Polyhedral oligomeric silsesquioxanes (POSS, T₈ and T₁₀) 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-T₈ or decastyryl-T₁₀ 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, N₂ physisorption analyses, solid-state NMR (²⁹Si and ¹³C), and TGA, which indicated that the T₈ and T₁₀ cages were incorporated and remained intact within the hybrid gel network, with no Si–C cleavage being observed via ²⁹Si 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 T₁₀ cages in such gels.

多面体低聚倍半硅氧烷（POSS，T ₈和T ₁₀）已分别通过八-和十（三乙氧基甲硅烷基化）-POSS前体的水解缩合而掺入杂化二氧化硅材料中。前体是通过硫醇-烯点击反应合成的，该反应涉及相应的辛基-T ₈或去甲酰基-T ₁₀分子和硫丙基三乙氧基硅烷。向前体溶液中加入水和HCl（作为催化剂）后，在几分钟内形成凝胶。所得杂种通过TEM，FTIR，N ₂物理吸附分析，固态NMR（²⁹ Si和¹³ C）和TGA表征，表明T ₈并结合了T ₁₀笼，并在混合凝胶网络中保持完整，通过²⁹ Si NMR未观察到Si-C裂解。FTIR数据表明，在环境温度下干燥和老化后，保留在凝胶中的水表现出不同寻常的“结缔”，冰状结构，表明在环境温度下固结和老化期间，水最初保留为凝胶网络的关键成分。老化后，根据凝胶的FTIR光谱，很容易通过在100°C抽真空除去水，而不会显着改变网络结构。据我们所知，这是在这种凝胶中掺入T ₁₀笼的首次报道。