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THE PHYSICAL CHEMISTRY of METALS in THEIR MOLTEN HALIDES THESIS Presented for the Degree of DOCTOR of PHILOSOPHY in the UNIVERSI

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THE PHYSICAL CHEMISTRY of METALS in THEIR MOLTEN HALIDES THESIS Presented for the Degree of DOCTOR of PHILOSOPHY in the UNIVERSI THE PHYSICAL CHEMISTRY OF METALS IN THEIR MOLTEN HALIDES THESIS presented for the degree of DOCTOR OF PHILOSOPHY in the UNIVERSITY OF LONDON By Lars-Ingvar Staffansson, Bergsingenjor, (Stockholm). London, December 1959, ABSTRACT The phase diagrams of the systems calcium- calcium chloride, calcium-calcium bromide and calcium- calcium iodide have been established by solubility measurements and differential thermal analysis. Each of the systems was found to have a eutectic a mono- tectic and a large miscibility gap. The eutectics are 3.3, 3.2 and 6.8 mole % calcium respectively, and the corresponding temperatures are 763, 728 and 760°C. The monotectics are at 99.5, 99.6 and 99.7 mole % calcium respectively and the corresponding temperatures are 826, 828 and 831°C. The consolute points are at 1338, 1335 and 1380°C and the corresponding compositions are 62, 64 and 74 mole % calcium. Discrepancies between this and previous work are mainly attributed to composition changes of the phases during quenching. A method has been developed that overcomes this difficulty. The depression of the freezing point of strontium by strontium chloride has also been determined. From the results of this work a model for the mutal solubility of metalS and their molten halides has been suggested. CONTENTS Page CHAPTER 1: INTRODUCTION 1 1.1 General Introduction 1 1.2 Relevant previous work on metal-molten salts. 4 1.2.1 General 4 1.2.2 Alkaline earth metal-metal halide systems. 12 CHAPTER 2: EXPERIMENTAL 24 2.1 Programme 24 2.2 Preparation and purity of materials 25 2.2.1 Calcium 25 2.2.2 Strontium 26 2.2.3 Calcium Chloride 26 2.2.4 Calcium Bromide 28 2.2.5 Calcium Iodide 28 2.2.6 Strontium Chloride 29 2.2.7 Pure Iron 30 2.2.8 Gases 31 2.3 Dry-box. 32 2.4 Solubility measurements 46 2.4.1 Furnace assembly 46 2.4.2 Gas analysis apparatus 50 2.4.3 Initial experiments 53 Pau_ 2.4.4 Segregation 59 2.4.5 Modified programme 64 2.4.6 Development of new method 65 2.4.7 Experimental procedure. 71 2.5 Differential thermal analysis. 76 2.5.1 The principle of the method 76 2.5.2 Initial experiments 78 2.5.3 Crucibles 80 2.5.4 Furnace and differential analysis assembly. 83 2.5.5 Experimental procedure 93 CHAPTER 3: RESULTS 99 3.1 Description 99 3.1.1 The Calcium-Calcium Chloride system. 99 3.1.1.1 Solubility measurements 99 3.1.1.2 Differential thermal analysis 102 3.1.2 The Calcium-Calcium Bromide system. 107 3.1.2.1 Solubility measurements. 107 3.1.2.2 Differential thermal analysis 107 3.1.3 The Calciuri-Calcium Iodide system 111 3.1.3.1 Solubility measurements 111 3.1.3.2 Differential thermal analysis 111 Page 3.1.4 The Strontium-Strontium Chloride system 114 3.1.4.1 Solubility measurements 114 3.1.4.2 Differential thermal analysis 115 3.2 Errors 119 3.2.1 Errors in the solubility measurements 119 3.2.1.1 Temperature measurements 119 3.2.1.2 Weighing 120 3.2.1.3 Gas analysis 120 3.2.1.4 Other errors. 120 3.2.2 Errors in the differential thermal analysis 121 3.2.2.1 Temperature measurements 121 3.2.2.2 Weighing 121 3.2.2.3 Other errors 121 3.3 Derived data 123 3.3.1 The heat of fusion of the investigated salts123 - 3.3.2 The monotectic compositions in the Ca Can2' 126 - Ca-CaBr2 and Ca CaI2 systems. nIAPTER 4: DISCUSSION 128 4.1 Comparison with previous work 12.8 4.2 Interpretation of the results 136 4.3 The nature of metal-molten halide solutions 142 ACKNOWLEDGMENTS 149 REFERENCES 150 LIST OF FIGURES Fig. no. Page 1. Phase diagram of the system Ca/CaF2. 15 2. Dry-box. 34 3. Glove port for dry-box. 35 4. Purification train for dry-box. 38 5. Equilibration furnace. 4.7 6. Gas-analysis apparatus. 51 7. Preliminary results in system Ca/CaBr2, 55 8. Photograph of section of quenched crucible. 60 9. Photograph of section of quenched crucible. 62 10. Crucibles for solubility measurements. 70 11. Glass envelope for premelting of salts. 73 12. Thermocouples for D.T.A. 77 13. Crucibles for D.T.A. 81 Y,-.1 Wilson seal. 86 15. Crucible arrangement for D.T.A. 87, Biasing circuit. 91 17. Temperature and differential curves. 97 18. Solubility versus tine in the system Ca/CaC12. 101 19. Phase diagram of the system Ca/CaC12. 106 20. Phase diagram of the system Ca/CaBr2 110 21. Phase diagram of the system Ca/CaI2. 112 22. Depression of freezing point of SrCl2 by Sr. 118 23. Depression of freezing point of Ca versus anion radius. 138 24. Electronegativity of anion versus consolute 141 composition. CHAPTER 1 1. INTRODUCTION 1,.1 General Introduction. Molten salts have long been of importance for the electrochemical production of the alkali and alkaline earth metals and aluminium. In recent years the importance of the fused salts has increased with the interest in metals such as titanium, molybdenum, beryllium, zirconium, thorium and uranium. The rapid progress in the field of nuclear power generation is the main reason for the sudden great demand for these metals. The metals are produced either by fused salt electrolysis or by reduction of their halides or oxides with either 1.2.3. sodium, magnesium or calcium In the reduction processes the salts are either reaction products or added deliberately to act as a flux. The development of these methods has been largely empirical. Much funda- mental research is therefore needed for a fuller understanding of the principles underlying these processes. If e.g. uranium is produced by reduction of uranium tetra- chloride with calcium according to the reaction UC1 + 2Ca -> U + 2CaC12 the activities of the calcium and the calcium chloride will be influenced by their mutual solubilities. A knowledge of the interaction between the calcium and its chloride in the 2. temperature region where the reaction occurs is there- fore important for the understanding of this reduction process. The solubility of metals in their fused salts is also of interest from the point of view of current efficiency in electrolysis. The current efficiency is often rather low in these fused salt electrolysEs and it was at one time thought that Faraday's law was not valid for these processes. However, work by Helfenstein4 b.nd Lorenz5'6 showed that this assumption was wrong and that 100% efficiency could be obtained if certain precautions were taken. The main reason for the low yield is that metal produced at the cathode dissolves in the salt and migrates to the anode or to the surface of the bath where it reacts. Even a very small solubility of the metal can thus cause great losses if stirring and convection currents allow the dissolved metal to react at the bath surface or the anode. To obtain further information for the theoretical background to processes such as those mentioned above, as well as to increase our knowledge of the nature of the solutions of metals in molten halides, research on metal-molten salts was started 3. some years ago in this laboratory by Rogers? and Taylor8. This research is a continuation of their work and is complementary to work on electrical properties of metal-molten halides carried out in this laboratory9. The object of this work was to make an extensive study of the solubility of metal in the metal halide systems of those Group II:a metals which had not previously been studied in detail. Initial experi- ments on the calcium-calcium bromide and calcium-calcium chloride systems, previously determined in this laboratory, showed, however, the earlier results to be in error. These systems had therefore to be redetermined before further work was carried out. 4. 1.2. Relevant previous work on metal-molten salts. 1.2.1 General. 10 Since H. Davy's observation of the dispersion of potassium in molten potassium hydroxide in 1807 many investigations on the solubility of metals in molten salts have been carried out. idest of the early work was carried out by Lorenz and his co-workers at the beginning of this century and was largely qualitative and concerned with the question whether the dispersion of the metal in the salt was a conoidal suspension or a true solution. That part of their work carried out before 1926 is summarised in the book "Pyrosole" by Lorenz and Eitelll and in a chapter contributed by Lorenz to Alexander's book "Colloid Chemistry"12. According to Lorenz the metal dissolved in the melt in a colloidal form with a particle size > 10001. It is surprising that the colloidal theory could survive Aten's important observation in 1910 that the melting point of cadmium,chloride was depressed by the addition of cadmium, as this indicated a true solution13. Although Eitel and Lange14 placed doubt on the veracity of the colloidal theory, from their investigations of metal-salt melts with a high temperature 5. ultra microscope, it was not until the work of Heymann and his associates that the colloidal theory was finally rejected. In their work on the distribution equilibrium of cadmium between molten cadmium chloride and a molten bismuth phase Heymann and Friedlander15 found a linear relation in the distribution of cadmium between the two phases. As bismuth did not react or dissolve in cadmium chloride, and because cadmium in bismuth was an atomic solution, this indicated that the solution of cadmium in cadmium chloride was also a true solution.
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