Black NiO powders were prepared by
a hydrothermal method. Moreover,
the visible light-driven Ag
3
PO
4
/NiO photocatalyst
composites were successfully synthesized by in situ precipitation
method. These samples were structurally characterized by X-ray diffraction
and Rietveld refinement. The strong interaction between the phases
and the defects in the samples was affected by the formation of the
composites, as identified by Fourier transform infrared spectroscopy
and Raman spectroscopy. UV–vis diffuse reflectance spectroscopy
exhibited enhanced light absorption for all Ag
3
PO
4
/NiO composites, suggesting the effective interaction between the
phases. Moreover, field-emission scanning electron microscopy images
revealed the presence of NiO microflowers composed of nanoflakes in
contact with Ag
3
PO
4
microparticles. The composite
with 5% NiO presented enhanced photocatalytic efficiency in comparison
with pure Ag
3
PO
4
, degrading 96% of rhodamine
B (RhB) dye in just 15 min under visible light; however, the recycling
experiments confirmed that the composite with 75% NiO showed superior
stability. The recombination of the electron–hole pairs was
considered for the measurement of the photoluminescence of the samples.
These measurements were performed to evaluate the possible causes
for the difference in the photocatalytic responses of the composites.
From these experimental results, possible photocatalytic mechanisms
for RhB degradation over Ag
3
PO
4
/NiO composites
under visible-light irradiation were proposed.