Various methods for the preparation
of inorganic nanosheets have
been established and they have contributed to the substantial development
of the research on diverse two-dimensional materials. Covalent surface
modification of layered metal hydroxides with alkoxy groups is known
to effectively weaken the interactions between layers, although the
modified ligands are irreversibly immobilized. This study proposes
the use of methanol as a removable surface modifier forming monodentate
alkoxy bonds to prepare nickel hydroxide nanosheets through hydrolysis.
Methoxylated layered nickel hydroxide, consisting of randomly stacked
nano-sized nickel hydroxide sheets (10–20 nm in size) having
Ni–OCH3 groups on its surface, was synthesized in
a powder form through the precipitation reaction of a nickel salt
in methanol at room temperature. After dispersing the aggregated methoxylated
nickel hydroxide in water, single-layer nickel hydroxide nanosheets
with a thickness of 1.2 nm and a lateral size of 460 nm at maximum,
which is larger than the size of original methoxylated nickel hydroxide
were found in the suspension. The time-course experiments during hydrolysis
suggested that two-dimensional crystal growth of exfoliated nickel
hydroxide sheets proceeded, resulting in the formation of the nanosheets.
Moreover, single-layer and nano-sized cobalt hydroxide was prepared
through a similar manner. This work demonstrates that two-dimensional
alkoxides consisting of polymeric M–O–M bonds are useful
precursors for the design of metal-hydroxide-based nanomaterials.