Department of Inorganic Chemistry, Fritz-Haber-Institut der Max-Planck-Gesellschaft, Berlin, Germany.
Department of Inorganic Chemistry, Fritz-Haber-Institut der Max-Planck-Gesellschaft, Berlin, Germany; Department of Heterogeneous Reactions, Max Planck Institute for Chemical Energy Conversion, Mülheim, Germany.
Ultramicroscopy. 2018 Dec;195:121-128. doi: 10.1016/j.ultramic.2018.09.001. Epub 2018 Sep 5.
We present a versatile grid reactor setup for transmission electron microscopy (TEM), which is able to track catalytic conversion on TEM amounts of sample. It is based on the concept of decoupling catalytic gas-phase reactions from the structural analysis of identical particles before and after reaction. The system has superior properties in terms of image resolution and long-term measurements compared to conventional in situ TEM analysis. Monitoring catalytic conversions on a TEM grid is enabled by proton-transfer reaction mass spectrometry. In addition, identical location imaging benefits from a secure transfer of the sample between TEM and the reactor system by vacuum transfer holders. Using Pt and Cu/ZnO/AlO as an example we show that structural changes of identical particles or areas of a Pt foil before and after reactive experiments can be tracked. During catalytic testing the samples are exposed to homogeneous reaction conditions. The concept minimizes electron-sample and electron-atmosphere interactions and can prospectively be considered as complementary tool to in situ TEM analysis.
我们提出了一种用于透射电子显微镜(TEM)的通用网格反应器设置,该设置能够跟踪 TEM 量样品上的催化转化。它基于将催化气相反应与反应前后相同颗粒的结构分析解耦的概念。与传统的原位 TEM 分析相比,该系统在图像分辨率和长期测量方面具有优越的性能。质子转移反应质谱法可实现 TEM 网格上的催化转化监测。此外,通过真空转移支架在 TEM 和反应器系统之间安全地转移样品,相同位置的成像也成为可能。使用 Pt 和 Cu/ZnO/AlO 作为示例,我们证明了在反应实验前后相同颗粒或 Pt 箔的相同区域的结构变化可以被跟踪。在催化测试中,样品暴露于均匀的反应条件下。该概念最大限度地减少了电子-样品和电子-气氛的相互作用,并且可以作为原位 TEM 分析的补充工具来考虑。