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Solution Processing for Copper Indium Sulfide Solar Cells

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Solution Processing for Copper Indium Sulfide Solar Cells SOLUTION PROCESSING FOR COPPER INDIUM SULFIDE SOLAR CELLS A DISSERTATION SUBMITTED TO THE DEPARTMENT OF CHEMISTRY AND THE COMMITTEE ON GRADUATE STUDIES OF STANFORD UNIVERSITY IN PARTIAL FULFILLMENT OF THE REQUIREMENTS FOR THE DEGREE OF DOCTOR OF PHILOSOPHY Stephen Thacker Connor August 2011 © 2011 by Stephen Thacker Connor. All Rights Reserved. Re-distributed by Stanford University under license with the author. This work is licensed under a Creative Commons Attribution- Noncommercial 3.0 United States License. http://creativecommons.org/licenses/by-nc/3.0/us/ This dissertation is online at: http://purl.stanford.edu/wr798sx5189 ii I certify that I have read this dissertation and that, in my opinion, it is fully adequate in scope and quality as a dissertation for the degree of Doctor of Philosophy. Yi Cui, Primary Adviser I certify that I have read this dissertation and that, in my opinion, it is fully adequate in scope and quality as a dissertation for the degree of Doctor of Philosophy. Christopher Chidsey I certify that I have read this dissertation and that, in my opinion, it is fully adequate in scope and quality as a dissertation for the degree of Doctor of Philosophy. T Stack Approved for the Stanford University Committee on Graduate Studies. Patricia J. Gumport, Vice Provost Graduate Education This signature page was generated electronically upon submission of this dissertation in electronic format. An original signed hard copy of the signature page is on file in University Archives. iii Abstract In recent years, the field of photovoltaics has become increasingly important due to rising energy demand and climate change. While most solar cells are currently composed of crystalline silicon, devices with thinner films of inorganic absorber materials might allow production at a greater scale due to their lower materials cost. In particular, thin films of CuInS 2 are promising solar absorber materials due to their high efficiencies and low required thicknesses. However, the fabrication of thin film solar cells currently requires expensive vacuum techniques. As an alternative, solution-based deposition techniques have been proposed as a route to low-cost and high-throughput electronic device fabrication. In this dissertation, I will describe two approaches developed to solution process CuInS 2 solar absorber layers from nanoparticle precursors. Many common solution techniques can quickly deposit thick layers of nanoparticulate material, but these layers must be subsequently converted into a final compact semiconductor thin film by annealing. The primary limitation in solution processed thin films tends to be the lack of grain growth during annealing, which degrades electrical properties. I have studied how film growth depends on precursor film quality, with the goal of producing large grained films of CuInS 2 through solution processing. In the first approach, we used solvothermal decomposition of organometallic precursors at moderate temperatures to produce nanoparticles of CuInS 2. In order to determine the growth mechanism of these nanoparticles, we analyzed the structure and phase of these nanoparticles by transmission electron microscopy and X-ray diffraction. Thin films of these nanoparticles were cast onto molybdenum coated glass and further processed to create CuInS 2 solar cells. We found that performance was dependent on film porosity, grain size, and stoichiometry of the nanoparticles. Films with grain sizes of ~200nm were attained, from which 1.3% efficient solar cells were made. In addition, we showed that this synthesis could be extended to produce CuInS 2 nanoparticles with partial substitution of Fe, Zn, and Ga. The substitution of In or Cu with other elements allows tuning of the band gap and is the first step in producing iv more complicated structures such as layers with graded compositions for improved device performance. In the second approach, we synthesized an air-stable hybrid organometallic/nanoparticle ink at room temperature in ambient conditions through a vulcanization reaction. This ink could be coated onto substrates in smooth layers, and further reactive annealing formed large grained CuInS 2 films. This process was characterized, and a correlation between residual carbon and grain growth was found. Additionally, the chemical transformation between precursor layers and final sulfide thin film was analyzed, with an emphasis on the difference between sulfurization and selenization. We demonstrated that the sulfurization process was producing morphological defects due to its nucleation limited growth mechanism. However, it was modified to more closely resemble the diffusion limited selenization mechanism, thus producing flat films of CuInS 2 with grain sizes of ~500nm. v Acknowledgements This dissertation wouldn’t have been possible without the help and support of a whole gaggle of people. Foremost I’d like to thank my girlfriend Egle Cekanaviciute who edited almost every word in this document and also tolerated late night microscopy and other such tragedies. Second, I thank my adviser, Yi Cui, for his extensive guidance and keen scientific insights through the years. The entire Cui research group has been amazing and exciting to work within; in particular Ben Weil and Ching-Mei Hsu have been sounding boards for all of my terrible ideas, and thus deserve countless thanks. I’d like to thank my collaborators: Sumohan Misra and Mike Toney at the Stanford Linear Accelerator; Jung-Yong Lee and Peter Peuman in the Department of Electrical Engineering; and Mary Tang at the Stanford Nanofabrication Facility. In addition, the staff members of the Moore and McCullough buildings have been wonderful; in particular I offer heartfelt thanks to Christina Konjevich and Benita Givens for helping avert administrative doom many times and Mark Gibson for literally keeping the Moore building together. Finally, I’d like to thank my family and friends for the years of emotional support and good times. My mother and father, Cindy Floyd and Gordon Connor, have always stood by me, for which I’m very lucky and grateful. Lastly, I’d like to honor the memory of Jeanne Connor; I will always aspire to one day be as brilliant and good as she believed I was. vi Table of Contents Abstract…………………….…………………………………………………………iv Acknowledgements…………..…………………………………………………….…vi Table of Contents…………………………………………………………………..…vii List of Tables……………………………………………………………….…………xi List of Figures…………………………………………………...……………………xii 1 Introduction and Background ............................................................................. 1 1.1 Solar Cell Design Principles ............................................................................ 2 1.1.1 Solar Spectrum ......................................................................................... 2 1.1.2 Structure and Performance ....................................................................... 3 1.1.3 Important Parameters ................................................................................ 5 1.2 Thin Film Solar Cell Development .................................................................. 6 1.3 Solution Processing .......................................................................................... 8 1.4 Solution Deposition Techniques ...................................................................... 9 1.4.1 Spray Coating ......................................................................................... 10 1.4.2 Spin Coating ........................................................................................... 10 1.4.3 Paste Coating .......................................................................................... 10 1.4.4 Bath Depositions .................................................................................... 11 1.5 Ink Compositions ........................................................................................... 11 1.5.1 Solution-based Inks ................................................................................ 12 1.5.2 Nanoparticle-based Inks ......................................................................... 13 1.5.3 Hybrid Approaches ................................................................................. 14 2 Methods ............................................................................................................... 16 2.1 CuInS 2 Precursor Films from Nanoparticle Ink ............................................. 16 2.1.1 Oleate Precursor Synthesis ..................................................................... 16 2.1.2 CuInS 2 Nanoparticle Synthesis ............................................................... 17 vii 2.1.3 Deposition of CuInS 2 nanoparticle film ................................................. 18 2.2 Cu-In-O Precursor Films from Hybrid Nanoparticle Ink .............................. 18 2.2.1 Preparation of Hybrid Ink ....................................................................... 18 2.2.2 Deposition of Cu-In-O Film ................................................................... 18 2.3 Sulfurization of Cu-In-O and CuInS 2 NP films ............................................. 19 2.4 Solar Cell Device Fabrication ........................................................................ 20 2.5 Analytical Techniques ................................................................................... 20 2.5.1 Transmission Electron Microscopy (TEM) ............................................ 20 2.5.2 Selected Area Electron Diffraction (SAED)
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