原位液相透射电子显微镜及其在纳米粒子表征方面的应用

刘玄玄; 国洪轩; 徐涛; 尹奎波; 孙立涛

doi:10.7498/aps.70.20201899

摘要

近年来, 基于透射电子显微技术、微纳加工技术和薄膜制造技术的发展, 原位液相透射电子显微技术产生, 为构建多种纳米级分辨率尺度下的微实验平台, 发展新型纳米表征技术和众多领域的相关研究提供了途径. 本文首先介绍了应用于原位液相透射电子显微技术的液体腔设计要求, 然后介绍了液体腔的发展和典型的制备工艺, 最后综述了近年来液体腔透射电子显微镜在纳米粒子成核和生长方面的应用研究, 并探讨了该技术前沿发展面临的机遇和挑战. 本文将为提高我国先进纳米表征技术和原子精准构筑技术提供相关讨论和支持.

关键词:

Abstract

Based on the improvement of transmission electron microscope (TEM), nano fabrication, and film deposition, and with the development of the in-situ liquid TEM and nano characterization platform, various relevant nano researches have been carried in different fields. In this article, the principle, basic design requirements, development and typical preparation technologies of the liquid cell are briefly introduced. Subsequently, the state-of-the-art applications of liquid cell transmission electron microscope in the nucleation and growth of nanoparticles are reviewed. Finally, the opportunities and challenges faced by the frontier development of this technology are also discussed. This article provides constructive discussion about and support for advanced nano characterization technology and precise manipulation of atomic structures.

Keywords:

in situ liquid transmission electron microscope /
nano characterization /
in situ liquid cell

作者及机构信息

1.
东南大学电子科学与工程学院, MEMS教育部重点实验室, 南京　210096

2.
东南大学FEI纳皮米中心, 南京　210096

3.
东南大学微电子学院, 无锡　214000

通信作者: 国洪轩, ghx@seu.edu.cn ; 孙立涛, slt@seu.edu.cn

基金项目: 国家自然科学基金(批准号: 11874105)和国家杰出青年科学基金(批准号: 11525415)资助的课题

Authors and contacts

1.
Key Lab of MEMS of Ministry of Education, School of Electronic Science and Engineering, Southeast University, Nanjing 210096, China

2.
FEI Nano-Pico Center, Southeast University, Nanjing 210096, China

3.
School of Microelectronics, Southeast University, Wuxi 214000, China

Corresponding author: Guo Hong-Xuan, ghx@seu.edu.cn ; Sun Li-Tao, slt@seu.edu.cn

Funds: Project supported by the National Natural Science Foundation of China (Grant No. 11874105) and the National Science Fund for Distinguished Young Scholars of China (Grant No. 11525415)

文章全文 : translate this paragraph

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施引文献

图 1 三类液体环境TEM实现方式示意图　(a)基于差分泵真空系统TEM结构示意图^[3]; (b), (c) 基于离子液体构建的液体环境TEM实验装置示意图^[4]; (d) 基于液体腔构建的液体环境TEM实验装置示意图; (e), (f)基于微纳加工制备的氮化硅窗口液体腔结构示意图^[6,7]; (g), (h)基于石墨烯窗口的液体腔结构示意图^[8,9]

Fig. 1. Schematic diagrams of three typical methods to observe liquid sample by TEM: (a) Environment TEM based on differential pump system^[3]; (b), (c) observation of the ionic liquid sample by TEM^[4]; (d) schematic diagram of closed liquid cell for TEM observation; (e), (f) schematic diagrams of the liquid cell with the silicon nitride window^[6,7]; (g), (h) schematic diagrams of the liquid cell with the graphene window^[8,9].

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图 2 典型的液体腔基本结构示意图

Fig. 2. Schematic diagram of the structure of a typical liquid cell.

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图 3 氮化硅窗口液体腔的发展情况

Fig. 3. The development of the silicon nitride window liquid cell.

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图 4 典型的TEM 原位液体腔制作工艺步骤示意图　(a) 液体腔的基本结构图, 为方便结构解析, (b), (c) 沿黑色虚线剖面结构; (b) 典型的制作工艺步骤, 通过不同工艺分别制作上下两部分结构, 最后组装成(c)结构; (c) 液体腔的基本结构图剖面图

Fig. 4. Typical TEM liquid cell manufacturing process: (a) The structure diagram of the liquid cell, where description (b) and (c) are cross-sectional diagram drawn along the black dash; (b) typical manufacturing process steps, the upper and lower parts are made by different processes structure, finally assembled into (c) the structure of the liquid cell with the cross-sectional view.

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图 5 附加功能的液体腔结构示意图　(a) 附加电极的流动式液体腔结构示意图^[6]; (b) 附加加热功能的液体腔结构示意图^[72]

Fig. 5. Liquid cell with additional functions: (a) Fluidic liquid cell with electrodes^[6]; (b) liquid cell with heater^[72]

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图 6 典型的石墨烯液体腔制作工艺步骤示意图　(a) 两个石墨烯沉积的TEM网格相互叠加; (b) 滴加溶液并吸去多余的溶液; (c) 少量残留的液体压入微米或纳米级的囊中; (d) 移除上层TEM网格

Fig. 6. Typical manufacturing process of the graphene liquid cell: (a) Two graphene deposited TEM grids are superimposed; (b) extra solution is removed by suction after dropping; (c) solution is entrapped between two graphene membranes after drying; (d) top TEM grid is removed.

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图 7 两种典型的石墨烯液体腔结构示意图　(a)石墨烯液体腔结构示意图; (b)硅基-石墨烯液体腔结构示意图

Fig. 7. Schematic diagram of two typical graphene liquid cell structures: (a) Graphene liquid cavity structure; (b) silicon-based graphene liquid cavity structure.

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图 8 金纳米颗粒的成核过程的TEM时序图像^[82]　(a)−(d)金纳米颗粒在溶液中的形核过程; (e)−(n) 选自(a)中黑框区域的成核情况, 圆圈标定的粒子在成核过程中溶解

Fig. 8. TEM time series images of the nucleation process of gold nanoparticles^[82]: (a)−(d) Nucleation process of gold nanoparticles in solution; (e)−(n) nucleation situation of the black frame area in (a) is selected, where particles demarcated by the circle are dissolved during the nucleation process.

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图 9 金和银在溶液中成核的三步途径^[85]　(a)金纳米粒子成核的三个阶段演化图像; (b)成核步骤示意图; (c)银纳米粒子成核的三个阶段演化图像

Fig. 9. The three-step pathway of gold and silver nucleation in solution^[85]: (a) Three-stage evolution image of gold nanoparticle nucleation; (b) schematic diagram of nucleation step; (c) three-stage evolution image of silver nanoparticle nucleation.

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图 10 原位液体电镜下纳米晶的生长过程　(a) Pt 纳米粒子生长的TEM时序图像, 左侧为纳米粒子通过单体生长的过程, 右侧为纳米粒子聚合生长过程^[7]; (b) Pt纳米粒子特定晶相的聚合生长过程的TEM时序图像^[8]

Fig. 10. Growth process of nanocrystals observed by in-situ liquid electron microscope: (a) TEM time series images of Pt nanoparticle growth, the left side is the process of nanoparticle growth through monomer, and the right side is the process of nanoparticle aggregation growth^[7]; (b) TEM time series images of the polymerization growth process of the specific crystal phase of Pt nanoparticles^[8]

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图 11 纳米晶体在溶液中的定向吸附过程^[69]　(a) 弛豫阶段纳米晶体的结构变化; (b)不同长度纳米线的矫直过程

Fig. 11. The directional adsorption process of nanocrystals in solution^[69]: (a) Structural evolution of nanocrystals in the relaxation phase; (b) straightening process of nanowires of different lengths.

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图 12 Pt二十面体上Au的生长^[93]　(a) TEM时序图像显示了Au在Pt二十面体纳米颗粒上的生长过程, 箭头代表Au的生长变化位置; (b) Pt纳米晶体上Au的成核和生长的定量分析, 方程是考虑了反应和扩散的增长率

Fig. 12. Au growth on a Pt icosahedron^[93]: (a) TEM sequence image shows the growth process of Au on Pt icosahedral nanoparticles, and the arrow represents the growth and change position of Au; (b) quantitative analysis of Au nucleation and growth on Pt nanocrystals, the equation is to consider the growth rate of reaction and diffusion.

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原位液相透射电子显微镜及其在纳米粒子表征方面的应用