Lewis acidic molten salt method is a promising synthesis
strategy
for achieving MXenes with controllable surface termination from numerous
MAX materials. Understanding the phase evolution chemistry during
etching and post-processing is highly desirable but remains a key
challenge due to the lack of suitable in-situ characterizations and
the complexity of the reaction process. Herein, we introduce an operando
synchrotron radiation X-ray diffraction (SRXRD) technique to unveil
the phase evolution process of Nb2GaC MAX under a molten-salt
ambient, proposing a controllable synthesis to achieve optimal etching
through precise temperature and time adjustment. Subsequently, the
phase structure of Nb2CT
x
MXenes
is successfully tailored from hexagonal to amorphous by time-dependent
persulfate oxidation. The resulting amorphous Nb2CT
x
with a well-patterned morphology and numerous
chloride terminations exhibits highly improved specific capacity,
rate capability, and long cycling for Li+ storage with
a Cl-containing surface protective film. Addressing the time-related
phase evolution during the entire molten salt strategy provides new
insights into achieving higher efficiency and controllability in preparing
MXenes and shows great potential in high-performance energy storage
systems based on MXenes.