Two-dimensional
(2D) nanomaterials have been the focus of substantial
research interest recently owing to their fascinating and excellent
properties. However, 2D porous materials have remained quite rare
due to the difficulty of creating pores in 2D nanostructures. Here,
we have synthesized a novel type of single-layered 2D mesoporous TiO<sub>2</sub> nanosheets with very uniform size and thickness as well as
ordered mesostructure from an unprecedented hydrothermal-induced solvent-confined
assembly approach. The F127/TiO<sub>2</sub> spherical monomicelles
are first formed and redispersed in ethanol and glycerol, followed
by a hydrothermal treatment to assemble these subunits into single-layered
2D mesostructure owing to the confinement effect of highly adhered
glycerol solvent. The obtained 2D mesoporous TiO<sub>2</sub> nanosheets
have a relative mean size at around 500 × 500 nm and can be randomly
stacked into a bulk. The TiO<sub>2</sub> nanosheets possess only one
layer of ordered mesopores with a pore size of 4.0 nm, a very high
surface area of 210 m<sup>2</sup> g<sup>–1</sup> and a uniform
thickness of 5.5 nm. The thickness can be further manipulated from
5.5 to 27.6 nm via simply tuning precursor concentration or solvent
ratio. Due to the well-defined 2D morphology and large mesoporosity
as well as crystalline anatase mesopore walls, these uniform TiO<sub>2</sub> nanosheets are capable of providing large accessible voids
for sodium ion adsorption and intercalation as well as preventing
volume expansion. As expected, these mesoporous TiO<sub>2</sub> nanosheets
have exhibited an excellent reversible capacity of 220 mAh g<sup>–1</sup> at 100 mA g<sup>–1</sup> as sodium-ion battery anodes, and
they can retain at 199 mAh g<sup>–1</sup> after numerous cycles
at different current densities. The capacity is retained at 44 mAh
g<sup>–1</sup> even at a large current density of 10 A g<sup>–1</sup> after 10 000 cycles, demonstrating a remarkable
performance for energy storage