Protonated
lanthanum titanium oxide H2La2Ti3O10 and oxynitride H2La2Ti3O10–3/2x
N
x
crystals were synthesized from the oxide, nitrided,
and reoxidized layered K2La2Ti3O10 crystals prepared by solid-state reaction through proton
exchange. Here, we investigated the holding time of nitridation of
oxide K2La2Ti3O10 crystals
influencing their crystal structure, shape, and absorption wavelength
and band gap energy. The XRD and SEM results confirmed that the crystal
structure and plate-like shape of the parent oxide were maintained
after nitridation at 800 °C for 10 h, and the color of crystals
was changed from white to dark green. However, no clear absorption
edges were observed in the UV–vis diffuse reflectance spectra
of the nitrided crystals due mainly to the reduced titanium species
(Ti3+), which act as the recombination center of the photogenerated
charge carriers. To decrease the amount of the reduced titanium species,
the nitrided crystals were further reoxidized at 400 °C for 6
h. After partial reoxidation, the absorption intensity in the longer
wavelength region was reduced, and the absorption edges appeared at
about 449–460 nm. The photocatalytic activity for the water
oxidation half-reaction was evaluated only for the protonated samples.
The protonated reoxidized K2La2Ti3O10 crystals showed the O2 evolution rate of
180 nmol·h–1 (for the photocatalytic water
oxidation) under visible-light irradiation, and the unexpected photocatalytic
decomposition of N2O adsorbed onto the photocatalyst surfaces
was observed for the protonated oxide and protonated nitrided layered
K2La2Ti3O10 crystals.
Furthermore, lanthanum titanium oxide [La2Ti3O10]2– and oxynitride [La2Ti3O10–3/2x
N
x
]2– nanosheets were successfully
fabricated by proton exchange and mechanical exfoliation (sonication)
of the oxide, nitrided, and reoxidized K2La2Ti3O10 crystals. The TEM results revealed that
the lateral sizes of the fabricated nanosheets grown along the ⟨001⟩
direction are 270–620 nm. Apparently, the colloidal suspensions
of the fabricated nanosheets showed a Tyndall effect, implying their
good dispersion and stability for several weeks in water.