Solvothermal preparation, processing, and characterization of nanocrystalline CuIn1-xAlxSe2 materials

Christopher L. Exstrom; Jiří Olejníček; Scott A. Darveau; Anatole Mirasano; David S. Paprocki; Megan L. Schliefert; Matt A. Ingersoll; Laura E. Slaymaker; R. J. Soukup; N. J. Ianno; C. A. Kamler

Solvothermal preparation, processing, and characterization of nanocrystalline CuIn_1-xAl_xSe₂ materials

Christopher L. Exstrom, Jiří Olejníček, Scott A. Darveau, Anatole Mirasano, David S. Paprocki, Megan L. Schliefert, Matt A. Ingersoll, Laura E. Slaymaker, R. J. Soukup, N. J. Ianno, C. A. Kamler

Chemistry

Research output: Chapter in Book/Report/Conference proceeding › Conference contribution

1 Scopus citations

Abstract

We report solvothermal preparations of nanocrystalline CuIn _1-xAl_xSe₂ materials prepared from the reaction of Se, CuX₂ (X = Cl^- or stearate), InCl₃, and Al(oleate)₃ in refluxing oleylamine for 30 minutes to 3 hours. Scanning electron microscopy (SEM) images reveal morphologies consisting of hexagonal plates (100-400 nm diameter) with smaller isomorphic nodules. Micro-Raman spectroscopy, x-ray diffraction, and optical bandgap data are consistent with Al³⁺ incorporation into the chalcopyrite structure. For aluminum-containing reactions, product Al/(In+Al) ratios are estimated to be between 0.15 and 0.35 regardless of the indium-aluminum stoichiometry employed in the reaction. When Se is added to the reaction last, the reaction pathway involves an early-formed Cu_2-xSe(s) intermediate that appears to react with Inand Al-containing species simultaneously. This intermediate is avoided when heating InCl₃, Al(oleate)₃, and Se together prior to Cu addition, but the final product includes Se contamination that must be removed or reacted by annealing.

Original language	English (US)
Title of host publication	Thin-Film Compound Semiconductor Photovoltaics - 2009
Pages	153-158
Number of pages	6
State	Published - 2010
Event	2009 MRS Spring Meeting - San Francisco, CA, United States Duration: Apr 13 2009 → Apr 17 2009

Publication series

Name	Materials Research Society Symposium Proceedings
Volume	1165
ISSN (Print)	0272-9172

Conference

Conference	2009 MRS Spring Meeting
Country/Territory	United States
City	San Francisco, CA
Period	4/13/09 → 4/17/09

ASJC Scopus subject areas

General Materials Science
Condensed Matter Physics
Mechanics of Materials
Mechanical Engineering

Cite this

Exstrom, C. L., Olejníček, J., Darveau, S. A., Mirasano, A., Paprocki, D. S., Schliefert, M. L., Ingersoll, M. A., Slaymaker, L. E., Soukup, R. J., Ianno, N. J., & Kamler, C. A. (2010). Solvothermal preparation, processing, and characterization of nanocrystalline CuIn_1-xAl_xSe₂ materials. In Thin-Film Compound Semiconductor Photovoltaics - 2009 (pp. 153-158). (Materials Research Society Symposium Proceedings; Vol. 1165).

Solvothermal preparation, processing, and characterization of nanocrystalline CuIn_1-xAl_xSe₂ materials. / Exstrom, Christopher L.; Olejníček, Jiří; Darveau, Scott A. et al.
Thin-Film Compound Semiconductor Photovoltaics - 2009. 2010. p. 153-158 (Materials Research Society Symposium Proceedings; Vol. 1165).

Research output: Chapter in Book/Report/Conference proceeding › Conference contribution

Exstrom, CL, Olejníček, J, Darveau, SA, Mirasano, A, Paprocki, DS, Schliefert, ML, Ingersoll, MA, Slaymaker, LE, Soukup, RJ, Ianno, NJ & Kamler, CA 2010, Solvothermal preparation, processing, and characterization of nanocrystalline CuIn_1-xAl_xSe₂ materials. in Thin-Film Compound Semiconductor Photovoltaics - 2009. Materials Research Society Symposium Proceedings, vol. 1165, pp. 153-158, 2009 MRS Spring Meeting, San Francisco, CA, United States, 4/13/09.

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abstract = "We report solvothermal preparations of nanocrystalline CuIn 1-xAlxSe2 materials prepared from the reaction of Se, CuX2 (X = Cl- or stearate), InCl3, and Al(oleate)3 in refluxing oleylamine for 30 minutes to 3 hours. Scanning electron microscopy (SEM) images reveal morphologies consisting of hexagonal plates (100-400 nm diameter) with smaller isomorphic nodules. Micro-Raman spectroscopy, x-ray diffraction, and optical bandgap data are consistent with Al3+ incorporation into the chalcopyrite structure. For aluminum-containing reactions, product Al/(In+Al) ratios are estimated to be between 0.15 and 0.35 regardless of the indium-aluminum stoichiometry employed in the reaction. When Se is added to the reaction last, the reaction pathway involves an early-formed Cu2-xSe(s) intermediate that appears to react with Inand Al-containing species simultaneously. This intermediate is avoided when heating InCl3, Al(oleate)3, and Se together prior to Cu addition, but the final product includes Se contamination that must be removed or reacted by annealing.",

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AU - Schliefert, Megan L.

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AB - We report solvothermal preparations of nanocrystalline CuIn 1-xAlxSe2 materials prepared from the reaction of Se, CuX2 (X = Cl- or stearate), InCl3, and Al(oleate)3 in refluxing oleylamine for 30 minutes to 3 hours. Scanning electron microscopy (SEM) images reveal morphologies consisting of hexagonal plates (100-400 nm diameter) with smaller isomorphic nodules. Micro-Raman spectroscopy, x-ray diffraction, and optical bandgap data are consistent with Al3+ incorporation into the chalcopyrite structure. For aluminum-containing reactions, product Al/(In+Al) ratios are estimated to be between 0.15 and 0.35 regardless of the indium-aluminum stoichiometry employed in the reaction. When Se is added to the reaction last, the reaction pathway involves an early-formed Cu2-xSe(s) intermediate that appears to react with Inand Al-containing species simultaneously. This intermediate is avoided when heating InCl3, Al(oleate)3, and Se together prior to Cu addition, but the final product includes Se contamination that must be removed or reacted by annealing.

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