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Sains Malaysiana 54(9)(2025): 2211-2226
http://doi.org/10.17576/jsm-2025-5409-09
Synthesis and Characterization of Fe3O4/rGO/Ag
Composites for Electrocatalytic Oxygen Reduction Reaction (ORR)
(Sintesis dan Pencirian Komposit Fe3O4/rGO/Ag
untuk Tindak Balas Pengurangan Oksigen Elektrokatalitik (ORR))
KOMATY MARAN1,
SARAH ILYANIE ROSWADI1, MOHD AFIFI JUSOH2 & FARHANINI
YUSOFF1,*
1Faculty
of Science and Marine Environment, Universiti Malaysia Terengganu, 21030 Kuala
Terengganu, Terengganu, Malaysia
Received: 11 September 2024/Accepted: 18 July
2025
Abstract
The oxygen reduction
reaction (ORR) plays a pivotal role in fuel cells, making the discovery of
efficient and cost-effective catalysts to substitute platinum crucial for the
progress of sustainable energy technologies. This study investigates a new
rGO/Fe3O4/Ag composite as a potential low-cost substitute
for platinum-based cathode materials in ORR applications due to platinum’s
drawbacks. Reduced graphene oxide incorporated with iron (III) oxide and
silver nanoparticles were synthesized through a modified one-pot process,
denoted as rGO/Fe3O4/Ag. This study is the first to
utilize rGO/Fe3O4/Ag as an ORR catalyst. Synthesis began
with the formation of graphene oxide, followed by its reduction, the addition
of Fe2+ and Fe3+, and the introduction of silver
nanoparticles via silver nitrate (AgNO3) to produce the novel
electrocatalyst. Physicochemical and electrochemical characterization was
performed using Fourier transform infrared (FTIR) spectroscopy, X-ray
diffraction (XRD), scanning electron microscopy-energy dispersive X-ray
(SEM-EDX), Brunauer-Emmett-Teller (BET) analysis, and cyclic voltammetry (CV).
FTIR confirmed the presence of functional groups such as O-H, C=C, C=O, C-O,
C-Fe, and C-Ag in the nanocomposites. XRD identified average crystalline sizes,
with diffraction peaks confirming the formation of rGO/Fe3O4/Ag.
SEM-EDX analysis showed well-dispersed Fe3O4 and Ag
nanoparticles on rGO sheets, and BET analysis indicated the nanocomposites were
mesoporous, with a surface area of 81.60 m2/g for rGO/Fe3O4/Ag.
Electrochemical characterization showed that the modified rGO/Fe3O4/Ag
exhibited significant redox responses, indicating enhanced electrochemical
activity compared to the bare GCE. In the ORR analysis, the rGO/Fe3O4/Ag
demonstrated a positive shift in the cyclic voltammogram, suggesting improved
current density and superior ORR performance relative to the bare GCE. These
results strongly suggest that rGO/Fe3O4/Ag can be an
effective replacement for platinum in ORR applications as a cathode material.
Keywords: Cyclic voltammetry; electrocatalyst;
graphene; iron oxide; oxygen reduction reaction (ORR)
Abstrak
Tindak balas pengurangan
oksigen (ORR) memainkan peranan penting dalam sel bahan api, menjadikan
penemuan pemangkin yang cekap dan kos efektif untuk menggantikan platinum
penting untuk kemajuan teknologi tenaga mampan. Penyelidikan ini mengkaji
komposit rGO/ Fe3O4/Ag baharu sebagai pengganti kos
rendah yang berpotensi untuk bahan katod berasaskan platinum dalam aplikasi ORR
disebabkan oleh kelemahan platinum. Grafena oksida terkurang yang digabungkan
dengan oksida besi (III) dan nanozarah perak telah disintesis melalui proses
satu periuk yang diubah suai, dilambangkan sebagai rGO/Fe3O4/Ag.
Penyelidikan ini
merupakan kajian pertama yang menggunakan rGO/Fe3O4/Ag
sebagai katalis ORR. Sintesis bermula dengan pembentukan grafin oksida, diikuti
oleh penurunannya, penambahan Fe2+ dan Fe3+ dan
pengenalan nanozarah perak melalui nitrat perak (AgNO3) untuk
menghasilkan elektrokatalis baru. Pencirian fizikal-kimia dan elektrokimia
dilakukan dengan menggunakan spektroskopi transformasi Fourier inframerah
(FTIR), pembelauan sinar-X (XRD), mikroskop elektron pengesan-tenaga-sebaran
X-ray (SEM-EDX), analisis Brunauer-Emmett-Teller (BET) dan voltametri berkitar
(CV). FTIR mengesahkan kehadiran kumpulan berfungsi seperti O-H, C=C, C = O,
C-O, C-Fe dan C-Ag dalam nanokomposit. XRD mengenal pasti saiz kristal purata
dengan puncak difraksi mengesahkan pembentukan rGO/Fe3O4/Ag.
Analisis SEM-EDX mendedahkan nanozarah Fe3O4 dan Ag yang
tersebar dengan baik pada permukaan rGO dan analisis BET menunjukkan
nanokomposit adalah ‘mesoporous’ dengan kawasan permukaan 81.60 m2/g
untuk rGO/Fe3O4/Ag. Pencirian elektrokimia menunjukkan
bahawa rGO/Fe3O4/Ag yang diubah suai menunjukkan respons
redoks yang signifikan; peningkatan aktiviti elektrokimia berbanding dengan
GCE. Dalam analisis ORR, rGO/Fe3O4/Ag menunjukkan
pergeseran positif dalam voltamogram kitaran yang menunjukkan peningkatan
kepadatan arus dan prestasi ORR yang lebih baik berbanding GCE sahaja. Hasil
ini menunjukkan bahawa rGO/Fe3O4/Ag boleh menjadi
pengganti platinum yang berkesan dalam aplikasi ORR sebagai bahan katod.
Kata kunci: Grafin; katalis; oksida besi;
tindak balas pengurangan oksigen (ORR); voltametri berkitar
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