Luminescence spectroscopic techniques are a set of powerful analytical techniques that study the optical properties of materials. These techniques depend on the interaction between absorbed energy and subsequent photon emission. It provides valuable information about the electronic and optical properties of substances. Luminescence spectroscopy has evolved as a crucial and indispensable tool for fundamental research in chemistry, physics, materials science, biology and environmental sciences. In this chapter, various luminescence spectroscopic techniques, including photoluminescence, electroluminescence, cathodoluminescence, chemiluminescence and thermoluminescence spectroscopy, are discussed. Each technique offers distinct insights into the luminescent properties of materials under different excitation sources. These techniques, along with others such as Raman spectroscopy, UV–visible spectroscopy and Fourier transform infrared spectroscopy, collectively contribute to the comprehensive characterisation of luminescent materials. These luminescence spectroscopic techniques offer essential tools for researchers in various scientific fields and contribute to the development of advanced materials and innovative technologies.