Development of a gas injection/specimen heating holder for use with transmission electron microscope

Author： Kamino Takeo Yaguchi Toshie Konno Mitsuru Watabe Akira Marukawa Tomotaka Mima Takayuki Kuroda Kotaro Saka Hiroyasu Arai Shigeo Makino Hiroshi Suzuki Yoshinao Kishita Keisuke

Publisher： Oxford University Press

ISSN： 0022-0744

Source： Journal of Electron Microscopy, Vol.54, Iss.6, 2005-12, pp. : 497-503

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Abstract

A new gas injection/specimen heating holder is developed for the purpose of in situ observation of gas reaction of materials at high temperatures in a transmission electron microscope at near-atomic resolution. A fine tungsten wire is employed as a heating element of the holder and a battery is used as the power source. Gas was injected onto specimens in the form of particles lying on the heating element via a nozzle. The maximum pressure near specimens was middle of 10⁻² Pa, while the pressure in the electron-gun chamber was kept to 2 × 10⁻⁴ Pa. This gas injection/specimen heating holder was applied to observe solid–gas reactions. The reactions observed include oxidation of pure In into In2O3, reduction of SiO2 into Si and re-oxidation of Si into SiO2.