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Synthesis, Ion-Exchange and Dehydration

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Synthesis, Ion-Exchange and Dehydration Microporous titanosilicate AM-2: Synthesis, ion-exchange and dehydration Inauguraldissertation der Philosophisch-naturwissenschaftlichen Fakultat¨ der Universitat¨ Bern vorgelegt von Nicola Dobelin¨ von Basel Leiter der Arbeit: Prof. Dr. T. Armbruster Laboratorium fur¨ chemische und mineralogische Kristallographie Von der Philosophisch-naturwissenschaftlichen Fakultat¨ angenommen. Bern, 12. Januar 2006 Der Dekan Prof. Dr. P. Messerli Contents 1. Abstract 6 2. Introduction 7 2.1. Zorite, ETS-4 . 8 2.2. ETS-10 . 9 2.3. Penkvilksite, ETS-14, AM-3 . 12 2.4. Umbite, AM-2 . 14 2.5. Silico-titanate, CST, TAM-5 . 15 2.6. Chemical variations . 17 References . 18 3. Synthesis 24 3.1. Experimental procedures . 24 3.1.1. Reproduction of previously published syntheses (TiS02) . 24 3.1.2. Doping with CsCl, NH4Cl, and RbCl (TiS03–TiS05) . 25 3.1.3. Lower SiO2 and TiCl3 concentrations (TiS08, TiS09) . 26 3.1.4. Agitation and different cooling rates (TiS11) . 26 3.1.5. Using anatase as Ti source and KF as F- source (TiS15) . 28 3.1.6. Seeds (TiS16) . 29 3.1.7. Adding TiCl3 solution prior to KOH (TiS20) . 29 3.1.8. Different fill levels of the autoclaves (TiS21–TiS23) . 30 3.1.9. Temperatures between 210 and 250 ◦C (TiS25–TiS28) . 30 3.1.10. Agitation and high temperature (TiS30–TiS31) . 31 3.1.11. Synthesis of UND-1 (TiS32–TiS33) . 31 3.1.12. Using HF as fluorine source (TiS34–TiS35) . 32 3.1.13. Adjusting the pH (TiS36–TiS42) . 32 3.1.14. Using higher concentrations of HCl (TiS43–TiS46) . 34 3.1.15. Ti deficiency (TiS48) . 34 3.2. Conclusion . 37 3.3. SEM images . 41 References . 59 3 Contents 4. Ion exchange and dehydration of Rb-exchanged AM-2 60 4.1. Abstract . 60 4.2. Experimental procedure . 60 4.3. Results . 64 4.4. Discussion . 69 4.5. Tables . 75 References . 84 5. Structural characterisation of ion-exchanged AM-2 85 5.1. Abstract . 85 5.2. Experimental procedure . 85 5.3. Results . 87 5.3.1. Ion exchange . 87 5.3.2. Thermo-gravimetric analysis . 89 5.3.3. Structure refinement . 89 5.3.4. Dehydration experiments . 95 5.4. Discussion . 99 5.5. Figures . 102 5.5.1. X-ray diffraction patterns . 102 5.5.2. Structures . 110 5.6. Tables . 113 5.6.1. Cell parameters . 113 5.6.2. Atomic coordinates, site occupancies, and Beq values . 115 5.6.3. Bond angles and distances . 118 5.6.4. Bond valence calculations . 125 5.6.5. Peak lists . 128 References . 130 6. Schreyerite, V2Ti3O9: New Occurrence and Crystal Structure 131 6.1. Abstract . 131 6.2. Introduction . 131 6.3. Geological setting and occurrence of schreyerite . 133 6.4. Experimental procedure . 134 6.4.1. Chemical analysis . 134 6.4.2. Structure determination . 134 6.5. Results . 135 6.5.1. Chemical composition . 135 6.5.2. Crystal structure . 136 6.6. Discussion . 138 6.7. Acknowledgements . 144 4 Contents References . 144 7. Heulandite-Ba, a new zeolite species from Norway 147 7.8. Abstract . 147 7.9. Introduction . 147 7.10. Heulandite-Ba occurrences . 148 7.11. Morphology, physical and optical properties . 148 7.12. Chemical composition . 150 7.13. X-ray crystallography and crystal structure determination . 151 7.13.1. Experimental procedures and results . 151 7.13.2. The tetrahedral framework . 153 7.13.3. The extra-framework sites . 154 7.14. Acknowledgements . 156 7.15. References . 156 8. The crystal structure of painite CaZrB[Al9O18] revisited 158 8.16. Abstract . 158 8.17. Introduction . 158 8.18. Experimental methods . 159 8.19. Discussion . 159 8.20. Acknowledgments . 161 8.21. References cited . 161 A. Appendix 162 A.1. A sample Fullprof input file . 162 A.1.1. Input PCR file with comments . 162 A.1.2. The input PCR file . 166 B. Acknowledgements 170 C. Curriculum Vitae 171 C.1. Personal Details . 171 C.2. Education . 171 5 1. Abstract Microporous titanosilicates have attracted great attention among mineralogists and mate- rial scientists during the last decades. Their variable chemical compositions and structural features suggest high potential for technical applications in the classical fields of zeolites such as ion-exchange, catalysis, adsorption, and gas separation, but also in new areas like optoelectronics, batteries, non-linear optics, magnetic materials and sensors. Some materi- als have been investigated thoroughly and are still subject of many studies (e. g. ETS-10, CST), whereas others have merely been synthesised without further investigation of the structure. The microporous structure AM-2 is an analogue of the natural zirconosilicate umbite, and has been synthesised in various chemical compositions (K2MSi3O9 · H2O, with M = Ti, Zr, Sn, Pb and others). Although several synthesis instructions have been published to date, none of them produces crystals large and pure enough for single-crystal X-ray diffraction (XRD). This technique, however, is preferred for structural analyses due to its higher resolu- tion compared to powder XRD. In the first part our study thus focuses on the optimisation of AM-2 synthesis, striving for larger crystals suitable for single-crystal XRD. Synthesis in- structions using colloidal silica and dissolved TiCl3 for hydrothermal reactions turned out to be most suitable for a starting point. By changing various parameters we found a de- pendence between crystal intergrowth and pH of the reaction gel, and to a limited extent between HCl concentration and crystal size. Maximum crystal sizes up to 30 µm were ob- tained, which is, however, too small for single-crystal XRD. On the other hand, some syn- thesis products contained aggregates with a high specific surface and crystallite sizes in the range of 1–20 µm, which guaranteed fast ion-exchange reactions and high-quality powder XRD patterns with sharp reflections and low risk for orientation and absorption effects. The ion-exchange properties of AM-2 of initial composition K2TiSi3O9 · H2O were anal- ysed by exchanging K+ for various mono- and divalent cations, namely Rb+, Cs+, Sr2+, Na+, Mn2+, Ca2+, and Cu2+. The exchanged structures were analysed for their dehydra- tion behaviour with the goal to provide a comprehensive characterisation of the Ti-AM-2 structure in terms of selectivity and exchange capacity for various cations, as well as ther- mal stability in general and as a function of the incorporated cation species. The ion ex- change reactions were monitored with ICP-OES and Rietveld refinement of powder XRD data. Dehydration was analysed with powder XRD and thermo-gravimetric analyses. In conclusion, the Ti-AM-2 structure has almost 100% exchange capacity for all analysed cations. The kinetics of the exchange reaction depend on the ionic radius and are faster for small cations than for large ones. In fully hydrated state the H2O concentration varies between 1 and 3 molecules per formula unit. H2O may easily be expelled by heating to 400–500 ◦C. For K- and Rb-bearing AM-2 the dehydration is completely reversible without compromising the structural integrity, whereas all other varieties gradually break down and reach complete amorphisation between 250 and 500 ◦C, depending on the cation species in the cavities. At higher temperatures (700–750 ◦C) new phases crystallise, with structures determined by the exchangeable cations. This phase change is irreversible. 6 2. Introduction Microporous titanosilicates (TS) constitute a novel family of zeotype materials built from TiO6-octahedra and SiO4-tetrahedra. Some species show promising properties.
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