Kliewer Chris E, Kiss Gabor, Demartin Gregory J
ExxonMobil Research and Engineering Company, 1545 Route 22 East, Annandale, NJ 08801-0998, USA.
Microsc Microanal. 2006 Apr;12(2):135-44. doi: 10.1017/S1431927606060077.
A fixed-bed reactor has been designed and constructed for ex situ transmission electron microscopy (TEM) studies of heterogeneous catalysts. The ex situ facility exposes a fully prepared TEM sample on a grid to actual process conditions (e.g., temperature, pressure, gas composition, etc.) by placing the grid at the exit section of a conventional fixed-bed reactor. A unique reactor design allows grid transfer into the electron microscope and back into the reactor again under a controlled (inert) environment, thus allowing time-resolved monitoring of catalyst morphology changes under realistic, well-controlled conditions. This facility stands completely independent of the TEM. Thus, no special TEM modifications are required and long-term ex situ studies do not impact microscope utilization. The utility of the facility is demonstrated via the oxidation of intermediate size ( approximately 20- approximately 80 nm) supported copper particles.
已设计并建造了一个固定床反应器，用于对多相催化剂进行非原位透射电子显微镜（TEM）研究。该非原位实验装置通过将载网放置在传统固定床反应器的出口处，使载网上完全制备好的TEM样品暴露于实际工艺条件（如温度、压力、气体组成等）下。独特的反应器设计允许在受控（惰性）环境下将载网转移到电子显微镜中，然后再转移回反应器，从而能够在真实、可控的条件下对催化剂形态变化进行时间分辨监测。该实验装置完全独立于透射电子显微镜。因此，无需对透射电子显微镜进行特殊改装，长期的非原位研究也不会影响显微镜的使用。通过对中等尺寸（约20 - 约80纳米）负载型铜颗粒的氧化反应，证明了该实验装置的实用性。
