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© 2014 Jin Zhang © 2014 Jin Zhang NEW HIGH PRESSURE PHASE TRANSITION OF NATURAL ORTHOENSTATITE AND SOUND VELOCITY MEASUREMENTS AT SIMULTANEOUS HIGH PRESSURES AND TEMPERATURES BY LASER HEATING BY JIN ZHANG DISSERTATION Submitted in partial fulfillment of the requirements for the degree of Doctor of Philosophy in Geology in the Graduate College of the University of Illinois at Urbana-Champaign, 2014 Urbana, Illinois Doctoral Committee: Professor Jay D. Bass, Chair and Director of Research Professor Xiaodong Song Assistant Professor Lijun Liu Associate Professor Przemyslaw Dera , University of Hawaii Abstract Studies of phase transformations and sound velocities of candidate mantle minerals under high-pressure high-temperature conditions are essential for understanding the mineralogical composition and physical processes of Earth’s interior. Phase transitions in candidate deep earth minerals under high-pressure high-temperature conditions is one of the main causes of the seismically observed discontinuities that define the boundaries between major layers of the Earth. The changes of sound velocities, including the directional dependencies of sound velocities, across phase transitions are still not well constrained. This is largely due to the lack of sound velocity measurements at sufficiently high pressure-temperature conditions and/or using only polycrystalline instead of single-crystal samples. To address the issues mentioned above, my dissertation involves two main topics Firstly, I discovered a new high-pressure Pbca -P2 1/c phase transition of natural orthoenstatite (Mg,Fe)SiO 3 using synchrotron single-crystal X-ray diffraction. This discovery contradicts with the widely accepted phase diagram of (Mg,Fe)SiO 3. I performed additional in situ Raman spectroscopy experiments addressing both compositional and high-temperature effects of this phase transition, providing solid evidences for the stability of orthoenstatite ( Pbca ) under average upper-most mantle conditions, and a potential stability/metastablity field for the new high-pressure P2 1/c phase. Furthermore, I measured in-situ the sound velocities change across this transition by single-crystal Brillouin spectroscopy, showing a pronounced increase of elastic anisotropy when transforming from the low to the high pressure phase. Secondly, I built the first laser-heating Brillouin spectroscopy system with the capability of performing single-crystal sound velocity measurements with laser heating to produce simultaneous high pressures and temperatures on samples in a diamond anvil cell. This experimental setup allows us for the first time to measure sound velocities of single-crystals of minerals under realistic P-T conditions of the Earth’s mantle. Sound velocity measurements of water and polycrystalline H2O ice as well as single-crystal San Carlos olivine were made utilizing this system. Our result provide the first experimental constrains on the effect of high ii temperature on the single-crystal elastic properties of olivine under high pressures. Our results indicate 1. Velocity gradient of olivine is far less than velocity gradient of AK135; 2. Olivine is the slow phase instead of fast phase at deeper than ~250km in depth; 3. Vs of olivine is almost constant or decreases from ~ 300km to ~410km. Based on the above observations, we expected much less olivine in the upper mantle (~ 25%), and much more pyroxene (both opx and cpx) in order to balance the velocity and velocity gradient discrepancy. In addition, this system has been designed so that the scattering angle can be changed continuously to any desired angle up to near back scattering (~141º) via a rotational stage and a compact 532nm diode-pumped solid-state (DPSS) laser. This novel setup allows us to probe a wide range of wave vectors q for investigation of phonon dispersion for crystals with large unit cells (~hundards of nms). This capability is demonstrated by dispersion measurements on cubic-close-packed polystyrene crystals. iii To Mom, Dad and Hao iv Acknowledgements I have spent almost six years in Urbana-Champaign, longer than any other places I have been except my hometown. I have a lot of good memories here and I owe a debt of thanks to many people. Beyond any shadow of doubt, the first person I have to thank is my advisor Prof. Jay Bass, for being so supportive and resourceful to let me try all types of wild ideas, being so knowledgeable and insightful to guide me all the way through, and especially, for being so patient and enduring to revise my endless drafts as well as deal with my occasional stubbornness. A traditional Chinese virtue is “a teacher for a day is a father forever”. My great respect and sincere gratitude will stay with me for a lifetime. I would also like to acknowledge all my instructors and colleagues all these years: Xiaodong Song, who broadened my knowledge of seismology and generously offered me lots of suggestions for my career development; Przemek Dera, who spent vast time and effort teaching and working with me on single-crystal X-ray diffraction; Lijun Liu, who greatly extended and deepened my understanding of the time-dependent dynamical processes of Earth and from whom I was benefited a lot through our discussions; Bruno Reynard, who introduced me into the world of Raman spectroscopy and gave me the benefit of his deep insight on subduction zones; Craig Lundstrom, who revised and graded my first term paper in English and is always helpful about my questions related to petrology; Steve Marshak, Jie Li, and professors from other departments, who taught me the tectonic history of Unites states, mineralogy and the mechanics-related courses. I also gained a significant amount of help from my fellow labmates, classmates and friends, for research and everyday life: Jingyun Wang, Bin Chen and Seiji Kamada, for their instructions in high-pressure experimental techniques; Liqin Sang, Guimiao Zhang, Jia Chen and Stephen Picek, for all the help and support in the lab; Xiaoxiao Li, a great life-time friend; Chong-Hwey Fee, for her kindness and delicious food; Zhen Xu, Xiangli Wang, Jing Jin, v Jiangtao Li, Quan Zhou, Jiashun Hu, Aiguo Han, Dongfang Li and many others, for the happy time we have spent together. In the end, I have to give my thankfulness to my parents; it is their unconditional love that gave me my strength and bravery. My husband, Hao, don’t worry, being a “Phd” will not really “Push Husband to Death”. vi Table of Contents Chapter 1 ....................................................................................................................................................... 1 Introduction ................................................................................................................................................... 1 1.1 Motivation ........................................................................................................................ 2 1.2 Experimental techniques review ...................................................................................... 6 1.3 Study framework and outline of this dissertation .......................................................... 11 References .................................................................................................................................. 12 Part I ............................................................................................................................................................ 21 New High Pressure Phase Transition of Natural Orthoenstatite ................................................................. 21 Chapter 2 ..................................................................................................................................................... 22 A new high-pressure polymorph of orthoenstatite: a synchrotron single-crystal X-ray diffraction study .. 22 Abstract ...................................................................................................................................... 23 2.1 Introduction .................................................................................................................... 24 2.2 Experimental Methods ................................................................................................... 25 2.3 Results ............................................................................................................................ 26 2.4 Discussion and conclusion ............................................................................................. 28 2.5 Acknowledgements ........................................................................................................ 29 References .................................................................................................................................. 29 Figures ....................................................................................................................................... 33 Tables ....................................................................................................................................... 37 Chapter 3 ..................................................................................................................................................... 40 Stability of orthoenstatite polymorphs: Effects from composition ............................................................. 40 Abstract ...................................................................................................................................... 41 3.1 Introduction
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