Transmission Electron Microscopy: New Advances and Applications for Earth and Planetary Sciences
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摘要: 近年来，各种微束分析技术的快速发展及其在地球和行星科学领域的广泛应用，极大地推动了纳米地球科学和行星科学的学科发展和科学研究.透射电子显微镜（简称透射电镜）因具有空间分辨率高和综合分析能力强等优点，在地球与行星物质的微纳尺度到原子水平的形貌、晶体结构、矿物相鉴定、化学成分、原子成像和微磁结构等研究中发挥着巨大作用.在简要回顾透射电镜的发展历程、物理结构和工作原理的基础上，结合本实验室过去几年的工作内容，重点介绍了透射电镜的基本功能、样品制备方法及其在地球和行星科学研究中的应用范例.通过与其他微束分析技术的简单对比，还初步分析了透射电镜在地球与行星科学研究领域的应用现状和未来趋势.Abstract: In recent years, researches on nanogeoscience and planetary sciences have achieved significant progresses mostly due to the applications of various microscopic and micro-spectroscopic approaches. Among these techniques, transmission electron microscopy (TEM), known as high spatial resolution and strong comprehensive analysis capability, plays an important role in simultaneously imaging and characterizing morphological, structural, chemical, and micromagnetic properties down to atomic scales. In this review it briefly introduces the development history, mechanical structure and working principles of transmission electron microscope, and the sample preparation involved in the TEM technique as well. Based on some recent progresses achieved in the Electron Microscope Lab at the IGGCAS, this review also shows and focus on the fundamental functions and applications of transmission electron microscope in some typical researches in earth and planetary sciences. Finally, it tentatively discusses the current situation and future trend of transmission electron microscopy in earth and planetary sciences.
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图 1 20世纪30年代初鲁斯卡（右）和克诺尔（左）研制的电子显微镜(Williams and Carter, 2009)（a）；最初的电子显微镜光路图（b）；现代球差校正透射电镜（JEM-ARM 300F，https://www.jeol.co.jp/en/products/detail/JEM-ARM300F.html）（c）；聚光镜像差校正透射电镜结构示意图（d）
Fig. 1. The earliest electron microscope built by Ruska (right) and Knoll (left), in Berlin in the early 1930s(a), schematic illustration of the electron optical systems of the earliest electron microscope(b), picture of one representative modern transmission electron microscope (JEM-ARM 300F, https://www.jeol.co.jp/en/products/detail/JEM-ARM300F.html) (c), schematic illustration of aberration-corrected transmission electron microscope(d)
图 2 入射电子与样品相互作用后产生的各种信号（a）；常规透射电子显微镜工作原理示意图（b）；扫描透射电子显微镜工作原理示意图（c）
Fig. 2. Multiphoton absorption and emission by interaction between incident electrons and matters(a), schematic diagram of working principle of conventional transmission electron microscope(b), schematic illustration of working principle of a scanning transmission electron microscope(c)
图 3 原子电子三维重构（AED）原理（Miao et al., 2016）
Fig. 3. The schematic layout of 3D atomic electron tomography (AET)
图 4 单晶衍射花样（橄榄石）（a）；多晶衍射花样（Fe3O4）（b）；非晶衍射花样（长石）（c）；会聚束衍射花样（晶体材料）（d）
Fig. 4. SAED pattern for single crystal (olivine) (a), SAED pattern for polycrystal (Fe3O4) (b), SAED pattern for amorphous material (feldspar) (c), central disk of CBED pattern for the crystal model(d)
图 5 DPC STEM工作原理示意图（修改自Shibata, 2019）（a）.分割探测器几何结构及其接收的电子束穿过原子柱时在衍射面产生的强度分布（修改自Sánchez-Santolino et al., 2018）（b）
Fig. 5. Schematic illustrations of DPC STEM(a), the segmented area detector geometry and the accepted intensity distribution in the diffraction plane when the electron probe passes close to a column(b)
图 6 洛伦兹电子显微术的Fresnel成像原理（修改自Du et al., 2015）（a）；离轴电子全息术原理（修改自Midgley and Dunin-Borkowski, 2009）（b）
Fig. 6. Schematic ray diagram in a Fresnel image of a ferromagnetic specimen containing two 180° domain walls(a), schematic diagram of off-axis electron holography (b)
图 7 固体块状样品的透射电镜样品制备方法
a.超薄切片法工作原理图（Wei and Li, 1997）；b.离子减薄工作原理图；c. FIB-SEM双束系统原理图；d. FIB-SEM制备TEM样品示意图
Fig. 7. Preparation methods of solid block sample for TEM
图 8 来自Apex燧石样品中的疑似细菌化石纳米结构和化学特征
图a和图b分别是提取用于TEM分析的超薄片之前和之后的光学显微照片.图c~f是伪化石薄片的明场TEM图像（c）和相应的TEM能量过滤像元素图，硅（d）、碳（e）和铝（f）.图g为碳、铁和铝的元素叠加图，碳（黄色）和铁（绿色）交错于铝硅酸盐（红色）之间（Brasier et al., 2015）
Fig. 8. Nanoscale structure and chemistry of a pseudofossil from sample Apex chert
图 9 趋磁杆菌WYHR-1及其子弹头形磁小体晶体生长机制
a, b.一个WYHR-1细菌的明场像和高角环形暗场STEM图像；c.STEM-EDXS研究WYHR-1细胞的化学成分分布；d.磁小体链的STEM-HAADF三维层析重构图像；e, f.WYHR-1磁小体链的ACOM晶体取向分布图；e.对照指数图；f.水平方向（X）的晶体取向图；g.磁小体的晶体长度与宽度对比图及其磁小体晶体的生长规律；h, i.WYHR-1磁小体晶体的3D层析重构图（h）和晶体模型（i）（修改自Li et al., 2020d）
Fig. 9. Morphology, chemistry, crystal orientation and morphological model of WYHR-1 magnetosomal magnetite analyzed by atomic resolution STEM
图 10 8种磁性矿物颗粒的TEM实验结果
a, b.类型1的单个磁铁矿颗粒TEM图像（a）和对应的高分辨像（b）以及电子衍射谱（图b插图）；c, d.类型2的TEM图像（八面体的磁铁矿颗粒，平均粒径为367.8±44.9 nm）（c）和对应的电子衍射谱（d）；e, f.类型3纳米级钛磁铁矿的TEM图像（e）和对应的高分辨像（f）以及电子衍射谱（图f插图）；g, h.类型4的TEM图像（硅酸盐矿物包裹的纳米级钛磁铁矿）（g）和对应的高分辨像（h）以及电子衍射谱（图h插图）；i, j.类型5的TEM图像（树枝状的磁铁矿颗粒）（i）和对应的高分辨像（j）以及电子衍射谱（图j插图）；k, m.类型6的TEM图像（化石磁小体）；n, o.类型7的超顺磁磁性矿物聚集体的TEM图像（n）和对应的电子衍射谱（o）；p, q.类型8的TEM图像（取向一致的超顺磁磁性矿物的聚集体）（p）和对应的电子衍射谱（q）；r, s.来自8种类型磁铁矿样品的EDXS成分分析，S1~S10表示图 10中十字叉位置（Li et al., 2020b）
Fig. 10. TEM results of eight types of magnetite mineral particles
图 11 卡林型金矿中纳米金的透射电镜表征
a.金粒子(较亮的点，箭头所指)的STEM-HAADF像；b~c.金晶粒的高分辨图像（HRTEM）(b)和对应的FFT图像(c)；d~e.金粒子的EDXS元素面分布图，分别是Au -Lα (d)、Fe-Kα (e)和S-Kα (f)（修改自Palenik et al., 2004）
Fig. 11. Characterization of gold nanoparticles in a Carlin-type deposit by TEM
图 12 RW-1独居石中放射成因Pb的透射电镜分析
a.独居石薄片的TEM明场像和相应的电子衍射谱；b. [010]带轴的高分辨像；c.图a独居石晶粒的EDXS谱图，其中插图是放大的EDXS谱图，红色箭头分别指示Pb-Mα和Pb-Lα峰. d~i.沿着[010]方向（d~f）和[100]方向（g~i）的独居石原子模型（d，g）、HAADF像（e，h）和对应的归一化强度mapping（f，i）；插图ex，hx分别是沿着[010]和[100]方向的放大的HAADF图像和相应的Ce原子模型，黄绿色球代表Ce原子；图f和i中白色-蓝色强度值（0.85）表示REEs分布，黄色-红色强度值（1.15）表示Pb和Th的分布（修改自Tang et al., 2020）
Fig. 12. TEM analysis of radiogenic Pb in RW-1 monazite
图 13 巴西Junia地区金刚石内多晶包裹体中集合体的STEM-HAADF图像（a）和EDXS元素分布（b~j）
Fig. 13. STEM-HAADF image (a) and elemental maps (b-j) of nanocrystalline aggregate in polymineralic inclusion from Juina, Brazil
图 14 Ⅰ型柯石英的TEM分析
a, b. NWA 8657火星陨石FIB薄片的HAADF图像；c, g. 元素Si，Al，Ca，K和Na的EDXS分布图；h. 图a局部区域的TEM暗场像；i. 柯石英的选区电子衍射图谱（来图h圆圈处）.SG.二氧化硅玻璃；Mask. 熔长石；Px. 辉石；Coe. 柯石英；Ves. 气孔.图据Hu et al.（2020）
Fig. 14. TEM analysis of Type Ⅰ coesite
表 1 透射电子显微镜的基本功能和相关技术
Table 1. Function and techniques of transmission electron microscope
分析功能 相关技术 获得信息 形貌像 BF-TEM、DF-TEM、SE 形貌、位错线和孪晶板条等 晶体结构与缺陷 SAED、CBED、NED、HRTEM、ACOM 晶体类型、晶粒取向、位错、孪晶、层错和界面结构等 原子成像 STEM-HAADF、ABF、DPC-STEM、iDPC-STEM 轻、重原子占位与分布、原子偏聚、原子电场/磁场分布 化学分析 (S)TEM-EDXS、STEM-EELS、EF-TEM 成分、原子尺度元素和空位偏析与分布、价态、键合成像等 磁结构表征 EH、Lorentz
TEM、EMCD磁场（电场）分布、磁交互作用、磁畴分布、磁化强度、轨道磁矩和自旋磁矩等 三维重构像 (S)TEM-3D ET、STEM-3D EDXS、AET 三维空间形态、结构和成分分布 原位和冷冻分析 In-situ TEM，cryo-TEM 实时、动态的形貌，成分和结构表征，特殊条件下（冷冻）电镜分析 注：BF-TEM. 明场像；DF-TEM. 暗场像；SE. 二次电子像；SAED. 选区电子衍射；CBED.会聚束电子衍射；NED. 纳米电子衍射；HRTEM. 高分辨透射电子显微像；TEM. 透射电子显微术（镜）；ACOM. 自动晶体取向成像术；STEM. 扫描透射电子显微术（镜）；STEM-HAADF. 高角环形暗场像；ABF. 环形明场像；DPC-STEM. 差分相位衬度成像；iDPC-STEM. 积分微分相位衬度成像；EDXS. X射线能量色散谱；EELS. 电子能量损失谱；EF-TEM. 能量过滤透射电子显微术；EH. 电子全息术；Lorentz TEM. 洛伦兹电子显微术；EMCD. 电子磁手性二向色性技术；3D ET. 电子三维重构技术；STEM-3D EDXS. X射线能量色散谱三维重构技术；AET. 原子电子三维重构技术；In-situ TEM. 原位透射电镜显微术；cryo-TEM. 冷冻透射电镜显微术. 
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表 2 TEM铜载网碳膜类型参数及其适用的纳米材料
Table 2. Types and applicability of carbon film coated TEM copper grid for nanomaterials
类别 特征 膜厚(nm) 衬度 适用样品 参考文献 纯碳膜 铜网和碳膜组成 15~30 一般 在有机溶剂或高温处理的材料(≥10 nm) Lu et al., 2013 微栅 有微孔的碳支持膜 15~20 优异 管状、棒状、纳米团聚物等 Tian et al., 2018 碳支持膜 铜网，方华膜和碳膜叠加 7~10 较好 粒径≥10 nm的纳米材料 Sun et al., 2019 超薄碳膜 在微栅上覆盖薄碳膜而成 3~5 优异 分散性好，粒径 < 10 nm的样品 Cai et al., 2019 双联网碳支持膜 2个碳支持膜相连，可折叠 7~10 一般 磁性纳米材料和矿物 He and Pan, 2020
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