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COO-2990-6 Distribution Category UC-94A COO-2990-6 Distribution Category UC-94a INVESTIGATION OF METAL FLUORIDE THERMAL ENERGY STORAGE MATERIALS AVAILABILITY, COST AND CHEMISTRY FINAL REPORT J. L. EICHELBERGER - NOTICE- This report was prepared as an account of work sponsored by the United States Government. Neither the United States nor the United States Energy Research and Development Administration, nor any of their employees, nor any of their contractors, subcontractor*, or their employees, makes any DECEMBER, 1976 warranty, express or implied, or assumes any legal liability or 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. CONTRACT NO. EY-76-C-02-2990*000 PREPARED FOR ENERGY RESEARCH AND DEVELOPMENT ADMINISTRATION OFFICE OF CONSERVATION DIVISION OF ENERGY STORAGE SYSTEMS PENNWALT CORPORATION TECHNOLOGICAL CENTER KING OF PRUSSIA, PENNSYLVANIA 19406 rSSTRIBOTION QF THIS DOCUMENT IS UNLIMITED DISCLAIMER This report was prepared as an account of work sponsored by an agency of the United States Government. Neither the United States Government nor any agency Thereof, nor any of their employees, makes any warranty, express or implied, or assumes any legal liability or 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 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. The views and opinions of authors expressed herein do not necessarily state or reflect those of the United States Government or any agency thereof. DISCLAIMER Portions of this document may be illegible in electronic image products. Images are produced from the best available original document. FOREWORD This report was prepared by Pennwalt Corporation, King Of Prussia, Pennsylvania, under U.S. Energy Research and ^Development Administration Contract EY-76-C-02-2990*000, formerly E(ll-l)-2990. The contract was issued by Harold N. Miller, Director, Chicago Contracts Management Office. Technical monitoring was begun by C. J. Swet, Thermal Energy Storage Program Manager of the Division of Conservation Research and Develop• ment, and was completed by William Masica and Joseph Joyce of the NASA-Lewis Research Center. This report covers the work carried out during the period July 15, 1976 - December 15, 1976 and was submitted by the author in December, 1976. li ACKNOWLEDGEMENTS In addition to the King of Prussia Technological Center of Pennwalt Corporation, the Ozark-Mahoning Division of Penn• walt, Tulsa, Oklahoma, made significant contributions to the performance of this contract. The most active participants assisting the principal investigator were Dr. Hyman Gillman and Mr. Fred Loomis of the Technological Center, and Dr. Charles Lindah.l, Dr. Dayal Meshri, and Mr. Charles Ramming of Ozark-Mahoning. 111 ABSTRACT Storage of thermal energy in the 400-1000°C range is attracting increasing consideration for use in solar power, central power, vehicular, and commercial process systems. This study investigates the practicality of using metal fluorides as the heat storage medium. The projected avail• ability of metal fluorides has been studied and is shown to be adequate for widespread thermal storage use. Costs are projected and discussed in relation to thermal energy storage applications. Phase diagrams, heats of fusion, heat capacities, vapor pressures, toxicity, stability, volume changes, thermal conductivities, fusion kinetics, corrosion, and container materials of construction for a wide range of fluorides have been examined. Analyses of these data in consideration of thermal energy storage requirements have resulted in selection of the most cost- effective fluoride or fluoride mixture for each of 23 temperature increments between 400 and 1000°C. Thermo- physical properties of these 23 materials are presented. Comparison of fluoride with non-fluoride materials shows that the fluorides are suitable candidates for high temperature applications on the bases of cost, heat capacity/unit volume, heat capacity/unit weight, corrosive properties, and availability. iv TABLE OF CONTENTS Page I. EXECUTIVE SUMMARY 1 Foreword 1 Metal Fluoride Availability 2 Metal Fluoride Costs 6 Metal Fluoride Chemistry 8 Major Study Conclusions 13 Recommendations 13 II. INTRODUCTION 14 III. APPLICATIONS 17 IV. AVAILABILITY 21 A. Fluorine Supply and Demand 22 B. Fluorine Occurrence and Geology 24 C. Calcium Fluoride Supply 27 1. World Reserves and Resources 27 2. U.S. Reserves and Resources 35 D. Fluosilicic Acid Supply 51 E. Other Fluorine Sources 69 F. Fluorine Demand 71 1. Fluorine Demand - Steel Production 75 2. Fluorine Demand - Aluminum Production 77 3. Fluorine Demand - Fluorocarbon Production 80 4. Fluorine Demand - Other Applications 83 G. Future Trends of Fluorine Supply and Demand 86 1. Demand 86 2. Supply 86 H. Supply - Demand of Metals 93 I. Supply - Demand of Metal Fluorides 105 J. Supply - Requirements of Metal Fluorides for 106 Heat Storage v TABLE OF CONTENTS (Continued) Page V. METAL FLUORIDE COSTS 108 A. Current Costs 108 B. Future Costs .115 C. Non-Accountable Costs 126 VI. CHEMISTRY EVALUATION 128 A. Classification and Data Quality 128 B. Metal Fluoride Synthesis 130 C. Purification 143 D. Vapor Pressure and Thermal Stability 146 E. Hydrolytic Stability 153 F. Corrosion 154 G. Melting Points and Phase Diagrams 163 H. Heat Contents 166 1. Heat of Fusion 167 2. Heat of Transition 175 3. Heat Capacity and Sensible Heat 175 I. Volume Changes and Density 186 J. Viscosity 190 K. Thermal Conductivity 193 L. Supercooling 199 M. Selected Fluoride Compositions 200 VII. EXPERIMENTAL 213 VIII. SAFETY 214 IX. RECOMMENDATIONS 216 X. REFERENCES 218 XI. APPENDIX VI TABLE OF TABLES Page I. Applications for Heat Storage 18 II. Fluorine Minerals 25 III. World Production and Reserves of Calcium Fluoride 28 IV. States of Mexico in Which Major Fluorspar Deposits Occur 32 V. Mexican Producers of Fluorspar 36 VI. Fluorspar reserves and resources in the U.S. by States 1974 37 VII. Domestic Fluorspar Producers by State 41 VIII. Some Companies Involved in Phosphate Production 53 IX. Some of the Companies Involved in Fluosilicic Acid Recovery and Conversion 66 X. Partial List of Inorganic Chemicals Containing Fluorine 85 XI. United States Projections and Forecasts for Fluorine by End Use, 1973 and 2000 87 XII. Summary of Forecasts of U.S. and Rest of World fluorine Demand, 1974-2000 88 XIII. Fluorine Supply Potential From The Phosphate Industry 91 XIV. Abundance, Mass, Reserves, and Resources of Some Metals in the Earth's Crust and in the United States Crust 95 XV. Abundance of Some Elements in the Earth's Crust 96 XVI. Production of Minerals (Metal Content) in 1974 99 XVII. Potential U.S. Resources of Some Important Mineral Commodities, in Relation to Minimum Anticipated Cumulative Demand to Year 2000 A.D. .100 XVIII. Supply Forecasts for Selected Minerals Based on Proven World Reserves 102 XIX. Prices and Estimated Production Costs of Fluoride Compound s 109 XX. Prices of Starting Materials for Metal Fluorides 111 XXI. Estimated Current Prices of Metal Fluoride Compounds 112 XXIa. Estimated Future Production Costs and Prices of Metal Fluorides 116 XXII. Vapor Pressure of Fluoride Salts 147 XXIII. Melting Points of Some Aluminum Fluoride Compositions 151 vn TABLE OF TABLES (Continued) Page XXIV. Gibbs Free Energies of Selected Fluorides 155 XXV. Fluoride-Metal Corrosion Experiments , 160 XXVI. Heats of Fusion of Fluoride Salts 168 XXVII. Heats of Fusion of Alkali and Alkaline Earth Fluorides 173 XXVIII. Heats of Transition of Fluoride Salts 177 XXIX. Thermodynamic Equations For Sodium Fluoride 178 XXX. Specific Heat and Heat Content Functions of Selected Metal Fluorides 180 XXXI. Heat Contents of Selected Metal Fluorides 182 XXXII. Densities and Volume Changes of Fluoride Salts 187 XXXIII. Viscosity of Fluoride Salts 191 XXXIV. Thermal Conductivity of Fluoride Salts 194 XXXV. Melting Points of Selected Metal Fluoride Salts 202 XXXVI. Selected Metal Fluoride Salts 207 viii TABLE OF FIGURES Page I. Metal Fluoride Selection Criteria 16 II. Relationships Among Sources of Supply and Demand for Fluorine - 23 III. CaF2 World Production 29 IV. CaF_ Known World Reserve 30 V. Mexico Fluorspar Production 33 VI. Canada Fluorspar Production 34 VII. Fluorspar in Canada, 1972 38 VIII. CaF2 Known U.S. Reserves 40 IX. CaF- U.S. Production Finished (All Grades) 44 X. U.S. Stocks : Mine 46 XI. CaF2 (97%) U.S. Stockpile 47 XII. U.S. Imports 48 XIII. U.S. Imports by Country of Origin 49 XIV. U.S. Fluorspar Equivalent From H2SiF6 64 XV. U.S. Fluorspar Consumption (All Grades) 73 XVI. U.S. Fluorspar Consumption and Imports 74 XVII. Historical Demand and Trend Projections of Fluorine Used in Steel Production 76 XVIII. Fluorine Values in the Aluminum Industry 79 XIX. Projections of Fluorine Use in the Aluminum Industry 81 XX. Historical Demand and Trend Predictions of Fluorine Used in Chemical Production 82 XXI. Historical Trend Projection of Fluorine Use in the Ceramic Industry 84 XXII. Fluorine Demand Projection 89 XXIIa. Change in World Proved Reserves 1950-70 103 XXIII. 1975 Imports Percentage of Minerals and Metals U.S. Consumption 104 XXIV. Time-Price Relationship for Fluorine 119 XXV. The Enthalpy and Enthalpy of Fusion of LiAlF , Na,AlF and K A1F fi° 176 j 6c 02. 6C XXVI. Heat Contents Above 298.16°K 183 ix TABLE OF FIGURES (Cont'd) Page XXVII. Enthalpy Curve, H° - H° _ _5 in kcal/mole for NaMgF3 * 184 XXVTII. Enthalpy Curve, Hi, - H° Q 15, in kcal/mole, for (0.782NaF + 0.21MgF2) 184 XXIX. Enthalpy Increments H - H2gQ ., _ and Enthalpy of Fusion of the Eutectic Mixture 21.8 mole % Na-AlFg + 78.2 mole % at 1162°K 185 XXX. Lithium Fluoride Thermal Conductivity Variation with Temperature 197 XXXI.
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