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MXenes, 2D transition metal carbides, nitrides, or carbonitrides, have garnered significant research attention due to their exceptional properties. Delaminated MXenes (d-MXenes) have further expanded interest due to their enhanced functionalities. However, their instability in aqueous solutions and oxygen-rich environments at room temperature, leading to surface oxidation, remains a critical challenge.
In this study, Ti3C2Tx and Mo2CTx multilayer MXenes were synthesized from their respective MAX phases (Ti3AlC2 and Mo2Ga2C) using a mixed etching solution of 12 M HCl, DI water, and 48% HF with ratios of 6:3:1 (for Ti3AlC2) and 6:1:3 (for Mo2Ga2C). The etched MXenes were further treated with 0.5 M LiCl to obtain delaminated MXene (d-MXene) sheets, dispersed in nitrogen-degassed DI water.
The d-MXenes were characterized using UV-visible spectroscopy, HRSEM, and EDS. Samples were aged at room temperature for 20 days, after which fresh samples were also prepared from the same MXene solutions for comparison.
HRSEM and EDS analyses revealed that 20-day-old d-MXene samples exhibited surface oxide formation, with Ti3C2Tx forming pinecone-like structures (TiO2) and Mo2CTx showing spherical oxide particles (MoO3). In contrast, freshly prepared d-MXene samples exhibited unoxidized smooth surfaces and sharp edges for Ti3C2Tx and uneven surfaces with bent edges for Mo2CTx.
After 45 days in aqueous solutions at room temperature, the Ti3C2Tx solution color changed from transparent green to whitish, and the Mo2CTx from transparent brown to blue, confirming significant oxidation. These findings emphasize the need for deoxygenated storage conditions to enhance the stability and lifespan of Ti3C2Tx and Mo2CTx d-MXenes in both liquid and solid forms.