We
describe a previously not reported “one-pot” synthesis
of nanocrystalline Ag(0)/CaTiO3 in aqueous suspension and
the following in situ photocatalytic testing in the same suspension
to generate hydrogen. The Ag(0)/CaTiO3 showed an enhancement
of photocatalytic hydrogen generation rate vs CaTiO3 precursor.
The obtained Ag(0)/CaTiO3 photocatalyst was ex situ characterized
by XPS, XRD, UV–vis diffuse reflectance spectroscopy (DRS),
and photoluminescence (PL) spectroscopy, and concluded to have metallic
silver nanoparticles on the surface of calcium titanate nanocrystals.
The three photocatalytic mechanisms in Ag(0)/CaTiO3 were
considered: (a) bandgap narrowing in CaTiO3, (b) enhanced
electron–hole separation in CaTiO3, and (c) excitation
of surface plasmon resonance (SPR) in metallic Ag nanoparticles. In
mechanistic studies, photocatalytic suspensions with CaTiO3 precursor, with silver precursor, and with both CaTiO3 and Ag precursors to form Ag(0)/CaTiO3 were illuminated,
flash-frozen to 77 K, and characterized by in situ “conventional”
PL spectroscopy and in situ synchronous luminescence spectroscopy.
On the basis of the complementary ex situ and in situ studies, an
enhanced electron–hole separation in Ag(0)/CaTiO3 is suggested.