The synthesis of layered metalates consisting of metalate
layers
with two types of metal ions and interlayer organic cations via an
aqueous solution process was studied for the preparation of metalate
nanosheets. First, layered perovskite Cs[Sr2Nb3O10] was synthesized hydrothermally and featured Cs+ ions, but not organic cations, as interlayer cations; the
formation of a strontium niobate layer required a high hydrothermal
temperature (≥150 °C). Next, bulky organic interlayer
cations N(CH3)4
+ and C16H33N(CH3)3
+ were used.
However, bulky cations inhibited the formation of layered compounds
at high temperature due to their thermal vibration. Then, layered
cesium tungstates were hydrothermally synthesized using alkylamines
at a temperature ≥150 °C. Alkylamines NH2C
n
H2n+1 with a
long alkyl chain n ≥ 10 provided a robust
layered structure at ≥150 °C, yielding layered cesium
tungstates with interlayer organic cations. Upon dispersing the product
in acetone solvent, cesium tungstate nanosheets [Cs4W11O36]2– were formed by exfoliation.
Overall, high temperature is required for the hydrothermal synthesis
of metalate layers featuring two types of metal ions, and the interlayer
organic cations are needed to contribute to the formation of layered
structures at high temperature.