Toshie Yaguchi

Structure of carbon nanotubes grown by microwave-plasma-enhanced chemical vapor deposition

Carbon nanotubes grown on a Ni substrate and an Fe–Ni–Cr alloy substrate by plasma-enhanced chemical vapor deposition were investigated by transmission electron microscope (TEM) and energy dispersive x-ray (EDX) analysis. TEM showed that the nanotubes on both substrates have a piled-cone structure with metal particles on top which determine the diameter of the nanotubes. Their diameter ranges from 60 to 80 nm. Moreover, EDX showed that the metal particles are composed of Ni when the nanotubes are grown on Ni substrate and of Fe and Ni in the case of the Fe–Ni–Cr alloy substrate.

CROSS-SECTIONAL SAMPLE PREPARATION BY FOCUSED ION BEAM : A REVIEW OF ION-SAMPLE INTERACTION

A focused ion beam (FIB) was applied for cross‐sectional sample preparation with both transmission electron microscopes (TEM) and scanning electron microscopes (SEM). The FIB sample preparation has the advantage of high positioning accuracy for cross sections. On the other hand, a broad ion beam (BIB) has been conventionally used for thinning TEM samples. Although both FIB and BIB use energetic ion beams, they are essentially different from each other in many aspects such as beam size, beam current density, incident angle of the beam with respect to cross sections, and beam scanning (i.e., dynamic or static beam). In this study, FIB cross‐sectioning is compared with BIB thinning. We review inherent characteristics such as positioning accuracy and uniformity of cross section, radiation damage, and beam heating. Discussion is held from a viewpoint of ion beam and sample interaction.

Observation of three-dimensional elemental distributions of a Si device using a 360°-tilt FIB and the cold field-emission STEM system

A technique for preparation of a pillar-shaped specimen and its multidirectional observation using a combination of a scanning transmission electron microscope (STEM) and a focused ion beam (FIB) instrument has been developed. The system employs an FIB/STEM compatible holder with a specially designed tilt mechanism, which allows the specimen to be tilted through 360 degrees [T. Yaguchi, M. Konno, T. Kamino, T. Hashimoto, T. Ohnishi, K. Umemura, K. Asayama, Microsc. Microanal. 9 (Suppl. 2) (2003) 118; T. Yaguchi, M. Konno, T. Kamino, T. Hashimoto, T. Ohnishi, M. Watanabe, Microsc. Microanal. 10 (Suppl. 2) (2004) 1030]. This technique was applied to obtain the three-dimensional (3D) elemental distributions around a contact plug of a Si device used in a 90-nm technology. A specimen containing only one contact plug was prepared in the shape of a pillar with a diameter of 200nm and a length of 5mum. Elemental maps were obtained from the pillar specimen using a 200-kV cold-field emission gun (FEG) STEM model HD-2300C equipped with the EDAX genesis X-ray energy-dispersive spectrometry (XEDS) system through a spectrum imaging technique. In this study, elemental distributions of minor elements with weak signals were enhanced by applying principal component analysis (PCA), which is a superior technique to extract weak signals from a large dataset. The distributions of elements, especially the metallization component Ti and minor dopant As in this particular device, were successfully extracted by PCA. Finally, the 3D elemental distributions around the contact plug could be visualized by reconstruction from the tilt series of maps.

Electron tomography of embedded semiconductor quantum dot

We performed an electron tomography for a single InAs quantum dot (QD) embedded in GaAs. A comprehensive three-dimensional image of indium distribution has been reconstructed by using a high-angle annular dark-field scanning transmission electron microscope. This was achieved by using a special nanopillar specimen prepared by a focused ion beam technique. The real structure of the embedded single QD has been found to have a complicated anisotropic structure reflecting the QD structure before being capped.

A FIB Micro-Sampling Technique and a Site Specific TEM Specimen Preparation Method

A FIB micro-sampling technique has been developed to facilitate TEM specimen preparation while allowing samples to remain intact. A deep trench is FIB-milled to remove a portion of the sample containing the region of interest. A micromanipulator is employed for the purpose of lifting out a small portion of the sample, i.e., the micro-sample. FIB assisted metal deposition is used to bond the micro-sample to the micromanipulator. The micro-sample is subsequently lifted out and mounted onto an edge of the micro-sample carrier using FIB assisted metal deposition. The micro-sample is then thinned to the thickness of about 0.1µm for TEM observation. All of the above steps are accomplished under vacuum in the same FIB system. This procedure is a reliable TEM specimen preparation technique when the evaluation or failure analysis of a specific site is required. Both cross sectional and plan view TEM specimen preparations are feasible with this technique. In addition, a technique to prepare TEM specimens from a specific site has also been developed. In this technique, an FIB system equipped with a FIB/TEM(STEM) compatible specimen holder is used for thinning of the samples, e.g., a micro-sample. The compatible specimen holder permits repeated alternating FIB milling and TEM(STEM) observation, enabling TEM specimen preparation from a specific site.

In-situ high-resolution electron microscopy study on a surface reconstruction of Au-deposited Si at very high temperatures

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.

Development of a technique for in situ high temperature TEM observation of catalysts in a highly moisturized air atmosphere.

To clarify the influence of moisture on the structural changes of heated nano materials, in situ high temperature transmission electron microscopy (TEM) has been carried out using a conventional analytical TEM combined with a gas injection-specimen heating holder. Air with high moisture content, above 94% relative humidity (RH), from a humidifier was directly injected onto the heated platinum catalyst dispersed on carbon black (Pt/CB), and the morphological changes of the specimens were observed at high magnification dynamically. The result of the experiment was compared with a result obtained from an experiment using air with a low moisture content, 34% RH. Active movement of the Pt particles, leading agglomeration and grain growth, occurred prior to degradation of the CB support at high moisture content. In contrast, the degradation of the CB support leading agglomeration and grain growth of the Pt particles occurred before the displacement of the Pt particles on the CB supports in a low humidity environment.

Formation and structural observation of cesium encapsulated single-walled carbon nanotubes

Cesium encapsulation inside single-walled carbon nanotubes (SWNTs) is for the first time realized by ion irradiation of SWNTs immersed in a magnetized alkali-metal plasma, the configuration of which is confirmed to comprise three varieties by field emission type transmission electron microscopy (FE-TEM) and scanning TEM (STEM) observation.

Electron microscopy of Mg2Ni-H alloy synthesized by reactive mechanical grinding

Abstract A new material containing 1.6 wt.% of hydrogen (Mg2NiH1.8) was synthesized by reactive mechanical grinding under hydrogen atmosphere by Orimo and Fujii [Orimo, S. and Fujii, H., J. Alloys and Compounds, 1996, 232, L16]. The microstructures of this alloy, Mg2NiH1.8, was investigated by high resolution transmission electron microscopy (HRTEM). It has been found from the HRTEM images that the texture mainly consists of nanocrystals of Mg2NiHx (x ≤ 0.3) with an average size of approximately 15 nm, and also found that heavily distorted regions exist around or between nanocrystals. The width or the thickness of these regions is thought to be approximately 1–2 nm. These results are consistent with the results deduced from the peak broadening of the X-ray diffraction pattern and magnetic analysis [Orimo S., Fujii, H. and Ikeda, K. Acta Metallurgica, accepted]. It is plausible to assume that these regions can contain an unexpected number of hydrogen atoms.

High-resolution environmental transmission electron microscopy: modeling and experimental verification

Quantitative modeling for high-resolution (phase contrast) gas cell environmental transmission electron microscopy (ETEM) imaging is presented in this paper. Concepts of pre-specimen scattering object (PreSO) and post-specimen scattering object (PoSO) are introduced to explain electron scattering caused by gas and window membranes associated with the gas environmental cell (E-cell). PreSO preserves the structural phase information and the effect can be evaluated by averaging the contrast transfer functions (CTFs) over random electron scattering. PoSO is treated as information loss and the unscattered electrons play a major role in determining the ETEM image quality. The theoretical model is compared and matched well with our systematic gas ETEM experimental results under various gas pressures. Extension of our approach to the aberration-corrected ETEM is discussed.