| In situ monitoring of events in transmission electron microscopy provides information on how materials behave in their true state while varying environmental conditions (i.e. temperature and pressure) and exposure to reactant gas mixtures. In-situ results are usually different from static, post-reaction observations because they provide valuable real time---rather than post mortem---information. To facilitate applications that demand in situ observations, a transmission electron microscope specimen holder assembly has been developed in this dissertation. This assembly incorporates a gas flow and heating mechanism along with a novel window-type environmental cell. A controlled mixture of up to four different gases can be circulated through the cell during an experiment. In addition, the specimen can be heated up to a temperature of 1500°C using a specially designed carbon dioxide laser mechanism. This heating technique provides major advantages over conventional methods in terms of product life, specimen heating time and design size. The cell design incorporates a gas reaction chamber less than 1 mm in height, enclosed between a pair of 20 nm thick silicon nitride windows. The chamber can accommodate a specimen or a grid having a diameter of 3 mm and thicknesses in the range of 50 to 100 microns. The volume for the gas environment within the chamber is approximately 3 mm 3 and the gas path length is less than 1 mm. This holder has been designed by incorporating cutting edge heating and Si3N4 window fabrication technology to achieve excellent resolution along with a low thermal drift. Successful application of the holder has been shown to provide scientists with an economical alternative to dedicated transmission electron microscopes for a vast array of in situ applications. These applications include understanding the basic material properties, catalysis reactions, semiconductor device development, and nano structure fabrication. |
