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Fabrication and characterisation of electrodeposited reduced graphene oxide modified molybdenum microdisk electrode for the reduction of dissolved carbon dioxide in aqueous solutions

Shafiee, Saiful 'Arifin and Saiful Adlee, Siti Aisyah and Rashidi, Daniel Mohamad and Mahat, Mohd Muzamir and Ismail, Mohamad Wafiuddin and Samad, Wan Zurina and Murad, Alyaa Syahirah A. and Zahaba, Maryam and Zakaria, Azmel and Hamdan, Khaled and Aizamddin, Muhammad Faiz and Danial, Wan Hazman (2026) Fabrication and characterisation of electrodeposited reduced graphene oxide modified molybdenum microdisk electrode for the reduction of dissolved carbon dioxide in aqueous solutions. Microchemical Journal, 225 (NA). pp. 1-14. ISSN 0026-265X

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Abstract

The rising atmospheric carbon dioxide (CO2) concentration and its dissolution in aquatic systems have intensified interest in electrochemical sensing technologies capable of sensitive detection of dissolved CO2. To address this, molybdenum (Mo) microdisk electrodes were surface modified with reduced graphene oxide (rGO) via a one-step electrochemical deposition method, following graphene oxide synthesis using a modified Hummers' approach. The morphology, elemental composition, and crystalline phases were characterised using scanning electron microscopy, energy dispersive X-ray, X-ray diffraction, and X-ray photoelectron spectroscopy confirming a successful rGO deposition alongside minor molybdenum oxide (MoO2) phases on the electrode surface. The scalable electrodeposition process employed herein eliminates the need for chemical reductants, offering an environmentally benign route for the development of graphene-based electrocatalysts. The cyclic voltammetry evaluation, conducted at a scan rate of 0.1 V s−1 within a potential window of −1.25 to 0.25 V (vs Ag/AgCl), demonstrates an enhanced CO2 reduction activity in 0.5 M sodium bicarbonate (NaHCO3) at −1.0 V vs Ag/AgCl compared with bare Mo, evidenced by higher cathodic currents, a linear response to CO2 bubbling time (R2 > 0.9981) from 2 to 20 min, and quasi-reversible electron transfer behaviour. The electrodes displayed high reproducibility with relative standard deviation, RSD = 1.57%. This research work aims at proposing a low cost, facile, sensitive and selective assembly of three electrode electrochemical reduction of dissolved CO2 which operates at room temperature in ambient conditions and highlights the potential for future studies exploring rGO integration on other metal microelectrodes. © 2026 Elsevier B.V.

Item Type: Article (Journal)
Uncontrolled Keywords: Carbon dioxide reduction; Dissolved carbon dioxide gas; Electrochemical sensor; Electrodeposition; Graphene oxide; Reduced graphene oxide
Subjects: Q Science > QD Chemistry
Kulliyyahs/Centres/Divisions/Institutes (Can select more than one option. Press CONTROL button): Kulliyyah of Science
Kulliyyah of Science > Department of Chemistry
Depositing User: Dr Wan Hazman Danial
Date Deposited: 28 Oct 2026 16:48
Last Update: 28 Oct 2026 16:48
Queue Number: 2026-10-Q5855
URI: http://irep.iium.edu.my/id/eprint/132286
Indexed In: WOS and SCOPUS, ERA, Google Scholar

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