Green synthesis of graphene oxide via electrochemical exfoliation and its characterization

Adilet Dautov, Тilek Kuanyshbekov, Zhandos Tolepov, San Orazova, Ahmed A. Abdala, Bayan Kurbanova, Nurkhamit Kantay, Amantur Umarov, Zhandos Shalabayev, Роза Аблакимовна Аубакирова

4 more authors

Tantybayeva Batima Smataevna, Zhazira Mukazhanova, Bakhyt Shaikhova, Nurkadam Tolep

2026

Full text Open access: Gold Metadata (CSL-JSON)
DOI 10.1016/j.rechem.2026.103746
Data confidence 70 medium
How this score is calculated

It is built from checkable properties of the record itself: whether the article has a DOI, how many independent sources confirmed its data, whether the required fields are filled in, and how recent the latest confirmation is. Disagreement between sources and a missing identifier lower it. A value of 80 or above means the record was published without further checking; 60 to 79 means it is published at reduced confidence, with a manual check advisable. A record verified by an editor by hand is never pushed below 90 by a recalculation. This scores our data about the article, not the article itself.

Abstract

Graphene oxide (GO) is a versatile carbon nanomaterial whose properties strongly depend on the synthesis route. In this study, an environmentally friendly electrochemical exfoliation (EE) method using 0.1 M ammonium sulfate electrolyte was developed and compared with the conventional Hummers' method (HM). The influence of electrolysis duration and purification on the structural and electrical properties of the obtained materials was systemically investigated. UV–Vis spectroscopy showed a characteristic absorption band at approximately 190 nm for electrochemically exfoliated samples, while prolonged electrolysis (8 h) resulted in the appearance of a weak shoulder near 230 nm, indicating gradual oxidation of the graphite structure. XRD analysis revealed that HM-derived GO exhibited a characteristic (001) reflection at 11.09° (d-spacing = 7.99 Å), whereas electrochemically exfoliated GO retained a broad (002) peak centered at 26.54°, corresponding to an interlayer spacing of 3.36 Å and indicating partial preservation of the graphitic structure. Raman spectroscopy demonstrated a lower defect density in electrochemically exfoliated GO, with an I D /I G ratio of 0.759 compared with 0.864 for HM-derived GO. FTIR spectra further confirmed the lower abundance of oxygen-containing functional groups in the electrochemically synthesized material. Electron microscopy revealed thin, transparent, wrinkled graphene-like nanosheets with significantly improved exfoliation after dialysis. Electrical resistivity measurements performed between 40 and 100 °C under laboratory air, humid atmosphere, and flowing argon demonstrated consistently lower resistivity for electrochemically exfoliated GO than for HM-derived GO, indicating higher electrical conductivity due to its lower oxidation degree and better preservation of the sp 2 carbon network. These results demonstrate that EE provides a simple, low-cost, and environmentally benign approach for producing conductive graphene-like materials with reduced oxygen functionalization while avoiding the hazardous oxidants required in the conventional Hummers' method.