Self‐Assembly and Characterization of Mesostructured Silica Films with a 3D Arrangement of Isolated Spherical Mesopores
Self‐Assembly and Characterization of Mesostructured Silica Films with a 3D Arrangement of Isolated Spherical Mesopores
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DOI：
10.1002/adfm.200390005
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发表时间：
2003-01
影响因子：
19
通讯作者：
Kui Yu;B. Smarsly;C. Brinker
中科院分区：
文献类型：
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作者：
Kui Yu;B. Smarsly;C. Brinker
我们报道了具有孤立球形孔的3D有序排列的介孔二氧化硅薄膜的自组装和表征。制备方法基于溶剂蒸发诱导自组装（EISA），以MTES（CH 3-Si（OCH 2CH 3）3）为二氧化硅前体，聚苯乙烯-嵌段-聚（环氧乙烷）（PS-B-PEO）二嵌段共聚物为结构导向剂。该合成方法旨在抑制硅氧烷网络的硅氧烷缩合速率，允许二氧化硅和两亲物的共自组装，随后PEO链从二氧化硅基质中缩回并进行基质固结，以不受阻碍地发生。煅烧后的膜保留了甲基配体，并且没有表现出可测量的微孔性，从而表明3D有序的球形中孔没有互连。溶剂介导的形成机制，提出了微孔的情况下。由于其封闭的孔隙率和疏水性，我们描述的MTES-基薄膜和MTES-TEOS（Si（OCH 2CH 3）4）-基杂化薄膜应该有希望用于低k值等应用。
We report the self‐assembly and characterization of mesoporous silica thin films with a 3D ordered arrangement of isolated spherical pores. The preparation method was based on solvent‐evaporation induced self‐assembly (EISA), with MTES (CH3–Si(OCH2CH3)3) as the silica precursor and a polystyrene‐block‐poly(ethylene oxide) (PS‐b‐PEO) diblock copolymer as the structure‐directing agent. The synthetic approach was designed to suppress the siloxane condensation rate of the siloxane network, allowing co‐self‐assembly of the silica and the amphiphile, followed by retraction of the PEO chains from the silica matrix and matrix consolidation, to occur unimpeded. The calcined films retained the methyl ligands and exhibited no measurable microporosity, thereby indicating that the 3D‐ordered spherical mesopores are not interconnected. A solvent‐mediated formation mechanism is proposed for the absence of microporosity. Due to their closed porosity and hydrophobicity, the MTES‐based films and MTES‐TEOS (Si(OCH2CH3)4)‐based hybrid films we describe should be promising for applications such as low‐k dielectrics.