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Proceeding Paper

Preparation of Cu4SnS4/CuCo2S4 Nanoparticles Using Combustion Reaction Accelerated by Organic Driving Agents under Microwave Irradiation †

Department of Chemistry, Iran University of Science and Technology (IUST), Tehran 16846-13114, Iran
*
Author to whom correspondence should be addressed.
Presented at the 24th International Electronic Conference on Synthetic Organic Chemistry, 15 November–15 December 2020; Available online: https://ecsoc-24.sciforum.net/.
Chem. Proc. 2021, 3(1), 51; https://doi.org/10.3390/ecsoc-24-08354
Published: 14 November 2020

Abstract

:
Copper-based sulfide-rich nanomaterials have recently attracted attention in various applications due to the lack of expense, abundance, and non-toxicity of their constituent elements. As the members of this family, Cu4SnS4 and CuCo2S4 have exhibited good capability in a stable manner in solar cells, energy storage electrodes, batteries, etc. In this work, through a facile and rapid combustion reaction accelerated by microwave irradiation, Cu4SnS4/CuCo2S4 nanoparticles were prepared. Thiourea was used as a sulphur source and also organic driving agent. The features of the synthesized product were studied using FT-IR, XRD, SEM, and EDX techniques. The FT-IR and XRD results showed the formation of a multi-components structure containing orthorhombic crystalline phase of Cu4SnS4 alongside carrollite CuCo2S4 phase.

1. Introduction

In recent years, copper-based sulfide rich nanomaterials have attracted lots of attention because of having more abundant, low-cost, easily available, and non-toxic constituents compared to cadmium and lead-based compounds [1]. Usually, sulfide-rich materials have a higher activity and conductivity, as well as a lower electronegativity and band gap, than metal oxides. These compounds have significant features such as layered structures and suitable band gaps for light absorption, which enable them to be semiconductor materials in various applications [2].
Copper-based ternary sulfides, such as Cu4SnS4 and CuCo2S4 (as the members of this large family), have been studied in variety of photovoltaic, energy storage, solar cells, and catalytic applications, among others [3,4,5]. The synthesis of hetero-structured building blocks consisting of these compounds to improve multifunctional features and create highly efficient products is notable. Amongst reported synthesis methods, such as the solvothermal/hydrothermal, hot-injection, and sol–gel approaches, microwave-assisted technique can be introduced as a simple and rapid method to prepare nanomaterials [6,7,8]. As a matter of fact, the synthesis of Cu4SnS4/CuCo2S4 heterostructure nanoparticles using a solvent-free microwave-assisted procedure has not been yet reported.

2. Experimental Section

2.1. Materials

All initial reactants were provided from valid Co. and used without further purification.

2.2. Synthesis Method

The proper stoichiometric amounts of metal sources in the presence of thiourea as a sulphur source and driving agent were mixed with each other, put into a microwave oven, and treated with microwave irradiation at a power of 900 W for 20 minutes. The resulting black powder was washed, dried overnight, and characterized by FT-IR, XRD, and SEM analyses.

2.3. Characterizations

XRD patterns were recorded by a DRON-8 powder diffractometer using Cu Kα radiation (λ = 1.54060 Å). FT-IR spectra were obtained by a Shimadzu-8400S spectrometer in the range of 400–4000 cm−1 using KBr pellets. SEM and energy-dispersive X-ray images were taken on a VEGA\\TESCAN S360 with gold coating.

3. Results and Discussion

Figure 1 indicates the FT-IR spectrum of the prepared sample. The observed strong peaks at 522, 569, and 664 cm−1 could be assigned to vibration frequencies of the Co-O, Sn-S, CoS, and Cu-S bands from the prepared heterostructure molecule [9,10]. The peaks at 2361 and 3403 cm−1 could have been related to the vibrational frequencies of the H-O and C-O-C functional groups from the adsorbed H2O and CO2 molecules on the product surface.
The recorded XRD pattern of Cu4SnS4/CuCo2S4 nanoparticles is shown in Figure 2. Based on this pattern, it can be said that the diffractions peaks were related to the formation of orthorhombic phase of Cu4SnS4 structure (JCPDS card No. 27-0196). In addition, the diffraction peaks at 26.59°, 31.26°, 32.70°, 38.88°, 44.88°, 48.84°, 51.89°, 54.73°, 58.29°, 61.74°, 64.79°, 66.11°, 68.14°, 71.39°, 75.36°, and 78.91°—in close accordance with the 220; 311,222; 400; 331; 422; 333,440; 531; 620; 533; 622,444; 711; 642; and 731 crystal planes—were attributed to the cubic phase of the carrollite CuCo2S4 structure (JCPDS card No. 75-1570). The slight shift at the 2 theta positions could have been a result of being the sandwich and crystallization of the carrollite CuCo2S4 phase between the Cu4SnS4 layers.
The elemental EDX analysis (Figure 3) revealed the presence of Cu, Sn, Co, and S elements, thus confirming the mentioned structural data of FT-IR and XRD analyses.
The recorded SEM images of the prepared product depicted aggregations of crystalline flake-like morphology with an average thickness of 40 nm and a width of 210 nm (Figure 4). This morphology could have originated from the role of thiourea as a driving agent, alongside being sulfide source. A particulate morphology with an average particle size of 60 nm was also observed.

4. Conclusions

Cu4SnS4/CuCo2S4 nanoparticles were well-synthesized by a microwave-assisted method. Amongst various chemical methods, the advantages of this synthesis technique include its simplicity, high speed, low energy consumption, and solvent-free reaction. In an effort to decrease the growth time, microwave heating treatment can be introduced as a capable technique to produce nanomaterials in the short reaction time compared to the conventional procedures with a long reaction time.

Funding

This research received no external funding.

Institutional Review Board Statement

Not applicable.

Informed Consent Statement

Not applicable.

Data Availability Statement

The necessary data has been given and this study does not report more data.

Acknowledgments

We gratefully acknowledge IUST for providing materials and facilities.

References

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Figure 1. FT-IR spectrum of the synthesized Cu4SnS4/CuCo2S4.
Figure 1. FT-IR spectrum of the synthesized Cu4SnS4/CuCo2S4.
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Figure 2. XRD pattern of the prepared Cu4SnS4/CuCo2S4 nanoparticles.
Figure 2. XRD pattern of the prepared Cu4SnS4/CuCo2S4 nanoparticles.
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Figure 3. EDX analysis of the resulting product.
Figure 3. EDX analysis of the resulting product.
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Figure 4. SEM images of the synthesized Cu4SnS4/CuCo2S4.
Figure 4. SEM images of the synthesized Cu4SnS4/CuCo2S4.
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MDPI and ACS Style

Aghaei, M.; Imani, M.; Tadjarodi, A. Preparation of Cu4SnS4/CuCo2S4 Nanoparticles Using Combustion Reaction Accelerated by Organic Driving Agents under Microwave Irradiation. Chem. Proc. 2021, 3, 51. https://doi.org/10.3390/ecsoc-24-08354

AMA Style

Aghaei M, Imani M, Tadjarodi A. Preparation of Cu4SnS4/CuCo2S4 Nanoparticles Using Combustion Reaction Accelerated by Organic Driving Agents under Microwave Irradiation. Chemistry Proceedings. 2021; 3(1):51. https://doi.org/10.3390/ecsoc-24-08354

Chicago/Turabian Style

Aghaei, Maede, Mina Imani, and Azadeh Tadjarodi. 2021. "Preparation of Cu4SnS4/CuCo2S4 Nanoparticles Using Combustion Reaction Accelerated by Organic Driving Agents under Microwave Irradiation" Chemistry Proceedings 3, no. 1: 51. https://doi.org/10.3390/ecsoc-24-08354

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