Synthesis and structure of nanocrystalline copper sulfides with djurleite and covellite structures

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Resumo

Method of chemical deposition from water solutions of copper nitrate and sodium sulphide, and also from water solutions of copper nitrate with use thiocarbonic acid diamide as sufidizer in the presence of Trilon stabilizer are synthesized nanocrystalline powders of copper sulfides with structures of covellite and djurleite. It is established, that as a result of sulfidization of copper nitrate by sodium sulphide forms powders of copper sulfides with the particle size of 3–6 nanometers having structure of hexagonal covellite and also monoclinic djurleite Cu2-xS with small nonstoichiometry of copper sublattice. Deposition from poorly alkaline water solutions of copper nitrate, thiocarbonic acid diamide and Trilon with heating to temperature ~90–100°C would allow to receive nanocrystalline powders CuS with the particle size of 45–55 nanometers having structure of hexagonal covellite.

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Sobre autores

S. Sadovnikov

Institute of Solid State Chemistry, Ural Branch of the RAS

Autor responsável pela correspondência
Email: sadovnikov@ihim.uran.ru
Rússia, Ekaterinburg, 620990

A. Gusev

Institute of Solid State Chemistry, Ural Branch of the RAS

Email: sadovnikov@ihim.uran.ru
Rússia, Ekaterinburg, 620990

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2. Fig. 1. X-ray diffraction patterns of nanocrystalline copper sulfides samples 1–3. Synthesized samples 1 and 2 are two-phase and contain the main hexagonal (sp. gr. P63/mmc) phase with a covellite structure and nanoparticle sizes of 3–6 nm, as well as a monoclinic (sp. gr. P21/n, No. 14) impurity phase of jarleyite with narrow reflections and particle sizes of ~70 nm. Sample 3 contains only covellite. The positions of jarleyite diffraction reflections according to [6, 13] are shown by vertical dashes at the bottom of the figure.

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3. Fig. 2. X-ray diffraction pattern of nanocrystalline copper sulfide CuS (sample 4) with a hexagonal (sp. gr. P63/mmc) covellite structure: experimental points are shown with an × sign, the calculated intensity is shown by a solid line. The difference between the experimental and calculated intensities (Iexp — Icalc) is shown at the bottom of the figure; vertical bars correspond to the positions of the diffraction reflections. RI is the Rietveld convergence factor.

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4. Fig. 3. TEM image of 40–50 nm particles of nanocrystalline hexagonal covellite CuS powder deposited from reaction mixture 4.

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5. Fig. 4. X-ray diffraction pattern of nanocrystalline copper sulfide CuS (sample 5) with a hexagonal (sp. gr. P63/mmc) covellite structure.

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6. Fig. 5. TEM image of 45–60 nm particles of nanocrystalline hexagonal covellite CuS powder deposited from reaction mixture 5.

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7. Fig. 6. Estimation of the average size of coherent scattering regions 〈D〉 based on the dependence of the reduced broadening β*(2θ ) = [β(2θ )cosθ ]/λ of diffraction reflections on the scattering vector s = (2sinθ )/λ for nanocrystalline copper sulfide CuS powders 4 and 5. The inset shows the position of the dependences and the reduced broadening at the origin of coordinates on an enlarged scale.

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