Polymer electrolyte fuel cells hold great potential for stationary and mobile applications due to high power density and low operating temperature. However, the structural changes during electrochemical reactions are not well understood. In this article, we detail the development of the sample holder equipped with gas injectors and electric conductors and its application to a membrane electrode assembly of a polymer electrolyte fuel cell. Hydrogen and oxygen gases were simultaneously sprayed on the surfaces of the anode and cathode catalysts of the membrane electrode assembly sample, respectively, and observation of the structural changes in the catalysts were simultaneously carried out along with measurement of the generated voltages.

Temperature is one of the most important factors affecting the state and behavior of materials. In situ heating transmission electron microscopy (TEM) is a powerful tool for understanding such temperature effects, and recently in situ heating TEM has made significant progress in terms of temperature available and resolution attained. This article briefly describes newly developed specimen-heating holders, which are useful in carrying out in situ heating TEM experiments. It then focuses on three main applications of these specimen holders: solid–solid reactions, solid–liquid reactions (including highresolution observation of a solid–liquid interface, size dependence of the melting temperatures of one-, two- and three-dimensionally reduced systems, size dependence of the contact angle of fine metal liquid, and wetting of Si with liquid Au or Al) and solid–gas reactions. These results illustrate the benefit of in situ heating TEM for providing fundamental information on temperature effects on materials.

One of the most important applications of a focused ion beam (FIB) workstation is preparing samples for transmission electron microscope (TEM) investigation. Samples must be uniformly thin to enable the analyzing beam of electrons to penetrate. The FIB enables not only the preparation of large, uniformly thick, sitespecific samples, but also the fabrication of lamellae used for TEM samples from composite samples consisting of inorganic and organic materials with very different properties. This article gives an overview of the variety of techniques that have been developed to prepare the final TEM specimen. The strengths of these methods as well as the problems, such as FIB-induced damage and Ga contamination, are illustrated with examples. Most recently, FIB-thinned lamellae were used to improve the spatial resolution of electron backscatter diffraction and energy-dispersive x-ray mapping. Examples are presented to illustrate the capabilities, difficulties, and future potential of FIB.

It is well known that analysis using transmission electron microscopes (TEM) yields very high resolution images of thin specimens. However, the applicability of TEM analysis is not universal due to the requirement that a high internal vacuum is required. This high vacuum precludes the TEM study of living specimens or specimens in a gas or liquid environment. In order to tackle this problem, L. Marton of Universite Libre in Brussels, Belgium was the first to design an environmental cell (E-cell) in 1935 that was sealed in the tip of a TEMsample holder [1]. Marton's design included two 0.5 μm aluminum foils as upper and lower windows sandwiching a biological sample to sustain a living environment. The electron transparent windows permitted the confined biological objects to be imaged in TEMmode. Since then, environmental TEM (E-TEM) has received increasing attention from biological scientists and eventually from materials scientists as well.

The processes of phase transformation in individual nanoparticles of FePt and FePtCu synthesized by the reverse micelle method, which are chemically homogeneous and monodisperse, have been investigated by an in-situ HREM observation in a FE-TEM. Polycrystalline FePt particles, initially of chemically disordered face-centered cubic phase (A1) were reconstructed into A1 single crystals between 25 °C and 650 °C, followed by phase transformation from A1 to chemically ordered face-centered tetragonal phase (L10) which began between 650 °C and 680 °C. The coalescence began concurrently with phase transformation, i. e., between 650 °C and 680 °C. They turned to be a round-shaped L10 particle between 680 °C and 720 °C. The single crystal formation, the phase transformation from A1 to L10, the coalescence and the round-shaped particle formation were also observed in the FePtCu nanoparticles. The temperatures of single crystal formation, phase transformation (and coalescence) and round-shaped particle formation of the FePtCu nanoparticles were between 25 °C and 500 °C, between 550 °C and 600 °C and between 600 °C and 650 °C, respectively. These temperatures were substantially lower than those for the FePt nanoparticles.

In characterization or failure analysis of new materials and semiconductor devices, the requirements for three dimensional observation and analysis are rapidly increasing. We discuss techniques for specimen preparation, three-dimensional observation, and elemental analysis of semiconductor devices that we developed using a system consisting of a dedicated focused ion beam (FIB) instrument and a scanning transmission electron microscope (STEM). The system utilizes a FIB-STEM compatible specimen holder with a specially designed rotation mechanism, which allows 360° rotation of a specimen on a conical stage (needle stub) around the ion beam axis of the FIB system and 360° rotation perpendicular to the electron beam in the STEM. A piece of sample (micro sample) is extracted from a specific-site by the micro-sampling technique and mounted on the needle stub. Instruments used in the study are the Hitachi FB-2100 FIB system with a micro-sampling attachment and the HD-2300 field emission 200kV STEM.

Extended abstract of a paper presented at Microscopy and Microanalysis 2004 in Savannah, Georgia, USA, August 1–5, 2004.

Extended abstract of a paper presented at Microscopy and Microanalysis 2004 in Savannah, Georgia, USA, August 1–5, 2004.

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.