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Nanoscale Heterogeneities in Visible Light Absorbing Photocatalysts

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Nanoscale Heterogeneities in Visible Light Absorbing Photocatalysts Nanoscale Heterogeneities in Visible Light Absorbing Photocatalysts: Connecting Structure to Functionality Through Electron Microscopy and Spectroscopy by Diane Michelle Haiber A Dissertation Presented in Partial Fulfillment of the Requirements for the Degree Doctor of Philosophy Approved November 2019 by the Graduate Supervisory Committee: Peter Crozier, Chair Candace Chan Jingyue Liu Michael Treacy ARIZONA STATE UNIVERSITY December 2019 ABSTRACT Photocatalytic water splitting over suspended nanoparticles represents a potential solution for achieving CO2-neutral energy generation and storage. To design efficient photocatalysts, a fundamental understanding of the material’s structure, electronic properties, defects, and how these are controlled via synthesis is essential. Both bulk and nanoscale materials characterization, in addition to various performance metrics, can be combined to elucidate functionality at multiple length scales. In this work, two promising visible light harvesting systems are studied in detail: Pt-functionalized graphitic carbon nitrides (g-CNxHys) and TiO2-supported CeO2-x composites. Electron energy-loss spectroscopy (EELS) is used to sense variations in the local concentration of amine moieties (defects believed to facilitate interfacial charge transfer) at the surface of a g-CNxHy flake. Using an aloof-beam configuration, spatial resolution is maximized while minimizing damage thus providing nanoscale vibrational fingerprints similar to infrared absorption spectra. Structural disorder in g-CNxHys is further studied using transmission electron microscopy at low electron fluence rates. In-plane structural fluctuations revealed variations in the local azimuthal orientation of the heptazine building blocks, allowing planar domain sizes to be related to the average polymer chain length. Furthermore, competing factors regulating photocatalytic performance in a series of Pt/g- CNxHys is elucidated. Increased polymer condensation in the g-CNxHy support enhances the rate of charge transfer to reactants owing to higher electronic mobility. However, active site densities are over 3x lower on the most condensed g-CNxHy which ultimately limits its H2 evolution rate (HER). Based on these findings, strategies to improve the cocatalyst configuration on intrinsically active supports are given. i In TiO2/CeO2-x photocatalysts, the effect of the support particle size on the bulk/nanoscale properties and photocatalytic performance is investigated. Small anatase supports facilitate highly dispersed CeO2-x species, leading to increased visible light absorption and HERs resulting from a higher density of mixed metal oxide (MMO) interfaces with Ce3+ species. Using monochromated EELS, bandgap states associated with MMO interfaces are detected, revealing electronic transitions from 0.5 eV up to the bulk bandgap onset of anatase. Overall, the electron microscopy/spectroscopy techniques developed and applied herein sheds light onto the relevant defects and limiting processes operating within these photocatalyst systems thus suggesting rational design strategies. ii This dissertation is dedicated to: DALTON, for his unwavering love, patience, advice, and long-distance drives to visit me. GOD and my FAMILY, for their faith and generosity. The one and only AUGGIE, my first dog, best friend, and writing buddy. iii ACKNOWLEDGEMENTS I extend my deepest thanks toward Prof. Peter Crozier, who recognized my potential and offered me a position within his research group. Your invaluable technical and professional guidance has shaped me into who I am today. Beyond that, your enthusiasm for materials science has rubbed off on me – just a little. I will forever be grateful. I want to acknowledge my committee members for providing critical feedback and instructive discussions which have allowed me to view my research from different perspectives. Special thanks to Dr. Candace Chan and her students for allowing me access to lab equipment. To all current and past members of the Crozier research group – your support is immensely appreciated. In particular, Dr. Barnaby Levin, Kartik Venkatraman, Dr. Qianlang Liu, and Dr. Ben Miller have contributed to this work and/or provided tips and tricks for doing advanced electron microscopy and spectroscopy. I want to thank Tara Boland, for helping with my research and most of all, being a best friend. I was fortunate to mentor undergraduate students Tu-Uyen Phan and Alex Bravenec, who both exceled in their endeavors and got some important projects off the ground. Much of this would not be possible without the assistance of ASU’s technical staff. For training and help with operating aberration-corrected microscopes, I thank John Mardinly, Dr. Toshihiro Aoki, Dr. Shery Chang, Dr. Katia Mark, and Karl Weiss. David Wright, Dr. Emmanuel Soignard, Diana Convey, and Douglas Daniel have helped on many aspects of my project including training on several tools for materials synthesis and characterization. Thanks to Sarah Kempkes, Adam Smith, Trevor Martin, and Dr. Gwyneth Gordon for helping me navigate the challenges of sample preparation for ICP-MS analysis. iv Conversations with Prof. Ray Egerton (University of Alberta) have been instrumental to the interpretation of vibrational EELS data. Prof. Michael Treacy graciously helped with producing correlographs and interpreting high resolution electron micrographs. Prof. Paul McMillan (University College London), thank you for explaining graphitic carbon nitrides in the most understandable way possible – your expertise at the beginning of graduate school was vital. I’ll never forget the enlightening conversation I had about disordered materials with Prof. Linn Hobbs (Massachusetts Institute of Technology); the small bit of time you dedicated to giving me feedback made all the difference. I would like to thank my parents and sisters for their continuous support throughout the years. To Dr. Marion Branch and Wilson Kong, our coffee chats were just what I needed to get me through a hard day. Thank you to the Arizona Shuffle Community and the authentic friendships I made since picking up this most awesome hobby – dancing my way through graduate school provided an essential balance. Most of all, I want to thank Dalton for gracefully undergoing this journey by my side as we start our lives together. I gratefully acknowledge the financial support from the U.S. Department of Energy (DE-SC0004954), ASU’s Deans Fellowship, and the Graduate College Completion Fellowship. For travel support, I thank the Microscopy Society of America, the Graduate and Professional Student Association, and the School for Engineering of Matter, Transport, and Energy. Finally, I acknowledge the John M. Cowley Center for High Resolution Electron Microscopy, the Eyring Materials Center, the W.M. Keck Foundation Laboratory, and the Goldwater Environmental Lab at ASU for access to advanced materials characterization equipment. v TABLE OF CONTENTS Page LIST OF TABLES ............................................................................................................ xii LIST OF FIGURES ......................................................................................................... xiii CHAPTER INTRODUCTION ..................................................................................................... 1 1.1 Motivation ................................................................................................... 1 1.2 Photocatalytic Water Splitting .................................................................... 8 Thermodynamic and Kinetic Considerations ................................ 10 Cocatalyst Loading Method .......................................................... 29 Performance Metrics ..................................................................... 32 1.3 Development of Visible Light Absorbing Photocatalysts ........................ 39 Synopsis of the Most Common Approaches and Advancements . 40 Graphitic Carbon Nitride Photocatalysts....................................... 52 TiO2-Supported CeO2-x Photocatalysts .......................................... 61 1.4 Objectives and Outline .............................................................................. 67 METHODS .............................................................................................................. 71 2.1 Materials Preparation ................................................................................ 71 Ionothermal Synthesis ................................................................... 71 Thermolytic Condensation ............................................................ 72 Hydrothermal Synthesis ................................................................ 73 Ce Impregnation onto TiO2 Nanoparticles .................................... 74 Pt Functionalization....................................................................... 74 vi CHAPTER Page 2.2 Measurement of H2 Evolution Rates......................................................... 78 Photoreactor System ...................................................................... 78 Gas Chromatography..................................................................... 82 2.3 Bulk Characterization ............................................................................... 87 X-ray Diffraction (XRD) ............................................................... 87 Vibrational Spectroscopies ............................................................ 90 Ultraviolet-Visible Absorption Spectroscopy
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