Environmental high resolution electron microscopy and applications to chemical science

TL;DR

This paper introduces an advanced environmental high resolution electron microscope (EHREM) capable of in situ chemical reaction studies at the atomic scale, enabling observation of catalyst dynamics and structural changes under controlled atmospheres.

Contribution

Development of a modified HRTEM and STEM system with an environmental cell for in situ gas-solid reaction analysis at near-ambient pressures, preserving samples and enabling dynamic studies.

Findings

Observation of metastable catalyst phases

Visualization of microstructural changes during reactions

Analysis of defect generation in oxide catalysts

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 C M30 HRTEM and 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 to 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 and annular dark field) and chemical and crystallographic microanalyses. Regular sample holders are used and include hot stages to higher than 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.