Institut de Science des Matériaux de Mulhouse, IS2M, UMR CNRS 7361, Université de Haute-Alsace , 15 rue Jean Starcky, BP 2488, 68057 Mulhouse Cedex, France.
Langmuir. 2014 Jan 14;30(1):297-307. doi: 10.1021/la402762v. Epub 2014 Jan 2.
An ordered microporous carbon material was prepared by the nanocasting process using the EMC-2 zeolite (EMT structure type) as a hard template. X-ray diffraction (XRD) and transmission electron microscopy (TEM) revealed long-range ordering in the material that resulted from the negative replication of the host template. The carbon porous network replicating the zeolite structure was modeled by overlapped spherical voids with diameters determined from the XRD pattern that displayed up to six distinct peaks. The surface delimiting the 3D interconnected porosity of the solid has a complex morphology. The pore size distribution calculated from the XRD-derived structural model is characterized by a maximum at 1.04 nm related to the long-range-ordered microporous network. Complementary studies by immersion calorimetry revealed that most of the porosity was characterized by a size above 1.5 nm. These porous features were compared to data resulting from classical analysis (DR, DFT, BET, etc.) of the N2 (77 K) and CO2 (low and high pressure, 273 K) physisorption isotherms. The limitations of these approaches are discussed in light of the pore size distribution consistently determined by XRD and immersion calorimetry measurements.
采用纳米铸型法，以 EMC-2 沸石（EMT 结构类型）为硬模板，制备了有序的微孔碳材料。X 射线衍射（XRD）和透射电子显微镜（TEM）表明，该材料具有长程有序性，这是由于主体模板的负复制所致。通过重叠的具有从显示多达六个不同峰的 XRD 图案确定的直径的球形空隙，对复制沸石结构的碳多孔网络进行建模。限定固体 3D 相互连通的孔隙率的表面具有复杂的形态。从 XRD 衍生的结构模型计算得到的孔径分布在 1.04nm 处具有最大值，这与长程有序的微孔网络有关。通过浸渍量热法进行的补充研究表明，大部分孔隙率的特征尺寸大于 1.5nm。将这些多孔特征与 N2（77K）和 CO2（低压和高压，273K）物理吸附等温线的经典分析（DR、DFT、BET 等）的数据进行了比较。根据 XRD 和浸渍量热法测量一致确定的孔径分布，讨论了这些方法的局限性。
