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Anl-79-94 High-Performance Batteries for Stationary A+J- ANL-79-94 ANL-79-94 HIGH-PERFORMANCE BATTERIES FOR ELECTRIC-VEHICLE PROPULSION AND STATIONARY ENERGY STORAGE Progress Report for the Period October 1978-September 1979 1STR A A ARGONNE NATIONAL LABORATORY, ARGONNE, ILLINOIS Prepared for the U. S. DEPARTMENT OF ENERGY under Contract W-31-106-Eng-38 "- , A IS ,,UANIE Distribution Category: Energy Storage- -Electrochemical- Advanced Batteries (UC-94cb) ANL-79-94 ARGONNE NATIONAL LABORATORY 9700 South Cass Avenue Argonne, Illinois 60439 HIGH-PERFORMANCE BATTERIES FOR ELECTRIC-VEHICLE PROPULSION AND STATIONARY ENERGY STORAGE Progress Report for the Period October 1978-September 1979 D. L. Barney Director, Ad anced Battery Projects R. K. Steunenberg Manager, Lithium/Metal Sulfide Battery Program A. A. Chilenskas Manager, Advanced Battery Technology Development E. C. Gay Section Manager, Battery Engineering J. E. Battles Group Leader, Materials Development F. Hornstra Group Leader, Battery Charging Systems W. E. Miller Group Leader, Industrial Cell and Battery Testing D. R. VIssers Group Leader, Cell Chemistry M. F. Roche Group Leader, Calcium/Metal Sulfide Battery Development H. Shimotake Group Leader, Cell Development and Engineering R. Hudson Program Manager, Eagle-Picher Industries, Inc. B. A. Askew Program Manager, Gould Inc. S. Sudar Program Manager, Rockwell International DISCLAIMER by aapavy he Up'ted Gttarnraet. f ,I10,1OrIre awlr tt~nt>1va1 t '+of 1 Of Stain. Nytt'lhi.' Urtell Staley,y +fy ripy '" ayWVy ttw'.0 Mir ay . en'V"%. malhes ay tfortIM ' tay. Iaa'ay, y.yritOwa'tmpta'J a ayyak'Wb aM y .atlaylt. N WOhb'fty March 1980 As Ildhiv a alrrl tatam t,ttatatttf. sayattaa ytadaat -a aSA' yar~kltb.b t teaw W 11 thUat ts.sa *ul at nu 'U f pyralday OaO~fd hyt i tera'y. hsa. alipenv 551'.. aammt'Udt at datl aV ... 'a . r v bly trde 'wm.taidW"5rl tta(M1aur. WU051*5' hasn t nut 41^101, anysttatSW y a',Iy +tH d~ttW'bI ' ofat yhGSS .g$SAf t tl a'.n rr Mrtr/~lln eaat5 by1a Unles Slat.Gao59"55n a' atoany a~y h th*.The aUSS tan pattnS ylt h baa the Uld Slat iGa tnUlt oran y euby thea9o SAU"IfV state d 0 Previous Reports ANL-78-21 October----December 1977 ANL-78-45 January-March 1978 ANL-78-94 October 1977-September 1978 ANL-79-39 October 1978-March 1979 TABLE OF CONTENTS Page ABSTRACT. 1 SUMMARY . 1 I. INTRODUCTION . 12 II. INDUSTRIAL CONTRACTS . 16 A. Eagle-Picher Industries, Inc. 16 1. Cell Development for the Murk IA Program . 16 2. Cell Experiments . 22 3. Mark IA Battery Development. 25 4. MERADCOM 6-V Battery . 27 5. Quality Assurance. 30 B. Gould Inc. 31 1. Cell Component Development . 31 2. Electrode Development. 38 3. Cell Testing and Post-Test Analysis. 42 4. Post-Test Cell Examinations. 45 5. Design and Cost Study. 46 C. Rockwell International. 51 1. Electric-Vehicle Cells . 51 2. Ceramic Separator Development. 54 3. Design and Cost Study of 100 MW-hr Plant . 57 D. General Motors Research Laboratory. 61 E. Institute of Gas Technology (IGT) . 66 III. CELL AND BATTERY TESTING . 68 A. Testing of ANL Cells. 68 1. Negative-to-Positive Capacity Ratio. 68 2. Positive-Electrode Capacity Density. 68 3. Design or Materinl Modifications . 70 4. Alternative Seprator Materials. 71 5. Multiplate Cells . 71 iii TABLE OF CONTENTS (contd) Page B. Testing of Go-ld Cells at ANL. .... 72 C. Testing of Eagle-Picher Cells at ANL . 75 1. Cell Swelling . 75 2. Capacity Fading . ." 76 3. Power Improvement . 78 4. Driving Prof ile Tests . 79 5. Cell Failure Studies. 81 D. Battery Testing . .. 83 1. Small Mark IA Battery . 83 2. MERADCOM Module Te;t . 84 3. Mark IA Battery . 86 IV. CELL PERFORMANCE AND LIFETIME SUMMARY . .. 97 A. Status Cell Tests.. ....... 97 1. Bicell Tests...... ........ 97 2. Multiplate Cell Tests . 97 B. Electrical Performance. ....... .... 98 C. Failure Mechanisms .... ........ 10) 1. Post-Test Examinations. 100 2. Failure Analysis of Mark IA Module D-001. 102 V. CELL DEVELOPMENT . .. 107 A. Cell Modeling Studies. 107 1. Macro-Modeling Studies. 107 2. Micro-Modeling Studies. 109 B. Reference Electrode System . 121 1. Development . 121 2. Electrode Potential Measuring Techniques. 124 3. Applications. 127 C. Cell Opt j iizatlon Studies. ................ 129 1. Electrolyte Alternative . .0 . 129 Ionic Conductance of Ceramic Separators . 130 3. Alternative Positive-Electrode Additive . 134 4. Electrode Discharge Processes...... 134 I, TABLE OF CONTENTS (contd) Page VI. MATERIALS AND COMPONENTS DEVELJPMENT..... ... 138 A. Electrode Development. .138 1. Li-Al Electrode Studies . 138 2. FeS Electrode Studies . 1.42 3. FeS2 Electrode Studies. 148 4. Physical Properties of Electrode Materials. 151 B. Separator Developmen L. .154 1. Bornn Nitride Felt Separators . 156 2. Porous, Sintered Ceramic Separators . 157 3. Magnesium Oxide Powder Separators . 157 4. Corrosion Rates of Candidate Ceramics for Cell Components.... ........ 157 C. Current Collector Development. .159 1. Current Collector Materials for FL.: Electrodes . 159 2. Resistivity Measurements of Candidate Collector Materials . 161 3. Ceramics for Current Collectors in FeS, Electrodes 162 VII. SYSTEMS DESIGN AND COST ANALYSIS. 172 A. Conceptual Designs of SLS Batteries. 172 B. Cost Analysis for Li/MS Cells . .. 173 C. Design and Development of In-Vehicle Testing Equipment. 176 1. Instrumentation for In-Vehicle Tes ting. 176 2. In-Vehicle Testing. 183 D. Desi6L and Development of Battery Sub-System . .. 188 1. Thermal Management. 188 2. Charger........ ... .. .. .... 192 VIII. CALCIUM/METAL SULFIDE BATTERY DEVELOPMENT... ... 198 A. Electrolyte Development. 198 1. Solubility Studie ................... 198 V TABLE OF CONTENTS (contd) Page 2. Vaporization of Sulfur. 200 3. Density....... .. .. 201 4. Conductivity. 202 5. Quaternary Salt Phases. 202 B. Positive Electrode Development 203 1. Cell Studies. 203 2. Cyclic Voltammetry of Metal Disulf ides 205 C. Large Cell Exploratory Studies 209 APPENDIX A. 217 APPENDIX B. 224 AFPENDIX C. 231 APPENDIX D. 238 APPENDIX E. ......................... 243 vi HIGH-PERFORMANCE BATTERIES >. ELECTRIC-VEHICLE PROPULSION AND STATIONARY ENERGY STORAGE Progress Report for the Period October 1978-September 1979 ABSTRACT This report covers the research, development, and management activities of the programs at Argonne National Laboratory (ANL) and at contractors' laboratories on high-temperature batteries during the period October 1978-September 1979. These batteries are being developed for electric-vehicle propulsion and for stationary energy-storage applications. The present cells, which operate at 400-500 C, are of a vertically oriented, pris- matic design with one or more inner positive electrodes of FeS or FeS2 , facing negative electrodes of lithium-aluminum or lithium-silicon alloy, and molten LiCl-KC1 electrolyte. During this reporting period, cell and battery development work has continued at ANL and contractors' laboratories. A 40 kW-hr electric-vehicle battery (designated Mark IA) was fabricated and delivered to ANL for testing. During the initial heal-up, one of the two modules failed due to a short circuit. A failure analysis was conducted and the Mark IA program com- pleted. Development work on the next electric-vehicle battery (Mark II) was initiated at Eagle-Picher Industries, Inc. and Gould Inc. Work on stationary energy-storage batteries during this period has consisted primarily of conceptual design studies. SUMMIIARY Industrial Contracts Most of the cell and battery development, design, and fabrication was subcontracted to two industrial firms--Eagle-Picher Industries, Inc. and Gould Inc. Eagle-Picher. In February 1978, Eagle-Picher was contracted to design, develop, and fabricate a 40 kW-hr lithium/iron sulfide battery (Mark IA) for testing in an electric van. In the cell development phase, Eagle-Picher fabricated about 130 multiplate Li-Al/FeS cells (assembled charged) of vary- ing designs, which were tested at their own laboratories or ANL. In general, tnese cells consisted of three positive and four negative electrodes, BN fabric separators, and LiCl-KC1 eutectic electrolyte. After testing of these developmental cells had been completed, the final design for the Mark IA cell was selected and testing indicated that they would meet our performance goals. In the course of cell development, performance data were obtained for individually cycled cells, but virtually no cell interaction data were 1 2 available for battery design. To this end, a cell-force test apparatus was designed and fabricated to determine the Mark IA cell characteristics when fully restrained; these data were used to define the maximum cell force that had to be restrained by the battery hardware during testing. In safety tests, the Budd Technical Center (under contract to Eagle-Picher) ruptured charged Mark IA cells at operating temperature, exposing the contents to room-tempera- ture air, by two methods: pressing the cell until rupture and dropping a 50 kg weight onto the cell at 48 km/hr (30 mph). No signs of fire or chemical reactions were observed after rupture of these cells. In conjunction with the cell development phase of the Mark IA program, Eagle-Picher constructed a small (6 V, 2 kW-hr) module consisting of five Mark IA cells connected in series and housed in a metal (Inconel 718) case insulated with vacuum-foil insulation. At Eagle-Picher, this module was operated for 10 cycles and exhibited acceptable performance. During cycles 3 and 5, the module was subjected to vibrations equivalent to 2.3 years of vehicle operation; the performance did not appear to be affected by the vibrations. Upon completion of these preliminary tests, the module was sent to ANL where it was used to test a charger/equalizer unit developed at ANL. Another small (6 V, 4 kW-hr) module was fabricated by eagle-Picher for perfor- mance testing at ANL. This module was fabricated for the U. S. Army to determine the viability of this system for fork-lift applications and con- sisted of five parallel connected pairs of Mark IA cells.
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