Commercially
available bulk niobium diselenide (NbSe2) reduced into
nanomaterials upon exfoliation typically contains
oxide and carbide impurities. Liquid-phase exfoliated two-dimensional
(2D) nanosheets of NbSe2 obtained from bulk powders provide
high charge mobility and large surface area but become self-passivated
and chemically inert as the presence of oxide impurities makes them
behave more semimetallic. In this article, we report the effects of
inherent impurities of liquid-phase exfoliated 2D NbSe2 (intended to be integrated as supercapacitor electrodes) on the
electrochemical performance. The highest specific capacitances achieved
using 1-butyl-3-methylimidazolium hexafluorophosphate (BMIMPF6) and sulfuric acid (1 M H2SO4) electrolytes
were 4955.5 ± 21.5 and 13 361.6 ± 31.8% mF/cm2, respectively, which were affected by the impurities, oxophilicity
of niobium defects, and moisture adsorption in the cell. Galvanostatic
charge–discharge profiles show moisture adsorption affecting
the high-energy charging procedure in the cell for BMIMPF6, resulting in leakage and decomposition of the electrolyte. Electrochemical
impedance spectroscopy provides insights into the solid-electrolyte
interphase and charge-transfer mechanisms at exfoliated 2D NbSe2 nanosheets, which affect the ion intercalation through heterogenous
phases of the nanosheets. Overall, the NbSe2 nanosheets
offer heterogenous phases because of the coexistence of Nb2O5 that influences the charge-transfer mechanism at the
exfoliated surfaces.