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New Developments in the Crystal Chemistry of Selected Borophosphates and Phosphates

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New Developments in the Crystal Chemistry of Selected Borophosphates and Phosphates New Developments in the Crystal Chemistry of Selected Borophosphates and Phosphates DISSERTATION zur Erlangung des akademischen Grades Doctor rerum naturalium (Dr. rer. nat.) vorgelegt der Fakultät Mathematik und Naturwissenschaften der Technischen Universität Dresden von M. Sc. Prashanth W. Menezes geboren am 02.05.1979 in Puttur, Indien Eingereicht am 09.07.2009 Die Dissertation wurde in der Zeit von Oktober 2004 bis Juni 2009 im Max-Planck-Institut für Chemische Physik fester Stoffe angefertigt. Hope is the companion of power and the mother of success. For who so hopes strongly has within him the gift of miracles. - Samuel Smiles Tag der Verteidigung: 19.10.2009 Gutachter: Prof. Dr. Rüdiger Kniep Prof. Dr. Michael Ruck Acknowledgement This is perhaps the easiest and hardest chapter that I have to write. It will be simple to name all the people that helped to get this done, but it will be tough to thank them enough. I will nonetheless try… In the first place, I would like to express my gratitude to my mentor and guide, Prof. R. Kniep, the director of Max Planck Institute for Chemical Physics of Solids for his supervision, advice, and guidance right from the nascent stage of this research till its completion. Above all he provided me unflinching encouragement and support in various ways. His passion towards science, his scientific intuition and foresight made him a constant oasis of ideas which enriched my growth as a student, a researcher and a scientist. His strong belief in the concept of “learning by doing” exceptionally inspired me during my failures and persuaded me to strive for success. I am truly indebted to him. I gratefully acknowledge my supervisor, Dr. S. Hoffmann for his advice and crucial contribution, which made him a backbone of this research and so to this thesis. His involvement, with his originality has triggered and nourished my intellectual maturity that I will benefit from, for a long time to come. Throughout my thesis–writing period, he provided encouragement, good teaching, good company, and lots of good ideas. I thank him for his detailed review and constructive criticism during the preparation of this thesis. I would have been lost without him. I sincerely thank Dr. Yu. Prots for single–crystal measurements and for his untiring help during my difficult moments especially with the single crystal structure refinements. I am obligated to him for reading my manuscripts. I have also benefited from the advice and guidance of Dr. G. Kreiner which was fruitful in shaping up my ideas and research. Collective and individual acknowledgments are also owed to my colleagues at MPI – CPfS whose presence perpetually refreshed and helped me in various ways. In particular, I would like to mention Dr. H. Borrmann, Dr. R. Cardoso and Mr. S. Hückmann for X–ray data collections and related discussions, Dr. G. Auffermann and Ms. A. Völzke for chemical analyses, Ms. Susann Scharsach for TG / DTA measurements, Dr. U. Burkhardt, Dr. R. Ramlau, and Mrs. P. Scheppan for SEM and EDX analyses, Dr. W. Schnelle and Mr. R. Koban for magnetic measurements and Ms. J. Buder for infrared measurements. This thesis research was made a lot easier by my lab mates, Dr. Y.-X. Huang, Dr. B. Ewald, Dr. W. Liu, Dr. M. Yang, Mr. Z. Lin, Ms. S. Chen, Mr. F. Gruchow and Mr. A. Topcu who created a pleasant working atmosphere. Without their constant support, my life at the institute would have been a lot less satisfying. I thank them all. Special thanks go to Dr. Y.-X. Huang and Dr. B. Ewald for all the interesting discussions and the critical reviews. I am grateful to the secretaries for assisting me in many different ways. Mrs. K. Demian, Mrs. C. Strohbach, Mrs. K. Klein and Ms. S. Zücker deserve special mention for their indispensable help dealing with travel, administration and bureaucratic matters during my stay in Dresden. I convey special acknowledgements to Dr. M. Schmidt, Dr. E. Dashjav and Dr. J. Hunger who amidst their busy schedules agreed to be internal referees for my papers. The last five years have been very rich and enjoyable owing to the presence of my colleagues and friends inside and outside the institute. It is pleasure to mention few of my friends and colleagues Dr. S. Nair, Dr. M. Kumar, Mr. J. Hirale, Dr. D. Kasinathan, Dr. A. Rajarajan, Mrs. A. Thomas, Dr. S. Rössler, Dr. H. Tlatlic, Dr. J. Makongo, Ms. K. Wagner, Dr. C. Göbel, Mr. Y. Ötzan, Dr. S. Singh, Dr. R. Nath, Mrs. J. Bendyna and Mr. S. Boulfelfel for the lunch meeting, tea breaks and weekend parties, also Dr. A. Wosylus for being such a good officemate and who always ready to lend a hand. I acknowledge the support of my friends Dr. S. Sapra, Dr. A. Sapra, Mr. K. Kumar, Dr. A. Bajpai, Dr. N. Kumar, Dr. M. Vyas, Dr. B. Gowd, Dr. B. Nandan, Mr. A. Nanjundan, Dr. N. Manik, Dr. K. Koepernik and Ms. S. Kuramoto for their great friendship outside office. They have been there through all my ups and downs. I was extraordinarily fortunate in having D. D. Sarma as my professor in Indian Institute of Science, India. I could never have embarked and started all of this without his prior teachings thus opened up unknown areas to me. Thank you. Words fail me to express my appreciation to my girlfriend Ms. R. Pais whose dedication, love and persistent confidence in me, has taken the load off my shoulder. Furthermore, I would like to thank Mr. R. Pais and Mrs. M. Pais for their constant support. None of these experiences would have occurred if not for the perpetual support of my parents, my father, Fredrick Menezes, my mother, Cecelia Menezes and my brothers Pradeep and Pramod, who deserve special mention for their inseparable support and prayers. The knowledge that they will always be there to pick up the pieces is what allows me to repeatedly risk getting shattered. To them I dedicate this thesis. Finally, I would like to thank everyone who was significant in the successful completion of my thesis as well as expressing my sincere apologies for failing to mention in person each and everyone. Thank you God for continuously showering your blessings upon me... CONTENTS 1 INTRODUCTION AND OBJECTIVE ............................................................. 1 1.1 General Introduction..................................................................................... 1 1.2 Structural Chemistry of Borophosphates ...................................................... 2 1.3 Transition Metal Borophosphates................................................................. 5 1.4 Aim of the Work ......................................................................................... 13 2 EXPERIMENTAL ............................................................................................ 16 2.1 Methods of Preparation ............................................................................... 16 2.2 Chemicals and Quality ................................................................................ 18 2.3 Materials Characterization.......................................................................... 18 2.3.1 Powder X–ray Diffraction................................................................... 18 2.3.2 Single Crystal X–ray Diffraction ........................................................ 19 2.3.3 Chemical Analysis............................................................................... 20 2.3.4 Scanning Electron Microscopy (SEM) and Energy Dispersive X–ray Analysis (EDX)................................................................................... 20 2.3.5 Thermal Analysis................................................................................ 21 2.3.6 Infrared Spectroscopy......................................................................... 21 2.3.7 Magnetic Susceptibility....................................................................... 22 3 RESULTS AND DISCUSSION ....................................................................... 23 3.1 Alkali–Metal Scandium Borophosphates.................................................... 23 I I 3.1.1 M Sc[BP2O8(OH)] (M = K, Rb).......................................................... 23 3.1.1.1 Synthesis.......................................................................................... 23 3.1.1.2 Crystal Structure Determination...................................................... 26 3.1.1.3 Crystal Structure Description.......................................................... 26 3.1.1.4 Thermal Analysis............................................................................ 28 3.1.2 CsSc[B2P3O11(OH)3] ........................................................................... 31 3.1.2.1 Synthesis.......................................................................................... 31 3.1.2.2 Crystal Structure Determination...................................................... 32 3.1.2.3 Crystal Structure Description.......................................................... 33 3.1.2.4 Thermal Analysis............................................................................ 38 3.1.3 Discussion ........................................................................................... 39 II CONTENTS 3.2 Alkali–Metal Scandium Hydrogenphosphates ............................................ 43 I I 3.2.1 Li2Sc[(PO4)(HPO4)] and M Sc(HPO4)2 (M = K, Rb, Cs, NH4) .......... 43 3.2.1.1 Synthesis.......................................................................................... 43 3.2.1.2 Crystal Structure Determinations .................................................... 48
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