Understanding
of the surface mechanism of electrode materials based
on MXenes, such as morphological evolution, is of great significance
for improving reaction kinetics and efficiency. In this paper, the
morphological evolutions of Ti3C2T
x
nanosheets and Fe3O4/Ti3C2T
x
nanocomposites
during potential cycling were explored by electrochemical atomic
force microscopy for the first time. The oxidation reaction of Fe
nanocomposites during potential cycling were explored by in situ electrochemical
atomic force microscopy for the first time. The oxidation reaction
of Fe3O4 to FeOOH and the accumulation of FeOOH
on the Fe3O4/Ti3C2T
x
nanocomposites during potential cycling resulted
in the appearance of deposits on the surface. After 70 cycles, cracks
formed in the Fe3O4/Ti3C2T
x
nanocomposites, which might be caused
by the falling of the deposits and the loss of Fe species during potential
cycling. The Ti3C2T
x
nanosheets became higher, and the volume expanded significantly
during potential cycling. The specific capacitance of Fe3O4/Ti3C2T
x
nanocomposites was higher than that of Ti3C2T
x
nanosheets. Their specific capacitances
gradually decreased during potential cycling, which could be assigned
to the morphological evolutions. The loading of Fe3O4 nanoparticles in the Ti3C2T
x
nanosheets played very important roles in morphological
evolutions and electrochemical properties. Comprehending morphological
evolutions of Ti3C2T
x
nanosheets and Fe3O4/Ti3C2T
x
nanocomposites during potential cycling
is very beneficial to design electrode materials and interfacial constructions
based on MXenes.