This document discusses the sol-gel synthesis and characterization of Titania-Zirconia matrices doped with rare earth ions and CdS. Chapter 1 provides a general introduction to sol-gel processing and its advantages. Chapter 2 discusses the spectroscopy of Tb3+ and Eu3+ ions in the Titania-Zirconia matrix. Chapter 3 details the structural and optical characterization of CdS/Tb3+/Eu3+ doped Titania-Zirconia matrices prepared via sol-gel processing. Various characterization techniques were used to analyze the materials' structure, composition, and optical properties.