Hostname: page-component-78c5997874-94fs2 Total loading time: 0 Render date: 2024-11-20T03:45:41.921Z Has data issue: false hasContentIssue false

Temperature Calibration for In Situ Environmental Transmission Electron Microscopy Experiments

Published online by Cambridge University Press:  06 October 2015

Jonathan P. Winterstein*
Affiliation:
FEI Company, 5350 NE Dawson Creek Drive, Hillsboro, Oregon 97124USA NIST, 100 Bureau Dr., Gaithersburg, MD, USA
Pin Ann Lin
Affiliation:
NIST, 100 Bureau Dr., Gaithersburg, MD, USA Maryland NanoCenter, University of Maryland, 225 Paint Branch Dr, College Park, MD 20740
Renu Sharma
Affiliation:
NIST, 100 Bureau Dr., Gaithersburg, MD, USA
*
*Corresponding author. [email protected]
Get access

Abstract

In situ environmental transmission electron microscopy (ETEM) experiments require specimen heating holders to study material behavior in gaseous environments at elevated temperatures. In order to extract meaningful kinetic parameters, such as activation energies, it is essential to have a direct and accurate measurement of local sample temperature. This is particularly important if the sample temperature might fluctuate, for example when room temperature gases are introduced to the sample area. Using selected-area diffraction (SAD) in an ETEM, the lattice parameter of Ag nanoparticles was measured as a function of the temperature and pressure of hydrogen gas to provide a calibration of the local sample temperature. SAD permits measurement of temperature to an accuracy of ±30°C using Ag lattice expansion. Gas introduction can cause sample cooling of several hundred degrees celsius for gas pressures achievable in the ETEM.

Type
Equipment and Techniques Development
Copyright
© Microscopy Society of America 2015 

Access options

Get access to the full version of this content by using one of the access options below. (Log in options will check for institutional or personal access. Content may require purchase if you do not have access.)

References

Allard, L.F., Bigelow, W.C., Jose-Yacaman, M., Nackashi, D.P., Damiano, J. & Mick, S.E. (2009). A new MEMS-based system for ultra-high-resolution imaging at elevated temperatures. Microsc Res Tech 72(3), 208215.Google Scholar
Baker, R.T.K. & Harris, P.S. (1972). Controlled atmosphere electron microscopy. J Phys E 5(8), 793.Google Scholar
Brintlinger, T., Qi, Y., Baloch, K.H., Goldhaber-Gordon, D. & Cumings, J. (2008). Electron thermal microscopy. Nano Lett 8(2), 582585.Google Scholar
Crozier, P. (2006). The fundamental role of in situ electron microscopy in catalytic science. Microsc Microanal 12(Suppl S02), 768769.Google Scholar
Gray, D.E. Ed. 1972). American Institute of Physics Handbook, 3rd ed. New York, NY: McGraw-Hill.Google Scholar
Hull, R., Demarest, J., Dunn, D., Stach, E.A. & Yuan, Q. (1998). Applications of ion microscopy and in situ electron microscopy to the study of electronic materials and devices. Microsc Microanal 4(3), 308316.Google Scholar
Krämer, S. & Mayer, J. (1999). Using the Hough transform for HOLZ line identification in convergent beam electron diffraction. J Microsc 194(1), 211.Google Scholar
Kreith, F. & Bohn, M.S. (1997). Principles of Heat Transfer. Boston, MA: PWS Publishing.Google Scholar
Mitchell, D.R.G. (2008). Circular Hough transform diffraction analysis: A software tool for automated measurement of selected area electron diffraction patterns within Digital Micrograph™. Ultramicroscopy 108(4), 367374.Google Scholar
Picher, M., Mazzucco, S., Blankenship, S. & Sharma, R. (2015). Vibrational and optical spectroscopies integrated with environmental transmission electron microscopy. Ultramicroscopy 150, 1015.Google Scholar
Ross, F.M. (2010). Controlling nanowire structures through real time growth studies. Rep Prog Phys 73(11), 114501.Google Scholar
Sharma, R. (2001). Design and applications of environmental cell transmission electron microscope for in situ observations of gas–solid reactions. Microsc Microanal 7(06), 494506.Google Scholar
Simmons, R.O. (1970). Use of fcc metals as internal temperature standards in X‐ray diffraction. J Appl Phys 41(5), 22352240.Google Scholar
Stach, E.A., Hull, R., Bean, J.C., Jones, K.S. & Nejim, A. (1998). In situ studies of the interaction of dislocations with point defects during annealing of ion implanted Si/SiGe/Si (001) heterostructures. Microsc Microanal 4(3), 294307.Google Scholar
Suh, I.-K., Ohta, H. & Waseda, Y. (1988). High-temperature thermal expansion of six metallic elements measured by dilatation method and X-ray diffraction. J Mater Sci 23(2), 757760.Google Scholar
Vendelbo, S.B., Kooyman, P.J., Creemer, J.F., Morana, B., Mele, L., Dona, P., Nelissen, B.J. & Helveg, S. (2013). Method for local temperature measurement in a nanoreactor for in situ high-resolution electron microscopy. Ultramicroscopy 133, 7279.Google Scholar
Yang, J.C. & Zhou, G. (2012). In situ ultra-high vacuum transmission electron microscopy studies of the transient oxidation stage of Cu and Cu alloy thin films. Micron 43(11), 11951210.CrossRefGoogle Scholar