DOI: 10.55525/tjst.1760043 ISSN: 1308-9080

Synthesis method of Ti3C2Tx MXene and the effect of synthesis conditions on MXene

Mustafa Yegin, Özge Hanay
With increasing industrialization, population growth, and rapidly rising consumption, the energy crisis and environmental pollution have become increasingly significant global concerns. Rapid industrial expansion, together with the industrial wastes it generates and the intensification of unplanned urbanization, has resulted in the contamination of existing surface and groundwater resources. In recent years, difficulties in accessing clean water and the emergence of water scarcity have begun to be felt worldwide. Therefore, new processes and novel materials are required both to prevent the pollution of current water resources and to remove contaminants from polluted water systems. Recent studies have shown a growing interest in nanomaterials. Among these, MXenes two-dimensional nanomaterials have been employed in various processes for the removal of toxic pollutants from aqueous environments due to their surface functional groups, high electrical conductivity, hydrophilic behavior, and large surface area. In this study, Ti₃C₂Tₓ MXene was synthesized from the Ti₃AlC₂ MAX phase through direct etching using HF and LiF+HCl solutions. The effects of synthesis conditions including temperature, etching duration, and etchant concentration on the surface terminations, morphological features, and chemical structure of the MXene were determined through SEM, EDS, XRD, and TGA analyses. Examination of the XRD data revealed that the 38.6° Al peak present in the MAX phase disappeared in the MXene structures synthesized by both routes, indicating the successful formation of the MXene phase. XPS results showed the presence of –F, –O, and –OH surface termination groups in MXenes synthesized via direct HF etching; together with the accordion-like morphology observed in SEM images, these features indicated the potential of the material to serve as an effective adsorbent for the removal of heavy metals and other pollutants. Contact angle measurements demonstrated that the MXene synthesized via HF (30 °C, 20% HF, 48 h) exhibited a contact angle of 40°, whereas MXene synthesized using LiF+HCl (33.13% HCl, 1.88 g LiF, 60 °C, 27 h) showed a contact angle of 26°, confirming a more hydrophilic behavior compared to the MAX phase (62°). TGA analysis further revealed that MXenes obtained through both synthesis routes remained stable without oxidation up to temperatures between 600 °C and 800 °C.