Scalable Synthesis of Ti3C2Tx Mxene

Scaling the production of synthetic two-dimensional (2D) materials to industrial quantities has faced significant challenges due to synthesis bottlenecks whereby few have been produced in large volumes. These challenges typically stem from bottom-up approaches limiting the production to the substrate size or precursor availability for chemical synthesis and/or exfoliation. MXenes are a large family of 2D carbides and/or nitrides that have applications in electrochemical energy storage, electromagnetic interface shielding, electrocatalysis, gas sensing, electrochromic devices, and many others. In contrast to other 2D materials, MXenes are produced via a top-down synthesis approach. The selective wet etching process does not have similar synthesis constraints as some other 2D materials. The reaction occurs in the whole volume; therefore the process can be readily scaled with reactor volume. In this study, the synthesis of 2D titanium carbide MXene (Ti₃C₂T_x) was studied in two batch sizes, 1 and 50 g, to determine if large-volume synthesis affects the resultant structure or composition of MXene flakes. Characterization of the morphology and properties of the produced MXene using scanning electron microscopy, X-ray diffraction (XRD), dynamic light scattering (DLS), Raman spectroscopy, X-ray photoelectron spectroscopy (XPS), UV-visible spectroscopy, and conductivity measurements showed that the materials produced in both batch sizes are essentially identical. This illustrates that MXenes experience no change in structure or properties when scaling synthesis, making them viable for further scale-up and commercialization.