Photophysical Probes to Reveal Sub-Nanometric Defect Sites on MXenes Prepared by Different Etching Methods
Hermenegildo GARCIA GOMEZ a, Carlos Balenzao b, Ana Primo a, Alberto GARCIA BALDOVÍ a, Dawid Kruguer a
a Instituto de Tecnología Química (ITQ-UPV-CSIC), 46022 Valencia, Spain.
b Instituto Superior Tecnico, Microlab, Lisboa, Portugal
Proceedings of MATSUS Fall 2025 Conference (MATSUSFall25)
E9 Frontiers in MXene Research: From Fundamentals to Applications - #MXFrontiers
València, Spain, 2025 October 20th - 24th
Organizers: Sara GOBERNA FERRON and Ana Primo
Invited Speaker, Alberto GARCIA BALDOVÍ, presentation 404
Publication date: 21st July 2025

MXenes are gaining increasing attention as heterogeneous catalysts[1, 2]. For these applications, surface defects – typically present at very low densities, often at sub-nanometric populations per gram – are believed to play a key role. However, due to this extremely low density, very few experimental techniques are sensitive enough to detect and monitor these types of sites.

In this presentation, I will show that pyrene photoemission, using borylated and amino-functionalized pyrene derivatives[3], can report on subtle surface differences in TiC MXenes prepared by different synthetic methods.

Specifically, TiC obtained by etching TiAlC with NHF, which introduces –F, –OH, and –O surface terminations, interacts strongly with boronic acid–functionalized pyrene. The binding of this molecule indicates the presence of surface –OH groups with a spatial arrangement similar to vicinal diols in organic molecules.

In contrast, 1-aminopyrene reveals unique properties when tested on TiCBr prepared by molten salt etching of TiAlC in a eutectic LiBr/KBr mixture. In this case, the characteristic excimer emission of 1-aminopyrene disappears upon binding to the surface, and only monomer fluorescence is observed. This indicates that NH groups strongly attach to specific sites on the Br-terminated MXene, which are sufficiently isolated to prevent π–π interactions between neighboring pyrene molecules (Fig. 1).

These results demonstrate the potential of photophysical probes to detect and monitor defect sites on MXene surfaces, even at sub-nanometric concentrations.

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