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A detailed ellipsometric porosimetry and positron annihilation spectroscopy study of porous organosilicate-glass films with various ratios of methyl terminal and ethylene bridging groups

: Rasadujjaman, M.; Wang, Y.; Zhang, L.; Naumov, S.; Attallah, A.G.; Liedke, M.O.; Koehler, N.; Redzheb, M.; Vishnevskiy, A.S.; Seregin, D.S.; Wu, Y.; Zhang, J.; Leu, J.; Wagner, A.; Vorotilov, K.A.; Schulz, S.E.; Baklanov, M.R.


Microporous and mesoporous materials 306 (2020), Art. 110434
ISSN: 1387-1811
Fraunhofer ENAS ()

Organosilicate-glass films with a varying ratio of terminal methyl and bridging ethylene groups are synthesized using 1,2-bis(trimethoxysilyl)ethane/methyltrimethoxysilane mixtures and sol-gel technology. The films are characterized by Fourier Transform Infrared spectroscopy, Ellipsometric Porosimetry and Positron Annihilation Spectroscopy. The hard bake at 400 °C generates the final pore structure, which depends on the curing environment. It is shown that ethylene bridge is destructed during the hard bake in the air via formation of peroxide radicals that form ≡SiOH during the transformation. Continuous hard bake leads to condensation of silanol groups and form a structure similar to the ordinary silica.
The pore size of highly porous materials (>30%) is larger in air cured films. Destruction of the ethylene bridge makes the films matrix soft and micropores collapse due to the capillary forces during the template evaporation. It leads to the film shrinkage, increases the size of internal voids. The air cured samples showed better mechanical properties than N2 cured ones although in the last case ethylene bridging groups were preserved. The reason is that the collapse of micropores increase the internal density and creates more favorable condition for condensation of silanol groups.