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Solvothermal Preparation, Processing, and Characterization of Nanocrystalline CuIn1-xAlxSe2 Materials

Published online by Cambridge University Press:  31 January 2011

Christopher L. Exstrom
Affiliation:
exstromc@unk.edu, University of Nebraska at Kearney, Chemistry, Kearney, Nebraska, United States
Jiří Olejníček
Affiliation:
olejn@fzu.cz, University of Nebraska at Kearney, Chemistry, Kearney, Nebraska, United States
Scott A. Darveau
Affiliation:
darveausa@unk.edu, University of Nebraska at Kearney, Chemistry, Kearney, Nebraska, United States
Anatole Mirasano
Affiliation:
mirasanoa1@unk.edu, University of Nebraska at Kearney, Chemistry, Kearney, Nebraska, United States
David S. Paprocki
Affiliation:
paprockids@unk.edu, University of Nebraska at Kearney, Chemistry, Kearney, Nebraska, United States
Megan L Schliefert
Affiliation:
schliefertml@unk.edu, University of Nebraska at Kearney, Chemistry, Kearney, Nebraska, United States
Matt A. Ingersoll
Affiliation:
ingersollma@unk.edu, University of Nebraska at Kearney, Chemistry, Kearney, Nebraska, United States
Laura E. Slaymaker
Affiliation:
slaymakerle@unk.edu, University of Nebraska at Kearney, Chemistry, Kearney, Nebraska, United States
Rodney J. Soukup
Affiliation:
rsoukup1@unl.edu, University of Nebraska-Lincoln, Electrical Engineering, Lincoln, Nebraska, United States
Natale J. Ianno
Affiliation:
nianno@unl.edu, University of Nebraska-Lincoln, Electrical Engineering, Lincoln, Nebraska, United States
Chad A. Kamler
Affiliation:
chadkamler@gmail.com, University of Nebraska-Lincoln, Electrical Engineering, Lincoln, Nebraska, United States
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Abstract

We report solvothermal preparations of nanocrystalline CuIn1-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 In- and 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.

Type
Research Article
Copyright
Copyright © Materials Research Society 2009

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