We discuss the advantages of V2O5-P2O5-Fe2O3-Li2O glass-ceramics as a cathode for lithium-ion batteries. The glass was prepared by using the melt quenching method. The glass-ceramics were produced by heat treatment in air. LixV2O5 crystal was only confirmed as the precipitated phase and the degree of crystallinity was approximately 90%. The total capacity of the glass-ceramics was 340 Ah/kg at a C/20 rate for 1.5-4.2 V cutoff ranges. It is 10% higher than the capacity of the glass cathode. Moreover, the charge-discharge performance of the glass-ceramics cathode showed good cycleability similar to that of the glass. The glass-ceramics had a 83% capacity retention after 40 cycles. These results show that glass-ceramics is a potential candidate for lithium-ion cathode materials.

Scanning confocal electron microscopy (SCEM) is a new imaging technique that is capable of depth sectioning with nanometer-scale depth resolution. However, the depth resolution in the optical axis direction (Z) is worse than might be expected on the basis of the vertical electron probe size calculated with the existence of spherical aberration. To investigate the origin of the degradation, the effects of electron energy loss and chromatic aberration on the depth resolution of annular dark-field SCEM were studied through both experiments and computational simulations. The simulation results obtained by taking these two factors into consideration coincided well with those obtained by experiments, which proved that electron energy loss and chromatic aberration cause blurs at the overfocus sides of the Z-direction intensity profiles rather than degrade the depth resolution much. In addition, a deconvolution method using a simulated point spread function, which combined two Gaussian functions, was adopted to process the XZ-slice images obtained both from experiments and simulations. As a result, the blurs induced by energy loss and chromatic aberration were successfully removed, and there was also about 30% improvement in the depth resolution in deconvoluting the experimental XZ-slice image.

As deposited amorphous and crystallized thin films of Ti 37.5% Si alloy deposited by pulsed laser ablation technique were irradiated with 100 keV Xe+ ion beam to an ion fluence of about 1016 ions-cm−2. Transmission electron microscopy revealed that the implanted Xe formed amorphous nanosized clusters in both cases. The Xe ion-irradiation favors nucleation of a fcc-Ti(Si) phase in amorphous films. However, in crystalline films, irradiation leads to dissolution of the Ti5Si3 intermetallic phase. In both cases, Xe irradiation leads to the evolution of similar microstructures. Our results point to the pivotal role of nucleation in the evolution of the microstructure under the condition of ion implantation.

We evaluated the depth resolution of annular dark-field (ADF) scanning confocal electron microscopy (SCEM) with a stage-scanning system by observation of nanoparticles. ADF-SCEM is a three-dimensional (3D) imaging technique that we recently proposed. An ADF-SCEM instrument involves a pinhole aperture before a detector for rejecting electrons from the out-of-focal plane in a specimen and an annular aperture under the specimen for collecting only scattered electrons. The stage-scanning system enables us to directly obtain optical slice images perpendicular and parallel to an optical axis at a desired position. In particular, the parallel slices visualize the elongation of nanoparticles along the optical axis, which depends on the depth resolution. ADF-SCEM effectively reduced the elongation length of the nanoparticles sufficiently to demonstrate depth sectioning, in comparison with scanning transmission electron microscopy and bright-field SCEM. The experimentally obtained length was nearly equal to the theoretically estimated one from the probe size considering the experimental conditions. Furthermore, we applied this ADF-SCEM technique to analysis of the 3D position of catalytic nanoparticles on carbon nanostructures.

A new TEM sample preparation technique using electron-beam-induced deposition combined with low-energy ion milling was used to fabricate for two different shapes of sample, conical and plate. High-quality HREM images can be obtained from samples prepared by this technique. A desired sample position can be obtained with high accuracy, and the total sample preparation time can be much less than conventional techniques. Because the gas deposition system used can easily be integrated in a conventional SEM, the method can be performed in any laboratory equipped with a SEM and an ion milling machine.

The process of electron-beam-induced deposition (EBID) was simulated with a dynamic Monte Carlo profile simulator, and the growth of carbon, silver, and tungsten supertips was investigated to study the dependence of material composition on the spatial resolution of EBID. Because light atoms have a smaller scattering angle and a longer mean free path, the carbon supertip has the smallest lateral size and the highest aspect ratio of a bottom tip compared to silver and tungsten supertips. Thus the best spatial resolution of EBID can be achieved on materials of low atomic number. The calculation also indicated a significant contribution of primary electrons to the growth of a supertip in EBID, which is consistent with the experimental observations. These results lead to a more comprehensive understanding of EBID, which is a complex interaction process between electrons and solids.

Initial results from an ultrahigh-vacuum (UHV) third-order spherical aberration (Cs) corrector for a dedicated scanning transmission electron microscopy, installed at the National Institute for Materials Science, Tsukuba, Japan, are presented here. The Cs corrector is of the dual hexapole type. It is UHV compatible and was installed on a UHV column. The Ronchigram obtained showed an extension of the sweet spot area, indicating a successful correction of the third-order spherical aberration Cs. The power spectrum of an image demonstrated that the resolution achieved was 0.1 nm. A first trial of the direct measurement of the fifth-order spherical aberration C5 was also attempted on the basis of a Ronchigram fringe measurement.

Thin film specimens of austenitic 304 stainless steel implanted with 100 keV Xe ions at room temperature were investigated. Microstructural evolution and phase transformation were characterized and analyzed in situ with conventional and high-resolution transmission electron microscopy. The phase transformation in a sequence from austenitic γ face-centered cubic (fcc) to hexagonal close-packed (hcp), and then to a martensitic α body-centered cubic (bcc) structure was observed in the implanted specimens. The fraction of the induced α(bcc) phase increased with increasing Xe ion fluence. Orientation relationships between the induced α(bcc) phase and austenitic γ(fcc) matrix were determined to be (011)α//(111)γ and [111]α//[011]γ. The relationship was independent of the induced process of the martensitic phase transformation for austenitic 304 stainless steel specimen, in agreement with the Kurdjumov–Sachs (K-S) rule. It is suggested that the phase transformation is induced mainly by the formation of the highly pressurized Xe precipitates, which generate a large stress level in stainless steels.

An H-terminated-surface conductive layer of B-doped diamond on a (111) surface was used to fabricate a metal insulator semiconductor field effect transistor (MISFET) using CaF2, SiO2 or Al2O3 gate insulators and a Cu-metal stacked gate. For a CaF2 gate, the maximum measured drain current (Idmax) was 240 mA/mm and the maximum transconductance (gm) was 70 mS/mm, and the cut-off frequency of 4 GHz was obtained. For a SiO2 gate, Idmax and gm were 75 mA/mm and 24 mS/mm, respectively, and for an Al2O3 gate, these characteristics were 86 mA/mm and 15 mS/mm, respectively. These values are among the highest reported DC and RF characteristics for a diamond homoepitaxial (111) MISFET.

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.

The reduction mechanism of particle surface oxide films on Al–Mg alloy specimens sintered by the pulse electric current sintering (PECS) process was investigated via transmission electron microscopy, energy dispersive x-ray spectroscopy, and thermodynamic calculation. The reduction products were either MgAl2O4 or MgO or both, which is dependent on the sintering temperature and Mg content in Al–Mg alloy. Comparing the experimental temperature of the reduction products with that from thermodynamic calculation, it was suggested that the temperature at interfaces between particles was higher than that inside particles. This difference of temperature enhanced reduction of surface oxide films of Al–Mg alloy powders and hence accelerated the sintering in the PECS process.

About 1 monolayer of palladium was deposited onto a silicon (111) 7 × 7 surface at a temperature of about 550 K inside an ultrahigh vacuum transmission electron microscope, resulting in formation of Pd2Si nanoislands and a 1 × 1 surface layer. Pd clusters created from an excess of Pd atoms on the 1 × 1 surface layer were directly observed by in situ plan view high-resolution transmission electron microscopy. When an objective aperture was introduced so that electron diffractions less than 0.20 nm were filtered out, the lattice structure of the 1 × 1 surface with 0.33 nm spacing and the Pd clusters with a trimer shape were visualized. It was found that image contrast of the 1 × 1 lattice on the specific height terraces disappeared, and thereby an atomic structure of the Pd clusters was clearly observed. The appearance and disappearance of the 1 × 1 lattice was explained by the effect of the kinematical diffraction. It was identified that a Pd cluster was composed of three Pd atoms without a centered Si atom, which is consistent with the model proposed previously. The feature of the Pd clusters stuck at the surface step was also described.

Real space, high-resolution transmission electron microscopy observations of Xe confined in nanometer size faceted cavities in Al yield information on both the inert gas and the matrix in which it is confined. At room temperature, Xe in such cavities can be liquid or an fcc solid. In larger cavities, Xe within can undergo melting and recrystallization. The Al surface energy can be deduced from the largest Xe nanocrystal at 300 K by setting the corresponding calculated Laplace pressure equal to the equilibrium pressure for melting of Xe, obtained from empirical bulk compression data. These surface energy values are 1.05 J m-2 for {111} facets and 1.10 Jm-2 for {200} facets. Because of the weak interactions, these values correspond to the surface tensions for Al at 300 K.

At room temperature, fluid Xe confined in small faceted cavities in aluminum has up to three ordered layers of Xe atoms at the Al interface. Conceptually in a three-dimensionally confined system of sufficiently small size, complete three-dimensional ordering of the fluid may occur. Molecular dynamics simulations have revealed that such ordering would result in fluid Xe confined to a small tetragonal volume solidifying as a body-centered cubic phase on compression.