Methylammonium Acetate Assisted Deposition of Hybrid Halide
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METHYLAMMONIUM ACETATE ASSISTED DEPOSITION OF HYBRID HALIDE PEROVSKITE FOR EFFICIENT DEVICES by Mehedhi Hasan, M.S. A dissertation submitted to the Graduate Council of Texas State University in partial fulfillment of the requirements for the degree of Doctor of Philosophy with a Major in Materials Science, Engineering and Commercialization August 2019 Committee Members: Alex Zakhidov, Chair Edwin L Piner Wilhelmus J. Geerts Casey Smith William Chittenden COPYRIGHT by Mehedhi Hasan 2019 FAIR USE AND AUTHOR’S PERMISSION STATEMENT Fair Use This work is protected by the Copyright Laws of the United States (Public Law 94-553, section 107). Consistent with fair use as defined in the Copyright Laws, brief quotations from this material are allowed with proper acknowledgement. Use of this material for financial gain without the author’s express written permission is not allowed. Duplication Permission As the copyright holder of this work I, Mehedhi Hasan, authorize duplication of this work, in whole or in part, for educational or scholarly purposes only. DEDICATION I would like to dedicate this dissertation to my family members for all the guidance, encouragement and support throughout my life. ACKNOWLEDGEMENTS First, I would like to take this opportunity to express my sincere gratitude to my advisor Dr. Alex Zakhidov for offering his guidance and the opportunity to work in his lab over the last four years. He helped me in numerous ways during the challenging research I was a part of and provided access to our excellent lab facilities. Dr. Zakhidov not only helped me in academic matters, but also in adjusting to the completely new culture as a newcomer from the other side of the world. Without his active supervision it would not be possible to complete my work and this thesis. I would also like to thank the other members of my dissertation committee, Dr. Edwin L. Piner, Dr. Wilhelmus J. Geerts, Dr. Casey Smith, Dr. William Chittenden for their time and valuable suggestions. I am especially grateful to Dr. Casey Smith, who helped me above and beyond his regular schedule regarding instruments and analysis. I would like to thank Dr. Dmitry Lyashenko for the technical training in the organic semiconductor lab and ARSC facilities. I would specially acknowledge my colleague Dr. Swaminathan Venkatesan. We worked together for the solar cell project from the beginning to end. I have achieved many technical skills, software skills and analysis skill thanks to him. v I would like to acknowledge Dr. Mark Hotlz for giving the opportunity to use the low temperature probe station. I am very thankful to Dr. Sanjoy Paul, who is an expert of low temperature transport study. He helped in data collection, analysis and report preparation for whole temperature dependent study. I am thankful to my fellow lab mate Dr. Chris Manspeaker, Kevin Lyon, Eric Welch, Tanjina Ahmed, Garrett Merrion, Nischal Khakurel, Aureliano Perez, Joseph Sadler. Dr. Manspeaker was my colleague for the longest time in the lab. He not only supported during the experimental work in the lab but did a thorough review of my dissertation from remote without any hesitation. My gratitude and appreciation are not enough for my wife Rafea Sultana Rea, whose support and encouragement has helped me greatly through these last few years. I look forward to helping her through her journey as she has helped me. Many thanks to my friend Anwar Siddique and Raju Ahmed for sharing their experience, characterization and analysis skills and endless support throughout the graduate life. I wish to thank Dr. Jennifer Irvin, Dr. Clois Powell and Dr. Gary Beall for their guidance and encouragement. I also like to thank MSEC staff Pizana Karla and Kelsie Crumpton; SRO staff Alissa Savage, Dr. Juan Gomez, Nate England, MSEC colleague Md. Dalim Mia, Joyce Anderson. vi I would like to acknowledge ONR HBCU/MI Instrumentation grant (#W911NF- 16-1-0518, Program Manager Dr. Paul Armistead) and American Chemical Society Petroleum Research Fund grant (#UNI656095-UNI6, Program Manager Dr. Askar Fahr) for financial support. Finally, I wish to acknowledge, all the members (this can be a very big list of names) of Bangladesh Student Association community who made San Marcos my second home also made the graduate life eventful. vii TABLE OF CONTENTS Page ACKNOWLEDGEMENTS ................................................................................................ v LIST OF TABLES ............................................................................................................ xii LIST OF FIGURES ......................................................................................................... xiii LIST OF ABBREVIATIONS .......................................................................................... xix ABSTRACT ................................................................................................................... xxiii CHAPTER 1. INTRODUCTION .......................................................................................................... 1 1.1 Overview ................................................................................................................... 1 1.2 Perovskite: Hybrid halide perovskites ....................................................................... 4 1.3 Optoelectronic properties of perovskite .................................................................... 7 1.4 Perovskite deposition techniques .............................................................................. 9 1.5 Crystal growth and optimum growth parameters .................................................... 12 1.6 Perovskite devices and device architecture ............................................................. 15 1.7 Organization of the thesis ........................................................................................ 17 2. CHARACTERIZATION TECHNIQUES .................................................................... 19 2.1 Introduction ............................................................................................................. 19 2.2 Morphological and Structural characterizations...................................................... 19 2.2.1 SEM and EDS…………………………………………………………………19 2.2.2 X-Ray diffraction (XRD) and XRD pole figure ............................................... 21 2.2.3 Atomic force microscopy (AFM) ..................................................................... 25 2.2.4 Surface profilometry ......................................................................................... 27 2.3 Electrical and Transport .......................................................................................... 27 viii 2.3.1 Current-voltage ................................................................................................. 28 2.3.2 Temperature dependent Current-Voltage ......................................................... 29 2.4 Optical ..................................................................................................................... 30 2.4.1 UV-Vis Spectroscopy ....................................................................................... 31 2.4.2 Ellipsometry...................................................................................................... 32 2.5 Electrochemical: Cyclic-voltammetry ..................................................................... 35 3. PEROVSKITE FILM PROCESSING OPTIMIZATION ............................................ 38 3.1 Introduction/literature review .................................................................................. 38 3.2 Experimental ........................................................................................................... 41 3.2.1 Synthesis of Methylammonium Acetate (MAAc) ...................................... 42 3.2.2 Preparation of Perovskite Thin Film ................................................................ 43 3.3 Film characterization ............................................................................................... 43 3.3.1 UV-Visible spectroscopy and optical imaging of the films ............................. 43 3.3.2 FTIR.................................................................................................................. 45 3.3.3 SEM Measurements .......................................................................................... 46 3.3.4 XRD .................................................................................................................. 49 3.3.5 Pole figure analysis ........................................................................................... 51 3.3.6 Crystal growth hypothesis and scope for future research ................................. 56 3.3.7 Ellipsometry...................................................................................................... 59 3.3.8 Thickness control of perovskite thin film ......................................................... 68 4. MAAc ASSISTED PEROVSKITE OPTOELECTRONIC DEVICES ........................ 73 4.1 Introduction ............................................................................................................. 73 4.2 Perovskite solar cell device architecture and operation .......................................... 74 4.3 Solar cell model and performance parameters ........................................................ 75 4.4 Solar cell fabrication ..............................................................................................