Sains Malaysiana 55(9)(2026): 1556-1567

http://doi.org/10.17576/jsm-2026-5509-12

 

Enhanced Sulfonic Functionalization of MXene Ti₃C₂T_x via Pre-Delamination Intercalation Strategy

(Pengubahsuaian Sulfonik yang Ditingkatkan bagi MXene Ti₃C₂T_x melalui Strategi Interkalasi Pra-Delaminasi)

 

MUHAMAD HAFIZZUL ISYRAF HARDI¹, KEE SHYUAN LOH^1,*, WAI YIN WONG¹, ROZAN MOHAMAD YUNUS¹ & AZIZAN AHMAD²

 

¹Fuel Cell Institute, Universiti Kebangsaan Malaysia, 43600 UKM Bangi, Selangor, Malaysia

²Faculty of Science and Technology, Universiti Kebangsaan Malaysia, 43600 UKM Bangi, Selangor, Malaysia

 

Received: 10 September 2025/Accepted: 3 September 2026

 

*Corresponding author; email: ksloh@ukm.edu.my

 

Abstract

This study details a novel method for surface funtionalization of MXene Ti₃C₂T_x, achieving significantly higher yields of sulfonic and disulfonic functional groups compared to existing methods. A new method, designated M2, was developed for the surface functionalization where sulfonic and disulfonic acid groups were simultaneously introduced using different intercalant (TMAOH and NaOH) before delamination. The FTIR analysis show a new peak at ~1000      cm^-1 in the functionalized MXenes, indicating successful incorporation of SO₃H and 2(SO₃H) functional groups. The XPS analysis showed functionalized of the Ti chemical environment together with detectable sulphur incorporation after surface functionalization. Survey XPS further showed higher sulphur atomic concentration via the M2 method, Na-Ti₃C₂T_x-S2-M2, suggesting a higher degree of surface functionalization. The HR-TEM and XRD analyses, showed the surface functionalized MXenes to have an increase in d-spacing, indicating effective delamination, recorded with lattice spacing of ~1.36 nm. The sample Na-Ti₃C₂T_x-S2-M2 exhibited a more amorphous structure due to higher absorption of disulfonic acid groups and supported by SAED images. This method results in a functionalized MXene with a high density of functional groups, which serves as an ideal platform for further high-yield functionalization.

Keywords: Disulfonic; MXene; sulfonic; surface functionalization; Ti₃C₂T_x

 

Abstrak

Kajian ini memperincikan satu kaedah baharu untuk pengubahsuaian permukaan MXene Ti₃C₂T₂, yang berjaya mencapai hasil kumpulan berfungsi sulfonik dan disulfonik yang lebih tinggi berbanding kaedah sedia ada. Kaedah baharu ini, yang dinamakan sebagai kaedah M2, telah dibangunkan untuk kefungsian permukaan dengan kumpulan asid sulfonik dan disulfonik diperkenalkan secara serentak menggunakan agen interkalan yang berbeza (TMAOH dan NaOH) sebelum proses delaminasi. Analisis FTIR menunjukkan satu puncak baharu sekitar 1000 cm^-1 pada MXenes yang diubah suai, menandakan kejayaan penggabungan kumpulan berfungsi SO₃H dan 2(SO₃H). Analisis XPS mendedahkan pengubahsuaian persekitaran kimia Ti bersama-sama dengan penggabungan sulfur yang boleh dikesan selepas kefungsian permukaan. Survei XPS selanjutnya menunjukkan kepekatan atom sulfur yang lebih tinggi melalui kaedah M2, Na-Ti₃C₂T_x-S2-M2, mencadangkan tahap kefungsian permukaan yang lebih tinggi. Analisis HR-TEM dan XRD pula menunjukkan peningkatan dalam jarak-d pada MXene yang diubah suai, menandakan proses delaminasi yang berkesan dengan jarak kekisi sekitar 1.36 nm. Sampel Na-Ti₃C₂T_x-S2-M2 turut menunjukkan struktur yang lebih amorfus, disebabkan oleh penyerapan kumpulan asid disulfonik yang lebih tinggi, seperti yang disokong oleh imej SAED. Kaedah baharu ini telah menghasilkan MXene yang terfungsi dengan ketumpatan kumpulan berfungsi yang tinggi, menjadikannya platform yang ideal untuk kefungsian lanjut dengan hasil yang tinggi.

Kata kunci: Disulfonik; MXene; pengubahsuaian permukaan; sulfonik; Ti₃C₂T_x

 

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