Template transformations in preparation of MCM-41 silica

Summary

Template transformation in MCM-41 material during thermal treatment under different conditions was investigated on the basis of thermogravimetry (TG-DTA), X-ray diffraction (XRD) and positron annihilation lifetime spectroscopy (PALS). Micelle templated silica was prepared using C18 trimethylammonium bromide. The pore structure of MCM-41 samples obtained after removal of the surfactant in air, argon flow and vacuum was analyzed on the basis of the adsorption isotherms of nitrogen at 77 K and XRD experiments. The TG-DTA experiments confirm the mechanism of the template removal known from literature. However, the sequence of the processes during thermal treatment of as-synthesized sample and temperature of transformations depended strongly on the presence of oxygen and the heating rate. The main template degradation took place below 573 K and was independent of the kind of atmosphere above the sample. Residual carbonaceous species are removed from pores and the external surface of MCM-41 silica upon heating to 823 K by combustion or evaporation. The latter process as well as translocation of liquid-like products of template degradation from the pore interior to external surface was confirmed by PALS experiment in vacuum.