The fluorination processes of layered rare-earth hydroxides (LRHs) intercalated with various anions, including organic ones, have been compared for the first time. The fluorination process was investigated for chloride-, nitrate-and 4-sulfobenzoate-intercalated Eu-doped layered yttrium hydroxides by interaction with aqueous solutions of sodium fluoride at 100-150 • C for 2-48 hours. The final product of fluorination in all cases is the hexagonal yttrium hydroxide fluoride (YHF) phase of Na y Y 0.95 Eu 0.05 (OH) 3+y−x F x • mH 2 O (x ∼ 3, y ∼ 0.2) composition. The formation rate of the YHF increases with the interlayer spacing of the Eu-doped layered yttrium hydroxide. KEYWORDS layered rare-earth hydroxides (LRHs), fluorination, luminescence, ion exchange, topotactic reactions, metal hydroxyfluorides.