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A series of Zn-Doped Magnesium Hydroxyfluoride, Mg1-xZnxFOH) samples with Oto 0.15 of x were prepared using a sol-gel synthesis and dried with vacuum technique. XRD characterization of the samples indicated the amorphous phase of Mgl-xZnxFOH similarity with MgF2. The Zn doped in magnesium hydroxyfluoride did not affected on the basic structure of magnesium hydroxyfluoride. The FUR spectra showed the samples had a broad band at 3000-3700 cm-1 and 1620 cm-1 was indicated of adsorbed H20 molecules and a bridging hydroxyl groups, respectively. The intensity of the 460, and 550 cm-1 bands correlates to Mg-F and Mg-O vibrations. The Zn-O stretching vibration of Zn-doped magnesium hydroxyfluoride appeared at 1634 and 621 cm-1. [ABSTRACT FROM AUTHOR]