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Journal of Electron Microscopy Advance Access published online on April 17, 2009
Journal of Electron Microscopy, doi:10.1093/jmicro/dfp020
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© The Author 2009. Published by Oxford University Press on behalf of Japanese Society of Microscopy. All rights reserved. For permissions, please e-mail: journals.permissions@oxfordjournals.org

An in situ heating TEM analysis method for an interface reaction

Toshiaki Tanigaki1,*, Katsuji Ito1, Yasuhira Nagakubo2, Takayuki Asakawa1 and Takashi Kanemura1

1 Hitachi High-Tech Manufacturing & Service Corporation, 1040 Ichige, Hitachinaka, Ibaraki 312-0033 and
2 Hitachi High-Technologies Corporation, 882 Ichige, Hitachinaka, Ibaraki 312-8504, Japan

* To whom correspondence should be addressed. E-mail: tanigaki-toshiaki{at}naka.hitachi-hitec.com

In order to analyze the thermal property of nano-sized materials, an in situ observation technique that allows highly sensitive energy dispersive x-ray spectroscopic (EDX) analyses and high-resolution in situ heating observation of precision specimens is required. A method for the in situ observation of the interface reaction using an analytical transmission electron microscopy (TEM) and a specimen-heating holder was developed. The specimen holder used in this study was a direct-heating type having a fine tungsten wire heater. For sensitive analyses including an EDX map of composition changes during the interface reaction, a space toward the EDX detector with a take-off angle of 20° was made in the specimen holder. Samples were prepared by attaching a micro-sample directly to the heater using the focused ion beam (FIB) micro-sampling technique. It was confirmed that the sensitive EDX map and electron diffraction analyses were possible during the reaction, and that the resolution of this technique was of the order of 0.223 nm at 550°C.

Keywords     in situ observation, interface, nano-sized materials, reaction, energy dispersive x-ray spectroscopic analysis, focused ion beam

Received     12 February 2009, accepted 23 March 2009


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