Effect of Sonication Approaches on the Silanization and Structural Quality of Multilayer Ti3C2Tx

MXenes have attracted attention due to their high specific surface area, excellent electrical conductivity, and considerable mechanical properties. Multilayer Ti 3 C 2 T x faces challenges related to restacking and agglomeration as well as its limited oxidation/degradation resistance in oxygen‐containing environments. In this study, multilayer Ti 3 C 2 T x is chemically functionalized by silanization with trimethoxy(octyl)silane while varying the dispersion approach. The impact of four sonication approaches on the success of silanization of Ti 3 C 2 T x by Fourier transform infrared spectroscopy, Raman spectroscopy, scanning electron microscopy coupled with energy dispersive X‐ray spectroscopy, and X‐ray photoelectron spectroscopy, is studied. Regardless of the approach, all procedures successfully silanize Ti 3 C 2 T x , demonstrating the robustness of each individual procedure. Moreover, the various sonication approaches do not affect the samples’ morphology. The two‐step sonication approach (method B) that consists of dispersing Ti 3 C 2 T x first in isopropanol for 20 min using bath‐sonication and then dispersing them for 30 min in isopropanol/toluene/trimethoxy(octyl)silane using bath sonication notably reduces the amount of amorphous carbon in Ti 3 C 2 T x , indicating an enhanced structural quality due to the reduced amount of defective carbon. The silanized Ti 3 C 2 T x obtained using method B shows an enhanced oxidation stability, a greater hydrophobicity, and an improved stability in apolar solvents compared to pristine Ti 3 C 2 T x .