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Sains Malaysiana 55(3)(2026): 549-559
http://doi.org/10.17576/jsm-2026-5503-15
Effect of Annealing Techniques in
Enhancing Nitrogen Doped Graphene Synthesis by Ball Milling Method
NURUL AIN HUZAIFAH MOHD NORIZAN1,
NORDIN SABLI1,2,*,
SHAMSUL IZHAR SIAJAM2 & ROSHASNORLYZA HAZAN3
1Institute
of Nanoscience and Nanotechnology (ION2), Universiti Putra Malaysia, 43400 UPM Serdang, Selangor, Malaysia
2Department
of Chemical and Environmental Engineering, Faculty of Engineering, Universiti Putra Malaysia, 43400 UPM Serdang, Selangor,
Malaysia
3Materials
Technology Group, Industrial Technology Division, Malaysian Nuclear Agency,
43000 Kajang, Selangor, Malaysia
Received: 5 November 2025/Accepted: 2 March 2026
Abstract
Catalysts
play a crucial role in addressing global challenges related to clean energy
conversion and environmental sustainability. Among various catalyst materials,
nitrogen-doped graphene (NDG) has emerged as a promising metal-free
electrocatalyst for oxygen reduction reactions (ORR) due to its tunable electronic structure and high surface area.
However, conventional synthesis of NDG via ball milling requires prolonged
processing times, limiting its scalability and energy efficiency. This study
focuses on optimizing NDG synthesis by employing annealing techniques to
explore the potential for reducing production durations. NDG was synthesized by
milling graphite and melamine, followed by annealing as a modification process
to expedite synthesis. Key results show significant improvements in structural
and catalytic properties. Raman Spectroscopy showed an ID/IG value of 1.73, indicating enhanced structural integrity. X-ray Diffraction (XRD)
analysis confirmed the formation of graphene layers with a broad peak at 26°.
X-ray Photoelectron Spectroscopy (XPS) identified a nitrogen content of 38%,
crucial for catalytic activity. Electrochemical performance, evaluated via Open
Circuit Potential (OCP) measurements, demonstrated a notable current of 19 mA,
with variations attributed to annealing temperature and milling duration. The
synthesis optimization through ball milling and annealing not only enhances
material properties but also addresses the challenge of time-intensive
production, making NDG more feasible for large-scale applications. These
advancements pave the way for efficient and scalable NDG catalyst production,
essential for advancing technologies in various industrial and environmental
sectors.
Keywords:
Annealing; ball milling; electrocatalysis; nitrogen doped graphene; synthesis
optimization
Abstrak
Pemangkin memainkan peranan penting dalam menangani cabaran global berkaitan penukaran tenaga bersih dan kelestarian alam sekitar. Dalam kalangan pelbagai bahan pemangkin, grafin terdop nitrogen (NDG) telah muncul sebagai pemangkin elektrokimia bebas logam yang berpotensi untuk tindak balas penurunan oksigen (ORR) kerana struktur elektroniknya yang boleh diubah suai serta luas permukaan yang tinggi. Walau bagaimanapun, sintesis konvensional NDG melalui kaedah penggilingan bola memerlukan tempoh pemprosesan yang panjang, sekali gus mengehadkan kebolehskalaan dan kecekapan tenaga proses tersebut. Penyelidikan ini memfokuskan kepada pengoptimuman sintesis NDG dengan menggunakan teknik penaikan suhu (anli) untuk meneroka potensi pengurangan tempoh pengeluaran. NDG disintesis melalui proses penggilingan grafit dan melamin, diikuti dengan proses anil sebagai proses pengubahsuaian bagi mempercepatkan sintesis.
Keputusan utama menunjukkan peningkatan ketara dalam sifat struktur dan keupayaan pemangkin. Spektroskopi Raman menunjukkan nilai ID/IG sebanyak 1.73, menandakan peningkatan keutuhan struktur. Analisis Pembelauan Sinar-X (XRD) mengesahkan pembentukan lapisan grafin dengan puncak lebar pada sudut 26°. Spektroskopi Fotoelektron Sinar-X (XPS) mengenal pasti kandungan nitrogen sebanyak 38%, penting untuk aktiviti pemangkin. Prestasi elektrokimia yang dinilai melalui pengukuran Potensi Litar Terbuka (OCP) menunjukkan arus sebanyak 19 mA dengan variasi yang dikaitkan dengan suhu penaikan (anil) dan tempoh penggilingan. Pengoptimuman sintesis melalui penggilingan bola dan penaikan suhu (anil) bukan sahaja meningkatkan sifat bahan tetapi juga menangani cabaran penghasilan yang memakan masa, menjadikan NDG lebih berdaya maju untuk aplikasi berskala besar. Kemajuan ini membuka jalan bagi penghasilan pemangkin NDG yang lebih cekap dan boleh diskalakan, penting untuk memajukan teknologi dalam pelbagai sektor industri dan alam sekitar.
Kata kunci: Elektrokatalis; grafin terdop nitrogen; penggilingan bola; pengoptimuman sintesis; penyepuhlindapan
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*Corresponding author; email:
nordin_sab@upm.edu.my
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