An innovative yet simple approach for the in situ growth
of black
phosphorus (BP) over MXene sheets has been carried out by a facile
and simple hydrothermal treatment. Basically, a dual strategy is adopted
to expand MXene interlayer spacing by in situ intercalation of BP
along with encapsulation with an antioxidant agent to prevent oxidation
at elevated temperatures. Detailed nucleation and growth mechanisms
are explained by optimizing the ratio of BP in MXene–BP hybrid
material supported by XRD, FE-SEM, FT-IR, Raman spectroscopy, and
XPS characterizations. The presence of surface terminations (−OH,
−O) at enlarged interlayers of MXenes chemically attached to
BP causes the production of Ti–O–P linkages at the junctions
of heterostructures, resulting in uniform in situ development of BP
over MXenes nanolayers. These interactions enhance the Coulombic reactions
between the core and valence states present at the interface (Ti–O–P)
bonds, which is beneficial for large electronic transfers. Further,
the optimized MXene–BP (10 mg) hybrid denoted as the MX–BP-10
sample was analyzed systematically with temperature-dependent Raman
spectroscopy at elevated temperatures to check its stability at high
temperatures. Moreover, a symmetric MX–BP-10 hybrid supercapacitor
device was fabricated, which reveals excellent specific capacitance
of 120 mF/cm2 at a current density of 0.4 mA/cm2 with an exceptional capacitance retention of 95% and Coulombic efficiency
of 92% even after 10 000 charge–discharge cycles. This
unique intercalation and encapsulation approach to passivate MXenes
gives multidimensional insights to tune its electrochemical properties
at high temperature so as to enhance its oxidation resistance.