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Locally Condensed Water as a Solution for In Situ Wet Corrosion Electron Microscopy
Microscopy and Microanalysis ( IF 2.9 ) Pub Date : 2020-02-13 , DOI: 10.1017/s1431927620000100
Majid Ahmadi 1 , Frans D Tichelaar 1 , Andreas Ihring 2 , Michael Kunze 3 , Sophie Billat 3 , Zahra Kolahdouz Esfahani 1 , Henny W Zandbergen 1
Affiliation  

In microstructural corrosion studies, knowledge on the initiation of corrosion on an nm-scale is lacking. In situ transmission electron microscope (TEM) studies can elucidate where/how the corrosion starts, provided that the proper corrosive conditions are present during the investigation. In wet corrosion studies with liquid cell nanoreactors (NRs), the liquid along the electron beam direction leads to strong scattering and therefore image blurring. Thus, a quick liquid removal or thickness control of the liquid layer is preferred. This can be done by the use of a Peltier element embedded in an NR. As a prelude to such in situ work, we demonstrate the local wetting of a TEM sample, by creating a temperature decrease of 10 ± 2°C on the membrane of an NR with planar Sb/BiSb thermoelectric materials for the Peltier element. TEM samples were prepared and loaded in an NR using a dual-beam focused ion beam scanning electron microscope. A mixture of water vapor and carrier gas was passed through a chamber, which holds the micro-electromechanical system Peltier device and resulted in quick formation of a water layer/droplets on the sample. The TEM analysis after repeated corrosion of the same sample (ex situ studies) shows the onset and progression of O2 and H2S corrosion of the AA2024-T3 alloy and cold-rolled HCT980X steel lamellae.

中文翻译:

局部冷凝水作为原位湿腐蚀电子显微镜的解决方案

在微观结构腐蚀研究中,缺乏关于纳米级腐蚀引发的知识。原位透射电子显微镜 (TEM) 研究可以阐明腐蚀开始的位置/方式,前提是在调查期间存在适当的腐蚀条件。在液体电池纳米反应器 (NR) 的湿腐蚀研究中,沿电子束方向的液体会导致强烈的散射,从而导致图像模糊。因此,优选液体层的快速液体去除或厚度控制。这可以通过使用嵌入 NR 中的 Peltier 元件来完成。作为这样的前奏原位工作,我们通过在具有用于珀尔帖元件的平面 Sb/BiSb 热电材料的 NR 膜上产生 10 ± 2°C 的温度降低来证明 TEM 样品的局部润湿。使用双束聚焦离子束扫描电子显微镜制备 TEM 样品并将其加载到 NR 中。水蒸气和载气的混合物通过一个装有微机电系统 Peltier 装置的腔室,并导致样品上快速形成水层/液滴。同一样品反复腐蚀后的 TEM 分析 (异地研究)显示 O 的发生和进展2和 H2AA2024-T3 合金和冷轧 HCT980X 钢片的 S 腐蚀。
更新日期:2020-02-13
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