Effect of Sonication Approaches on the Silanization and Structural Quality of Multilayer Ti ₃ C ₂ T _<i>x</i>

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 .