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MATERIALS TRANSACTIONS Vol. 51 (2010), No. 2

ISIJ International
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オンライン版ISSN: 1347-5320
冊子版ISSN: 1345-9678
発行機関: The Japan Institute of Metals and Materials

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MATERIALS TRANSACTIONS Vol. 51 (2010), No. 2

Conjugated Silicon–Based Polymer Resists for Nanotechnologies: EB and UV Meditated Degradation Processes in Polysilanes

Frantisek Schauer, Petr Schauer, Ivo Ku\\v{r}itka, Hua Bao

pp. 197-201

抄録

The comparison of the susceptibility of aryl-substituted polysilanes to the photodegradation by electron beam (EB) and UV radiation is examined on the prototypical material, poly[methyl(phenyl)silylene] (PMPSi). The main purpose of this paper is to compare the photoluminescence (PL) and cathodoluminescence (CL) after major degradation, predominantly in the long wavelength range of 400–600 nm, studying the disorder due to dangling bonds, conformational transformations and weak bonds created by the degradation process. The UV degradation was a completely reversible process, whereas the EB degradation process was only reversible, provided certain material specific level of degradation was not exceeded. This observation supports different paths and final states in both UV and EB degradations. The results serve for the optimization of polysilane nanoresists.

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Photonic Crystal Structure of Wing Scales in Sasakia Charonda Butterflies

Ji\\v{r}ina Mat\\v{e}jková-Plšková, Dalibor Jancik, Miroslav Mašlá\\v{n}, Satoshi Shiojiri, Makoto Shiojiri

pp. 202-208

抄録

The hindwings of the male Sasakia charonda charonda butterflies comprise iridescent purple-blue areas, iridescent white-pearl areas, yellow spots and red spots as well as brown background. We have examined the microstructure of their scales by scanning electron microscopy, for applying their photonic crystal structures to fine light manipulators such as reflection elements in laser diodes. The scales in the yellow spots, red spots and brown background have almost the same structure, which is an optical diffraction grating made of ridges with two cuticle layers. Their difference comes from the contained pigments. The scales in the iridescent purple-blue and white-pearl are also the same in structure. They have seven tilted cuticle layers lapped on the ridges, which also constitute a grating. The widths of the ridge and groove in the grating are different between scales of the two kinds. It is shown that the vivid iridescence is mainly attributed to multiple interferences caused between rays reflected from the seven cuticle layers with air gaps.

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Study of Thermal Stability of Ultrafine-Grained Copper by means of Electron Back Scattering Diffraction

Ond\\v{r}ej Man, Libor Pant\\v{e}lejev, Ludvík Kunz

pp. 209-213

抄録

Thermal stability of ultrafine-grained (UFG) structure of 99.9% pure copper produced by eight equal channel angular pressing (ECAP) passes was studied. The annealing experiments were conducted at 180°C in a tube furnace under argon as a covering gas. The dwell times were in the range of 10 min to 120 min. The electron backscattering diffraction (EBSD) analyses were performed before and after annealing at exactly the same area in order to quantify the degree of decomposition of the UFG structure. Definition of grain boundaries was based on the misorientation angle of 1°. More advanced analysis of the EBSD results based on a kernel average misorientation (KAM) parameter was performed. Inverse pole figure maps with included grain networks did not reveal any substantial changes of UFG microstructure due to annealing. Some shift in the KAM modus in comparison with the initial state was observed but its magnitude was found negligible. Also changes in texture were found to be minor. On the other hand the microhardness increases with increasing time of annealing.

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Mapping the Local Density of States by Very-Low-Energy Scanning Electron Microscope

Zuzana Pokorná, Lud\\v{e}k Frank

pp. 214-218

抄録

Reflection of very slow electrons from solid surfaces has been reported to be inversely proportional to the local density of electronic states coupled to the incident electron wave. The reflected electron flux at units of eV used as the image signal in a scanning electron microscope allows mapping of the local density of states at high spatial resolution. Good performance of the microscope at very low energies is enabled by introducing the beam-retarding immersion lens (the cathode lens) with a biased specimen serving as the cathode. Results of demonstration experiments on aluminum are provided.

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Structure and Electro-Optical Properties of Thin Films Grown by Alternate Atomic Layer Deposition of ZnO and Al2O3 on the Sapphire Substrate

Miran \\v{C}eh, Hsing-Chao Chen, Miin-Jang Chen, Jer-Ren Yang, Makoto Shiojiri

pp. 219-226

抄録

Al-doped ZnO thin films were prepared on the (0001) sapphire (c-Al2O3) substrates by atomic layer deposition (ALD) using alternating pulses of Zn(C2H5)2, Al(CH3)3 and H2O precursors and post-deposition high-temperature annealing. Photoluminescence (PL) spectroscopy showed that the threshold of stimulated emission decreases with increasing Al concentration, from 49.2 kW/cm2 of the ZnO film to 12.2 kW/cm2 of the ZnO film nominally containing 4% Al. This reduction is attributable to the increase in the optical scattering resulting from segregation of excess Al in heavily Al-doped ZnO films. The structure of these films was investigated by analytical scanning-transmission electron microscopy (STEM) as well as X-ray diffraction (XRD). It was revealed that a single crystal ZnO layer containing a small amount of Al is formed with the orientation relation with respect to the c-Al2O3: [0001]ZnO || [0001]Al2O3 and [01\\bar10]ZnO || [2\\bar1\\bar10]Al2O3, and that a polycrystalline ZnAl2O4 layer is formed between the ZnO layer and the c-Al2O3 substrate. The electron microscopy observation accounts for the results of the electro-optical experiments. The growth mechanism of the observed two layers is discussed.

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Gold Substitution Effect on Structure and Superconductivity Properties in Filled Skutterudite La(Pt1−xAux)4Ge12

Lingwei Li, Eitaro Sakada, Katsuhiko Nishimura

pp. 227-230

抄録

A series of single-phased La(Pt1−xAux)4Ge12 compounds were prepared by an arc-melting method. The crystal structure and basic superconductivity parameters have been systematically investigated by X-ray diffraction and by examining the temperature and field dependences of electrical resistivity, magnetization and heat capacity. The lattice parameter a increases and the superconducting transition temperature Tc decreases gradually with increasing Au content x. The low critical field Hc1(T) and the upper critical field Hc2(T) were estimated from the isothermal magnetization (M-H-T) and electrical transport (ρ-H-T) measurements, respectively. The evaluated Hc1(0) and Hc2(0) indicate a decrease tendency with increasing x, and enable us to deduce the coherence length ξ(0), penetration depth λ(0), Ginzburg-Landau parameter κ(0) and thermodynamic critical field Hc(0). The present results are compared with those of the related systems.

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Ultra-Fast Spectrometric Cathodoluminescence Scanning Microscopy for Materials Analysis

Hiroshi Saijo, Makoto Shiojiri

pp. 231-236

抄録

We have constructed a cathodoluminescence (CL) detection system that records the CL spectra emitted from each point raster-scanned by the incident electron probe in a conventional scanning electron microscope. The CL spectrum is detected by a 32 channel high-speed high-sensitive photoelectron multiplier array set behind the spectrometer. The shortest signal sampling time is 8 s for a frame of 512×512 pixels and all the imaging and spectroscopic signals are stored in two 8-megabyte files. Maximum image size is 2048×2048 pixels. The microscope displays a spectral accurate full color (whole spectrum) CL image, twenty-nine monochromic images and the spectrum of each pixel point in the corresponding secondary electron image. The spatial resolution of CL image reaches 25 nm by reducing the quantum noise and the phosphorescent delay effect using a slow signal sampling time of 40 s with a 6-keV incident electron probe. Some examples are demonstrated using SnO2-doped ZnO-Ba2O3 ceramics and photosensitive cyanine dyes.

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Profiling N-Type Dopants in Silicon

Miloš Hovorka, Filip Mika, Petr Mikulík, Lud\\v{e}k Frank

pp. 237-242

抄録

Variously doped n-type structures (dopant concentration between 1.5*1016 cm−3 and 1.5*1019 cm−3) on a lightly doped p-type silicon substrate (doped to 1.9*1015 cm−3) have been examined by a photoemission electron microscope equipped with a high-pass energy filter and by an ultra-high vacuum scanning low energy electron microscope. High contrast have been observed between the n-type areas and the p-type substrate and its monotone dependency on the doping level of structures has been manifested. The relation between the energy spectra of photoelectrons and the doping level has been studied, too. The scanning electron microscope images obtained with the landing energy of the primary beam in the low keV range exhibit contrasts similar to those appearing in the full threshold photoemission micrographs.

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UV Light Activation of TiO2-Doped SnO2 Thick Film for Sensing Ethanol at Room Temperature

Wen Zeng, Tianmo Liu, Zhongchang Wang

pp. 243-245

抄録

TiO2-doped SnO2 nanopowder is synthesized via a sol-gel method and characterized by atomic force microscopy and X-ray diffraction. Using this nanopowder, we have fabricated a novel semiconductor gas sensor that is sensitive to UV light illumination. We find that gas-sensing properties of TiO2-doped SnO2 sensor can be enhanced significantly under the exposure of UV light. The sensor exhibits a high sensitivity of 25 and rapid response-recovery times of 8 s and 24 s, respectively, under an ethanol gas of up to 100 ppm at room temperature (323 K). This suggests the possibility of development of a gas sensor for detecting ethanol at room temperature.

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Effect of Substrate Temperature, Biasing and Sputter Cleaning on the Structure and Properties of Nanostructured TiB2 Coatings on High Speed Steel

Prasonk Sricharoenchai, Nurot Panich, Patama Visuttipitukul, Panyawat Wangyao

pp. 246-252

抄録

Fabrication and development of TiB2-based nanostructured coatings was investigated in the present work. By varying the sputter-target power density, substrate temperature, deposition time, substrate-to-target distance, substrate biasing and substrate sputter cleaning, the relationship between the sputtered structure, properties and sputtering conditions were established. The experimental results showed that the target-to-substrate distance played a major role in the coating structure and properties. Sputter cleaning of substrate helped to improve TiB2 coating hardness and adhesion. The deposition process could be controlled to produce a TiB2 coating with both high hardness and good adhesion strength. This was achieved by introducing substrate sputter-cleaning and then biasing for the early stage of deposition, followed by deposition without biasing.

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Fabrication of ZnO Nanopillars by Atomic Layer Deposition

Mong-Kai Wu, Miin-Jang Chen, Feng-Yu Tsai, Jer-Ren Yang, Makoto Shiojiri

pp. 253-255

抄録

A new method was developed to fabricate high-quality ZnO nanopillars with good uniformity using atomic layer deposition (ALD). The ZnO island seeds were prepared on the (0001) sapphire by the initial 5∼20 ALD cycles at 180°C and then heat-treated at 900°C for 1 h. Afterwards, the ALD growth of ZnO at a temperature as high as 300°C proceeded preferentially on the ZnO island seeds over the sapphire substrate, leading to the formation of ZnO nanopillars. The average diameter and height of the nanopillars are about 60 nm and 50 nm, which can be effectively controlled by the numbers of initial ALD cycles and the following high-temperature ALD cycles, respectively. The ZnO nanopillars have high crystallinity with the [0001] orientation, and exhibit a significant ultraviolet luminescence at room temperature.

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Crystallization Studies on Se-Te-Cd Chalcogenide Glasses

M. A. Abdel Rahim, A. El-Korashy, S. Al-Ariki

pp. 256-260

抄録

The thermal crystallization behavior of bulk Se90−xTe10Cdx (x=0, 3, 9, and 15 at%) glasses was studied by differential thermal analysis, (DTA), under non-isothermal conditions. The glass transition temperature, (Tg), the onset crystallization temperature, (Tc), and the peak temperature of crystallization, (Tp), were found to be dependent on both the composition and the heating rates. From the dependence on the heating rates (α) of (Tg) and (Tp), the activation energy for the glass transition, (Et), and the activation energy for crystallization, (Ec), were calculated and their composition dependence is discussed. The crystalline phases resulting from DTA and scanning electron microscopy (SEM) have been identified using X-ray diffraction. The results indicate one dimensional growth from the surface to the inside for all the studied compositions. The kinetic parameters determined have made it possible to discuss the glass forming ability.

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Preparation of Pyrochlore Potassium Tantalate Thin Films on Ta/ITO Glass via Mild Hydrothermal Growth

T. Hashizume, A. Saiki, K. Terayama

pp. 261-264

抄録

Potassium tantalate with perovskite structure (KTaO3) is an incipient ferroelectric material that has promising functions in electromechanical and sensing sectors. Potassium tantalate with pyrochlore structure (K2Ta2O6) appears promising in a photocatalystic field. Potassium tantalate powders and bulks were fabricated at high temperature such as over 400°C from Ta2O5 and KOH. A sheet of tantalum was hard to react with potassium hydroxide in the mild hydrothermal condition at 100–150°C and low alkaline concentrations (0–2 M). Pyrochlore potassium tantalate film was synthesized with a mild hydrothermal method (100–150°C) at short reaction time by using a sputtered tantalum substrate on ITO glass. Synthesis of this film employed significantly low concentrations of KOH solution (0.1–1 M). The potassium tantalate film fabricated by the hydrothermal condition of 0.5 M-KOH solution, 100°C and 3 h reaction time was a smooth surface and became transparent. The particle size of this film was 150 nm.

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Very Low Energy Scanning Electron Microscopy of Free-Standing Ultrathin Films

Ilona Müllerová, Miloš Hovorka, Renáta Hanzlíková, Lud\\v{e}k Frank

pp. 265-270

抄録

Instrument and methodology is presented for very low energy scanning transmission electron microscopy. The detector system provides simultaneous acquisitions of total reflected and transmitted electron fluxes. Introductory experiments incorporated examination of ultrathin foils of gold, carbon and graphene flakes. Extremely sensitive thickness contrast obtained at units of eV is demonstrated. The phenomenon of electron transmissivity apparently exceeding 100% owing to the contribution of secondary electrons released near to the exit surface is described and discussed.

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Oxidation Resistance of CrAlN Films with Different Microstructures Prepared by Pulsed DC Balanced Magnetron Sputtering System

S. Khamseh, M. Nose, T. Kawabata, K. Matsuda, S. Ikeno

pp. 271-276

抄録

CrAlN films were prepared using a pulsed DC balanced reactive sputtering system under different N2/Ar ratios and pulse widths. We investigated the oxidation resistance of two CrAlN films with different microstructures; i) with a fcc-CrN structure, lower internal stress and moderate hardness, and ii) with a mixed structure of hcp-AlN and hcp-Cr2N phases, higher internal stress and super high hardness of 41 GPa. The CrAlN film (i) having the single fcc-CrN structure showed good oxidation resistance up to 900°C. The plastic hardness of this film increased to a maximum of 38.5 GPa at 900°C. In contrast, the CrAlN film (ii) with the mixed structure of hcp-AlN and hcp-Cr2N phases was stable up to 800°C. The plastic hardness of this film decreased gradually with annealing.

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Effect of Tin Addition on the Properties of Electroless Ni-P-Sn Ternary Deposits

Yong Zou, YanHai Cheng, Lin Cheng, Wen Liu

pp. 277-281

抄録

In this study, the ternary Ni-P-Sn alloy coatings were prepared using electroless plating, and the effect of tin element on amorphous formation and anticorrosive properties of deposits in different corrosion medium were investigated. The different tin contents in deposits could be obtained by adjusting the amount of NaSnO3·3H2O in plating bath. The X-ray results indicate that the small amount of tin addition can improve the formability of the amorphous phase. At the same time, the hardness of deposit decreases and the crystalline temperature shifts to lower temperature with increasing amount of Sn. The electrochemical corrosive experiments of deposits resulted that the addition tin improves the anticorrosion property in 3.5 mass% NaCl solution, but reduces the anticorrosion ability in sulfuric acid solution.

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Microstructure and Properties of TiAlN/a-C Nanocomposite Coatings Prepared by Reactive Sputtering

Masateru Nose, Tokimasa Kawabata, Sara Khamseh, Kenji Matsuda, K. Fujii, Susumu Ikeno, Wen-An Chiou

pp. 282-287

抄録

TiAlN/a-C nano-composite coatings were synthesized by a reactive co-sputtering process to investigate the effects of sputtering conditions on the microstructure and mechanical properties. Coating films were deposited on square plates of Si and high speed steel (ANSI M2) by the co-sputtering of TiAl (pulsed-d.c. sputtering) and C (d.c. sputtering) targets using a “Facing Target-type Sputtering” system at an atmosphere with a mixture of Ar and N2 but without hydrocarbon gas. The structure of the coatings was investigated by means of XRD, XPS and HRTEM with GIF (Gatan Imaging Filter). Mechanical properties of coating films were measured by a submicron indentation system.
Though TiAlN and a-C coatings showed hardness of about 32 and about 10 GPa, respectively, TiAlN/a-C coatings containing 4.6 at% of C showed higher hardness of 43 GPa. The energy filter images depicted that a change of contrast in the zero-loss image corresponded to nanometer-size of Ti agglomerates in Ti map. C1s spectrum in XPS analysis revealed that carbon in the coatings was bounded as C-C and C-N without bonding of Ti-C or Al-C. These results indicated that the TiAlN/a-C nano-composite coatings consisted of complicated mixture of nanocrystalline Ti-Al-N phase and a-C phase (including C-N bonding).

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Preparation and Thermoelectric Properties of Bi-Doped Mg2Si0.8Sn0.2 Compound

Weijun Luo, Meijun Yang, Fei Chen, Qiang Shen, Hongyi Jiang, Lianmeng Zhang

pp. 288-291

抄録

The Bi-doped Mg2Si0.8Sn0.2 single phase compound is prepared by a solid state reaction (SSR)-spark plasma sintering (SPS) method. The effect of the Bi content on the thermoelectric properties of the Bi-doped Mg2Si0.8Sn0.2 compound is mainly investigated. The results show that the thermoelectric properties of the obtained samples are sensitive to the Bi content. With the increase in Bi content, the electrical conductivity (σ) and Seebeck coefficient (α) of the samples are increased, while the thermal conductivity (κ) is decreased slightly between 300 K and 850 K. When the Bi content is greater than 3.0 at%, the sample shows a maximum figure of merit (ZT) value (1.17±0.05) at 850 K.

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Grain Contrast Imaging in UHV SLEEM

Šárka Mikmeková, Miloš Hovorka, Ilona Müllerová, Ond\\v{r}ej Man, Libor Pant\\v{e}lejev, Lud\\v{e}k Frank

pp. 292-296

抄録

Study of the grain structure in the equal channel angular pressing processed copper by means of the cathode lens equipped ultrahigh vacuum scanning low energy electron microscope is reported. The grain contrast was found achieving its maximum at electron energies below about 30 eV where it alternated its sign and exhibited dependence on electron energy specific for the grain orientation. The energy dependence of the electron reflectance seemed to be capable of serving as a fingerprint enabling determination of the crystalline orientation. In the cathode lens mode at hundreds of eV fine details of the microstructure are also observable including twins and low angle grain boundaries. This is explained by acquisition of high-angle backscattered slow electrons, normally not acquired in standard scanning electron microscopes. The very low energy electron reflectance is promising as an alternative to the EBSD method owing to its high resolution and fast data acquisition.

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Effect of Pulsed Electrical Field on Deposition of YSZ Thin Films in an Aqueous Solution

Atsushi Saiki, Takashi Hashizume, Kiyoshi Terayama

pp. 297-300

抄録

In this study we investigated YSZ thin film deposition from an aqueous solution by applying constant electrical field and the effect of a pulsed electrical field upon the growth condition of films. The precursor was an aqueous solution of Zr(NO2)3-2H2O, Y(NO3)3-6H2O, and 0.5 vol% NH3(aq). The thin film was deposited on the minus electrode side of the glass substrate, which was placed above the minus electrode with a gap distance of 48–530 μm. By applying the electrical field, the thin film was effectively deposited on glass substrates under an applied voltage of 2.5 V for 300 s at room temperature. The as-deposited film was amorphous, and a crystalline phase with a transparent and smooth surface can be obtained after annealing at 773 K for 3 h in air. When a pulse bias is applied to the electrical field, the film thickness, surface defects, and roughness were changed with the frequency. At 2 Hz, the film was fabricated effectively, and a thick film was obtained, but films with smoother and fewer defect surfaces were obtained in a range of about 10–100 Hz.

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HRTEM Observation of Metastable Phases in a Mg–15%Gd–6.4%Sc Alloy

Tokimasa Kawabata, Kenji Matsuda, Susumu Ikeno

pp. 301-304

抄録

The aging behavior of a ternary Mg–15%Gd–6.4%Sc (mass%) alloy was examined by high-resolution transmission electron microscopy. During the first stage of age hardening of the alloy, a contrast corresponding to a precursor of the β″ phase was observed predominantly. The β″ and β′ phases coexist in the second stage of hardening, up to the point of maximum hardness. In the over-aging stage, the spheroidal contrast of the β′ phase became longer along the ⟨1\\bar100⟩Mg direction. The addition of Sc to the Mg-Gd alloys is useful to clarify the precipitation behavior and contribution of the β″ and β′ phases to age hardening, as indicated by the two stage in the early stage of aging.

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Microstructure Evolution of a Novel Super304H Steel Aged at High Temperatures

Xin-mei Li, Yong Zou, Zhong-wen Zhang, Zeng-da Zou

pp. 305-309

抄録

The microstructure evolution of a novel Super304H stainless steel aged at different temperatures was investigated using various analysis methods. The results reveal that the microstructure of the Super304H steel after aging at 973–1623 K consists of the primary γ matrix and a small amount of precipitated phases. Grain size of γ-matrix shows a slow increase when the aging temperature is lower than 1373 K and it increases quickly when the aging temperature is beyond 1423 K. The lattice parameter of γ-matrix varies at different aging temperatures, and this variation corresponds to the phases precipitated or redissolved. The variation of grain size and precipitated phases can affect the performance of the steel when exposing to steam oxidation and be subject to creep at high temperatures.

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Effect of Silver Addition on the β′-Phase in Al-Mg-Si-Ag Alloy

J. Nakamura, K. Matsuda, T. Kawabata, T. Sato, Y. Nakamura, S. Ikeno

pp. 310-316

抄録

The metastable β′-phase that forms in an alloy with composition Al-1.0 mass% Mg2Si-0.5 mass% Ag, over aged at 523 K, has been investigated by transmission electron microscopy (TEM) in order to understand the effect of Ag-addition on the crystal structure of this phase. According to the results of analyses of selected area diffraction pattern, high resolution TEM (HRTEM), energy dispersive X-ray spectroscopy (EDS), the elemental maps by energy-filtered TEM (EFTEM) and high angle annular dark field scanning transmission electron microscopy (HAADF-STEM), this precipitate consists of Mg, Si and Ag, and has a hexagonal unit cell which is similar to that of β′ phase in Al-Mg-Si alloys without Ag. However, the unit cell a-axis of β′ with Ag was 0.69 nm, which is slightly smaller than the corresponding dimension in Ag-free β′ (0.71 nm). The bond overlap population (BOP) was also calculated for the bonding between atoms in the small cluster in the β′-phase by the discrete-variational (DV)-Xa method, suggesting the bonding in β′ with Ag was higher than in the Ag-free β′.

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Precipitation Kinetics in Supersaturated Al-2.0 at% Cu-1.0 at% Mg Alloy

N. Afify, A. Gaber, A. M. Abousehly, Y. M. Abou Deif

pp. 317-320

抄録

In Al-2.0 at%Cu-1.0 at%Mg alloy, fine-scale precipitates that occur during aging have been investigated by using differential scanning calorimetry (DSC) to search for the phase transition temperatures (formation and dissolution of precipitates). The microhardness measurements (HV) are used to correlate between the developed reaction peaks in DSC and the observed peaks in the microhardness (HV). The scanning electron microscopy (SEM) is utilized to examine the surface microstructure of the precipitated phases and to confirm the obtained results. During the aging treatment the supersaturation is gradually reduced. The strength increases when fine coherent and/or semicoherent precipitates nucleate. The precipitation kinetics can be characterized by analyzing the DSC curves. The kinetics of the early stage precipitates were found to be controlled by the migration of Cu and Mg atoms in the matrix. Whereas, the later precipitates as S″, S′ and S are controlled by diffusion of Mg and Cu in the alloy.

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First-Principles Study on Stability and Electronic Structures of Pt-Rh Bimetallic Nanoparticles

Koretaka Yuge, Takayuki Ichikawa, Jun Kawai

pp. 321-324

抄録

Energetic stability and electronic structures of Pt atoms in Pt-Rh nanoparticle is investigated by first-principles calculation. Pt atom energetically prefer surface sites (vertex, edge, and (100)) rather than subsurface and core site, which is attributed to lower Pt surface energy compared with Rh. Vertex of nanoparticle is the most favorable site for Pt atom, which has lowest coordination numbers. Band center of d-state electronic contribution for Pt atom measured from the Fermi energy exhibit negative dependence with respect to Pt coordination number. This can be attributed to positive dependence of second-order moment of density of states for the Pt d-band on the coordination number. Pt segregation to the surface is expected due mainly to contribution from Pt on-site segregation energy compared with weak ordering tendency of Pt-Rh unlike-atom pairs.

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Combined Effect of Pre-Straining and Pre-Aging on Bake-Hardening Behavior of an Al-0.6 mass%Mg-1.0 mass%Si Alloy

Tetsuya Masuda, Yasuo Takaki, Takeo Sakurai, Shoichi Hirosawa

pp. 325-332

抄録

The effect of pre-straining in combination with pre-aging on bake-hardening behavior of an Al-0.6 mass%Mg-1.0 mass%Si alloy was investigated by means of Vickers hardness test, electrical conductivity measurement, differential scanning calorimetry (DSC) and transmission electron microscopy (TEM). Hardness change and DSC analysis revealed that only 3% pre-strain suppresses the formation of clusters; i.e. cluster(1), during single aging below 343 K. On the other hand, by combining with pre-aging at 343 K, pre-straining was found to improve bake-hardening response during final aging at 443 K. TEM observation confirmed that the improvement of bake-hardening response by pre-straining is mainly due to the enhanced precipitation of β″ phase in the matrix. These results are explained by the consideration that dislocations induced by pre-straining reduce the concentration of quenched-in excess vacancies, resulting in both the suppressed clustering of solute atoms during pre-aging and the accelerated precipitation of the β″ phase from more supersaturated solute atoms in final aging.

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Transmission Electron Microscopy Study on the Grain Boundaries and Magnetic Domains in Nd–Fe–B Based Magnets

Kohei Sato, Yasukazu Murakami, Daisuke Shindo, Satoshi Hirosawa, Akira Yasuhara

pp. 333-340

抄録

The effect of post-sintering heat treatment on the coercivity of Nd–Fe–B based permanent magnets was studied by observing their crystallographic and magnetic microstructures. High-resolution transmission electron microscopy revealed meandering grain boundaries in the as-sintered state, and the smoothness of the boundaries was improved by the post-sintering heat treatment. Electron holography demonstrated that magnetization reversal occurred in a stepwise manner in individual grains in the specimen subjected to the post-sintering heat treatment, whereas reversal was occurred simultaneously in different grains in the as-sintered specimen.

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Effect of Cold Forging and Static Recrystallization on Microstructure and Mechanical Property of Magnesium Alloy AZ31

Jianzhong Liu, Tianmo Liu, Hanqi Yuan, Xiuling Shi, Zhongchang Wang

pp. 341-346

抄録

We perform a cold forging and annealing technique on Mg alloy AZ31 and investigate the impact on microstructure evolution and mechanical property. In particular, we focus on how twin and static recrystallization behave during the forging process followed by the annealing. Interestingly, we find that a large number of thick-lenticular {10\\bar12} twins emerge at initial stage of deformation and subsequently evolve into narrow-band {10\\bar11} and {30\\bar32} twins. The transformable twins are found to be crucial for inducing static recrystallization via providing recrystallization sites and refined grains. Moreover, the alloy forged at room temperature and annealed at 623 K is found to have optimal microstructure due to the complete recrystallization and therefore exhibit the highest micro-hardness, largest compressive strength, and most significantly enhanced compressive ratio. The improved mechanical properties are comparable or even superior to those of the alloy deformed using other techniques, rendering the cold forging a promising way for further tailing properties of Mg alloy.

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Effects of Grain Size on Hydrogen Environment Embrittlement of High Strength Low Alloy Steel in 45 MPa Gaseous Hydrogen

Koichi Takasawa, Yoru Wada, Ryoji Ishigaki, Rinzo Kayano

pp. 347-353

抄録

The effect of grain size on the susceptibility of high-strength low alloy steels to hydrogen environment embrittlement in a 45 MPa gaseous hydrogen atmosphere was examined in term of the hydrogen content penetrating the specimen during the deformation. Notch tensile tests were performed in a 45 MPa hydrogen environment using specimens with different prior austenite grain size numbers varying from 2.5 to 5.4. The hydrogen content was measured by thermal desorption analysis with a quadrupole mass spectrometer before and after the tensile test. The fracture stress of the notch tensile test increased with increasing grain size number; this showed that grain refinement was effective in reducing the susceptibility of the specimens to hydrogen environment embrittlement in a high-pressure hydrogen atmosphere. The addition of nickel did not affect the fracture stress. A remarkable increase in the content of diffusive hydrogen was observed after the notch tensile test. Assuming that part of the diffusive hydrogen desorbed from grain boundaries, it can be inferred that grain refinement can reduce the mass of hydrogen in the unit grain boundary area, and the susceptibility to high-pressure hydrogen environment embrittlement.

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Characteristic Variation of Niobium Powder Produced under Various Reduction Temperature and Amount of Reductant Addition

Jae-sik Yoon, Shoji Goto, Byung Il Kim

pp. 354-358

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This article was retracted. See the Notification.

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Wettability of Sodium Chloride Aqueous Solutions on SUS304 Stainless Steel with Current Flow

Rongguang Wang

pp. 359-365

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The wettability of NaCl solutions on SUS304 stainless steel was investigated under cathodic and anodic current. It was found that the contact angle became small when a cathodic current of 1.0 mA was applied, with a tendency of higher wettability for higher concentrations (between 0.01% and 0.1%). However, the decrease in the contact angle is irreversible even if the current is stopped or anodic current is applied. This phenomenon can be attributed to changes in the electric charge and the passive film at the interface.

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Separation and Determination of Zirconium Carbide in Zr50Al10Ni5Cu30 Bulk Metallic Glass Matrix Composites Containing ZrC Particles

Mikio Ishikuro, Kazuaki Wagatsuma

pp. 366-370

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The method of separation and determination of zirconium carbide in Zr50Al10Ni5Cu30 bulk metallic glass matrix composites containing zirconium carbide particles has been developed.
The zirconium carbide was not dissolved though the metallic glass specimen was dissolved with 6 kmol·m−3 hydrochloric acid of the room temperature.
After complete dissolution of the metallic glass matrix specimen with 6 kmol·m−3 hydrochloric acid of the room temperature, the undissolved zirconium carbide was separated by filtration with the membrane filter having the pore size of 0.2 μm. The separated zirconium carbide was fused with the potassium hydrogen sulfate in the platinum crucible. The concentrations of zirconium, copper, aluminum and nickel in the filtrate and the insoluble residue were determined respectively by inductively coupled plasma-optical emission spectrometry.
The zirconium concentration in the filtrate and the insoluble residue were constant irrespective of the dissolution time. Copper, aluminum and nickel were not detected in the insoluble zirconium carbide.
It was confirmed that the zirconium carbide in the Zr50Al10Ni5Cu30 bulk metallic glass matrix had been quantitatively separated and determined.

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Cold Crack Criterion for ADC12 Aluminum Alloy Die Casting

Shuxin Dong, Yasushi Iwata, Yoshio Sugiyama, Hiroaki Iwahori

pp. 371-376

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A cold crack criterion for JIS ADC12 aluminum alloy die casting is proposed. Through investigating the temperature dependence of the fracture strain of JIS ADC12 aluminum alloy die casting, it was found that the fracture strain features a turning point at a temperature, Tc (we called “critical temperature to the ductility”, about 573 K for the present composition), i.e. stays low while below Tc, rises rapidly to a high level beyond Tc. Focusing on this character of the fracture strain, we analyzed the equivalent plastic strain (εc) of the castings introduced below Tc in casting processes by thermal stress simulations and compared with the occurrence of cold cracks in the die casting experiments. It was found that the εc of the cracking positions in the castings exceeded, while the εc of the castings without crack were much lower than the fracture strain of JIS ADC12 aluminum alloy die casting below Tc. That is to say, the occurrence of the cold crack in a die casting can be judged by comparing the εc with the fracture strain below Tc. Based on this proposed criterion, it is possible to predict the appearance of the cold cracks in ADC12 die castings by thermal stress simulations.

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Fabrication of Beta-Ti-Type Ti-Nb-Ta-Zr (TNTZ) Wire with High-Ductility by Arc-Melt-Type Melt-Extraction Method

Takeshi Nagase, Takayoshi Nakano, Yukichi Umakoshi, Mitsuo Niinomi

pp. 377-380

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Beta-Ti-type Ti-30Nb-10Ta-5Zr (TNTZ) wires with high-ductility were developed using the arc-melt-type melt-extraction method. The continuous melt-extracted wire with very smooth surface and small fluctuations in the diameter realizes the high tensile strength and superior bending ductility of TNTZ alloy. The melt-extracted Beta-Ti wire shows the possibility for the use in biomedical applications. The arc-melt-type melt-extraction method is very effective for developing new Beta-Ti-based biomaterials.

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Heterogeneity along the Height in Disc Specimens of Graphite/Tungsten Powder Mixtures with Sub-Stoichiometric Carbon Atom Ratios Heated by Concentrated Solar Beam to 1600°C

Nobumitsu Shohoji, Teresa Magalhães, Fernando Almeida Costa Oliveira, Luís Guerra Rosa, Jorge Cruz Fernandes, José Rodríguez, Inmaculada Cañadas, Diego Martínez

pp. 381-388

抄録

Compositional heterogeneity along the thickness of compacted disc specimens of graphite/tungsten powder mixtures with sub-stoichiometric carbon atom ratios (0.35, 0.50 and 1.00) heated by concentrated solar beam to 1600°C was characterised by X-ray diffraction. Top surface of any examined test piece was consisted purely of mono-carbide WC while the bottom surface showed different constitution depending on the net initial C/W ratio of the test piece; almost pure metallic W for the C/W=0.35 specimen, dominant metallic W associated with small proportion of W2C for the C/W=0.50 and dominant W2C with trivial proportion of WC for the C/W=1.0. In the intermediate zone between the top and the bottom layers, the constitution held virtually constant depending on the nominal C/W ratio of the starting material: co-existing metallic W and W2C for the C/W=0.35, pure W2C for the C/W=0.50 and predominant WC with trace W2C for the C/W=1.00. Unlike for the top surface of the C/W=0.35 test piece heated in a solar furnace to 1900°C reported earlier, no evidence of formation of nano-meter scale WC whisker was detected for the top surface in any sample heated to 1600°C in the present work.

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Fitness-for-Service Evaluation of a Pipe with an Incomplete Penetration Flaw

Soo-Keun Park, Tae-Woon Nam

pp. 389-393

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Serious deformation on the pipe transporting hot water for heating was occurred by the cyclic heat impact during trial operation. Non-destructive inspection (RT, UT, MT, PT) and continuous indentation test were carried out to observe the flaw on the pipe and the variation of mechanical property for pipe material respectively. It was newly found by radiographic test that incomplete penetration flaws exist on every welding zone, which had been generated during the process of production. Ultrasonic test showed the length of incomplete penetration flaw reached 2/3 of circumference and its depth reached up to 60% of width. The mechanical property of material was found to be well uniform along the tube by the continuous indentation test. The incomplete penetration flaw was assumed to be a keen notch, and fitness for service was examined to observe the possibility of breakage crack and spread of crack in incomplete penetration area. As a result, it was observed to be usable under current operating condition, considering safety factor.

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Life Cycle Assessment of Copper Sulfide-Dispersed Lead-Free Bronze

Hidekazu Sueyoshi, Yuki Yamano, Yoshikazu Maeda, Kosaku Yamada

pp. 394-398

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Inventory analyses of manufacturing systems for Pb-bronze (JIS: CAC406), Pb-free bronze produced by Bi addition (JIS: CAC902) and copper sulfide-dispersed Pb-free bronze were assessed from the viewpoint of life cycle assessment. The results show that the manufacturing system of copper sulfide-dispersed Pb-free bronze significantly reduces such environmental impacts as energy consumption, global warming, acidification and resource consumption as compared with that of CAC902.

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Structure–Properties Relations in Friction Stir Spot Welded Low Carbon Steel Sheets for Light Weight Automobile Body

Seung-Wook Baek, Don-Hyun Choi, Chang-Yong Lee, Byung-Wook Ahn, Yun-Mo Yeon, Keun Song, Seung-Boo Jung

pp. 399-403

抄録

Low carbon steel plates were joined by friction stir spot welding (FSSW) with lap configuration. The tool penetration depth exerted a strong effect on the failure mode of the joined samples and a weak effect on the joint shear strength. With increasing tool penetration depth, and consequently with increasing depth of the tool shoulder pressing into the top sample, the failure mode in a lap-shear test changed from brittle to ductile and concentrated near the pinhole located away from the weld towards the base metal. No mechanically mixed layer was formed between the top and bottom plates at the weld nugget due to the limited tool penetration and the fact that the pin height of the welding tool was less than the steel plate thickness. The region under the pin exhibited a fully recrystallized microstructure, with grain growth and a different texture.

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Effects of Strontium Ion Doping on the Thermoelectric Properties of Dysprosium Cobalt Oxide

Hideki Hashimoto, Takafumi Kusunose, Tohru Sekino

pp. 404-407

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We prepared Dy1−xSrxCoO3−δ (x=0,0.025) ceramics and evaluated their thermoelectric performances at temperatures up to 873 K. The sample in which x=0.025 showed a higher electrical conductivity and a lower Seebeck coefficient than that in which x=0. Due to phonon scattering, the thermal conductivity of the x=0.025 sample was lower than that of the x=0 sample over the entire range measured although the carrier component of thermal conductivity of the x=0.025 sample was slightly larger than that of the x=0 sample. Due to the effects of an increase of the electrical conductivity and a decrease of the thermal conductivity, the sample in which x=0.025 showed the highest figure of merit, Z=5.7×10−5 K−1, at 773 K in the present system. These results imply that the partial substitution of a larger and lighter divalent cation for the trivalent cation of the A-site effectively enhanced the thermoelectric performance of the RCoO3 system.

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Influence of Post-Annealing on the Oxide Layer of AZ91 Mg Alloy Prepared by Plasma Electrolytic Oxidation

Duck Young Hwang, Young Gun Ko, Yong Min Kim, Bongyoung Yoo, Dong Hyuk Shin

pp. 408-412

抄録

The influence of the post-annealing (PA) treatment on plasma electrolytic oxidation (PEO) treated AZ91 Mg alloy was investigated and the dependence of the dehydration reaction on the PA temperature was also studied. In this study, a series of PA treatments were carried out on the coated samples at four different temperatures, i.e. 373, 423, 473, and 523 K for 10 h. In contrast to the sample without PA treatment, the samples annealed at temperatures higher than 423 K exhibited a significant difference in terms of surface morphology since the MgO content in the oxide layer increased with increasing PA temperature. With increasing PA temperature, the dehydration of Mg(OH)2 led to the increase in the relative amount of the MgO, which was a hard phase. From the nano-indentation results, the applied loads of the samples were seen to increase as PA temperatures increased. Moreover, the corrosion resistance of the sample annealed at 423 K was higher than that of the samples annealed at three different PA temperatures.

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Dissolution Kinetics of Complex Sulfides Using Acidophilic Microorganisms

Debabrata Pradhan, Dong Jin Kim, Gautam Roy Chaudhury, Jeong Soo Sohn, Seoung Won Lee

pp. 413-419

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Bioleaching studies were conducted to evaluate a complex sulfide concentrate using an acidophilic microorganism. The leaching kinetics were found to vary based on pulp density, Fe and pH. In addition, the leaching efficiency increased as the Fe(II) concentration increased up to 20 kg·m−3, after which it decreased due to an increase in iron precipitation. Furthermore, the bacterial activity was good based on observation of the iron oxidation rate and pH and Eh studies. The leaching efficiencies decreased below 2 and 5% (w/v) in the pH and pulp density studies, respectively. Furthermore, the XRD analyses revealed the presence of various product layers, while the SEM-EDX analyses showed partial contact between different sulfide minerals that resulted in formation of a galvanic couple. The dissolution rate followed a product diffusion model. The diffusivity of Fe(III) for chalcopyrite and sphalerite were calculated.

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