Citation: YUAN En-Hui, XING Jun-Ling, PANG Jun-Ling, JIANG Shu-Hua, JIANG Jin-Gang, ZHANG Kun. Formation Mechanism of Highly Ordered MCM-48 via Phase Transformation[J]. Chinese Journal of Inorganic Chemistry, ;2015, (12): 2358-2364. doi: 10.11862/CJIC.2015.310
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Highly ordered mesoporous molecular sieve MCM-48 with Ia3d cubic structure was hydrothermally synthesized using new surfactant cetyltrimethylammonium tosylate (CTATos) as template via phase transformation (PT). Structural study by small angle X-ray diffraction (XRD), scanning electron microscopy (SEM), high-resolution transmission electron microscopy (HR-TEM) and nitrogen adsorption-desorption shows the time-dependent structural change in M41S mesoporous silica from MCM-41 to MCM-48 and MCM-50. The driving force for this transformation seems to be an increase of the local effective surfactant packing parameter (g), which resulted from the leaching of surfactant counter anions (Tos-) in the pore with the prolongation of the reaction time. One-dimensional solid state 29Si NMR spectra, X-ray diffraction patterns, and infrared spectra show the progression of molecular organization in the self-assembled mesophases from structures with initially amorphous silica networks into sheets with very high degrees of atomic order when the phase transformation is happening. The finally obtained self-assembled lamellar silica-surfactant mesophase composites with crystal-like ordering in the silica frameworks can be an ideal precursor to fabricate the three-dimensional microporous zeolites with the expanded pore size.
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