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Sol–gel processing of polyhedral oligomeric silsesquioxanes: nanohybrid materials incorporating T8 and T10 cages
Ist Teil von
Journal of sol-gel science and technology, 2020-09, Vol.95 (3), p.760-770
Ort / Verlag
New York: Springer US
Erscheinungsjahr
2020
Quelle
SpringerNature Journals
Beschreibungen/Notizen
Polyhedral oligomeric silsesquioxanes (POSS, T
8
and T
10
) have been incorporated in hybrid silica materials via hydrolysis-condensation of octa- and deca(triethoxysilylated)-POSS precursors, respectively. The precursors were synthesized via a thiol-ene Click reaction involving the corresponding octastyryl-T
8
or decastyryl-T
10
molecules and thiopropyltriethoxysilane. Following addition of water and HCl (as catalyst) to a solution of the precursors, gels were formed within a few minutes. The resulting hybrids were characterized by TEM, FTIR, N
2
physisorption analyses, solid-state NMR (
29
Si and
13
C), and TGA, which indicated that the T
8
and T
10
cages were incorporated and remained intact within the hybrid gel network, with no Si–C cleavage being observed via
29
Si NMR. FTIR data indicated that water retained within the gels following drying and aging at ambient temperature exhibited an unusual “connective”, ice-like structure, suggesting that it is initially retained as a key component of the gel network during consolidation and aging at ambient temperature. Following aging, the water was readily removed by evacuation at 100 °C without significantly modifying the network structure, on the basis of the FTIR spectrum of the gel. To the best of our knowledge, this is the first report of the incorporation of T
10
cages in such gels.
Highlights
New precursors developed, incorporating POSS cages covalently bound to hydrolysable –Si(OEt)
3
groups.
Intact T
8
and T
10
POSS covalently incorporated in hybrid silica materials with no Si–C cleavage.
First report of materials incorporating intact T
10
POSS cages.