Pb/Pb₃O₄ Metal-Semiconductor Nanocomposite Obtained on 4A Zeolite─Optical and Structural Properties

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 4f_7/2 and Pb 4f_5/2 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.