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Optimization of Layered Battery Cathode Materials Synthesized Via Spray Pyrolysis Miklos Lengyel Washington University in St

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Optimization of Layered Battery Cathode Materials Synthesized Via Spray Pyrolysis Miklos Lengyel Washington University in St Washington University in St. Louis Washington University Open Scholarship All Theses and Dissertations (ETDs) Spring 4-14-2014 Optimization of layered battery cathode materials synthesized via spray pyrolysis Miklos Lengyel Washington University in St. Louis Follow this and additional works at: https://openscholarship.wustl.edu/etd Part of the Engineering Commons Recommended Citation Lengyel, Miklos, "Optimization of layered battery cathode materials synthesized via spray pyrolysis" (2014). All Theses and Dissertations (ETDs). 1246. https://openscholarship.wustl.edu/etd/1246 This Dissertation is brought to you for free and open access by Washington University Open Scholarship. It has been accepted for inclusion in All Theses and Dissertations (ETDs) by an authorized administrator of Washington University Open Scholarship. For more information, please contact [email protected]. WASHINGTON UNIVERSITY IN ST. LOUIS School of Engineering and Applied Science Department of Energy, Environmental and Chemical Engineering Dissertation Examination Committee: Richard L. Axelbaum, Chair Pratim Biswas William E. Buhro Cynthia Lo Venkat Subramanian Xiaofeng Zhang Optimization of Layered Battery Cathode Materials Synthesized via Spray Pyrolysis by Miklós Lengyel A dissertation presented to the Graduate School of Arts and Sciences of Washington University in St. Louis in partial fulfillment of the requirements for the degree of Doctor of Philosophy May 2014 St. Louis, Missouri © 2014 Miklos Lengyel Chapters 3 and 5 are Reproduced by permission of ECS – The Electrochemical Society Table of Contents List of Figures ................................................................................................................................ vi List of Tables ................................................................................................................................. xi Acknowledgments........................................................................................................................ xiii Preface........................................................................................................................................... xx Chapter 1 ......................................................................................................................................... 2 Introduction ..................................................................................................................................... 2 1.1 Demand for Li-ion Batteries ............................................................................................ 2 1.2 Lithium-ion Battery Basics .............................................................................................. 4 1.3 Anode Materials for Li-ion Batteries ............................................................................... 7 1.4 Cathode Materials in Li-ion Batteries .............................................................................. 8 1.5 Batteries beyond conventional lithium ion chemistries ................................................. 13 1.6 Overview of Synthesis Processes for Cathode Materials ............................................... 15 1.7 Objectives and Dissertation Outline ............................................................................... 21 Chapter 2 ....................................................................................................................................... 23 Research Methodology ................................................................................................................. 23 2.1 Powder Synthesis – Spray Pyrolysis .............................................................................. 23 2.2 Annealing heat-treatment ............................................................................................... 26 2.3 Particle Size Measurements ........................................................................................... 27 ii 2.4 Crystallographic Analysis - Powder Diffraction ............................................................ 28 2.5 Morphological Studies ................................................................................................... 28 2.5 Other Characterization Techniques ................................................................................ 29 2.6 Battery Performance Evaluation .................................................................................... 29 Chapter 3 ....................................................................................................................................... 35 Composition Optimization of Layered Lithium Nickel Manganese Cobalt Oxide Materials Synthesized Via Ultrasonic Spray Pyrolysis................................................................................. 35 3.1 Introduction ......................................................................................................................... 35 3.2. Experimental ...................................................................................................................... 38 3.3 Physical and crystal properties............................................................................................ 40 3.4 Electrochemical testing results ........................................................................................... 49 3.5 Voltage Fade ....................................................................................................................... 59 3.6 Conclusions ......................................................................................................................... 63 Chapter 4 ....................................................................................................................................... 65 Effects of synthesis conditions on the physical and electrochemical properties of Li1.2Mn0.54Ni0.13Co0.13O2 prepared by spray pyrolysis .................................................................. 65 4.1 Introduction ......................................................................................................................... 65 4.2 Experimental ....................................................................................................................... 67 4.3 Results and Discussion ....................................................................................................... 71 iii Chapter 5 ....................................................................................................................................... 98 Effects of surface area and lithium content on the electrochemical performance of Li1.2Mn0.54Ni0.13Co0.13O2 ............................................................................................................... 98 5.1 Introduction ......................................................................................................................... 98 5.2. Experimental .................................................................................................................... 101 5.3 Results and Discussion ..................................................................................................... 104 5.4. Conclusions ...................................................................................................................... 120 Chapter 6 ..................................................................................................................................... 122 Trace level doping to improve capacity retention and prevent voltage fade .............................. 122 6.1. Introduction ...................................................................................................................... 122 6.2 Experimental ..................................................................................................................... 125 6.3 Results and Discussion ..................................................................................................... 127 6.4 Conclusions ....................................................................................................................... 144 Chapter 7 ..................................................................................................................................... 145 Development of a Scalable Spray Pyrolysis Process for the Production of Non-hollow Battery Materials ..................................................................................................................................... 145 7.1 Introduction ....................................................................................................................... 145 7.2. Experimental .................................................................................................................... 146 7.3 Results and Discussion ..................................................................................................... 149 iv 7.4 Conclusions ....................................................................................................................... 153 Chapter 8 ..................................................................................................................................... 155 Summary and recommendations for future work ....................................................................... 155 7.1 Summary of Results ..................................................................................................... 155 7.2 Recommendations for Future Work ............................................................................
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