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Generalized One-Pot Synthesis of Copper Sulfide, Selenide-Sulfide, and Telluride-Sulfide Nanoparticles

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Department of Nanochemistry, Istituto Italiano di Tecnologia, via Morego 30, 16163 Genova, Italy
*E-mail: [email protected]
Cite this: Chem. Mater. 2014, 26, 3, 1442–1449
Publication Date (Web):January 9, 2014
https://doi.org/10.1021/cm4035598
Copyright © 2014 American Chemical Society
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    Abstract

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    Here we report a facile approach to synthesize copper chalcogenide (Cu2–xS, Cu2–xSeyS1–y and Cu2–xTeyS1–y) nanocrystals without employing hot-injection, at moderate reaction temperatures (200–220 °C) and free of phosphines. Scaling up of the synthesis yields monodisperse nanoparticles without variations in their morphology. We have observed the formation of alloyed copper selenide-sulfide and telluride-sulfide nanocrystals due to the incorporation of sulfur by using 1-dodecanethiol as a ligand along with oleic acid. The materials obtained possess localized surface plasmon resonances in the near-infrared region, which are demonstrated to be widely tunable via a controlled oxidation generating copper vacancies. Copper sulfide nanoparticles with well-defined initial chalcocite crystal phase were subjected to oxidation followed by structural characterization. Structural rearrangement of the oxidized chalcocite Cu2–xS crystal lattice to roxbyite by aging is proven to release the copper vacancies. Further oxidation again can create new copper vacancies in the roxbyite lattice, however its structure does not evolve into covellite CuS. These findings suggest that besides nonstoichiometry (i.e., the value of x) induced by oxidation, crystal structure is an important factor responsible for plasmonic properties of copper chalcogenide nanocrystals. Furthermore, successful water solubilization of Cu2–xTeyS1–y nanoparticles with preservation of their plasmon band has been realized via a ligand exchange approach employing a mPEG-SH stabilizer.

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    Histograms displaying size distributions of Cu2–xS, Cu2–xSeyS1–y, and Cu2–xTeyS1–y NCs. TEM images demonstrating a spontaneous self-assembly of Cu2–xS and Cu2–xSeyS1–y NCs. TEM images of Cu2–xSeyS1–y NCs obtained from scaled up synthesis as well as of Cu2–xTeyS1–y NCs synthesized in DDT. Absorbance spectra of DDT and the mixture of DDT with Te powder after heating. Crystal structures of high and low chalcocite Cu2S unit cells. Electron diffraction patterns of Cu2–xS, Cu2–xSeyS1–y and Cu2–xTeyS1–y NCs. HRTEM images of individual Cu2–xS, Cu2–xSeyS1–y and Cu2–xTeyS1–y particles, crystal structures of which differ from the corresponding dominant phases. XRD patterns of as-synthesized Cu2–xS NCs, oxidized by addition of CAN, aged by storage and additionally CAN-oxidized aged sample. Absorbance spectra of Cu7S4 NC colloid before and after a stepwise addition of CAN. TEM images of Cu2–xS NCs before and after oxidation. Absorbance spectra of small size Cu2–xSeyS1–y NCs before and after their oxidation. Details of the ligand exchange on Cu2–xTeyS1–y NCs. Absorbance spectra and TEM images of Cu2–xTeyS1–y NCs before and after the ligand exchange and water solubilization. This information is available free of charge via the Internet at http://pubs.acs.org.

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