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Fluoride phase separation is the initial stage of nanocrystallization in oxyfluoride glasses, and it is a key step in achieving transparent glass‐ceramics with good luminescence. In this work, we combine molecular dynamics (MD) simulations and experimental studies to investigate the phase separation, nanocrystallization and photoluminescence in fluoroaluminosilicate glass and glass‐ceramics containing alkali earth fluoride (MF₂). The results reveal different phase separation behaviors due to the field strength difference of M²⁺. The composition and size similarity between the fluoride‐rich regions in the MD simulated glass and the fluoride nanocrystals in the experimental prepared glass‐ceramics are observed, suggesting that the separated fluoride phase is the structural origin of the observed MF₂nanocrystals. Besides, in order to understand the M²⁺dependent glass structural features, the crystallization temperatures, the luminescent properties of Eu³⁺and Eu²⁺doped glass‐ceramics, and the lasing performance of Er³⁺doped glass‐ceramics are discussed. Based on these comprehensions, some strategies are proposed to help to efficiently design oxyfluoride glass with desired luminescence performance.