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Processing of Cuinse2-Based Solar Cells: Characterization of Deposition Processes in Terms of Chemical Reaction Analyses

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Processing of Cuinse2-Based Solar Cells: Characterization of Deposition Processes in Terms of Chemical Reaction Analyses June 2001 • NREL/SR-520-30391 Processing of CuInSe2-Based Solar Cells: Characterization of Deposition Processes in Terms of Chemical Reaction Analyses Final Report 6 May 1995―31 December 1998 T.J. Anderson and B.J. Stanbery University of Florida Gainesville, Florida National Renewable Energy Laboratory 1617 Cole Boulevard Golden, Colorado 80401-3393 NREL is a U.S. Department of Energy Laboratory Operated by Midwest Research Institute • Battelle • Bechtel Contract No. DE-AC36-99-GO10337 NOTICE This report was prepared as an account of work sponsored by an agency of the United States government. Neither the United States government nor any agency thereof, nor any of their employees, makes any warranty, express or implied, or assumes any legal liability or responsibility for the accuracy, completeness, or usefulness of any information, apparatus, product, or process disclosed, or represents that its use would not infringe privately owned rights. Reference herein to any specific commercial product, process, or service by trade name, trademark, manufacturer, or otherwise does not necessarily constitute or imply its endorsement, recommendation, or favoring by the United States government or any agency thereof. The views and opinions of authors expressed herein do not necessarily state or reflect those of the United States government or any agency thereof. Available electronically at http://www.doe.gov/bridge Available for a processing fee to U.S. Department of Energy and its contractors, in paper, from: U.S. Department of Energy Office of Scientific and Technical Information P.O. Box 62 Oak Ridge, TN 37831-0062 phone: 865.576.8401 fax: 865.576.5728 email: [email protected] Available for sale to the public, in paper, from: U.S. Department of Commerce National Technical Information Service 5285 Port Royal Road Springfield, VA 22161 phone: 800.553.6847 fax: 703.605.6900 email: [email protected] online ordering: http://www.ntis.gov/ordering.htm Printed on paper containing at least 50% wastepaper, including 20% postconsumer waste June 2001 • NREL/SR-520-30391 Processing of CuInSe2-Based Solar Cells: Characterization of Deposition Processes in Terms of Chemical Reaction Analyses Final Report 6 May 1995―31 December 1998 T.J. Anderson and B.J. Stanbery University of Florida Gainesville, Florida NREL Technical Monitor: Bolko von Roedern Prepared under Subcontract No. XAF-5-14142-10 National Renewable Energy Laboratory 1617 Cole Boulevard Golden, Colorado 80401-3393 NREL is a U.S. Department of Energy Laboratory Operated by Midwest Research Institute • Battelle • Bechtel Contract No. DE-AC36-99-GO10337 This Dissertation by Dr. Billy J. Stanbery describes in great detail many aspects of the research carried out by Billy Stanbery in pursuing his degree at the University of Florida (UF) under the direction of Prof. Tim Anderson. This project was initiated after the Boeing Company decided to terminate its photovoltaic research and development efforts, and donated some research equipment to UF. Billy Stanbery, who was part of the Boeing team, decided then to enroll at UF to pursue a Ph.D degree. As such these events constituted a rare direct technology transfer from industry to a university. This helped to preserve more than the published legacy of the solar cell efforts at Boeing, and jump-started a comprehensive, multifaceted, and multidisciplinary copper indium diselenide solar cell research effort at UF. Bolko von Roedern Technical Monitor, May 2001 Copyright 2001 By Billy Jack Stanbery To those dedicated teachers whose encouragement enabled me and whose vision inspired me to persevere: B. M. Stanberry M. E. Oakes W. T. Guy, Jr. G. C. Hamrick S. C. Fain M. P. Gouterman R. A. Mickelsen W. S. Chen L. E. Johns, Jr. R. Narayanan ACKNOWLEDGMENTS The long voyage of discovery I have labored to share in this dissertation could not have been realized without the contributions of a multitude of others that have chosen to invest their hope and efforts in mine. My study of this subject began over two decades ago, and prior to coming to the University of Florida was conducted mostly while employed by The Boeing Company. Their generous donation to the University of the key research equipment used to conduct this research provided irreplaceable physical assets that have made it possible. This would not have happened without the advocacy within Boeing of Dr. Theodore L. Johnson, for which I am very grateful. This research would likewise not have been possible without the financial support of the United States Department of Energy provided through contract numbers XCG–4–14194–01, XAF–5–14142–10 and XAK–8–17619–32 from the National Renewable Energy Laboratory. Although these contracts were won through competitive procurement processes, the encouragement of K. Zweibel and J. Benner, providing me hope that I might succeed (but could only if I tried), was indispensable motivation, and I thank them both. I would like to thank my advisor, Professor T. J. Anderson, for recruiting me to the University, providing laboratory space at the University's iv MicroFabritech facility, and assembling the interdisciplinary research team within which I worked over the course of this doctoral research program. Every member of that team has contributed to this work, but I must particularly thank Dr. Albert Davydov and Dr. Chih–Hung (Alex) Chang who were always available, capable, and willing to engage in the intellectual exchanges that I have found to be the most compelling fount of insight. I am also indebted to Dr. Weidong Zhuang who provided me an advanced copy of the results of the critical assessment of the binary Cu–Se system that he and Dr. Chang performed. Those familiar with laboratory research recognize the enormous value of those who help a researcher with the essential but unglamorous and tedious tasks that actually absorb most of the time and effort required to conduct successful research of this sort. I thank W. P. Axson who helped me turn an empty space and truck full of unfinished, disassembled equipment into a productive and safe laboratory filled with operational state-of-the-art research systems, and taught me plumbing and electrical skills in the process. The control automation system that finally tamed the reactor and consolidated the data acquisition process was the work of my research assistant S. Kincal, whom I thank as well. Without his assistance the quadrapole mass spectrometric measurements could not have been performed. The EDX composition measurements vital to calibration and data interpretation were the work of my other laboratory assistant S. Kim, whom I also thank. I reaped the benefits of the support of the entire staff of MicroFabritech, especially S. Gapinski and v D. Badylak, who providing a dependable and indispensable laboratory infrastructure. I also thank the following University staff, faculty, and students who helped with advice, parts, measurements, and characterization: W. Acree, M. Davidson, D. Dishman, E. Lambers, and J. Trexler. Outside of this University, I would like to thank Dr. S. P. Ahrenkiel (NREL), who provided TEM measurements; Dr. G. Lippold (Universität Leipzig), who provided Raman measurements; and Dr. M. Klenk (Universität Konstanz), who provided XRF measurements. I would also like to thank some of those in the scientific community at large who have shared their time and thoughts with me during the course of this graduate program: Dr. M. Al–Jassim, Dr. R. Noufi, Dr. K. Ramanathan, Prof. A. Rockett, Dr. B. von Roedern, Prof. E. Vlieg, and Prof. J. Venables. Finally, I would like to thank Sue Wagner and my parents, Martha and Bill Stanberry, without whose faith, hope, support, help, encouragement, and love I could not have succeeded. vi TABLE OF CONTENTS page ACKNOWLEDGMENTS ...............................................................................................iv LIST OF TABLES .............................................................................................................. x LIST OF FIGURES ...........................................................................................................xi ABSTRACT................................................................................................................... xvii CHAPTERS 1 REVIEW OF PRIOR RESEARCH: CIS MATERIALS FOR PHOTOVOLTAIC DEVICES................................................................................. 1 Phase Chemistry of Cu–III–VI Material Systems ................................................3 The Cu–In–Se (CIS) Material System..................................................................4 The Cu–Ga–Se (CGS) Material System ...............................................................7 The Cu–In–S (CISU) Material System .................................................................9 Crystallographic Structure of the Ternary CIS Compounds............................. 10 α–CIS (Chalcopyrite CuInSe2)............................................................................ 11 δ–CIS (Sphalerite) ................................................................................................13 β–CIS (Cu2In4Se7 and CuIn3Se5)......................................................................... 14 γ–CIS (CuIn5Se8)................................................................................................... 17 Metastable Crystallographic Structures — CuAu–ordering........................18 Defect Structure of α–CIS ..................................................................................
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