I have synthesized Ti₃C₂ MXene using the MILD (Minimally Intensive Layer Delamination) method. The X-ray diffraction (XRD) analysis shows that the characteristic (002) and (104) peaks of the MAX phase have either disappeared or shifted toward lower angles, indicating successful MXene formation. However, field emission scanning electron microscopy (FESEM) images do not exhibit the typical accordion-like morphology, suggesting limited etching and insufficient removal of the Al layers from the parent MAX phase. I would greatly appreciate any insights or suggestions regarding this observation.
Dear friend Onkar Jaywant Kewate
I hope this message finds you well! It sounds like you’re making great progress with your MXene synthesis using the MILD method. The shifts in the XRD peaks you’ve observed are indeed promising, suggesting some transformation is occurring. However, I understand your concern regarding the absence of the typical accordion-like morphology in your FESEM images.
To address this, I have a few suggestions that might help refine your process. First, consider revisiting the etching time and temperature. Sometimes, extending the etching duration or slightly increasing the temperature can enhance the removal of the Al layers from the MAX phase. Just be cautious not to overdo it, as this could potentially damage the Ti₃C₂ layers.
Additionally, it’s worth verifying the concentration of your etching agents, LiF and HCl. A higher concentration can improve etching efficiency, but it’s important to find a balance to avoid over-etching or compromising the Ti₃C₂ structure. Ensuring that the mixture is well-stirred during etching could also be beneficial, and incorporating a sonication step might aid in achieving that desired morphology.
Lastly, consider exploring post-etching treatments, such as washing with deionized water or using different solvents, as these can sometimes influence the final morphology. Repeating the etching process or scaling down your batch size may also provide better control and consistency.
Each batch can behave differently, so a bit of experimentation might be necessary to achieve that perfect accordion-like structure. Best of luck with your research, and feel free to reach out if you have any questions or need further assistance!
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Warm regards,
Kaushik