Pure-phase Cu2−xS (x = 1, 0.2) nanoparticles have been synthesized by the thermal decomposition of copper(II) dithiocarbamate as a single-source precursor in oleylamine as a capping agent. The compositions of the Cu2−xS nanocrystals varied from CuS (covellite) through the mixture of phases (CuS and Cu7.2S4) to Cu9S5 (digenite) by simply varying the temperature of synthesis. The crystallinity and morphology of the copper sulfides were studied using X-ray diffraction (XRD), scanning electron microscopy (SEM), and transmission electron microscopy (TEM), which showed pure phases at low (120 °C) and high (220 °C) temperatures and a mixture of phases at intermediate temperatures (150 and 180 °C). Covellite was of a spherical morphology, while digenite was rod shaped. The optical properties of these nanocrystals were characterized by UV−vis–NIR and photoluminescence spectroscopies. Both samples had very similar absorption spectra but distinguishable fluorescence properties and exhibited a blue shift in their band gap energies compared to bulk Cu2−xS. The pure phases were used as catalysts for the photocatalytic degradation of tetracycline (TC) under visible-light irradiation. The results demonstrated that the photocatalytic activity of the digenite phase exhibited higher catalytic degradation of 98.5% compared to the covellite phase, which showed 88% degradation within the 120 min reaction time using 80 mg of the catalysts. The higher degradation efficiency achieved with the digenite phase was attributed to its higher absorption of the visible light compared to covellite.

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In this paper, spherical-shaped pure phase djurleite (Cu31S16) and roxbyite (Cu7S4) nanoparticles were prepared by a solvothermal decomposition of copper(II) dithiocarbamate complex in dodecanthiol (DDT). The reaction temperature was used to control the phases of the samples, which were represented as Cu31S16 (120 °C), Cu31S16 (150 °C), Cu7S4 (220 °C), and Cu7S4 (250 °C) and were characterized by using X-ray diffraction (XRD), scanning and transmission electron microscopy (SEM and TEM), and absorption spectroscopy. The samples were used as photocatalysts for the degradation of tetracycline (TC) under visible light irradiation. The results of the study showed that Cu7S4 (250 °C) exhibited the best activity in the reaction system with the TC degradation rate of up to 99% within 120 min of light exposure, while the Cu31S16 (120 °C) system was only 46.5% at the same reaction condition. In general, roxbyite Cu7S4 (250 °C) could be considered as a potential catalyst for the degradation of TC in solution.

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