Oleyl phosphate-modified
HLaNb2O7·xH2O nanosheets (OP_HLaNb nanosheets) were prepared
via phase transfer from an aqueous phase, comprising a dispersion
of HLaNb2O7·xH2O (HLaNb) nanosheets, formed through the intercalation of tetrabutylammonium
ion (TBA+) in the interlayer space of HLaNb and subsequent
delamination, to a cyclohexane phase containing oleyl phosphate (OP,
a mixture of monoester and diester). The modification of HLaNb nanosheets
with OP was essentially completed within 3 days at a pH value of 2
or 4. Both infrared and solid-state 13C cross-polarization
and magic-angle spinning (MAS) nuclear magnetic resonance (NMR) spectra
of the OP_HLaNb nanosheets showed the presence of OP and/or related
species and TBA+ on the HLaNb nanosheet surface. The solid-state 31P MAS NMR spectra of OP_HLaNb nanosheets exhibited new signals
at −2 and 0 ppm, the former of which indicates the formation
of Nb–O–P bonds. These whole data set obtained by complementary
techniques clearly point out the modification of the HLaNb nanosheet
surface by OP moieties causing a phase transfer. OP_HLaNb nanosheets
showed higher dispersibility in cyclohexane than the OP_HLaNb_interlayer
nanosheets, which were prepared via stepwise substitution reactions
in the interlayers of HLaNb to achieve surface modification with OP
and subsequent exfoliation in cyclohexane. The presence of TBA+ on the HLaNb nanosheets and the use of a liquid–liquid
biphasic system were likely to improve the dispersibility. These results
show that the preparation of OP-modified HLaNb nanosheets which could
be well-dispersed in the cyclohexane phase was successful because
of the use of a liquid–liquid biphasic system.