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Solar Energy to Hydrogen Fuel Via Highly Efficient Iii-V Semiconductors

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Solar Energy to Hydrogen Fuel Via Highly Efficient Iii-V Semiconductors SOLAR ENERGY TO HYDROGEN FUEL VIA HIGHLY EFFICIENT III-V SEMICONDUCTORS by James L. Young B.S., University of Illinois at Urbana-Champaign, 2010 A thesis submitted to the Faculty of the Graduate School of the University of Colorado in partial fulfillment of the requirement for the degree of Doctor of Philosophy Materials Science and Engineering Program 2016 ProQuest Number: 10108680 All rights reserved INFORMATION TO ALL USERS The quality of this reproduction is dependent upon the quality of the copy submitted. In the unlikely event that the author did not send a com plete manuscript and there are missing pages, these will b e noted. Also, if material had to be rem oved, a note will indicate the deletion. Pro ProQuest 10108680 Published by ProQuest LLC (2016). Copyright of the Dissertation is held by the Author. All rights reserved. This work is protected against unauthorized copying under Title 17, United States Code Microform Edition © ProQuest LLC. ProQuest LLC. 789 East Eisenhower Parkway P.O. Box 1346 Ann Arbor, Ml 48106 - 1346 This thesis entitled: Solar energy to hydrogen fuel via highly efficient III-V semiconductors written by James L. Young has been approved for the Materials Science and Engineering Program Steven M. George Todd G. Deutsch Date The final copy of this thesis has been examined by the signatories, and we find that both the content and the form meet acceptable presentation standards of scholarly work in the above mentioned discipline. Abstract Young, James Luke (Ph.D., Materials Science and Engineering) Solar energy to hydrogen fuel via highly efficient III-V semiconductors Thesis directed by research advisor Todd G. Deutsch and academic advisor Steven M. George A sustainable energy economy depends critically on the conversion of renewable energy resources, whose inherent variability requires a storage mechanism. Pathways for conversion of solar energy, being the most abundant, to fuel represent crucial areas of research. Hydrogen as a chemical energy carrier is storable and transportable, while being a feedstock for ammonia fertilizer that is essential to global food supply. Direct photoelectrochemical conversion of sunlight via water splitting is a prominent concept for clean, scalable, cost-effective, and locally produced hydrogen, but the technology is not yet commercially viable. Here, we address the technical challenges of realizing economical solar hydrogen production using III-V semiconductor-based devices: high conversion efficiency and extended lifetime in aqueous electrolyte. Solar-to-hydrogen conversion efficiency is a fundamental metric for evaluating progress that will impact introduction of commercial solar water-splitting systems. Its definition is generally agreed upon, but measurement technique standards are not well defined. We demonstrate common practices, show how they can lead to significant error, and introduce methodology and cross-validation practices for improved accuracy. The advanced techniques are relevant to device configurations based on tandem absorbers, necessary for achieving maximum conversion efficiency. We outline the development pathway for III-V tandem devices to reach maximum efficiency, demonstrate progress toward 15% enabled by a new architecture allowing lower bandgaps, and investigate alternative p-i and p-n PEC junction doping profiles that enhance photovoltage. We identify reflection as the primary loss and model anti-reflective Ti02 coatings that demonstrate improved photocurrent. We present findings on the intrinsic stability of III-V photocathodes and the development of stabilizing surface modifications. We show that water vapor reversibly passivates p-GaInP2 surfaces and derive a model describing the behavior. Bare p-GaAs photocathodes etch ~100x slower than other III-V photocathodes due to residual surface As. Bare p-GaInP2 is unstable, but surface modification involving nitridation and/or PtRu alloy co-catalyst deposition offers corrosion resistance. We show that sputtered PtRu consistently provides better initial performance than other treatment variations, making it preferable for device development. Department of Energy progress milestones are exceeded for STH efficiency and approached for durability, while considerable reduction of device processing cost remains to be addressed. iv Acknowledgements I gratefully acknowledge support from the National Science Foundation through a Graduate Research Fellowship (Grant No. DGE1144083). Further financial support was provided by the U.S. Department of Energy (DOE) under Contract No. DE-AC36-08GO28308 with the National Renewable Energy Laboratory. Thank you to my research advisor, Todd Deutsch, for introducing me to the field and continued opportunity and support throughout. Thank you to Henning Doscher and John Turner for countless valuable and challenging discussions; to Myles Steiner and Ryan France for device design; Waldo Olavarria and Alan Kibbler for operating the epitaxy systems; to Michelle Young, Arrelaine Dameron, and Anna Duda for device processing assistance; and to John Geisz for use of the band bending calculator. Thank you to Steven George for academic advising, providing ALD advice, use of reactors and related equipment; and to Chris Bowman and Sabria Khushad for advising specific to the Materials Science and Engineering Program. V Table of Contents Title page ......................................................................................................................................................i Signature page ...........................................................................................................................................ii A bstract ......................................................................................................................................................iii Acknowledgements ..................................................................................................................................iv Table of contents ....................................................................................................................................... v List of tables .............................................................................................................................................. vi List of figures ...........................................................................................................................................vii List of publications .................................................................................................................................. ix 1. Introduction and background ............................................................................................................1 1.1 Renewable hydrogen from abundant sunlight......................................................................1 1.2 Tandems: III-V PEC state of the art ..................................................................................... 6 2. Development of auxiliary components and techniques ..............................................................14 2.1 Evaluation of common characterization practices .............................................................14 2.2 Components for on-sun and two-source solar simulation ............................................... 24 2.3 Photoelectrode mounting and compression cell design ................................................... 32 2.4 Measuring the spectral response of tandems .................................................................... 38 3. Tandem III-V semiconductor devices for water splitting .......................................................... 42 3.1 Toward maximum efficiency with III-Vs ........................................................................42 3.2 Light-limited photocurrent: Band gap and reflection .......................................................47 3.3 Photocurrent onset potential: Improving with doping profiles ....................................... 54 3.4 Design and demonstration of anti-reflective Ti02 coating ..............................................65 4. Stability and stabilization of III-Vs ................................................................................................71 4.1 Surface passivation of GaInP2 by water vapor ..................................................................71 4.2 Remarkable stability of unmodified GaAs photocathodes .............................................. 83 4.3 Stabilizing GaInP2 with nitridation and Pt/Ru sputtering ................................................96 5. Conclusions and outlook ................................................................................................................. 117 4.1 Conclusions .......................................................................................................................... 117 4.1 Outlook ..................................................................................................................................118 Complete bibliography ........................................................................................................................ 120 vi List of tables Chapter 2 Tables 2.2.1 Collimating tube design parameters ........................................................................................ 27 Chapter 4 Tables 4.3.1 Tabulated Pt and Ru loading averages ...................................................................................102 4.3.2 Summary of durability metrics ...............................................................................................106
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