Crystalline catalysts of orthorhombic MoO3 have been prepared via a va
por phase deposition method, and their crystallographic structure has
been affirmed by XRD and FTIR investigations. A chemical etching metho
d has been developed for restructuring these thermally processed catal
ysts. Using a 0.1 M NaOH etchant, {001} and {100} plane areas of the c
atalysts can be significantly increased while surface steps, ledges, a
nd terraces are created. Moreover, alternate crystal plane combination
s of either {100} and {010} or the {001} and {010} are observed on cry
stal edges and rectangular etch pits in the basal planes {010}. Both m
aterials chemistry of MoO3 and etching mechanisms have been studied on
the basis of the surface morphological evolution of etching patterns
of the catalysts. Technological merits and the processing parameters o
f this new method have also been identified. Following the findings of
the current work, it is believed that the chemically carved surface s
tructures may be crucial for certain MoO3-involving catalytic reaction
s.