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Characterization of Nanostructured Semiconductors by Ultrafast CHARACTERIZATION OF NANOSTRUCTURED SEMICONDUCTORS BY ULTRAFAST LUMINESCENCE IMAGING by Jolie Blake A dissertation submitted to the Faculty of the University of Delaware in partial fulfillment of the requirements for the degree of Doctor of Philosophy in Chemistry and Biochemistry Summer 2017 c 2017 Jolie Blake All Rights Reserved CHARACTERIZATION OF NANOSTRUCTURED SEMICONDUCTORS BY ULTRAFAST LUMINESCENCE IMAGING by Jolie Blake Approved: Murray Johnston, Ph.D. Chair of the Department of Chemistry & Biochemistry Approved: George H. Watson, Ph.D. Dean of the College of Arts & Sciences Approved: Ann L. Ardis, Ph.D. Senior Vice Provost for Graduate and Professional Education I certify that I have read this dissertation and that in my opinion it meets the academic and professional standard required by the University as a dissertation for the degree of Doctor of Philosophy. Signed: Lars Gundlach, Ph.D. Professor in charge of dissertation I certify that I have read this dissertation and that in my opinion it meets the academic and professional standard required by the University as a dissertation for the degree of Doctor of Philosophy. Signed: Andrew V. Teplyakov, Ph.D. Member of dissertation committee I certify that I have read this dissertation and that in my opinion it meets the academic and professional standard required by the University as a dissertation for the degree of Doctor of Philosophy. Signed: Mathew DeCamp, Ph.D. Member of dissertation committee I certify that I have read this dissertation and that in my opinion it meets the academic and professional standard required by the University as a dissertation for the degree of Doctor of Philosophy. Signed: Joshua Zide, Ph.D. Member of dissertation committee ACKNOWLEDGEMENTS These past 6 years have been truly transformative. I have deepened my knowl- edge of chemistry, fallen in and out of love with my work and gained a mind flexible enough to tackle any problem. More importantly, this period has taught me about my- self, my weaknesses and strengths and provided a thorough and invaluable education on human nature. I am grateful for being given the opportunity to experience all of these things, the good and especially the bad. I must acknowledge all the people that helped shaped this experience. I would like to thank the members of the Gundlach Group, past and present, because without them this work would not be possible. In particular, I would like to thank Dr. Lars Gundlach for his hands-on help in the lab, help with preparing this dissertation and for having an open door policy. I would also like to thank Dr. Jesus Nieto-Pescador for this constant willingness to help me align my NOPA and for his patience in teaching me optical alignment. I thank Dr. Peter Eldridge for his work with Igor, which made it possible to efficiently collect and analyze data and hence significantly speed up the period towards publication. I am thankful to Baxter Abraham for his help with the optics, his great sense of humor and his resourcefulness in procuring things we needed in the lab. Additionally, I thank Dr. Zide who took the time to provide insight on semiconductor material properties, which turned out to be truly invaluable to completing this dissertation. I want to acknowledge Dr. Sharon Neal whose grace and wisdom I hope to someday acquire. I am truly grateful for the talks that we had and how, like a sage, you always knew what to say and had the right answers to every situation. Your advice and mentorship were instrumental to me completing my Ph.D. iv I am thankful for the other members of the Chemistry & Biochemistry Depart- ment such as Doug Nixon and Susan Cheadle. I want to thank Doug for helping me learn how to handle different types of glass, for quickly repairing my numerous cracked quartz tubes and for his useful input in helping me manifest many of my ideas. Susan Cheadle was always ready to help with the necessary paper work at each stage of my academic career. I especially want to thank her for helping me sort out my immigration documents to ensure my continued enrollment in the program. I am also thankful for the University of Delaware NOBCChE student chapter and its members. The chapter's events would not have been possible if it was not for the support of Dr. Murray Johnston who pledged his support for the group from the beginning. I want to thank the NOBCChE student members for supporting me and the other founding members in the creation of this chapter and for helping me with my vision of establishing our professional network. To Ornella Sathoud, supportive NOBCChE board member and friend, thank you for being a fellow black female scientist in this marginalizing environment and for being a formidable and resilient force of nature. I am grateful for our long talks on racism, prejudice and perseverance in this program despite the odds. I truly admire your determination. I have discovered the beauty in being constantly undermined, disparaged, treated less than and having your ability questioned is that it acts as a refining process. It polishes you into a person who does not rely on external validation or acknowledgment in pursuit of your highest potential. It helps you to recognize that your place here was not acquired by charity or luck but hard earned. If you have not already realized this effect I strongly believe you will soon. I cannot forget my undergraduate advisor Dr. Katherine Plass. If it was not for you sharing your undying passion and enthusiasm for research with me I probably would not be here today. If it was not for your insightful advice early on in this program, I definitely would not have been here today completing my Ph.D. Thank you for being a great teacher, advisor and mentor. Thank you for giving me the opportunity to work in your lab, encouraging me to pursue graduate school and for believing that v I had what it took to be a good researcher and chemist. Lastly, I want to thank my mom, my significant other Jonathan and the rest of my family. Jonathan, thank you for being so selfless, understanding and patient and for all those long nights you sat in my office waiting for me while I worked in the lab. It would not have been possible without you. Mom, I dedicate this dissertation to you. You were my first teacher, my biggest supporter, my one-woman fan club and the one person who never once doubted my ability to do anything especially completing this program. Thank you for your sacrifice, constant encouragement and prayers. You may write me down in history With your bitter, twisted lies, You may trod me in the very dirt But still, like dust, I'll rise. You may shoot me with your words, You may cut me with your eyes, You may kill me with your hatefulness, But still, like air, I'll rise. Maya Angelou (1921-2014) vi TABLE OF CONTENTS LIST OF TABLES :::::::::::::::::::::::::::::::: x LIST OF FIGURES ::::::::::::::::::::::::::::::: xi ABSTRACT ::::::::::::::::::::::::::::::::::: xviii Chapter 1 INTRODUCTION :::::::::::::::::::::::::::::: 1 1.0.1 Measuring the electronic properties of nanostructures ::::: 6 1.1 Amplified Spontaneous Emission :::::::::::::::::::: 7 1.2 Objectives ::::::::::::::::::::::::::::::::: 11 2 EXPERIMENTAL METHODS :::::::::::::::::::::: 13 2.1 Ultrafast Kerr-gated Microscope ::::::::::::::::::::: 13 2.1.1 Kerr-electro-optic effect ::::::::::::::::::::: 13 2.1.2 Laser system ::::::::::::::::::::::::::: 17 2.1.3 Microscope optical setup ::::::::::::::::::::: 19 2.1.4 Ultraviolet Configuration ::::::::::::::::::::: 20 2.1.5 Modes of operation :::::::::::::::::::::::: 20 2.2 Sample Preparation :::::::::::::::::::::::::::: 21 3 KERR-GATED MICROSCOPY IN THE VISIBLE DETECTION vii RANGE :::::::::::::::::::::::::::::::::::: 24 3.1 Cadmium Sulfide Selenide Semiconductor material ::::::::::: 24 3.1.1 CdSxSe1−x Nanostructure Synthesis ::::::::::::::: 25 3.2 Ultrafast Measurements ::::::::::::::::::::::::: 26 3.2.1 Spatial Variation in Carrier Dynamics ::::::::::::: 26 3.3 Extracting non-radiative recombination rates in a single CdSxSe1−x nanowire :::::::::::::::::::::::::::::::::: 35 3.3.1 Introduction :::::::::::::::::::::::::::: 35 3.3.2 Materials and Methods :::::::::::::::::::::: 36 3.3.3 Results and discussion :::::::::::::::::::::: 38 3.3.4 Conclusions :::::::::::::::::::::::::::: 41 4 ZINC OXIDE SEMICONDUCTOR MATERIAL :::::::::: 42 4.1 Historical Timeline :::::::::::::::::::::::::::: 42 4.2 Fundamental properties and applications :::::::::::::::: 43 4.2.1 Crystal structure ::::::::::::::::::::::::: 45 4.3 Synthesis and growth ::::::::::::::::::::::::::: 46 4.3.1 Vapor Phase Synthesis of ZnO :::::::::::::::::: 48 4.3.2 Solution based Synthesis of ZnO ::::::::::::::::: 55 4.4 Point defects :::::::::::::::::::::::::::::::: 69 5 ULTRAVIOLET FEMTOSECOND KERR-GATED MICROSCOPY ::::::::::::::::::::::::::::::: 75 5.1 Kerr Medium Selection for the UV ::::::::::::::::::: 75 5.2 Preliminary Ultrafast Measurements :::::::::::::::::: 78 5.2.1 ZnO single nanowire samples :::::::::::::::::: 78 5.2.2 Steady State Measurements ::::::::::::::::::: 78 5.2.3 Time-resolved Spectroscopy ::::::::::::::::::: 82 viii 5.2.4 Time-resolved Imaging :::::::::::::::::::::: 85 5.3 Conclusion ::::::::::::::::::::::::::::::::: 87 6 KERR-GATED MICROSCOPY FOR MEASURING DEFECT DENSITY ::::::::::::::::::::::::::::::::::: 89 6.1 Introduction :::::::::::::::::::::::::::::::: 89 6.2 Results and Discussion :::::::::::::::::::::::::: 92 6.2.1 Steady state measurements :::::::::::::::::::: 92 6.2.2 Time resolved measurements ::::::::::::::::::: 95 6.2.3 Recombination rates from the Amplified Spontaneous
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