Luminescent materials emit light without heating in response to a stimulus such as exposure to light, temperature, or the introduction of an electrical current. For example, photoluminescent materials respond to light exposure. These materials absorb UV radiation and emit visible light. Luminescent materials are widely used in optoelectronic devices, solar cells, bioimaging, targeted drug delivery, and therapeutic applications. The emission efficiency varies greatly depending on the synthesis process used for the preparation of the materials. There are various methods, such as the solid-state reaction method, hydrothermal method, sol–gel method, facile molten salt synthesis method, combustion method, co-precipitation method, etc., that are followed for the synthesis of different luminescent materials. The synthesis methods can be dry synthesis techniques and solution-based synthesis. The samples prepared using dry synthesis techniques fail to reach the precise homogeneity needed for application-optimized materials due to the mechanical mixing of the starting components. Nevertheless, only solution-based synthesis methods can meet the required standards of ideal particle size and morphology. The advantages of the solution combustion synthesis (SCS) method are that it requires less time for preparation of samples, including cost effectiveness, whereas the sol–gel combustion method is the most promising method due to its advantages like particle homogeneity, fine distribution of particle size, etc. The co-precipitation method is a simple and conventional technique for synthesizing luminescent nanomaterials. One of the key benefits of this method is that it may immediately create water-soluble nanoparticles. Hydrothermal synthesis is one of the widely used methods for the synthesis of nanomaterials. In this chapter, different synthesis techniques used for the preparation of luminescent materials are discussed.