Abstract The focused ion beam(FIB) technique, developed for the microelectronics industry has become a major method for site specific transmission electron microscopy(TEM) specimen preparation in a wide range of materials[l]. The FIB lift-out technique has improved the specimen preparation procedures by removing complicated initial fabrication required prior to the FIB milling[2]. However, conventional FIB techniques are still having increased difficulty in meeting failure analysis needs from high technology industries such as microelectronics. We have developed a site specific TEM specimen preparation method using a combination of an FIB instrument and an intermediate voltage TEM equipped with a scanning attachment [3]. In this method, the specimen is mounted on an FIB-TEM compatible specimen holder, so that localization of the specific site can be carried out in the FIB and TEM using the same holder. The scanning electron imaging mode may be used to observe surface structures of the milled area, and the scanning transmission electron microscopy(STEM) mode may be used to observe structures inside of the milled surface.
Abstract The results of our previous studies revealed that the specimen heating holder with the heating elements of spiral shaped fine metal wires of high melting point enable us to observe high resolution transmission electron microscopy(TEM) images at elevated temperatures. In fact, the holder was applied for high resolution TEM study of a formation of SiC crystal at 1500°C and a surface reconstruction of Au deposited Si particle at 1000°C successfully. However, because the heating holder was single tilt type, there was a certain limitation in its application. In this paper, development of a double tilt specimen heating holder with a heating element of spiral shaped fine metal wire and its application for the study of microstructural changes of Si3N4 during sintering at very high temperature. Photograph of the newly developed double tilt specimen heating holder is shown in Fig. 1. The heating element is mounted on the electrically isolated tilting frame of the holder and the heating current is supplied via tilting rod which is also electrically isolated from other parts of the holder.
An environmental cell for high-temperature, high-resolution transmission electron microscopy of nanomaterials in near atmospheric pressures is developed. The developed environmental cell is a side-entry type with built-in specimen-heating element and micropressure gauge. The relationship between the cell condition and the quality of the transmission electron microscopic (TEM) image and the diffraction pattern was examined experimentally and theoretically. By using the cell consisting of two electron-transparent silicon nitride thin films as the window material, the gas pressure inside the environmental cell is continuously controlled from 10(-5) Pa to the atmospheric pressure in a high-vacuum TEM specimen chamber. TEM image resolutions of 0.23 and 0.31 nm were obtained using 15-nm-thick silicon nitride film windows with the pressure inside the cell being around 5 × 10(-5) and 1 × 10(4) Pa, respectively.
A gallium (Ga) focused-ion-beam (FIB) has been popularly used to prepare cross-sectional samples for transmission electron microscopes (TEMs) and scanning electron or ion microscopes. However, characteristics of the FIB-prepared cross sections such as ion concentration and radiation damage have been little studied either in theory or in experiment. In the present study, cross sections prepared by 30 keV Ga FIB are modeled using a combination of analytical and Monte Carlo methods to calculate the implanted Ga concentration. It is found that the Si/W layered sample is cross sectioned at grazing angles β≈2.5° and 6° for these layers, respectively. The implanted Ga ions for the cross-sectioned Si and W layers are concentrated very near their surfaces of <10 nm to yield the Ga concentrations CGa of about 4 and 9 at % for these layers, respectively. Although there is some differences in sample materials between the calculations and the experiments, the calculated CGa values for Si and W layers roughly agree with the experimental values for the magneto-optical disk TEM sample. This agreement firmly supports the present modeling of FIB-milled cross sections.
Abstract In-situ high-temperature high-resolution electron microscopy was applied to a study of the surface modification of Au-deposited Si. The experiment was carried out above the melting points of small particles of Au (approximately several nanometres in diameter) in a 300 kV high-resolution analytical transmission electron microscope equipped with a direct-heating-type specimen-heating holder in a vacuum of 4–6 × 10−6 Pa. Facet-unfacet transformation and reconstruction of the Si{111}, {001}, {211} and {311} surfaces induced by wetting of molten Au atoms have been observed at near-atomic resolution. It is concluded that molten Au atoms remove a surface amorphous layer on the Si surface, making the surface clean even in a non ultra-high vacuum.
Journal Article High Resolution Tem Observation and Eels Analysis of Carbon Nanotubes at Elevated Temperatures Get access T Yaguchi, T Yaguchi Hitachi Science Systems, Ltd., 882 Ichige, Hitachinaka, Ibaraki, 312-8504 Japan Search for other works by this author on: Oxford Academic Google Scholar T Sato, T Sato Hitachi Science Systems, Ltd., 882 Ichige, Hitachinaka, Ibaraki, 312-8504 Japan Search for other works by this author on: Oxford Academic Google Scholar T Kamino, T Kamino Hitachi Science Systems, Ltd., 882 Ichige, Hitachinaka, Ibaraki, 312-8504 Japan Search for other works by this author on: Oxford Academic Google Scholar T Hashimoto, T Hashimoto Hitachi High-technologies cooperation, 882 Ichige, Hitachinaka, Ibaraki, 312-8504 Japan Search for other works by this author on: Oxford Academic Google Scholar K Motomiya, K Motomiya Dept. of Geoscience and Technology, Tohoku Univ., Sendai, 980-8579, Japan Search for other works by this author on: Oxford Academic Google Scholar K Tohji, K Tohji Dept. of Geoscience and Technology, Tohoku Univ., Sendai, 980-8579, Japan Search for other works by this author on: Oxford Academic Google Scholar A Kasuya A Kasuya Center for Interdisciplinary Research, Tohoku Univ., Sendai, 980-8578, Japan Search for other works by this author on: Oxford Academic Google Scholar Microscopy and Microanalysis, Volume 8, Issue S02, 1 August 2002, Pages 1152–1153, https://doi.org/10.1017/S1431927602103837 Published: 01 August 2002
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