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article · Inorganic Chemistry Communications

Synthesis, physicochemical and electrochemical characterization of graphene oxide nanosheets obtained through improved and modified Hummers methods

202539 citationsOpen accessAbdelmalek Essaâdi University

In plain language

This research evaluates two distinct graphene oxide nanosheets, synthesised through an improved method and a modified Hummers method, to enhance electrochemical sensing devices. Physical and chemical analyses confirmed the nanosheet morphology, functional groups, and structural dimensions of both materials, with particle sizes measuring approximately 342 nanometres and 615 nanometres. The graphene oxide materials were dispersed using ultrasound to prepare modified carbon paste electrodes. When tested electrochemically, the modified electrodes significantly lowered charge transfer resistance compared to bare carbon paste electrodes. Testing with caffeic acid as a model detection molecule demonstrated that the incorporation of graphene oxide markedly increased charge transfer coefficients and oxidation rates, showing that both synthesis routes produce materials capable of enhancing sensor sensitivity.

Key takeaways

  • Graphene oxide nanosheets prepared by both improved and modified Hummers methods exhibited distinct particle sizes and interlayer spacings.
  • Modifying carbon paste electrodes with graphene oxide reduced charge transfer resistance from 847.6 ohms to as low as 106.6 ohms.
  • Electrodes modified with graphene oxide demonstrated improved peak separation and higher charge transfer coefficients during the oxidation of caffeic acid.

Why it matters

Electrochemical sensors rely on efficient electron transfer to detect target compounds accurately. By refining the synthesis of graphene oxide and integrating it into electrode designs, this work demonstrates how nanomaterials can substantially cut electrical resistance and speed up catalytic reactions, providing a basis for developing more sensitive and responsive analytical tools.

Commercialisation angle

The research points toward applications in voltammetric quantification and sensitive electrochemical sensor devices, with potential relevance for instrument designers and analytical testing laboratories. Tested using caffeic acid as a model target in a laboratory setup, the technology is at an early experimental stage, requiring further target testing and validation before real-world sensing products can emerge.

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Abstract

• Synthesis and characterization of graphene oxide nanosheets using various methods. • Ultrasound enabled GO dispersion for carbon paste electrode preparation. • GO-graphite materials showed excellent electrochemical performance . • Caffeic acid was used as a model molecule for detection evaluation. Graphene oxide (GO), with its large specific surface area, oxygenated functional groups, and conductive properties, is an efficient and versatile material for enhancing the sensitivity and selectivity of electrochemical devices. This study examines the electrocatalytic activity of two types of GO synthesized via an improved method (IGO) and a modified Hummers method (HGO + ), aimed at optimizing devices for voltammetric quantification. Characterizations showed particle sizes of 342.0 ± 24.3 nm (IGO) and 615.1 ± 81.5 nm (HGO + ), with zeta potentials of –33.5 ± 0.557 mV and −34.667 ± 0.635 mV. UV–visible spectra showed bands at 228 nm (IGO) and 231.5 nm (HGO + ). XRD analysis revealed characteristic peaks at 10.40° (IGO) and 11.25° (HGO + ), corresponding to interlayer spacings of 0.860 nm and 0.786 nm, while FTIR confirmed functional groups (C=O, C=C, C-O-C, CH 2 -OH). SEM revealed nanosheet morphology. GO-modified CPEs were synthesized using high-power ultrasound (60 s, 20 % amplitude) producing IGO/CPE and HGO + /CPE. EIS showed GO reduced charge transfer resistance from 847.6 Ω for CPE to 130.1 Ω (IGO/CPE) and 106.6 Ω (HGO + /CPE). Cyclic voltammograms showed peak separations of 60 mV (IGO/CPE) and 45 mV (HGO + /CPE), compared to 120 mV for CPE. Surface coverages were 7.3 × 10 −6 mol/cm 2 (IGO/CPE) and 1.3 × 10 −5 mol/cm 2 (HGO + /CPE). Electrocatalytic performance was tested with caffeic acid. Charge transfer coefficients increased from 0.418 ± 0.06 (CPE) to 0.731 ± 0.03 (IGO + /CPE) and 0.736 ± 0.04 (HGO + /CPE), improving oxidation rates. GO-modified CPEs exhibited superior electrocatalytic performance, demonstrating their potential as sensitive electrochemical sensors.

Research topics

  • Graphene research and applications
  • Advancements in Battery Materials
  • Graphene and Nanomaterials Applications

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DOI: 10.1016/j.inoche.2025.114120

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