摘要

Hierarchically nanoporous silicon hydrogen compound particles were synthesized by dissolving template method, and the hierarchically nanoporous Pd-HSiO1.5 were further prepared by in-situ synthesis method. The microstructure and morphology of the nanoparticles were characterized by the transmission electron microscopy (TEM). In addition, the hierarchically nanoporous P-dHSiO(1.5)/Ni-Co composite electrode was fabricated by the method of nanocomposite electrodeposition, in which hierarchically nanoporous Pd-HSiO1.5 particles were used as composite nanoparticles on the Ni-Co electroplating bath. The surface morphology was characterized by the scanning electron microscopy (SEM). Finally, the sensor was used to detect the tetracycline antibiotics with different classes. Results showed that the hierarchically nanoporous silicon hydrogen compound particles were with hollow spherical structure. The size of the hollow spheres was about 70 nm, and the thickness of the spherical shell was about 10 nm. The Pd nanoparticles were successfully loaded on the inside and surface of the hierarchically nanoporous silicon hydrogen compound. The size of the inside Pd nanoparticles was about 3 nm, and the size of surface Pd nanoparticles was 10-30 nm. In addition, the SEM image showed that the hierarchically nanoporous Pd-HSiO1.5 particles were uniformly inlaid on the surface of the hierarchically nanoporous Pd-HSiO1.5/Ni-Co composite electrode. The composite electrode had high electrocatalytic activity and showed high electrochemical sensitivity in the detection of the oxytetracycline and deoxytetracycline in alkaline medium. The obtained detection limits were 1.0 x 10(-8) M and 5.0 x 10(-8) M for oxytetracycline and deoxytetracycline, respectively.