Abstract
Crystallization of aluminum-free zeolite-Beta from viscous gel and incorporation of titanium into its framework were investigated by several spectroscopic techniques. Hydrothermal synthesis was stopped at different times and the gels obtained from the autoclaves were analyzed by liquid-state 29Si NMR spectroscopy. The gels were subsequently dried and inspected by solid-state 29Si NMR, Fourier-transform infrared, and X-ray absorption spectroscopy. NMR spectroscopy distinguished signals from oligomers and from two populations of nanoparticles with different typical dimensions. It also provided information about the composition of the oligomers and nanoparticles, in terms of the relative fractions of Qn units within them. Investigation showed that the synthesis of zeolite Ti-Beta started with a quick formation of oligomers. After 20 h of the hydrothermal treatment, oligomers with a high fraction of Q3 units gradually aggregated into primary nanoparticles with a diameter of ∼2 nm. During first 20 h, primary n...
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