Using P25 as the titanium source and based on a hydrothermal route, we have synthesized CaTiO₃ nanocuboids (NCs) with the width of 0.3–0.5 μm and length of 0.8–1.1 μm, and systematically investigated their growth process. Au nanoparticles (NPs) of 3–7 nm in size were assembled on the surface of CaTiO₃ NCs via a photocatalytic reduction method to achieve excellent Au@CaTiO₃ composite photocatalysts. Various techniques were used to characterize the as-prepared samples, including X-ray powder diffraction (XRD), scanning/transmission electron microscopy (SEM/TEM), diffuse reflectance spectroscopy (UV-vis DRS), Fourier transform infrared spectroscopy (FTIR), and X-ray photoelectron spectroscopy (XPS). Rhodamine B (RhB) in aqueous solution was chosen as the model pollutant to assess the photocatalytic performance of the samples separately under simulated-sunlight, ultraviolet (UV) and visible-light irradiation. Under irradiation of all kinds of light sources, the Au@CaTiO₃ composites, particularly the 4.3%Au@CaTiO₃ composite, exhibit greatly enhanced photocatalytic performance when compared with bare CaTiO₃ NCs. The main roles of Au NPs in the enhanced photocatalytic mechanism of the Au@CaTiO₃ composites manifest in the following aspects: (1) Au NPs act as excellent electron sinks to capture the photoexcited electrons in CaTiO₃, thus leading to an efficient separation of photoexcited electron/hole pairs in CaTiO₃; (2) the electromagnetic field caused by localized surface plasmon resonance (LSPR) of Au NPs could facilitate the generation and separation of electron/hole pairs in CaTiO₃; and (3) the LSPR-induced electrons in Au NPs could take part in the photocatalytic reactions.

In this work, we have synthesized BiOCl nanoplates (diameter 140–220 nm, thickness 60–70 nm) via a co-precipitation method, and then created Bi nanoparticles (diameter 35–50 nm) on the surface of BiOCl nanoplates via a NaBH₄ reduction method. By varying the NaBH₄ concentration and reaction time, the evolution of Bi nanoparticles was systematically investigated. It is demonstrated that with increasing the NaBH₄ concentration (at a fixing reaction time of 30 min), BiOCl crystals are gradually reduced into Bi nanoparticles, and pure Bi nanoparticles are formed at 120 mM NaBH₄ solution treatment. At low-concentration NaBH₄ solutions (e.g., 10 and 30 mM), with increasing the reaction time, BiOCl crystals are partially reduced into Bi nanoparticles, and then the Bi nanoparticles return to form BiOCl crystals. At high-concentration NaBH₄ solutions (e.g., 120 mM), BiOCl crystals are reduced to Bi nanoparticles completely with a short reaction time, and further prolong the treatment time leads to the transformation of the Bi nanoparticles into a two-phase mixture of BiOCl and Bi₂O₃ nanowires. The photodegradation performances of the samples were investigated by choosing rhodamine B (RhB) as the model pollutant and using simulated sunlight as the light source. It is demonstrated that an enhanced photodegradation performance can be achieved for the created Bi@BiOCl hybrid composites with appropriate NaBH₄ treatment. The underlying photocatalytic mechanism was systematically investigated and discussed.