Tornberg Marcus, Maliakkal Carina B, Jacobsson Daniel, Wallenberg Reine, Dick Kimberly A
Centre for Analysis and Synthesis, Lund University, Box 124, 22100 Lund, Sweden.
National Center for High Resolution Electron Microscopy (nCHREM), Lund University, 22100 Lund, Sweden.
Microsc Microanal. 2022 May 30:1-9. doi: 10.1017/S1431927622000769.
The world of environmental microscopy provides the possibility to study and analyze transformations and reactions during realistic conditions to understand the processes better. We report on the design and development of a metal-organic chemical vapor deposition (MOCVD) system integrated with an environmental transmission electron microscope intended for real-time investigations of crystal growth. We demonstrate methods for achieving a wide range of precisely controlled concentrations of precursor gas at the sample, as well as for calibrating the sample partial pressure using the pressure measured elsewhere in the microscope column. The influences of elevated temperature and reactive gas within the pole-piece gap are evaluated with respect to imaging and spectroscopy. We show that X-ray energy-dispersive spectroscopy can be strongly affected by temperatures beyond 500$^{\circ }$C, while the spatial resolution is largely unaffected by heat and microscope pressure for the relevant conditions. Finally, the influence of the electron beam on the investigated processes is discussed. With this work, we aim to provide crucial input in the development of advanced in situ electron microscopy systems for studies of complex reactions in real time under realistic conditions, for instance as used during formation of semiconductor crystals.
环境显微镜领域提供了在实际条件下研究和分析转变与反应的可能性,以便更好地理解这些过程。我们报告了一种与环境透射电子显微镜集成的金属有机化学气相沉积(MOCVD)系统的设计与开发,该系统旨在对晶体生长进行实时研究。我们展示了在样品处实现广泛精确控制的前驱体气体浓度的方法,以及使用在显微镜柱其他位置测量的压力来校准样品分压的方法。针对成像和光谱分析,评估了极靴间隙内高温和反应性气体的影响。我们表明,超过500℃的温度会对X射线能量色散光谱产生强烈影响,而在相关条件下,空间分辨率在很大程度上不受热量和显微镜压力的影响。最后,讨论了电子束对所研究过程的影响。通过这项工作,我们旨在为开发先进的原位电子显微镜系统提供关键投入,以便在实际条件下实时研究复杂反应,例如在半导体晶体形成过程中使用的情况。