This work describes a controlled and low-cost synthesis method to obtain Pb/Pb3O4 nanocomposites using synthetic zeolite 4A. The nanostructures obtained have a core-shell configuration with 5-25 nm diameters. High-resolution transmission electron microscopy (HRTEM), BF, high-angle annular dark-field annular scanning transmission electron microscopy (HAADF-STEM), energy-dispersive X-ray spectroscopy (EDS), X-ray photoelectron spectroscopy (XPS), and ultraviolet-visible (UV-vis) characterization techniques were used. Crystallographic planes (111), (200), and (220) for the core and planes (110) and (211) for the shell, corresponding to FCC and tetragonal structures for Pb and Pb3O4, respectively, were determined using HRTEM. The HAADF-STEM images allowed the analysis of intensity contrast images proportional to the number of atoms. XPS spectral analysis showed a 4.8 eV difference in binding energy between Pb 4f7/2 and Pb 4f5/2 for lead and lead oxide. EDS elemental mapping, XPS, and UV-vis spectroscopy analyses revealed the simultaneous presence of lead and lead oxide in the same structure. The band gap obtained for the shell was determined to be 4.50 eV. Consequently, Pb/Pb3O4 nanocomposites show a higher response to high-energy photons, making them suitable for UV photocatalysis applications.
© 2024 The Authors. Published by American Chemical Society.