Two‐Step Synthetic Method for 2D MXene Through Tungsten Carbide Nanoparticles and Their Characterization

ABSTRACT MXenes, a unique family of two‐dimensional (2D) transition metal carbides, have attracted growing interest due to their outstanding electrical, mechanical, and catalytic properties. However, traditional synthesis methods often rely on hazardous chemical etchants and complex procedures, limiting their scalability and environmental feasibility. In this work, we introduce a simplified, etchant‐free two‐step method for transforming tungsten carbide into MXene‐like materials, utilizing basic laboratory equipment and moderate temperature conditions. This novel approach involves the initial synthesis of metal carbide nanoparticles followed by their successful delamination in ethanol through a sonication‐assisted method. The prepared WC nanoparticle and its MXenes were characterized using FTIR, XRD, Raman, SEM with EDAX, TEM, and XPS analysis. FTIR analysis confirmed the formation of MXenes through the appearance of a new peak at 1232 cm −1 and the weakening of characteristic carbide peaks at 1112 and 832 cm −1 . XRD patterns revealed distinct reflections at 32.3°, 35.0°, 41.2°, and 48.0°, alongside a notable reduction in crystallite size from 48.52 nm in carbide to 35.67 nm in MXene. Elemental analysis showed a shift in the tungsten‐to‐carbon ratio from 1:4 to 1:12, while tungsten signal intensity dropped from 3.2 to 1.8 counts per second, suggesting encapsulation by carbon layers. Morphological transitions were evident in SEM images, evolving from amorphous particles to layered sheet‐like structures. TEM imaging further revealed clear lattice fringes at the 2‐nm scale. Raman spectroscopy exhibited a blue shift in the A₁g mode from 802to 798 cm −1 , indicating enhanced layering. XPS results confirmed surface functionalization and changes in tungsten oxidation states, affirming this method as an efficient, scalable, and environmentally friendly approach to MXene synthesis.