Structural and optical properties of nanostructured copper sulfide semiconductor synthesized in an industrial mill

doi:10.1007/s11705-018-1755-2

Front. Chem. Sci. Eng.

2019, Vol. 13

Issue (1) : 164-170 https://doi.org/10.1007/s11705-018-1755-2

RESEARCH ARTICLE

Structural and optical properties of nanostructured copper sulfide semiconductor synthesized in an industrial mill

Marcela Achimovičová^1,²(

), Erika Dutková², Erika Tóthová², Zdenka Bujňáková², Jaroslav Briančin², Satoshi Kitazono³

¹. Institute of Mineral and Waste Processing, Waste Disposal and Geomechanics, Clausthal University of Technology, Clausthal 38678, Germany
². Institute of Geotechnics, Slovak Academy of Sciences, Košice 04001, Slovakia
³. Nakase Refinery, Nihon Seiko Co., Ltd., Yabu-shi, Hyogo 667-1111, Japan

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Abstract

Chalcogenide nanostructured semiconductor, copper sulfide (CuS) was prepared from copper and sulfur powders in stoichiometric ratio by a simple, fast, and convenient one-step mechanochemical synthesis after 40 min of milling in an industrial eccentric vibratory mill. The kinetics of the mechanochemical synthesis and the influence of the physical properties of two Cu powder precursor types on the kinetics were studied. The crystal structure, physical properties, and morphology of the product were characterized by X-ray diffraction (XRD), the specific surface area measurements, particle size distribution and scanning electron microscopy. The XRD analysis confirmed the hexagonal crystal structure of the product-CuS (covellite) with the average size of the crystallites 11 nm. The scanning electron microscopy analysis has revealed that the agglomerated grains have a plate-like structure composed of CuS nanoparticles. The thermal analysis was performed to investigate the thermal stability of the mechanochemically synthesized CuS. The optical properties were studied using UV-Vis and photoluminescence spectroscopy. The determined optical band gap energy 1.80 eV responds to the value of the bulk CuS, because of agglomerated nanoparticles. In addition, a mechanism of CuS mechanochemical reaction was proposed, and the verification of CuS commercial production was performed.

Keywords copper sulfide industrial mechanochemical synthesis thermal analysis optical properties

Corresponding Author(s): Marcela Achimovičová

Just Accepted Date: 13 June 2018 Online First Date: 03 December 2018 Issue Date: 25 February 2019

Cite this article:

Marcela Achimovičová,Erika Dutková,Erika Tóthová, et al. Structural and optical properties of nanostructured copper sulfide semiconductor synthesized in an industrial mill[J]. Front. Chem. Sci. Eng., 2019, 13(1): 164-170.

URL:

https://academic.hep.com.cn/fcse/EN/10.1007/s11705-018-1755-2
https://academic.hep.com.cn/fcse/EN/Y2019/V13/I1/164

Fig.1 XRD patterns of Cu_a/S mixture milled for 40 and 60 min. l-CuS; □-Cu₂S

Fig.2 XRD patterns of Cu_e/S mixture milled for 5 and 40 min.. l-CuS; □-Cu₂S

Fig.3 Dependence of the phase composition of CuS products and the content of unreacted S⁰ on the milling time

Fig.4 SEM image of CuS product

Fig.5 SEM image of a selected CuS grain with the typical EDX spectrum (inset)

Tab.1 Quantification of the EDX spectra taken at the different spots of the CuS product sample

Fig.6 TG/DTG-DTA curves of CuS product, the heat effects and the mass losses in the function of temperature

Fig.7 UV-Vis absorption spectrum (inset Tauc’s plot) of CuS product

Fig.8 PL emission spectrum of CuS product

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