Structural Solution of Porous Materials on the Mesostructural Scale by Electron Microscopy

doi:10.6023/A22030136

Acta Chimica Sinica ›› 2022, Vol. 80 ›› Issue (8): 1203-1216.DOI: 10.6023/A22030136 Previous Articles

Review

介观尺度多孔材料的电子显微学结构解析

邓权政^a, 毛文婷^b, 韩璐^a^,^*()

a 同济大学化学科学与工程学院上海 200092
b 上海交通大学化学化工学院金属基复合材料国家重点实验室上海 200240

投稿日期:2022-03-29 发布日期:2022-09-01
通讯作者: 韩璐

作者简介:

邓权政, 同济大学化学科学与工程学院2019级在读博士生, 本科毕业于同济大学, 现主要从事孔材料的电子显微学结构解析研究.

毛文婷, 2015年获得东华大学理学学士学位, 2021年获得上海交通大学(导师韩璐教授)理学博士学位.

韩璐, 同济大学化学科学与工程学院教授, 博士生导师. 2006年获上海交通大学理学学士学位, 2010年及2011年分别获得斯德哥尔摩大学及上海交通大学博士学位, 2011年入职上海交通大学, 2017年加入同济大学. 获2013年度全国优秀博士学位论文奖, 2014年度教育部自然科学奖一等奖(第二完成人), 2019年受自然科学基金优秀青年基金资助. 主要研究方向为介观结构材料的合成及电子显微学结构研究.

基金资助:
国家自然科学基金(21922304); 国家自然科学基金(21873072); 上海自然科学基金(18ZR1442400)

Structural Solution of Porous Materials on the Mesostructural Scale by Electron Microscopy

Quanzheng Deng^a, Wenting Mao^b, Lu Han^a()

a School of Chemical Science and Engineering, Tongji University, Shanghai 200092, China
b School of Chemistry and Chemical Engineering, State Key Laboratory of Metal Matrix Composites, Shanghai Jiao Tong University, Shanghai 200240, China

Received:2022-03-29 Published:2022-09-01
Contact: Lu Han
Supported by:
National Natural Science Foundation of China(21922304); National Natural Science Foundation of China(21873072); Natural Science Foundation of Shanghai(18ZR1442400)

Ordered porous materials on the meso-structural scale have attracted great attention due to their ordered porous structure, large surface area and unique spatial confinement effect, which may find widespread applications in adsorption, separation, catalysis, sensing, drug delivery, energy storage, etc. The in-depth analysis of the structural characteristics of these porous materials is not only essential for understanding their properties and performances, but also the key for the future materials synthesis and their formation mechanism. The structural solution of porous materials on the meso-structural scale by using electron microscopy for last decades was outlined, which shows great advantages in the structural solution of the porous solids through diffractometry and imaging. Several representative examples including ordered mesoporous materials and macro-porous scaffolds, have been solved by appropriate methods. Then, the electron microscopy methods applicable to different types of porous materials were summarized. Finally, the advantages, limitations and future development of electron microscopy towards new porous materials, as well as the feasibility of using this technique for other materials were concluded.

Key words: mesoporous material, macro-porous material, electron microscopy, 3D reconstruction, crystal defect

Cite this article

Quanzheng Deng, Wenting Mao, Lu Han. Structural Solution of Porous Materials on the Mesostructural Scale by Electron Microscopy[J]. Acta Chimica Sinica, 2022, 80(8): 1203-1216.

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Fig. & Tab. 26

Figure 1. Structure determination of porous materials on the meso- structural scale by electron crystallography

Figure 2. HRTEM image of MCM-41 with different pore size. (a) 2 nm, (b) 4 nm, (c) 6.5 nm, (d) 10 nm. The schematic drawing of two- dimensional hexagonal structure is overlaid on the HRTEM image. (e) Powder X-ray diffraction pattern of calcinated MCM-41. Adapted with permission[4]

Figure 3. HRSEM images of (a) MCM-41, (b) KIT-6 and (c, d) SBA-15. Adapted with permission[18-19]

Figure 4. (a) HRTEM image and (b) Fourier diffractogram of the 2D-p2gg structure. The pore shape of (c) 2D-p6mm and (d) p2gg. Adapted with permission[20]

Figure 5. (a~c) Illustration of two layers stacking. (d~h) TEM images (up), SAED images and scheme of stacking at different angle. Adapted with permission[23]

Figure 6. (a~c) TEM images with different magnification, showing two typical lattice fringes (indicated by arrows and arrowheads) with different spacings. (d) Simulated TEM image. (e, f) Schematic diagrams of the electron beam incident along perpendicular direction and titled by 15°. (g, h) Simulated TEM image along perpendicular direction. (i, j) Simulated TEM image by an angle θ=15°. Adapted with permission[7-8]

Figure 7. HRTEM images of SBA-12 viewed along (a) [100] and (b) [110]; (c) PXRD of SBA-12. (d) Cubic close-packed cage structure model. Adapted with permission[27]

Figure 8. HRTEM images of SBA-16 viewed along (a) [100], (b)?[110], (c) [111]. (d) Electrostatic potential map of SBA-16. (e, f) 3D structure of SBA-16. Adapted with permission[24]

Figure 9. HRTEM images of SBA-8 viewed along (a) [100], (b) [110], (c) [111], and (d) [210] respectively. (e) The structure model of SBA-6. Adapted with permission[26]

Figure 10. (a) HRTEM image taken from the $[\overline{1}10]$ direction of AMS-8 type material; (b~e) the structural description employing polyhedral packing model. Adapted with permission[31]

Figure 11. (a~d) HRTEM images of the planar defect in the AMS-8 type structure and (e, f) its structural model. Adapted with permission[32]

Figure 12. HRTEM images of the intergrowth of the $Fm\overline{3}m$ (top and bottom) and $Fd\overline{3}m$ (middle) structures. Each domain is taken along (a) ${{[\overline{1}\overline{1}0]}_{Fm\overline{3}m}}$ and ${{[\overline{2}\overline{1}1]}_{Fd\overline{3}m}}$ (b) ${{[\overline{2}\overline{1}1]}_{Fm\overline{3}m}}$ and ${{[\overline{1}01]}_{Fd\overline{3}m}}$directions. Adapted with permission[35]

Figure 13. (a) SEM image, (b) the crystal planes shown in (a), and (c) TEM image of the samples. (d, e) SEM images of the SBA-1. Adapted with permission[36-37]

Figure 14. (a) SEM image of the calcined HSMCs. (b~d) Cross-sectional images of HSMCs. Adapted with permission[38]

Figure 15. (a, b) SEM and (c) HRTEM images of the sample with dodecagonal quasi-crystalline meso-structure. (d~g) frequently observed defects. (h) HRTEM image taken from the central part of the sliced sample. Adapted with permission[13]

Figure 16. HRTEM images of (a~c) MCM-48, (e~g) AMS-10 taken from main zone with corresponding Fourier diffractograms (FDs). (d) MCM-48, (h) AMS-10 3D-view along the [111]. Adapted with permission[41]

Figure 17. (a) MCM-48, and (b) AMS-10. Comparison of the experimental and simulated HRTEM images of (c) calcinated MCM-48 (cT=78.3?%) along [111] and (d) AMS-10 (cT=75.3?%) along [100] direction. Adapted with permission[42]

Figure 18. 3D reconstruction and actual g value distribution of the (a) D and (b) G structure. Adapted with permission[43]

Figure 19. (a~c) HRTEM images and the corresponding Fourier diffractograms of IBN-9 taken along the [001], [100] and [110] direction, respectively. (d) PXRD of IBN-9. (e) The 3D pore structure of IBN-9. (f) One single-channel system along the c axis. (g) The tri-continuous mesoporous channel system. (h) The rod model. Adapted with permission[16]

Figure 20. (a) SEM image of the scale. (b) High-magnification image of the scale. (c) Single gyroid crystallites viewed at an inclination of ca. 50°. (d) X-ray tomography cross section showing faceted gyroids. (e) High-resolution X-ray tomography of single crystallites. Adapted with permission[48]

Figure 21. (a, b) SEM images of slices at different height. (c) Structure reconstructed by successive FIB milling and SEM observations. (d) Theoretical model for (c) based on the I-WP-type photonic crystal. (e, f) The single unit cell for reconstruction structure and theoretical structure, respectively. Adapted with permission[49]

Figure 22. (a) Photographs of intense opalescence of phenolic inverse opal and its (b) SEM image taken from the fractured (111) facet; (c, d) SEM images of a (111) facet of a glassy carbon inverse opal. Adapted with permission[50]

Figure 23. (a, b) The typical SEM images of SDD structure. (c~f) TEM images of SDD recorded from (c) [010], (d) [001], (e) [101], (f) [111] directions, respectively. (g) 3D structure reconstructed from the HRTEM images. (h, i) 3D porous system with the stick model superimposed in the hollow channels. Adapted with permission[53]

Figure 24. (a~c) SEM images of SG viewed along different orientations; TEM images of SG structure recorded from (d) [100], (e) [110], (f) [111] directions, respectively. (g, h) 3D structure reconstructed from the TEM images. Adapted with permission[55]

Figure 25. (a~c) SEM images of SD viewed along different orientations; TEM images of SD recorded from (d) [110], (e) [112], (f) [111] and (g) [100] directions, respectively. (h, i) 3D structure reconstructed from the TEM images. Adapted with permission[56]

Figure 26. (a1-5, b1-5, c1-5) projections and (a6, b6, c6) side-view of the 3D electrostatic potential maps reconstructed with CSFs extracted from (a1-6) the HAADF-STEM images. (b1-6) under focused TEM images, and (c1-6) in focused TEM images. Skeletal models and the symmetry-averaged images are overlapped on corresponding projections. Adapted with permission[57]

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介观尺度多孔材料的电子显微学结构解析

Structural Solution of Porous Materials on the Mesostructural Scale by Electron Microscopy

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