A new MEMS‐based system for ultra‐high‐resolution imaging at elevated temperatures

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‐Ångström 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°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. Microsc. Res. Tech., 2009. © 2009 Wiley‐Liss, Inc.

[1]  Pratibha L. Gai,et al.  Developments in in situ Environmental Cell High-Resolution Electron Microscopy and Applications to Catalysis , 2002 .

[2]  T. Kamino,et al.  Development of a technique for high resolution electron microscopic observation of nano-materials at elevated temperatures. , 2005, Journal of electron microscopy.

[3]  P. Batson Motion of Gold Atoms on Carbon in the Aberration-Corrected STEM , 2007, Microscopy and Microanalysis.

[4]  N. H. Packan,et al.  Electron microscope in situ annealing study of voids induced by irradiation in aluminum , 1970 .

[5]  Konno Mitsuru,et al.  Development of a specimen heating holder with an evaporator and gas injector and its application for catalyst. , 2006, Journal of electron microscopy.

[6]  K. Sasaki,et al.  In Situ Heating Transmission Electron Microscopy , 2008 .

[7]  S. Sepúlveda-Guzmán,et al.  Three-layer core/shell structure in Au-Pd bimetallic nanoparticles. , 2007, Nano letters.

[8]  R. Baker In Situ Electron Microscopy Studies of Catalyst Particle Behavior , 1979 .

[9]  Renu Sharma Design and Applications of Environmental Cell Transmission Electron Microscope for In Situ Observations of Gas–Solid Reactions , 2001, Microscopy and Microanalysis.

[10]  H. Makino,et al.  Development of a gas injection/specimen heating holder for use with transmission electron microscope. , 2005, Journal of electron microscopy.

[11]  Renu Sharma,et al.  Development of a TEM to study in situ structural and chemical changes at an atomic level during gas‐solid interactions at elevated temperatures , 1998, Microscopy research and technique.

[12]  L. Allard,et al.  Atomic structure of three-layer Au/Pd nanoparticles revealed by aberration-corrected scanning transmission electron microscopy , 2008 .

[13]  M. O'Keefe,et al.  Early Results from an Aberration-Corrected JEOL 2200FS STEM/TEM at Oak Ridge National Laboratory , 2006, Microscopy and Microanalysis.

[14]  D. L. Douglass,et al.  Oxide nucleation on thin films of copper duringin Situ oxidation in an electron microscope , 1975 .