Petkov N, Hölzl M, Metzger T H, Mintova S, Bein T
Department of Chemistry, LMU, Butenandtstr. 11, 81377 Munich, Germany.
J Phys Chem B. 2005 Mar 17;109(10):4485-91. doi: 10.1021/jp0444969.
A new synthesis method for preparation of thin films and powders consisting of zeolite beta nanocrystals embedded in ordered mesoporous silica matrix is described. The final structures possessing bimodal porosity, i.e., high degree of mesophase order and spatially defined microporous zeolite nanocrystals are obtained via simultaneous solvent evaporation of preformed silica/surfactant/ethanol/nanosized zeolite beta assemblies. The films were characterized with grazing-incident diffraction (GID), nitrogen sorption based on gravimetric measurements with quartz crystal microbalance (QCM) devices, and transmission electron microscopy (TEM). It is shown that the incorporation of beta nanocrystals in the mesoporous silica matrix and the mesophase order itself can be controlled through the variation of the fractional amounts of the zeolite nanoparticles and silica/surfactant solutions. The HR-TEM measurements showed that the nanosized Beta microporous crystals are separated and at the same time connected through an ordered mesostructured matrix.
描述了一种制备由嵌入有序介孔二氧化硅基质中的β-沸石纳米晶体组成的薄膜和粉末的新合成方法。通过同时蒸发预先形成的二氧化硅/表面活性剂/乙醇/纳米尺寸β-沸石聚集体的溶剂,获得具有双峰孔隙率的最终结构,即高度的中间相有序和空间定义的微孔沸石纳米晶体。用掠入射衍射(GID)、基于石英晶体微天平(QCM)装置重量测量的氮吸附以及透射电子显微镜(TEM)对薄膜进行了表征。结果表明,通过改变沸石纳米颗粒与二氧化硅/表面活性剂溶液的分数含量,可以控制β-纳米晶体在介孔二氧化硅基质中的掺入以及中间相本身的有序性。高分辨率透射电子显微镜(HR-TEM)测量表明,纳米尺寸的β-微孔晶体是分离的,同时通过有序的介观结构基质连接。