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Advanced Transition Metal Phosphide Materials from Single-Source Molecular Precursors

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Advanced Transition Metal Phosphide Materials from Single-Source Molecular Precursors RICE UNIVERSITY Advanced transition metal phosphide materials from single-source molecular precursors by Adam Caleb Colson A THESIS SUBMITTED IN PARTIAL FULFILLMENT OF THE REQUIREMENTS FOR THE DEGREE Doctor of Philosophy APPROVED, THESIS COMMITTEE enton H. "tmire, Chair Professor of Chemistry Associate Dean for Academic Affairs Wiess School ofNatural Sciences Lon J. Wilson Professor of Chemistry Emilia Morosan Assistant Professor of Physics and Astronomy and Chemistry HOUSTON, TEXAS December 2011 Abstract Advanced transition metal phosphide materials from single-source molecular precursors by Adam Caleb Colson In this thesis, the feasibility of employing organometallic single-source precursors in the preparation of advanced transition metal pnictide materials such as colloidal nanoparticles and films has been investigated. In particular, the ternary FeMnP phase was targeted as a model for preparing advanced heterobimetallic phosphide materials, and the iron-rich Fe3P phase was targeted due to its favorable ferromagnetic properties as well as the fact that the preparation of advanced Fe3P materials has been elusive by commonly used methods. Progress towards the synthesis of advanced Fez-xMnxP nanomaterials and films was facilitated by the synthesis of the novel heterobimetallic complexes FeMn(CO)a(1.1-PR1R2) (R1 = H, RZ = H or R1 = H, RZ= Ph), which contain the relatively rare 1.1-PHZ and 11-PPhH functionalities. Iron rich Fez-xMnxP nanoparticles were obtained by thermal decomposition of FeMn(CO)a(Jl-PHz) using solution-based synthetic methods, and empirical evidence suggested that oleic acid was responsible for manganese depletion. Films containing Fe, Mn, and P with the desired stoichiometric ratio of 1:1:1 were prepared using FeMn(CO)a(Jl-PHz) in a simple low-pressure metal-organic chemical vapor deposition (MOCVD) apparatus. Although the elemental composition of the precursor was conserved in the deposited film material, spectroscopic evidence indicated that the films were not composed of pure-phase FeMnP, but were actually mixtures of crystalline FeMnP and amorphous FeP and MnxOy. A new method for the preparation of phase-pure ferromagnetic Fe3P films on quartz substrates has also been developed. This approach involved the thermal decomposition of the single-source precursors HzFe3(CO)gPR (R =tBu or Ph) at 400 °C. The films were deposited using a simple home-built MOCVD apparatus and were characterized using a variety of analytical methods. The films exhibited excellent phase purity, as evidenced by X-ray diffraction, X-ray photoelectron spectroscopy, and field-dependent magnetization measurements, the results of which were all in good agreement with measurements obtained from bulk Fe3P. As-deposited Fe3P films were found to be amorphous, and little or no magnetic hysteresis was observed in plots of magnetization versus applied field. Annealing the Fe3P films at 550 oc resulted in improved crystallinity as well as the observation of magnetic hysteresis. Acknowledgments During my time at Rice, I have benefited from a tremendous amount of support, guidance, and fellowship from friends, colleagues, and mentors, and I would be remiss if I did not acknowledge the individuals who have made this work possible. First, I would like to express my gratitude to Professor Kenton H. Whitmire for accepting the challenge of mentoring an uncultured and stubborn aspiring scientist from rural Idaho. In addition to teaching me a great deal about inorganic chemistry, he has also taught me about temperance, patience, and industriousness, and I am truly a better person for having spent time in his research group. I would also like to thank Professor Lon J. Wilson for being a member of my thesis committee and for chairing my qualifying exam committee, in addition to being an excellent source of professional and personal advice. My thanks are also extended to Professor Emilia Morosan for agreeing to be a member of my thesis committee and especially for being an ideal collaborator. I am grateful to the past and present members of the Whitmire research group for providing a welcoming and warm environment. Thanks to Dr. Cristina Hofmann, Dr. Anna Kelly, and Dr. Trinanjana Mandai for pointing me in the right direction, and thanks to Sean Walsh for having the metaphorical (and literal) fire extinguisher ready all these years. I am also indebted to the many friends I have made in the chemistry department who have lifted my spirits when I've been discouraged and who have been a sounding board to my occasional frustrations. v I would also like to acknowledge Chih-Wei Chen from the Morosan research group for his diligence and professionalism in obtaining magnetic measurements, and I wish him success in his own research efforts. Additionally, I would like to thank Dr. Caroline McNeil for her help in teaching and her assistance with GC-MS data collection. I am indebted to the research scientists from the Chemistry Department and the Shared Equipment Authority, especially Richard Crouse, Dr. Bo Chen, Dr. Wenh Guo, Dr. Christopher Pennington, and Dr. Lawrence B. Alemany. Without their tireless efforts, none of this work would have been possible. I would also like to acknowledge the support and guidance of the Rice University faculty and staff who have selflessly given logistical, professional, and personal advice. I will be forever grateful for the support and encouragement of my family members. I thank my mom and dad for the daily sacrifice of their time and resources that they have made on my behalf for over three decades. They are my heroes and they have always kept me grounded in reality. I also thank my grandparents, in­ laws, and extended family for teaching me about the important things in life. My wife Jenna will never know how much she means to me, and I do not have the words to express my gratitude for the sacrifices she has made over the years. My son Caleb is the inspiration for everything I do, and he is my daily source of pride and joy. Finally, I humbly acknowledge the Divine Presence that has given me strength and guided my path throughout my life. Table of Contents Abstract .......................................................................................................................................................... ii Acknowledgments .................................................................................................................................... iv Table of Contents ...................................................................................................................................... vi List of Figures ............................................................................................................................................. ix List of Tables ........................................................................................................................................... xvii Chapter 1. General Introduction ......................................................................................................... 1 1.1 Survey of the Bulk Metal Pnictides ........................................................................................ 1 1.2 Advanced Metal Pnictide Materials ....................................................................................... 6 1.2.1 Metal Pnictide Nanoparticles ........................................................................................... 6 1.2.2 Metal Pnictide Films ............................................................................................................ 9 1.3 Summary and Thesis Overview............................................................................................ 12 Chapter 2. Synthesis and Characterization of Single-source Molecular Precursors to Advanced Fez-xMnxP Materials .......................................................................................................... 14 2.1 Introduction .................................................................................................................................. 14 2.2 Experimental ................................................................................................................................ 16 2.3 Results and Discussion ............................................................................................................. 24 2.4 Conclusions ................................................................................................................................... 42 Chapter 3. Synthesis of Fez-xMnxP Nanoparticles from Single-Source Molecular Precursors .................................................................................................................................................. 44 vii 3.1 Introduction .................................................................................................................................. 44 3.2 Experimental ................................................................................................................................ 46 3.3 Results and Discussion............................................................................................................. 53 3.4 Conclusions ................................................................................................................................... 79 Chapter 4. Synthesis of Ferromagnetic Fe3P Films from Single-Source Molecular Precursors .................................................................................................................................................
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