An in situ heating TEM analysis method for an interface reaction.
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 degrees 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 degrees C.
Tanigaki
Toshiaki
T
Hitachi High-Tech Manufacturing & Service Corporation, 1040 Ichige, Hitachinaka, Ibaraki, Japan. tanigaki-toshiaki@naka.hitachi-hitec.com
Ito
Katsuji
K
Nagakubo
Yasuhira
Y
Asakawa
Takayuki
T
Kanemura
Takashi
T