Synthesis of highly ordered, three-dimensional, macroporous structures of amorphous or crystalline inorganic oxides, phosphates, and hybrid composites
Synthesis of highly ordered, three-dimensional, macroporous structures of amorphous or crystalline inorganic oxides, phosphates, and hybrid composites
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DOI：
10.1021/cm980666g
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发表时间：
1999-03-01
影响因子：
8.6
通讯作者：
Stein, A
中科院分区：
文献类型：
--
作者：
Holland, BT;Blanford, CF;Stein, A
高度有序的大孔材料的合成已经在简单的一步反应中完成。由Si、Ti、Zr、Al、W、Fe、Sb和Zr/Y混合物的氧化物组成的无机框架由金属醇盐前体围绕聚苯乙烯（胶乳）球模板形成。通过离心将单分散乳胶球排列成紧密堆积的阵列。醇盐渗透到乳胶球之间的空隙中，水解缩合。干燥后形成无机框架。通过在450和1000 ℃之间的温度下煅烧或用四氢呋喃/丙酮混合物萃取来实现胶乳球的去除。所得产物由延伸超过数百微米的单分散亚微米孔的周期性互连网络组成。根据模板去除的技术，可以形成无机氧化物的各种相。例如，在二氧化钛的情况下，在TiO 2的萃取和通过在450 ℃下煅烧的结晶时形成无定形相。该合成也已扩展到其他组合物，包括铝磷酸盐和混合有机硅酸盐，以及具有中孔和大孔的双峰分布的硅酸盐。本文中提出的材料显示了这种技术可实现的大孔材料的多样性。这些结构可以潜在地用作色谱支持材料、固体催化剂、电池材料、热绝缘体或光子晶体。
The synthesis of highly ordered macroporous materials has been accomplished in a straightforward, single-step reaction. Inorganic frameworks composed of oxides of Si, Ti, Zr, Al, W, Fe, Sb, and a Zr/Y mixture were formed from metal alkoxide precursors templated around polystyrene (latex) spheres. Monodisperse latex spheres were ordered into close-packed arrays by centrifugation. The interstices between latex spheres were permeated by the alkoxide, which hydrolyzed and condensed. An inorganic framework was formed upon drying. Removal of the latex spheres was accomplished by either calcination at temperatures between 450 and 1000 degrees C or extraction with a tetrahydrofuran/acetone mixture. The resulting products consisted of periodic, interconnected networks of monodisperse submicron pores extending over hundreds of micrometers. Depending on the technique of template removal, various phases of the inorganic oxide could be formed. For example, in the case of titania, an amorphous phase was formed upon extraction of TiO2 and anatase by calcination at 450 degrees C. The synthesis has also been expanded to other compositions including aluminophosphates and hybrid organosilicates, as well as silicates with bimodal distributions of meso- and macropores. The materials presented in this paper show the diversity of macroporous materials achievable with this technique. These structures could potentially find applications as chromatographic support materials, solid catalysts, battery materials, thermal insulators, or photonic crystals.