A bilayered rare-earth-based metal–insulator–semiconductor,
Dy
2
O
3
@SiO
2
@ZnO core–shell
nanospheres, was synthesized by a stepwise synthesis for enhanced
visible photocatalytic activity. The prepared material was characterized
by Fourier transform infrared spectroscopy, X-ray diffraction, ultraviolet–visible
diffuse reflectance spectroscopy, field-emission scanning electron
microscopy, energy-dispersive spectroscopy, high-resolution transmission
electron microscopy, selected area electron diffraction, atomic force
microscopy, X-ray photoelectron spectroscopy, Brunauer–Emmett–Teller,
and electron paramagnetic resonance techniques. Dy
2
O
3
@SiO
2
@ZnO core–shell nanospheres were found
be in a spherically arranged cauliflower-like morphology (40–60
nm). The high-resolution transmission electron microscopy analysis
proved the core–shell morphology of the prepared material with
a single Dy
2
O
3
core and two shells comprising
SiO
2
and ZnO. The material possessed a surface roughness
of 4. 98 nm (2 × 2 μm area) and a band gap energy of 2.82
eV. The in situ generation of OH radicals was confirmed by electron
paramagnetic resonance. Electron hopping through the SiO
2
layer from ZnO to Dy
2
O
3
played a major role
in trapping electrons in the f-shells of lanthanides, thus, preventing
the recombination of electron–hole pair. X-ray photoelectron
spectroscopy studies proved the band alignment of the material. Brunauer–Emmett–Teller
analysis further showed the core–shell surface area was 14
m
2
/g. The visible photocatalytic activity was tested against
2,4-D (2,4-dichlorophenoxyacetic acid), an endocrine disruptor. The
kinetic studies showed that the photocatalytic degradation process
followed a pseudo-first-order pathway. The photocatalyst was found
to be reusable even up to the third cycle.