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The synthesis of lanthanide-activated phosphors is pertinent to many emerging applications, ranging from high-resolution luminescence imaging to next-generation volumetric full-color display. In particular, the optical processes governed by the 4f-5d transitions of divalent and trivalent lanthanides have been the key to enabling precisely tuned color emission. The fundamental importance of lanthanide-activated phosphors for the physical and biomedical sciences has led to rapid development of novel synthetic methodologies and relevant tools that allow for probing the dynamics of energy transfer processes. Here, we review recent progress in developing methods for preparing lanthanide-activated phosphors, especially those featuring 4f-5d optical transitions. Particular attention will be devoted to two widely studied dopants, Ce³⁺ and Eu²⁺. The nature of the 4f-5d transition is examined by combining …