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According to the wide application of muscovite in various industries, many studies have focused on its fabrication. However, the process of its synthesis faces long-standing challenges mainly related to the elevated temperature and pressure ambient, together with time and cost-consuming processes. This research work aims at synthesizing muscovite through a straightforward and direct wet thermal oxidation of an ash sample produced from biotite-rich coal tailings. For this purpose, the lab ash powder was mixed with 35% H2O2 at the room temperature of 25 °C while stirring at 480 rpm. Then, the temperature was gradually raised to 80 °C, and the process ran for 180 min. The dried product and the raw lab ash were characterized by the X-ray diffraction (XRD), scanning electron microscopy (SEM) and Fourier-transform infrared spectroscopy (FTIR) methods. The XRD results indicated that the biotite was efficiently converted to the muscovite as the number of relevant peaks was significantly increased in the synthesized product’s pattern. The SEM and FTIR results showed some structural changes, from pseudo-hexagonal in the starting material to amorphous pseudo-crystals in the synthetic product, as well as the growth of the product’s crystals. The crystallographic study and lattice parameter calculations revealed that the starting material and product peaks matched to International Center for Diffraction Data (ICDD reference patterns of 01-080-1110 and 01-082-2450 for the biotite and the muscovite, respectively. Moreover, the calculation of the mean crystallite size of the starting material and treated samples were obtained as 55 nm and 87 nm, respectively. Finally, according to the characterization properties of synthesized muscovite, the presented method was introduced as an effective technique. Therefore, we highly suggest it for further consideration and its development in future investigations.

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