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The Structural Chemistry of Euxenite, .Fergusonite and Related Oxides

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The Structural Chemistry of Euxenite, .Fergusonite and Related Oxides THE STRUCTURAL CHEMISTRY OF EUXENITE, .FERGUSONITE AND RELATED OXIDES Thesis submitted for the Degree of DOCTOR OF PHILOSOPHY to the University of London by VASANT VIRUPAX DESHPANDE, M.Sce,Ph.D.(Bom.),A.R.I.C. (JULY 1961) ABSTRACT. Euxenite (YNbTiO6) and fergusonite (YNbO4) have been synthesized from their component oxides. X-Ray investigation showed that they are identical in structure with the natural metamict minerals. The composition range of existence of euxenite has been investigated by the study of the ternary system Y203-Nb205-Ti02 and also by substituting the cations TO+, ThYt-, U114- 9 0e4+ and NO+ and studying the resulting solid solutions. In the course of this study the new compounds NdNbTi06, NdTaTiO6, CeNbTiO6 and CeTaFe06 have been isolated, and their X-ray structure data are given. Cation substitution of Ta5+, Ce"- and in the fergusonite structure has also been investigated, and solid solution studies are reported. A new compound CeTa04 has been isolated, and its X-ray data are given. The systems Nb205-Ti029 Zr02-Nb205, Zr02-Ta205 and Zr02-Ti02 have been studied in a preliminary manner and the existence of the compounds, ZrTiO4, 6Zr029 Nb205 and 6Zr02,Ta205 has been confirmed. In the system Th02-Ti02 a new compound ThTi20e, with a complex structure has been prepared; its unit•-cell dimensions could not be determined. A brief preliminary study of the systems Ce02-Ti02, Be0-Nb2059 Be0-Ta208 and U308-Ti02 is also reported. ACKNOWTEDGEMENTS. I am very grateful to my supervisor Dr. A. J. E. Welch for his kindness, advice, and guidance throughout the course of this work. I thank Dr. D. F. Evans and Dr. L. Pratt, for their helpful discussions. I also thank my colleagues in Room 78, Dr. B. D. Joyce, Dr. B. E. Baughan, Messrs. P. E. D. Morgan, M. J. Gregory, A. C. Skapski, G. C. Nicholson, R. A. Brown and Miss T. Nyein for their cooperation. I gratefully acknowledge the award of a Central Overseas Scholarship by the Govt. of Maharashstra and Govt. of India, which made this study possible. Finally I thank Mrs. Y. Dolejsi for her help in the laboratory. Inorganic Chemistry Research Laboratories, Imperial College of Science and Technology, London, S.W.7. CONTENTS. PAGE CHAPTER I. INTRODUCTION. 1 1. The Metamict Minerals. 2 2. Euxenite. 3 3. Fergusonite and Formanite. 4. The System Ti02-Nb205. 13 5. The System Zr02-Ti02, 14 6. The Systems Zr02-Nb205 and Zr02-Ta205. 15 7. The System Th02-Ti02. 16 8. The System Ce02-Ti02 16 9. The Systems Be0-Nb205 and 17 Be0-Ta205. 10. The System U308-Ti02. 17 CHAPTER II. EXPERIMENTAL TECHNIQUES. 18 1. Materials. 19 2. Preparation of Oxide Mixtures. 20 3. Furnace Equipment. 21 4. Method of X-Ray Powder Photography. 22 CHAPTER III. EXPERIMENTAL RESULTS. 23 PART I. 1. Synthetic Euxenite. 24 2. The Ternary System Y203-Nb205-Ti02. 24 3. The System YNbTi06-YTaTi06. 28 4. The System YNbTi06-ThTip6. 30 5. The System YNbT106-ThIleNb06. 33 6. The System YNbTi06-CeNbTi06. 36 7. The System YNbTi06-CenFe06. 38 Page 8. The System YNbTi06-NdNbTi06. 41 9. The System YNbTi06-UTi206. 43 10. The System YTaTi06-NdTaTi06. 46 11. The System CeNbFe06-CeTaFe06. 48 PART II. THE FERGUSONITE SERIES. 12. Synthetic Fergusonite. 50 13. The System YNb04-YTa04. 52 14. The System YNb04-CeNb04. 54 15. The System YNb04-ThTiO4. 56 16. The System YNI004-UTiO4. 58 17. The System YTa04-CeTa04 . 61 PART III. 18. The System Nb205-Ti02. 63 19. The System Zr02-Ti02. 65 20. The Systems Zr02-Nb205 sand 67 Zr02-Ta205. 21. The System Th02-Ti02. 70 22. The System Ce02-T102. 72 23. The Systems Be0-Nb205 and 74 Be0-Ta206. 24. The System U308-Ti02 75 CHAPTER IV. DISCUSSION. 78 APPENDIX (Containing X-ray Powder Data). 92 REFERENCES 119 CHAPTER 1. INTRODUCTION. 2. 1. THE AETAMICT MINERALS. Radioactive minerals are of general interest because they frequently contain uranium and related elements, but they hold a special interest mineralogically because they include most of the minerals classed as metamict". The possession of this characteristic is probably the main reason why certain of these minerals have not been effectively studied previously by X-ray diffraction methods. Probably these minerals were originally crystalline, but they have been transformed into a glass- like, isotropic mass with a conchoidal fracture, although the original external forms of the crystals have often remained unchanged. The term "metamict' was introduced by BrAger (1893). Characteristic metamict minerals are orthite, gadolinite, samarskite, euxenite, polycrase, polymignite, aeschynite, fergusonite, and yttrotantalite. Although various theories of the metamict state in minerals have been put forward from time to time (e.g. by Goldschmidt and Thomassen (1924), Mugge (1922), and Vegard (1927)), it is now generally accepted that the disordering of the crystal lattice arises from atom 3. displacements due to radioactive disintegration of constituents of the mineral. All minerals that are commonly metamict have fairly complex compositions, involving a large amount of isomorphous substitution. They usually contain, among other elements, metals of the lanthanide group, uranium, or thorium. A characteristic of these minerals is their isotropy, as well as the lack of short X-ray diffraction lines. 2. EUXENITE. On account of its structural interest, this rare mineral was selected for synthesis and further study. The name of the mineral is derived from a Greek word meaning "friendly to strangers, hospitable", in allusion to the rare elements that it contains. It is found in granite pegmatites, sometimes in large amounts, associated with biotite, muscovite, ilmenite, monazite, xenotime, zircon, beryl, magnetite, garnet, gadolinite, blomstrandine and less frequently, thorite, uraninite, betafite, and columbite. Discolorations and radial fractures are frequently noted in the matrix of the crystals or masses of euxenite and other metamict or highly radioactive minerals. '4. Known occurences of euxenite are predominantly in Norway, Sweden, Madagascar, Congo Republic, Brazil, and Canada. Euxenite is ordinarily metamict (Goldschmidt and Thomassen, 1924), in common with most rare-earth oxides of niobium, tantalum, and titanium and it becomes crystalline only on ignition. Arnott (1950), working on mineral euxenite, ignited it at 800°C and found that the material was cryptocrystalline. He was, therefore, unable to obtain single crystals of the mineral. X-Ray powder photographs taken of the mineral after heating at 400° to 800°C showed considerable variations, chiefly in the presence or absence of particular lines. However, samples heated at 1000°C and above gave similar diffraction patterns. Faessler (1942) found that the crystalline structure of the mineral gadolinite is regained rapidly by heating at 800°C, and regained more slowly by heating at low temperatures. In the case of euxenite the uniformity of structure after heating at 1000°C suggests that the temperature of rapid recovery of the crystal structure lies between 800° and 1000°C, the variations at low temperature may then be the result of incomplete recovery of the crystalline structure when the sample is heated. Euxenite is an oxide or titanate-columbate of the type AB206 (Machatschki, 1929) with A = Y, Ce, Ca, U, Th. Ti, Nb, Ta, Fes+. The predominant constituents are yttrium, calcium, titanium, niobium and tantalum. The high titanium end member is called polycrase and the high niboium-tantalum member euxenite. The normal member of the series contains more niobium than tantalum although tantalum varieties are not uncommon. The ratios Ti o Nb + Ta lie between 2 : 3 and 3 : 1. Some reported analysis include up to 9% of A1203 and as much as 21% of Si02, but these constituents do not occur in appreciable amounts in homogeneous samples. The morphological similarity of euxenite and polycrase was first recognized by Scheerer (1847) and the chemical relationship by BrAger (1906). According to the morphological evidence, these minerals crystallige in the dipyramidal class of the orthorhombic system and have an axial ratio of a o b o c = 0.3789 : 1 : 0.3527 (Palache, Berman and Frondel, 1944). They show two 6. kinds of habit, prismatic and massive, showing no crystal faces. They are black with a brilliant sub- metallic or somewhat vitrous lustre, giving a brown streak. Their hardness is 5.5 - 6.5 and density 5.10 - 5.40. X-Ray Structure Analysis of Euxenite. Arnott (1950) carried out an X-ray analysis of mineral euxenite after igniting it at 1000°C. He indexed the powder pattern on the basis of orthorhombic symmetry, with the unit cell dimensions a = 5.53 A, b = 14.60 A, and c = 5.17 A. Euxenites obtained from different sources gave slightly different lattice dimensions. Using the above values for the unit cell dimensions, the spacings of all possible planes were calculated down to a spacing of 2.00 A. By comparing these possible reflections with those actually observed in the powder pattern, Arnott derived the probable space-group of euxenite as either Pccn or Pcmn. Both these space-groups satisfy the observed reflections on the X-ray powder photograph. Alexandrov and Pytenko (1959) calcined samples of euxenite obtained from different sources at 800°C to crystallize them, and obtained X-ray powder 7. photographs of the products. Some of the samples calcined at 800°C gave unsatisfactory powder photographs and had to be heated at 1100°C to develop good crystallinity. The X-radiograms of these samples were different from those of samples crystallized at 800°C in containing extra lines which could not be indexed from the orthorhombic unit cell of euxenite. These, however, fit a cubic unit cell of fluorite type with a = 5.07 - 5.-13 A. The content of this cubic component was particularly high in samples which were originally highly hydrated and decomposed.
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