This paper presents an investigation into high temperature imaging of metals through the use of a novel heat stage for in situ Scanning Electron Microscopy (SEM). The results obtained demonstrate the benefits and challenges of SEM imaging at elevated temperatures of up to 850 °C using Secondary Electron (SE) and Electron Backscatter Diffraction (EBSD) detectors. The data collected using the heat stage demonstrate good beam, vacuum, and detector stability at high temperatures without the need for shielding or detector modification owing to the heat stage geometry. SE imaging highlighted one possible application: carrying out thermal etching, a process in which surface grooves form along a material's grain boundaries during heating in situ. The data suggest that using the heat stage to perform imaging during the process gives a more accurate representation of a material's microstructure at temperature than examining the thermally etched specimen after cooling. This study also highlights some of the challenges of high temperature in situ EBSD imaging in both steel and nickel at a variety of temperatures and time scales. In particular, the data demonstrate the effect of surface roughness on EBSD imaging and how microstructural changes during heating may affect this. Additionally, the ease with which a material can be imaged using EBSD at temperature may be affected by the material's magnetic properties. For the first time, it is shown that at temperatures close to the Curie temperature of ferromagnetic materials, in this case Nickel, there is a loss of EBSD image quality. Quality was regained when temperatures were further increased. Despite these challenges, good quality EBSD scans were produced, further highlighting the benefits of in situ testing for providing information on grain boundaries, orientations, and phase change at elevated temperatures.

中文翻译：

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高温下原位扫描电子显微镜 (SEM) 成像实验研究

本文通过使用新型热台进行原位扫描电子显微镜 (SEM) 对金属的高温成像进行了研究。获得的结果证明了使用二次电子 (SE) 和电子背散射衍射 (EBSD) 探测器在高达 850 °C 的高温下进行 SEM 成像的优势和挑战。使用热台收集的数据在高温下显示出良好的光束、真空和探测器稳定性，而无需由于热台几何形状而需要屏蔽或探测器修改。SE 成像突出了一个可能的应用：进行热蚀刻，这是一种在原位加热过程中沿材料的晶界形成表面凹槽的过程。数据表明，与在冷却后检查热蚀刻样品相比，在该过程中使用热台进行成像可以更准确地表示材料在温度下的微观结构。这项研究还强调了钢和镍在各种温度和时间尺度下高温原位 EBSD 成像的一些挑战。特别是，数据证明了表面粗糙度对 EBSD 成像的影响，以及加热过程中的微观结构变化如何影响这一点。此外，材料在温度下使用 EBSD 成像的难易程度可能会受到材料磁性的影响。首次表明，在接近铁磁材料居里温度的温度下，在这种情况下为镍，EBSD 图像质量会有所下降。当温度进一步升高时，质量恢复。尽管存在这些挑战，但还是产生了高质量的 EBSD 扫描，进一步突出了原位测试在提供高温下晶界、取向和相变信息方面的优势。