A pyrochlore-type crystal structure photocatalytic nanomaterial, Ho
2FeSbO
7, was successfully synthesized using a hydrothermal method. Additionally, a fluorite-structured Bi
0.5Yb
0.5O
1.5 was prepared via rare earth Yb doping. Finally, a novel Ho
2FeSbO
7/Bi
0.5
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A pyrochlore-type crystal structure photocatalytic nanomaterial, Ho
2FeSbO
7, was successfully synthesized using a hydrothermal method. Additionally, a fluorite-structured Bi
0.5Yb
0.5O
1.5 was prepared via rare earth Yb doping. Finally, a novel Ho
2FeSbO
7/Bi
0.5Yb
0.5O
1.5 heterojunction photocatalyst (HBHP) was fabricated using a solvothermal method. The crystal structure, surface morphology, and physicochemical properties of the samples were characterized using XRD, a micro-Raman spectrometer, FT-IR, XPS, ultraviolet photoelectron spectroscopy (UPS), TEM, and SEM. The results showed that Ho
2FeSbO
7 possessed a pyrochlore-type cubic crystal structure (space group Fd-3m, No. 227), while Bi
0.5Yb
0.5O
1.5 featured a fluorite-type cubic structure (space group Fm-3m, No. 225). The results of the degradation experiment indicated that when HBHP, Ho
2FeSbO
7, or Bi
0.5Yb
0.5O
1.5 was employed as a photocatalytic nanomaterial, following 140 min of visible light irradiation, the removal efficiency of ciprofloxacin (CIP) reached 99.82%, 86.15%, or 73.86%, respectively. This finding strongly evidenced the remarkable superiority of HBHP in terms of photocatalytic performance. Compared to the individual catalyst Ho
2FeSbO
7, Bi
0.5Yb
0.5O
1.5, or N-doped TiO
2, the removal efficiency of CIP by HBHP was 1.16 times, 1.36 times, or 2.52 times higher than that by Ho
2FeSbO
7, Bi
0.5Yb
0.5O
1.5, or N-doped TiO
2, respectively. The radical trapping experiments indicated that in the CIP degradation process, the hydroxyl radical owned the strongest oxidation ability, followed by the superoxide anion and the photoinduced hole. These studies are of great significance for the degradation of antibiotics and environmental protection.
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