纳米多孔金属表面结构与成分的三维电子层析表征

doi:10.11900/0412.1961.2022.00133

金属学报

2023, Vol. 59

Issue (10): 1291-1298 DOI: 10.11900/0412.1961.2022.00133

研究论文

本期目录 | 过刊浏览

纳米多孔金属表面结构与成分的三维电子层析表征

段慧超¹^,², 王春阳¹, 叶恒强¹^,³, 杜奎¹(

)

^1.中国科学院金属研究所沈阳材料科学国家研究中心沈阳 110016
^2.中国科学技术大学材料科学与工程学院沈阳 110016
^3.季华实验室佛山 528000

Electron Tomography Analysis on the Structure and Chemical Composition of Nanoporous Metal Surfaces

DUAN Huichao¹^,², WANG Chunyang¹, YE Hengqiang¹^,³, DU Kui¹(

)

^1.Shenyang National Laboratory for Materials Science, Institute of Metal Research, Chinese Academy of Sciences, Shenyang 110016, China
^2.School of Materials Science and Engineering, University of Science and Technology of China, Shenyang 110016, China
^3.Ji Hua Laboratory, Foshan 528000, China

引用本文:

段慧超, 王春阳, 叶恒强, 杜奎. 纳米多孔金属表面结构与成分的三维电子层析表征[J]. 金属学报, 2023, 59(10): 1291-1298.
Huichao DUAN, Chunyang WANG, Hengqiang YE, Kui DU. Electron Tomography Analysis on the Structure and Chemical Composition of Nanoporous Metal Surfaces[J]. Acta Metall Sin, 2023, 59(10): 1291-1298.

全文: PDF(2008 KB) HTML

摘要:

结合扫描透射电子显微技术、电子层析技术及能量色散谱(EDS)成分的三维重构对纳米多孔Au和纳米多孔Au-Pt孔棱的表面结构和成分进行了分析。利用原子分辨率的电子层析技术分析了纳米多孔Au孔棱表面的原子结构，发现表面的缺陷可以分为2类，一类是{111}平台上的扭折和台阶，一类是表面凹坑。相比于扭折和台阶，表面凹坑会引入更多低配位位点。将原子级电子层析与EDS成分三维重构相结合，分析了Pt元素在孔棱表面的偏聚情况，证明了Pt在孔棱表面低配位位点的偏聚。

关键词 ：电子层析技术, 能量色散谱, 纳米多孔金属, 表面偏聚

Abstract：

Nanoporous metals have a porous structure with bicontinuous nanoscale voids and ligaments. Thus, nanoporous metals differ from their bulk counterparts in mechanical, physical, and chemical characteristics due to their unique ligament structure and high surface-to-volume ratio. The surface structure and chemistry of nanoporous metals play critical roles in their applications in catalysis, sensing, and other fields. The surfaces of nanoporous metals contain a substantial number of low-coordination sites, which are vital for improving their catalytic performance. Moreover, the addition of platinum to nanoporous gold has a massive impact on its catalytic and mechanical characteristics. High-resolution transmission electron microscopy (TEM) and high-resolution scanning transmission electron microscopy (STEM) are commonly used to study the atomic structure of crystals. However, since these techniques only provides two-dimensional projection images, it is usually hard or even impossible to directly and quantitatively resolve the three-dimensional (3D) structure of nanocrystals, especially their surface crystallography and coordination information. Compared to traditional TEM and STEM imaging technologies, electron tomography with atomic resolution provides a powerful means to resolve 3D atomic-resolution information of materials. In this work, the surface structure and chemical composition of nanoporous gold and nanoporous gold-platinum were analyzed using STEM, electron tomography, and three-dimensional reconstruction of energy dispersive spectroscopy (EDS) results. The atomic structure of the ligament surface was examined using electron tomography with atomic resolution. It was observed that, surface defects can be separated into two categories: kinks and steps on the {111} terrace, and dents and pits. Surface dents and pits introduce a greater number of low-coordination sites than kinks and steps. Furthermore, the segregation of Pt on the ligament surface was discovered by combining the atomic-resolution electron tomography with the 3D reconstruction of EDS results.

Key words： electron tomography energy dispersive spectroscopy nanoporous matal surface segregation

收稿日期: 2022-03-23

ZTFLH:

TG146.3

基金资助:国家自然科学基金项目(52171020);国家自然科学基金项目(91960202)

通讯作者: 杜奎，kuidu@imr.ac.cn，主要从事结构材料形变与相变的定量电子显微学研究

Corresponding author: DU Kui, professor, Tel: (024)83970725, E-mail: kuidu@imr.ac.cn

作者简介: 段慧超，男，1992年生，博士生

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图1 纳米多孔Au的孔棱和孔隙结构高角环形暗场(HAADF)像

图2 低倍下纳米多孔Au结构和成分的三维(3D)重构结果

图3 纳米多孔Au孔棱的原子分辨率电子层析3D重构及表面配位分析

图4 纳米多孔Au-Pt表面凹坑的原子级3D重构结果

图5 纳米多孔Au-Pt表面偏聚的3D分析

图6 表面Pt偏聚的3D探测尺寸

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