Microwave-assisted green fabrication of nickel foam–reduced graphene oxide–nickel sulfide nanocomposite: Structural, spectroscopic, and electrochemical performance evaluation for supercapacitor applications

Authors

  • Prabaharan Panchanathan Department of Chemistry, Government Polytechnic College Tiruchirappalli– 620 022, India. and Department of Chemistry, Cauvery College for Women (A), Tiruchirappalli – 620 018, India, Affiliated to Bharathidasan University https://orcid.org/0009-0007-9562-4703
  • Maadathi Sivakumar Department of Chemistry, Cauvery College for Women (A), Tiruchirappalli –620 018, India. Affiliated to Bharathidasan University
  • Gunasekaran Marudhai Department of Chemistry, J J College of Engineering and Technology, Tiruchirapalli - 620 009
  • Brindha Ganesan Department of chemistry, V.S.B. Engineering College Autonomous Karur - 639111. India
  • Sivasankari Gnanam Department of Chemistry, Cauvery College for Women (A), Tiruchirappalli – 620 018, India, Affiliated to Bharathidasan University https://orcid.org/0000-0001-9745-8322
  • Boobalan Sivalingam Department of Chemistry, Indra Ganesan College of Engineering, Manikandam, Tiruchirappalli – 620012. India
  • Devi Selvaraj Department of Chemistry, Cauvery College for Women (A), Tiruchirappalli – 620 018, India, Affiliated to Bharathidasan University https://orcid.org/0000-0001-8811-5870

DOI:

https://doi.org/10.20450/mjcce.2026.3562

Keywords:

Green synthesis, Nickel sulfide nanoparticles, Reduced graphene oxide nanocomposite, Coccinia grandis leaf extract, Supercapacitor electrode materials

Abstract

A microwave-assisted green synthesis route was employed to fabricate a nickel foam–reduced graphene oxide–nickel(II) sulfide (Ni foam–rGO–NiS) nanocomposite using Coccinia grandis leaf extract as the bio-reducing and stabilizing agent for supercapacitor applications. The Ultraviolet - Visible (UV) spectrum revealed an absorption peak of 239 nm (rGO) and 313 nm (NiS), confirming the formation of a composite that facilitates efficient electron transfer between the two components, potentially reducing the band gap energy. Fourier Transform Infrared spectra (FTIR) confirmed successful loading of NiS nanoparticles onto rGO, with associated phytochemical functional groups acting as reducing, capping, and stabilizing agents. X-ray Diffraction (XRD) patterns validated formation of hexagonal NiS and reduction in the sheet structure of rGO, thereby elucidating the nature of the nanocomposite. The average crystallite size, estimated using the   Debye–Scherrer equation, was approximately 2–5 nm (NiS) and approximately 30.4 nm (rGO). The surface morphology of the nanocomposite displayed an exfoliated wrinkled sheet structure, with NiS particles uniformly dispersed throughout. Elemental analysis verified that the material had achieved the expected purity levels, with no detectable impurities, while the Dynamic Light Scattering (DLS) indicated a particle size of approximately 100 nm in solution. The Ni foam–rGO–NiS electrode demonstrated significantly enhanced electrochemical performance. Cyclic voltammetry conducted at the same scan rate revealed intense redox peaks, thus confirming pseudocapacitive behavior. Electrochemical impedance spectroscopy (EIS) indicated low charge-transfer resistance with high electrochemical activity. This electrode achieved a high specific capacitance of approximately 633.3 F g1 at 1 A g1 and approximately 422.2 F g1 at 5 A g1, as well as exhibiting good rate capability and cycling stability, with 80–85% capacitance retention over 3000 cycles. The synergistic combination of highly conductive rGO, redox-active NiS, and porous Ni foam enhanced charge storage and transportation. The prepared green-synthesized, reduced graphene oxide–nickel(II) sulfide nanocomposite is proposed as a promising electrode nanomaterial for supercapacitor applications.

References

Simon, P.; Gogotsi, Y. Materials for electrochemical capacitors. Nat. Mater. 2008, 7, 845–854.

https://doi.org/10.1038/nmat2297

Miller, J. R.; Simon, P. Electrochemical capacitors for energy management. Science 2008, 321, 651–652.

https://doi/10.1126/science.1158736

Winter, M.; Brodd, R. J. What are batteries, fuel cells, and supercapacitors? Chem. Rev. 2004, 104, 4245–4269. https://doi.org/10.1021/cr040110e

Antony Sakthi, S.; Priyadarshini, K.; Mani, C.; Rusho Robin Prasad, S.; Dominic, A. Synthesis and characteri-zation of NiCo2S4-MOF-ZIF-67@rGO for efficient elec-trochemical energy storage. J. Phys.: Conf. Ser. 2024, 2801, 012001.

https://doi.org/10.1088/1742-6596/2801/1/012001

Sankari P.; Sivasankari, G.; Kannagi, K.; Pavithra , N.; et al. Study of structural and spectroscopic characterization of ZnS nanoparticles and its application as supercapacitor. Mod. Phys. Lett. B 2023, 37, 2350150.

https://doi.org/10.1142/S0217984923501506

Liu, C.; Li, F.; Ma, L. P.; Cheng, H. M. Advanced mate-rials for energy storage. Adv. Mater. 2010, 22, E28–E62. https://doi.org/10.1002/adma.200903328

Antony Sakthi, S.; Rakini Chanderasekaran, J. H.; Nire-sha Gnana Mary, A.; Surendra Varma, M.; Lakhsmi Prabha, P. Synthesis and characterization of 3D MnNi2O4@MnNi2S4/NF-MOF-67-rGO nanoflower@ nanosheet for ultra-high capacity electrode material. J. Phys.: Conf. Ser. 2024, 2801, 012009.

https://doi.org/10.1088/1742-6596/2801/1/012009

Antony Sakthi, S.; Priyadarshini, K.; Mani, C.; Rusho Robin Prasad, S. Synthesis and spectral characterization of high-performance supercapacitor ZIF-67@RGO nano-composite electrode materials. Rasayan J. Chem. 2023, 16, 1462–1472.

http://doi.org/10.31788/RJC.2023.1638206

Conway, B. E. Electrochemical Supercapacitors: Scien-tific Fundamentals and Technological Applications; Springer: New York, NY, USA, 1999.

https://doi.org/10.1007/978-1-4757-3058-6

Rishav K. Baranwal, Nisantika Biswas, Buddhadeb Or-aon, Gautam Majumdar, Advances in Surface Engineer-ing for Improved Energy Storage, Encyclopedia of Re-newable and Sustainable Materials, Elsevier, 2020, 245–249, ISBN 9780128131961.

https://doi.org/10.1016/B978-0-12-803581-8.11053-7.

Augustyn, V.; Simon, P.; Dunn, B. Pseudocapacitive oxide materials for high-rate electrochemical energy stor-age. Energy Environ. Sci. 2014, 7, 1597–1614.

https://doi.org/10.1039/C3EE44164D

Simon, P.; Gogotsi, Y.; Dunn, B. Where do batteries end and supercapacitors begin? Science 2014, 343, 1210–1211. http://dx.doi.org/10.1126/science.1249625

Novoselov, K. S.; et al. A roadmap for graphene. Nature 2012, 490, 192–200.

https://doi.org/10.1038/nature11458

Zhu, Y.; Murali, S.; Cai, W.; et al. Graphene and gra-phene oxide: Synthesis, properties, and applications. Adv. Mater. 2010, 22, 3906–3924.

https://doi.org/10.1002/adma.201001068

Dreyer, D. R.; Park, S.; Bielawski, C. W.; Ruoff, R. S. The chemistry of graphene oxide. Chem. Soc. Rev. 2010, 39, 228–240. https://doi.org/10.1039/B917103G

Zheng, M.; Xiao, X.; Li, L.; et al. Hierarchically nanostructured transition metal oxides for supercapaci-tors. Sci. China Mater. 2018, 61, 185–209.

https://doi.org/10.1007/s40843-017-9095-4

Wang, X.; Liu, X.; Rong, H.; et al. Layered manganese-based metal–organic framework as a high capacity elec-trode material for supercapacitors. RSC Adv. 2017, 7, 29611–29617. https://doi.org/10.1039/C7RA04374K

Wang, H.; Casalongue, H. S.; Liang, Y.; Dai, H. Ni(OH)2 nanoplates grown on graphene as advanced electrochemical pseudocapacitor materials. J. Am. Chem. Soc. 2010, 132, 7472–7477.

https://doi.org/10.1021/ja102267j

Yan, J.; Wang, Q.; Wei, T.; Fan, Z. Recent advances in design and fabrication of electrochemical supercapacitors with high energy densities. Adv. Energy Mater. 2013, 4, 1300816.

https://doi.org/10.1002/aenm.201300816

Iravani, S. Green synthesis of metal nanoparticles using plants. Green Chem. 2011, 13, 2638–2650.

https://doi.org/10.1039/C1GC15386B

Lee, Y.; Joo, N. Identification and quantification of key phytochemicals, phytohormones, and antioxidant proper-ties in Coccinia grandis during fruit ripening. Antioxi-dants 2022, 11, 2218.

https://doi.org/10.3390/antiox11112218

Raj, R. A.; AlSalhi, M. S.; Devanesan, S. Microwave-assisted synthesis of nickel oxide nanoparticles using Co-riandrum sativum leaf extract. Materials 2017, 10, 460. https://doi.org/10.3390/ma10050460

Marcano, D. C.; Kosynkin, D. V.; Berlin, J. M.; Sinitskii, A.; Sun, Z.; Slesarev, A.; Alemany, L. B.; Lu, W.; Tour, J. M. Improved synthesis of graphene oxide. ACS Nano 2010, 4, 4806–4814.

https://doi.org/10.1021/nn1006368

Cullity, B. D. Elements of X-Ray Diffraction, 2nd ed.; Addison-Wesley Publishing Company Inc.: Reading, MA, USA, 1978. ISBN 0-201-01174-3.

Soheila F.: Farid N A, Microwave-assisted synthesis of metal oxide/hydroxide composite electrodes for high power supercapacitors - A review. J. of. Pow. Sou. 2014, 263, 338–360.

https://doi.org/10.1016/j.jpowsour.2014.03.144

Wang, G.; Zhang, L.; Zhang, J. A review of electrode materials for electrochemical supercapacitors. Chem. Soc. Rev. 2012, 41, 797–828.

https://doi.org/10.1039/C1CS15060J

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Published

2026-06-22

How to Cite

Panchanathan, P. ., Sivakumar, M. ., Marudhai, G. ., Ganesan, . B., Gnanam, S., Sivalingam, B. ., & Selvaraj , D. . (2026). Microwave-assisted green fabrication of nickel foam–reduced graphene oxide–nickel sulfide nanocomposite: Structural, spectroscopic, and electrochemical performance evaluation for supercapacitor applications. Macedonian Journal of Chemistry and Chemical Engineering, 45(1). https://doi.org/10.20450/mjcce.2026.3562

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Section

Analytical Chemistry