介观尺度多孔材料的电子显微学结构解析

doi:10.6023/A22030136

化学学报 ›› 2022, Vol. 80 ›› Issue (8): 1203-1216.DOI: 10.6023/A22030136 上一篇

综述

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)

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摘要/Abstract

孔径在介观尺度的多孔材料由于其规整的孔道结构、大比表面积、特殊的空间限域效应使其在吸附、分离、催化、传感、载药、能源等领域都具有广阔的应用前景. 深入解析材料的结构特征不仅是理解其物理化学性能和应用的关键, 也是研究材料的形成机理及新材料制备的重要反馈和支持. 电子显微学以电子为探针, 通过电子衍射和高分辨像对材料结构展开探索, 可以研究更小尺寸晶体的结构, 揭示局部结构信息如缺陷及共生等, 对介观尺度多孔材料的结构解析至关重要. 对近年来通过电子显微学方法解析的介观尺度多孔材料工作进行了综述, 主要针对有序介孔材料以及有序大孔材料展开, 归纳了不同结构类型的介观尺度多孔材料所适用的电子晶体学方法, 在此基础上提出电子显微学在介观尺度孔材料结构解析上的优势、不足和未来发展的方向, 以及将电子显微学用于其它材料结构解析的可行性.

关键词: 介孔材料, 大孔材料, 电子显微学, 三维重构, 晶体缺陷

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

引用此文

邓权政, 毛文婷, 韩璐. 介观尺度多孔材料的电子显微学结构解析[J]. 化学学报, 2022, 80(8): 1203-1216.

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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图/表 26

图1. 电子显微学用于介观尺度孔材料结构解析

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

图2. 具有不同孔径MCM-41的HRTEM图像. 孔径分别为: (a) 2 nm, (b) 4 nm, (c) 6.5 nm, (d) 10 nm; 右下角插图为二维六方的结构模型. (e) 锻烧后MCM-41的XRD图谱

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]

图3. (a) MCM-41的HRSEM图像. (b) KIT-6的HRSEM图像. (c, d) SBA-15的HRSEM图像

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

图4. 二维p2gg结构的(a) HRTEM图像及(b)傅立叶变换图谱. (c) p6mm与(d) p2gg的结构对比

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]

图5. (a~c)双层堆叠的示意图. (d~h)以不同角度堆叠样品的TEM图像, SAED和示意图

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]

图6. (a~c) 手性介孔材料不同放大率的TEM图像, 显示了同时存在10与11两种晶格条纹. (d) TEM图像模拟. (e, f) 电子垂直入射和倾斜15°示意图. (g, h) 电子束垂直入射的TEM模拟图. (i, j) 材料倾斜15°的TEM模拟图

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]

图7. 沿(a) [100]和(b) [110]方向SBA-12的HRTEM图像. 插图为对应的SAED图像. (c) XRD图谱. (d)立方密堆积笼结构模型

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]

图8. SBA-16沿(a) [100]、(b) [110]、(c) [111]方向的HRTEM. (d) SBA-16的静电势图. (e, f) SBA-16三维孔道结构

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]

图9. SBA-6分别沿(a) [100]; (b) [110]; (c) [111]和(d) [210]晶向的HRTEM图像. (e) SBA-6的结构模型

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]

图10. (a) AMS-8材料沿 $[\overline{1}10]$方向拍摄的HRTEM图像. (b~e)通过多面体堆积模型对其结构进行构筑

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]

图11. (a~d) AMS-8型结构中具有单斜对称性的面缺陷的HRTEM图像和(e, f)结构示意图

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]

图12. (a)沿 ${{[\overline{1}\overline{1}0]}_{Fm\overline{3}m}}$和 ${{[\overline{2}\overline{1}1]}_{Fd\overline{3}m}}$方向, (b)沿 ${{[\overline{2}\overline{1}1]}_{Fm\overline{3}m}}$和 ${{[\overline{1}01]}_{Fd\overline{3}m}}$方向拍摄的 $Fm\overline{3}m$(顶部和底部)和 $Fd\overline{3}m$(中间)结构的共生的HRTEM图像

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]

图13. (a)样品的SEM图像, (b) (a)中所示晶面, (c)样品的TEM图像. (d, e) SBA-1的SEM图像

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]

图14. (a)二氧化硅介孔晶体的SEM图像. (b~d)二氧化硅介孔晶体横截面的SEM图像

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

图15. 具有准晶介孔结构样品的(a, b) SEM及(c) HRTEM图像; (d~g) 观察到的缺陷; (h) 超薄切片样品中心区域HRTEM图像

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]

图16. (a~c) MCM-48, (e~g) AMS-10沿主带轴的HRTEM图像及相应的傅立叶衍射图. (d) MCM-48, (h) AMS-10沿[111]的3D视图

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]

图17. (a) MCM-48和(b) AMS-10. (c) 煅烧后的MCM-48 (cT=78.3%)沿[111]的HRTEM及(d) AMS-10 (cT=75.3%)沿[100]的HRTEM图像, 均与模拟HRTEM图像高度一致

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]

图18. (a) D和(b) G结构的3D 重建和实际g值分布

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

图19. (a~c) 分别沿[001], [100], [110]方向拍摄的IBN-9的HRTEM图像, 插图为对应的傅立叶衍射图像; (d) IBN-9的PXRD图谱. (e) IBN-9的重建孔结构. (f)沿c轴观察的单孔道. (g)三维连续孔道. (h)棍棒模型

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]

图20. (a)鳞片的SEM. (b)高放大倍率图像. (c)以约50°的倾斜角度观察的单个G骨架微晶. (d) X射线断层摄影术的横截面. (e)单晶的高分辨率X射线断层扫描

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]

图21. (a, b) 甲虫翅膀表面不同高度切片的SEM图像. (c) 通过连续FIB-SEM技术重建的3D结构. (d) 基于I-WP型光子晶体的理论模型. (e, f) 分别为重建结构和理论结构的单个晶胞

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]

图22. (a) 酚醛反蛋白石强烈反光的图像及 (b) (111)断裂表面的SEM图像; (c, d) 玻璃状碳反蛋白石的(111)断裂表面的SEM图像

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]

图23. (a, b) SDD结构典型的SEM图像; (c~f) 分别沿[010]、[001]、[101]和[111]方向拍摄的TEM图像; (g) 从HRTEM图像中重构出的SDD的3D结构; (h, i) SDD结构的三维孔道系统模型

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]

图24. (a~c) 沿不同方向观察的SG的SEM图像. (d~f) 分别沿[100], [110], [111]方向拍摄的TEM图像. (g, h) 从TEM图像中重构出的SG的3D结构

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]

图25. (a~c) 沿不同方向观察的SD的SEM; (d~g) 分别沿[110]、[112]、[111]、[100]方向拍摄的SD的TEM图像. (h, i)从HRTEM图像中重构出的SD的3D结构

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]

图26. 从HAADF-STEM (a1-5), 欠焦TEM (b1-5), 正焦TEM (c1-5)图像重构的SDD结构投影和3D电视密度图

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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