Layered protonated
titanates (LPTs) are promising support materials for catalytic applications
because their high surface area and cation exchange capacity provide
the possibility of achieving a high metal dispersion. However, the
reported LPT nanomaterials are mainly limited to free-standing nanoparticles
(NPs) and usually require high temperature and pressure conditions
with extended reaction time. In this work, a high-throughput microwave-assisted
hydrothermal method was developed for the direct synthesis of conformal
LPT nanoarray coatings onto the three-dimensional honeycomb monoliths
as well as other substrate surfaces at low temperature (75–95
°C) and pressure (1 atm). Using TiCl3 as the titanium
source, H2O2 as the oxidant, and hydrochloric
acid as the pH controller, a peroxotitanium complex (PTC) was formed
and identified to play an essential role for the formation of LPT
nanoarrays. The gaseous O2 released during the decomposition
of PTC promotes the mass transfer of the precursors, making this method
applicable to substrates with complex geometries. With the optimized
conditions, a growth rate of 42 nm/min was achieved on cordierite
monolith substrates. When loaded with Pt NPs, the LPT nanoarray-based
monolithic catalysts showed excellent low-temperature catalytic activity
for CO and hydrocarbon oxidation as well as satisfactory hydrothermal
stability and mechanical robustness. The low temperature and pressure
requirements of this facile hydrothermal method overcome the size-
and pressure-seal restrictions of the reactors, making it feasible
for scaled production of LPT nanoarray-based devices for various applications.