteries 18 2.4 Objective 19 2.5 Charging Protocol for Lithium Ion Batteries 19 2.6 Experimental Design 21 iv 2.6.1 Effect of Charge Rate on Cycle life Performance 23 2.6.2 Effect of Discharge Rate on Cycle Life Performance 32 2.6.3 Effect of Charge Voltage Cutoff on Cycle Life 36 Performance 2.6.4 Effect of DOD on Cycle Life Performance 37 2.6.4.1 Sony Lithium Ion Cells at 100 and 80% DOD 37 2.6.4.2 Wilson Greatbatch Lithium Ion Cells at 80 and 40 60% DOD 2.6.5 Effect of Temperature on Cycle Life Performance 41 2.6.6 Comparison of Sony, Wilson Greatbatch and Quallion 43 2.6.7 Comparison of Sony and WG at 80% DOD 48 2.7 Comparison of Implantable battery technologies 49 2.7.1 Cycle life of Quallion and WG at 60% DOD 49 2.7.2 Cycle Life of WG and Quallion at 100% DOD 52 2.6.3 Long term tests on WG and Quallion 52 2.8 Comparison of Charge Times for New and Used Quallion cells 54 2.9 Conclusions 61 Works Cited 62 3.0 Platinum Negative Electrode – Testing and Activation 65 3.1 Introduction – Platinum Electrode 65 3.2 Characterization of the ESNS Electrode in a Liquid Cell 67 Configuration 3.2.1 Hydrogen Evolution Reaction Kinetics 68 3.2.2 Electrochemical Impedance Spectroscopy 69 3.2.3 Potentiodynamics 73 3.2.4 Conclusions 75 3.3 Characterization of the ESNS Electrode in Double Negative Cell 75 Configuration 3.3.1 Testing of Fresh ESNS Electrodes 76 v 3.3.2 Conditioning of ESNS Electrodes with Cyclic 78 Voltammetry 3.3.3 Effect of Rest 81 3.3.4 Effect of soaking in KOH for days 82 3.4 Testing of Current Collectors 83 3.5 Testing of Separators 85 3.6 Conclusions 85 Works Cited 87 4.0 Testing of ‘D Cell’ Nickel Hydroxide Electrode 89 4.1 Estimation of Specific Capacity 89 4.2 Performance of D cell Electrode in Liquid Cell 89 4.2.1 Description of the Experimental Setup 89 4.2.2 Charge-Discharge Experiments 90 4.2.3 Impedance Analysis 90 4.3 Performance of the D cell Electrode in Nickel-Hydrogen Cell 93 4.4 Performance of the D cell Electrode in Series Cell 97 4.5 Conclusions 102 Works Cited 102 5.0 Fabrication and Formation of Nickel Hydroxide Electrode 103 5.1 Introduction 103 5.2 Existing Methods of Fabrication 103 5.2.1 Pasted Nickel Electrode 104 5.2.2 Plastic Bonded Electrode 104 5.2.3 Sintered Electrode 105 5.3 Fabrication Methodology 105 5.3.1 Substrate 105 5.3.2 Paste Formulation 106 5.3.3 Screen Printing 107 5.4 Formation of the Nickel hydroxide Electrode 109 vi 5.4.1 Overview of Reactions in the Nickel Hydroxide 110 Electrode 5.4.2 Overview of Electrochemical Voltage Spectroscopy 111 5.4.3 Mechanism of Formation 112 5.4.4 Effect of Incomplete Formation 117 5.4.5 Effect of Different Rates of Formation 121 5.4.6 Effect of Overcharging during Formation 123 5.4.6.1 No Overcharge during Formation 123 5.4.6.2 50% Overcharge during Formation 124 5.4.6.3 Comparison of No Overcharge and 50% 125 Overcharge 5.5 Characterization of Nickel Hydroxide Electrode 129 5.5.1 Effect of PVDF Content on Electrode Performance 129 5.5.2 Effect of Loading Density 135 5.5.3 Effect of Fine Ni 139 5.5.3.1 Electronic Conductivity Studies 139 5.5.3.2 Comparison of electrodes Containing 0% and 142 8.8% Ni 5.5.3.3 Comparison of Electrodes Containing 5.2% 147 and 8.7% PVDF in the Presence of Fine Ni 5.5.4 Effect of Pressing the Electrode 148 5.6 Other Methods of Fabrication 148 5.6.1 Mechanical Impregnation Using Spatula 148 5.6.2 Mechanical Impregnation Using Hot Press 150 5.7 Conclusions 151 Works Cited 152 6.0 Assembly and Testing of Low Pressure Nickel Hydrogen Battery 155 6.1 Description of Experimental Setup 155 6.2 Performance of the Ni-H2 Cell in Comparison to the Liquid Cell 157 6.3 Columetric Efficiency of the Ni-H2 Cell 162 vii 6.3.1 Effect of Depth of Charge on Columetric Efficiency 162 6.3.2 Effect of Rest Period on Columetric Efficiency – Self- 165 discharge 6.4 Pressure Data Analysis 169 6.4.1 Pressure Variations During Charge 171 6.4.2 Pressure Variations During the Rest Period 174 6.4.3 Self Discharge at Different Depths of Charge 177 6.4.4 Recombination in the Ni-H2 Cell During Charge and 178 Rest Period 6.4.5 Pressure Contributions – Self discharge and 180 Recombination 6.4.6 Efficiency Loss – Self Discharge and Recombination 180 6.5 Comparison of Efficiency Based on Charge Data and Pressure 183 Data 6.6 Ni-H2 Cell Tests – Below Atmospheric Pressure 183 6.7 Cycle Life Tests 185 6.8 Conclusions 190 7.0 Low Pressure Nickel-Hydrogen Battery with Metal Hydride 192 7.1 Metal hydrides for hydrogen storage 192 7.1.1 Metal Hydride – Advantages and Applications 192 7.1.2 Factors Affecting Cycle Life of Metal Hydride 193 Electrodes 7.1.3 Comparison of Metal Hydride in Ni-MH and Low 195 Pressure Ni-H2 Cell 7.2 Pressure Composition Isotherm of the Metal Hydride 197 7.3 Testing of Metal Hydride Exposed to Air 198 7.4 Testing of Metal Hydride Exposed to KOH Solution 199 7.5 Testing of Ni-H2 Battery with Metal Hydride 200 7.5.1 Columetric efficiency Based on Charge-Discharge Data 203 7.5.2 Pressure Variations During the Charge-Discharge Cycle 206 viii 7.5.3 Pressure Variations During Charge 207 7.5.4 Pressure Variations During Rest after Discharge 208 7.5.5 Pressure Variations During Rest after Charge 210 7.5.6 Correlation of Pressure Variations During Discharge to 212 Pressure Composition Isotherm – Fuel Gauging 7.5.7 Correlation of Pressure Variations During Charge to 216 Pressure Composition Isotherm – Fuel Gauging 7.5.8 Self discharge at Different Depth of Charge 218 7.5.9 Recombination During Charge and Rest 218 7.5.10 Prediction of State of Charge 219 7.6 Problems associated with Ni-H2 Battery 219 7.7 Conclusions 224 Works Cited 225 8.0 Conclusions and Recommendations for Future Work 228 8.1 Conclusions 228 8.2 Recommendations for Future Work 231 9.0 Bibliography 232 ix LIST OF TABLES Page Number Table 2.1: Comparison of Quallion and Wilson Greatbatch lithium ion cells. 19 Table 2.2: Description of Sony lithium ion cells subjected to different test 24 conditions. Table 2.3: Comparison of parameters and errors estimated by fitting the 30 =+ discharge capacity as a function of cycle life to equation Ckkcycled 12 for C and C/5 rate of charging. Table 2.4: Comparison of parameters and errors estimated by fitting the 46 =+ discharge capacity as a function of cycle life to equation Ckkcycled 12 for lithium ion cells of different manufacturers charged at C/5 rate and discharged at C rate. Table 2.5: Linear fit parameters and their error estimations of the end of 52 discharge voltage data. Wilson Greatbatch and Quallion lithium ion cells were charged and discharged at C rate to 60% DOD. Table 2.6: Linear fit parameters and their error estimations of the end of 54 discharge voltage data. Wilson Greatbatch and Quallion lithium ion cells were charged and discharged at C/5 and C/4 rate, respectively. Table 3.1: Impedance analysis in the potential range 0 to -0.5 V. 70 Table 3.2: Impedance analysis at in the potential range 0 to -20V. 72 x Table 3.3: Estimated parameters for fresh electrodes based on the linear fit 77 applied to the CV data. Table 3.4: Estimated parameters for fresh electrodes based on the linear fit 81 applied to the CV data.
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