In recent years, an increasing number of laboratories have been applying in situ heating (and ultimately, gas reaction) techniques in electron microscopy studies of catalysts and other nanophase materials. With the advent of aberration-corrected electron microscopes that provide sub-Angström image resolution, it is of great interest to study the behavior of materials at elevated temperatures while maintaining the resolution capabilities of the microscope. In collaboration with Protochips Inc., our laboratory is developing an advanced capability for in situ heating experiments that overcomes a number of performance problems with standard heating stage technologies. The new heater device allows, for example, temperature cycling from room temperature to greater than 1000 degrees C in 1 ms (a heating rate of 1 million Centigrade degrees per second) and cooling at nearly the same rate. It also exhibits a return to stable operation (drift controlled by the microscope stage, not the heater) in a few seconds after large temperature excursions. With Protochips technology, we were able to demonstrate single atom imaging and the behavior of nanocrystals at high temperatures, using high-angle annular dark-field imaging in an aberration-corrected (S)TEM. The new capability has direct applicability for remote operation and (ultimately) for gas reaction experiments using a specially designed environmental cell.
Introduces and qualifies the Fusion platform. The authors perform quantitative experiments that show drift and settle time performance. Experiments include heating AuPd core shell particles at atomic resolution using a JEOL 2200FS Cs corrected STEM.