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In this study, we discuss a method for cross-sectional thin specimen preparation from a specific site using a combination of a focused ion beam (FIB) system and an intermediate voltage transmission electron microscope (TEM). A FIB-TEM compatible specimen holder was newly developed for the method. The thinning of the specimen using the FIB system and the observation of inside structure of the ion milled area in a TEM to localize a specific site were alternately carried out. The TEM fitted with both scanning transmitted electron detector and secondary electron detector enabled us to localize the specific site in a halfway milled specimen with the positional accuracy of better than 0.1 µm. The method was applied to the characterization of a precipitate in a steel. A submicron large precipitate was thinned exactly at its center for the characterization by a high-resolution electron microscopy and an elemental mapping.
A focused ion beam (FIB) technique was applied to cross-sectional specimen preparation to observe an interface between a plasma sprayed coating and an aluminum (Al) substrate by transmission electron microscopy (TEM). The surface of the sprayed coating film has a roughness of several tens of microns. Sputter rates for the coating film and the substrate are greatly different. The rough surface and the difference in sputter rate cause problems in making TEM specimens with smooth side walls. The top surface of the coating film was planerized by the FIB before fabricating the TEM specimen. The interfaces were investigated by TEM and energy-dispersive X-ray (EDX) analysis. The TEM observation revealed that there is a 10 nm thick amorphous layer at the interface between the coating film and substrate. The coating film consists of two kinds of sublayers with bright and dark contrast. The bright contrast sublayers were amorphous layers with thickness of 2~10 nm. The Al/Fe X-ray intensity ratio was larger in bright contrast sublayers than that in dark contrast sublayers.
A technique to cut out small pieces of samples directly from chips or wafer samples in a focused ion beam (FIB) system has been developed. A deep trench is FIB milled to cut out a small, wedge-shaped portion of the sample from the area of interest A micromanipulator with tungsten (W) probe is employed for lifting the micro-sample. The lifted micro-sample is then mounted on a carrier to prepare electron transparent thin foil specimens for transmission electron microscope (TEM) observation. We have also developed a method for site-specific TEM specimen preparation. In this method, FIB system and TEM/scanning transmission electron microscope (STEM) equipped with secondary electron (SE) detector are employed. An FIB–TEM/STEM compatible specimen holder has also been developed so that a specimen can be milled in the FIB system and observed in a TEM/STEM without remounting the specimen. STEM and scanning electron microscopy (SEM) images are used for locating a specific site on a specimen. SEM image observation at an accelerating voltage of 200kV enabled us to observe not only surface structures but also inner structures near the surface of a cross section with depth of field of around 1 micrometer. The STEM image allows the observation of inner structures of 3-5 micrometer thick specimens. Milling of a specimen by FIB and observation of the milled sample by SEM and STEM are alternately carried out until an electron transparent thin foil specimen is obtained. The position accuracy of the method in TEM specimen preparation is approximately 100nm.
A new method for transmission electron microscope (TEM) specimen preparation using a focused
ion beam (FIB) system that results in a lower rate of gallium (Ga) implantation has been developed. The
method was applied to structural and analytical studies of composite materials such as silicon (Si)-devices and
magneto-optical disk. To protect the specimens against Ga ion irradiation, amorphous tungsten (W) was
deposited on the surface of the specimen prior to FIB milling. The deposition was quite effective in reducing
the Ga implantation rate, and energy-dispersive X-ray (EDX) analysis of these specimens detected 0.3Ð1.5% Ga
incorporated in the thinned area. FIB milling times for these specimens were 1.5Ð2 hr. Although the milling rate was high, all the materials were properly prepared for TEM study,
and clear crystal lattice images were observed on all specimens.
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