Effect of Vacuum Treatment Temperature on the Structure, Morphology, and Porous Characteristics of Reduced Graphene Oxide

Editorial Board PCSS Journal; R.I. Zapukhlyak; A.O. Kotsyubynsky; R.G. Abaszade; V.M. Boychuk; V.O. Kotsyubynsky; V.T. Hoi; M.М. Klymyuk; I.R. Kos; D.O. Lynnyk

doi:10.15330/pcss.27.3.468-475

Authors

R.I. Zapukhlyak Vasyl Stefanyk Carpathian National University, Ivano-Frankivsk, Ukraine
A.O. Kotsyubynsky Ivano-Frankivsk National Technical University of Oil and Gas, Ivano-Frankivsk, Ukraine
R.G. Abaszade Azerbaijan State Oil and Industry University, Baku, Azerbaijan; Department of Ecology, Azerbaijan University of Architecture and Construction, Baku, Azerbaijan; Tashkent State Technical University named after Islam Karimov, Tashkent, Uzbekistan; Turan International Research Institute, Baku, Azerbaijan
V.M. Boychuk Vasyl Stefanyk Carpathian National University, Ivano-Frankivsk, Ukraine
V.O. Kotsyubynsky Vasyl Stefanyk Carpathian National University, Ivano-Frankivsk, Ukraine
V.T. Hoi Vasyl Stefanyk Carpathian National University, Ivano-Frankivsk, Ukraine
M.М. Klymyuk Vasyl Stefanyk Carpathian National University, Ivano-Frankivsk, Ukraine
I.R. Kos Vasyl Stefanyk Carpathian National University, Ivano-Frankivsk, Ukraine
D.O. Lynnyk Vasyl Stefanyk Carpathian National University, Ivano-Frankivsk, Ukraine

DOI:

https://doi.org/10.15330/pcss.27.3.468-475

Keywords:

graphene oxide, reduced graphene oxide, thermal reduction, turbostratic structure, porosity, pore size distribution

Abstract

The effect of thermal reduction temperature on the structural, morphological, and porous characteristics of graphene oxide-derived materials was investigated. Graphene oxide films were thermally treated in vacuum at temperatures from 200 to 600^оC, and the resulting materials were characterized by XRD, FTIR, SEM, and low-temperature nitrogen adsorption–desorption measurements with BET, NLDFT, and FHH analyses. The results showed that vacuum heat treatment induces a gradual transformation of graphene oxide into a disordered turbostratic reduced graphene oxide structure. Increasing treatment temperature is accompanied by progressive deoxygenation, morphological evolution from fragmented lamellar films to open frameworks of thin weakly stacked sheets, and pronounced development of porosity. The BET specific surface area increases from 61 m² g^-1 for the material obtained at 200^оC to 112, 197, 276, and 331 m² g^-1 for the materials obtained at 300, 400, 500, and 600^оC, respectively. It was demonstrated that thermal treatment temperature is a key parameter controlling the transformation of GO into porous turbostratic rGO.

References

S.C. Ray, Application and uses of graphene oxide and reduced graphene oxide, Applications of Graphene and Graphene-Oxide Based Nanomaterials, 6(8), 39 (2015); https://doi.org/10.1016/B978-0-323-37521-4.00002-9.

L.G. Guex, B. Sacchi, K.F. Peuvot, R.L. Andersson, A.M. Pourrahimi, V. Ström, R.T. Olsson, Experimental review: chemical reduction of graphene oxide (GO) to reduced graphene oxide (rGO) by aqueous chemistry, Nanoscale, 9(27), 9562 (2017); https://doi.org/10.1039/C7NR02943H.

I. Sengupta, S. Chakraborty, M. Talukdar, S.K. Pal, S. Chakraborty, Thermal reduction of graphene oxide: How temperature influences purity, Journal of Materials Research, 33(23), 4113 (2018); https://doi.org/10.1557/jmr.2018.338.

A.A. Zhou, J. Bai, W. Hong, H. Bai, Electrochemically reduced graphene oxide: Preparation, composites, and applications, Carbon, 191, 301 (2022); https://doi.org/10.1016/j.carbon.2022.01.056.

X. Mei, X. Meng, F. Wu, Hydrothermal method for the production of reduced graphene oxide, Physica E: Low-Dimensional Systems and Nanostructures, 68, 81 (2015); https://doi.org/10.1016/j.physe.2014.12.011.

V. Agarwal, P.B. Zetterlund, Strategies for reduction of graphene oxide–A comprehensive review, Chemical Engineering Journal, 405, 127018 (2021); https://doi.org/10.1016/j.cej.2020.127018.

P.P.A. Jose, M.S. Kala, N. Kalarikkal, S. Thomas, Reduced graphene oxide produced by chemical and hydrother¬mal methods, Materials Today: Proceedings, 5(8), 16306 (2018); https://doi.org/10.1016/j.matpr.2018.05.124.

P.V. Kumar, N.M. Bardhan, G.Y. Chen, Z. Li, A.M. Belcher, J.C. Grossman, New insights into the thermal reduction of graphene oxide: Impact of oxygen clustering, Carbon, 100, 90 (2016); https://doi.org/10.1016/j.carbon.2015.12.087.

M. Ostermann, P. Velicsanyi, P. Bilotto, J. Schodl, M. Nadlinger, G. Fafilek, M. Valtiner, Development and up-scaling of electrochemical production and mild thermal reduction of graphene oxide, Materials, 15(13), 4639 (2022); https://doi.org/10.3390/ma15134639.

R. Singh, S. Ullah, N. Rao, M. Singh, I. Patra, D.A. Darko, V. Vijayan, Synthesis of three-dimensional reduced-graphene oxide from graphene oxide, Journal of Nanomaterials, 2022(1), 8731429 (2022); https://doi.org/10.1155/2022/8731429.

V. Kotsyubynsky, Y.Z. Khimyak, R. Zapukhlyak, V. Boychuk, L. Turovska, V. Hoi, NaOH-assisted hydrothermal reduction of graphene oxide, Journal of Physics: Condensed Matter, 36(49), 495701 (2024); https://doi.org/10.1088/1361-648X/ad75dc.

D. Öztekin, H. Arbağ, S. Yaşyerli, Preparation of rGO with enhanced electrical conductivity: effects of sequential reductions of L-ascorbic acid and thermal, Arabian Journal for Science and Engineering, 50(13), 9905 (2025); https://doi.org/10.1007/s13369-024-09915-5.

V.O. Kotsyubynsky, V.M. Boychuk, I.M. Budzuliak, B.I. Rachiy, R.I. Zapukhlyak, M.A. Hodlevska, A.A. Malakhov, Structural Properties of Graphene Oxide Materials Synthesized Accordingly to Hummers, Tour and Modified Methods: XRD and Raman Study, Physics and Chemistry of Solid State, 22(1), 31 (2021); https://doi.org/10.15330/pcss.22.1.31-38.

B. Schwenzer, T.C. Kaspar, Y. Shin, D.W. Gotthold, Spectroscopic study of graphene oxide membranes exposed to ultraviolet light, The Journal of Physical Chemistry C, 120(23), 12559 (2016); https://doi.org/10.1021/acs.jpcc.6b03033.

M. Rosillo-Lopez, C.G. Salzmann, Detailed investigation into the preparation of graphene oxide by dichromate oxidation, ChemistrySelect, 3(24), 6972 (2018); https://doi.org/10.1002/slct.201801594.

T. Jiao, H. Guo, Q. Zhang, Q. Peng, Y. Tang, X. Yan, B. Li, Reduced graphene oxide-based silver nanoparticle-containing composite hydrogel as highly efficient dye catalysts for wastewater treatment, Scientific Reports, 5(1), 11873 (2015); https://doi.org/10.1038/srep11873.

D. Khalili, Graphene oxide: a promising carbocatalyst for the regioselective thiocyanation of aromatic amines, phenols, anisols and enolizable ketones by hydrogen peroxide/KSCN in water, New Journal of Chemistry, 40(3), 2547 (2016); https://doi.org/10.1039/C5NJ02314A.

G.M. Das, E. Hulkko, A. Emelianov, M.G. Santiveri, P. Myllyperkiö, A. Johansson, M. Pettersson, Nano-FTIR identification of functionalization in two-photon oxidized graphene, Carbon, 245, 120851 (2025); https://doi.org/10.1016/j.carbon.2025.120851.

C. Gao, X.Y. Yu, R.X. Xu, J.H. Liu, X.J. Huang, AlOOH-reduced graphene oxide nanocomposites: one-pot hydrothermal synthesis and their enhanced electrochemical activity for heavy metal ions, ACS Applied Materials & Interfaces, 4(9), 4672 (2012); https://doi.org/10.1021/am3010434.

P.H. Borges, M.V. da Silva, J.S. Stefano, R.R. Barreto, A.de Siervo, E.M. Richter, E. Nossol, Synergistic charge redistribution and structural evolution in three-dimensionally printed Mn-Prussian blue analogue-based electrodes for energy storage, ACS Nanoscience Au (2026); https://doi.org/10.1021/acsnanoscienceau.5c00167.

B. Sahouli, S. Blacher, F. Brouers, Applicability of the fractal FHH equation, Langmuir, 13(16), 4391 (1997); https://doi.org/10.1021/la962119k.

S.V. Sklepova, N. Ivanichok, P. Kolkovskyi, V. Kotsyubynsky, V. Boychuk, B. Rachiy, L. Ropyak, Porous structure and fractal dimensions of activated carbon prepared from waste coffee grounds, Materials, 16(18), 6127 (2023); https://doi.org/10.3390/ma16186127.

D. Liu, W. Zhou, J. Wu, T. Huang, Fractal characterization of graphene oxide nanosheet, Materials Letters, 220, 40 (2018); https://doi.org/10.1016/j.matlet.2018.02.134.