Environmental high resolution electron microscopy and applications to chemical science

Abstract

Abstract An environmental cell high resolution electron microscope (EHREM) has been developed for in situ studies of dynamic chemical reactions on the atomic scale. It allows access to metastable intermediate phases of catalysts and to sequences of reversible microstructural and chemical development associated with the activation, deactivation and poisoning of a catalyst. Materials transported through air can be restored or recreated and samples damaged, e.g. by dehydration, by the usual vacuum environment in a conventional electron microscope can be preserved. A Philips CM30 HRTEM/STEM system has been extensively modified in our laboratory to add facilities for in situ gas-solid reaction studies in controlled atmospheres of gas or vapor at pressures of 0–50 mbar, instead of the regular TEM high vacuum environment. The integrated new environmental cell capability is combined with the original 0.23 nm TEM resolution, STEM imaging (bright field/annular dark field) and chemical and crystallographic microanalyses. Regular sample holders are used and include hot stages to > 1000°C. Examples of applications include direct studies of dynamic reactions with supported metal particle catalysts, the generation of defects and structural changes in practical complex oxide catalyst systems under operating conditions and carbon microstructures.