Sintering and oxidation using a novel ultrahigh vacuum transmission electron microscope with in situ magnetron sputtering

The synthesis and processing of materials is often highly sensitive to the presence of trace contaminants and a number of technologically important materials demand the clean conditions associated with an ultrahigh vacuum environment. With increasing interest in understanding materials phenomena occurring on smaller and smaller length scales, the transmission electron microscope is finding increasing application in the characterization of new materials and processes. The need for ex situ sample preparation prior to analysis can raise questions regarding the validity of the data, however, due to contamination and the introduction of microstructural artifacts. In this paper we discuss the application of the ultrahigh vacuum transmission electron microscope to in situ studies of materials synthesis. To illustrate the capabilities of the electron microscope in this context, we present two case studies: the synthesis and subsequent sintering of supported copper nanoparticles, and the initial stages of the growth of Cu₂O on clean (001) Cu. We describe the novel aspects of the instrumentation used, the methods of sample preparation, and our application of the plan-view imaging technique to in situ investigations.