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ONLINE ISSN: 1347-5320

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The Japan Institute of Metals and Materials

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MATERIALS TRANSACTIONS
Vol. 52 (2011), No. 4

MATERIALS TRANSACTIONS Vol. 52 (2011), No. 4

Phase Transformation and Lattice-Strain Formation in Ti_1.0V_1.1Mn_0.9 during First Absorption and Desorption

Saishun Yamazaki, Jin Nakamura, Kouji Sakaki, Yumiko Nakamura, Etsuo Akiba

pp. 586-590

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Phase Transformation and Lattice-Strain Formation in Ti_1.0V_1.1Mn_0.9 during First Absorption and Desorption

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DOI:10.2320/matertrans.MA201004

Abstract

We used powder X-ray diffraction (XRD) and Rietveld refinement to study phase transformation and the lattice strain introduced into each hydride phase of Ti_1.0V_1.1Mn_0.9 during first absorption and desorption. Hydrogenation proceeded from a solid-solution phase to a dihydride phase via a monohydride phase. Each single-phase region was observed beside two clear plateau regions on the pressure–composition (P–C) isotherm. In contrast, the desorption P–C isotherm showed only one clear plateau, corresponding to a two-phase region of the dihydride and the monohydride. The plateau was connected to a two-phase region of the monohydride and a solid-solution phase, and to another region of solid-solution phases. The monohydride single-phase region was not clearly observed during desorption. Isotropic lattice strain was introduced, and increased with phase transformation during the first absorption. The strain increased further in the subsequent phase transformation during desorption, particularly upon formation of a solid-solution phase.
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Hydrogen Vibrational Excitation Spectra of CaF₂-Type Metal Hydrides Synthesized from Ti-Based BCC Solid Solution Alloys

Yumiko Nakamura, Takashi Kamiyama, Etsuo Akiba

pp. 591-594

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Hydrogen Vibrational Excitation Spectra of CaF₂-Type Metal Hydrides Synthesized from Ti-Based BCC Solid Solution Alloys

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DOI:10.2320/matertrans.MA201014

Abstract

Hydrogen vibrational excitation was studied for CaF₂-type metal hydrides synthesized from Ti-based BCC solid solution alloys using inelastic incoherent neutron scattering (IINS). Ti_1.0V_1.1Mn_0.9H_4.5 and Ti_0.7V_1.2Cr_1.1H_4.8 showed IINS spectra similar to that reported for TiH₂. The first three peaks were isolated but the higher excitation peaks were not clear. Analysis of the spectra using curve-fitting with Gauss functions revealed that the hydrogen vibration of Ti_1.0V_1.1Mn_0.9H_4.5 is harmonic but that of the Ti_0.7V_1.2Cr_1.1H_4.8 is deviated from harmonic, which reflects a trumpet-type potential. The relation between metal-hydrogen distance and vibrational excitation energy for the above two hydrides and Ti_1.1Cr_1.4Mo_0.3H_∼5 was compared with a series of CaF₂-type binary metal hydrides. All the hydrides of the Ti-based alloys had lower vibrational excitation energies than the binary metal hydrides for the corresponding metal-hydrogen distances.
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In Situ X-ray Diffraction Measurements of Aluminum Pulverization prior to the Hydrogenation Reaction

Hiroyuki Saitoh, Yuka Okajima, Yasuhiro Yoneda, Akihiko Machida, Yoshinori Katayama, Katsutoshi Aoki

pp. 595-597

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In Situ X-ray Diffraction Measurements of Aluminum Pulverization prior to the Hydrogenation Reaction

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DOI:10.2320/matertrans.MA201011

Abstract

The hydrogenation process of aluminum, especially pulverization of aluminum prior to the hydrogenation reaction was investigated by in situ synchrotron radiation X-ray diffraction measurements at high pressure and high temperature. Changes in the crystal grain sizes during the hydrogenation process were observed using the angle dispersive method, while weak Bragg peaks from aluminum and AlH₃ with small X-ray scattering factors were detected using focused monochromatic X-rays as the incident beam. The in situ measurement system monitored the pulverization of aluminum at several pressure-temperature conditions where AlH₃ was thermodynamically stable.
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3. Effect of Internal Strain on Martensitic Transformations in NiTi Shape Memory Alloys MATERIALS TRANSACTIONS Vol.52(2011), No.3
Structural and Hydrogen Desorption Properties of Aluminum Hydride

Kazutaka Ikeda, Hidetoshi Ohshita, Naokatsu Kaneko, Junrong Zhang, Masao Yonemura, Toshiya Otomo, Kentaro Suzuya, Hiroshi Yukawa, Masahiko Morinaga, Hai-Wen Li, Satoshi Semboshi, Shin-ichi Orimo

pp. 598-601

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Structural and Hydrogen Desorption Properties of Aluminum Hydride

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DOI:10.2320/matertrans.MA201019

Abstract

The structural and hydrogen/deuterium desorption properties of AlH₃/AlD₃ were investigated by Raman spectroscopy, high-intensity X-ray/neutron diffraction, and thermogravimetric analysis. The latter revealed that more than 9.6 mass% of hydrogen/18.1 mass% of deuterium desorbs from AlH₃/AlD₃, respectively. The presence of χ-Al₂O₃ on the surface may prevent the hydrogen/deuterium desorption reaction of AlH₃/AlD₃ to Al at room temperature.
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3. Effect of Internal Strain on Martensitic Transformations in NiTi Shape Memory Alloys MATERIALS TRANSACTIONS Vol.52(2011), No.3
Hydrogenation of Al₃Ti at High Pressure and High Temperature

Hiroyuki Saitoh, Akihiko Machida, Yoshinori Katayama, Katsutoshi Aoki

pp. 602-604

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Hydrogenation of Al₃Ti at High Pressure and High Temperature

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DOI:10.2320/matertrans.MA201006

Abstract

An Al₃Ti alloy was immersed in hydrogen at high pressures and high temperatures. An anomalous expansion of the Al₃Ti metal lattice was observed by in situ powder X-ray diffraction measurements at 625°C and 10 GPa, suggesting that Al₃Ti is hydrogenated to form Al₃TiH_x. The hydrogen content is roughly estimated to be x∼0.4. However, the formed hydride phase is dehydrogenated during depressurization, and cannot be recovered at ambient conditions.
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Aging of Cu-3 at% Ti Alloys in Hydrogen Atmosphere: Influence of Hydrogen Pressure on Strength and Electrical Conductivity

Satoshi Semboshi, Tomoya Nishida, Hiroshi Numakura

pp. 605-609

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Aging of Cu-3 at% Ti Alloys in Hydrogen Atmosphere: Influence of Hydrogen Pressure on Strength and Electrical Conductivity

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DOI:10.2320/matertrans.D-MA201031

Abstract

The influence of hydrogen pressure during isothermal aging on the mechanical strength, electrical conductivity, and microstructure of Cu-3 at% Ti alloys was investigated under various hydrogen pressures from 0 to 0.8 MPa. The variation of hardness with aging time was not significantly different among all specimens aged under the hydrogen pressures. This is because the hardness is improved primarily by the precipitation strengthening of Cu₄Ti particles, which is less affected by hydrogen pressure. The electrical conductivity increased more significantly for specimens aged under higher hydrogen pressure, due to a rapid reduction in the concentration of Ti dissolved in the matrix, which is attributed to the accelerated formation of TiH₂. The conductivity at peak-hardness was improved by a factor of approximately 1.4 in the specimens aged at both 773 and 723 K under the highest hydrogen pressure, compared to that for the specimen aged in vacuum. Therefore, aging under high hydrogen pressure assisted in the significant improvement of both strength and electrical conductivity.
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Ta-W Alloy for Hydrogen Permeable Membranes

H. Yukawa, T. Nambu, Y. Matsumoto

pp. 610-613

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Ta-W Alloy for Hydrogen Permeable Membranes

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DOI:10.2320/matertrans.MA201007

Abstract

The alloying effects of tungsten on the hydrogen solubility, the resistance to hydrogen embrittlement and the hydrogen permeability are investigated for Ta-based hydrogen permeable membranes. The hydrogen solubility is found to decrease by the addition of tungsten into tantalum or by increasing the temperature. It is also found that the mechanical properties (i.e., strength and ductility) for Ta-based alloy is better than that for Nb-based alloy in hydrogen atmosphere at high temperature. It is demonstrated that the Ta-5 mol%W alloy possesses excellent hydrogen permeability without showing any hydrogen embrittlement when used under appropriate permeation conditions. For example, the hydrogen flux for Ta-5 mol%W alloy measured at 773 K under the pressure condition of inlet/outlet = 0.15/0.01 MPa is about 5 times higher than that for Pd-27 mol%Ag alloy measured at the same testing condition.
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Molecular Dynamics Study of the Particle Size Dependency of Structural Change in Hydrogenated Model f.c.c. Nanoparticles

Hiroshi Ogawa

pp. 614-617

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Molecular Dynamics Study of the Particle Size Dependency of Structural Change in Hydrogenated Model f.c.c. Nanoparticles

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DOI:10.2320/matertrans.MA201017

Abstract

Hydrogen absorption in f.c.c. nanoparticles of 1–8 nm diameter was investigated using molecular dynamics simulation with model interatomic potentials. Atomic configuration with five-fold symmetries was observed in both hydrogen-free and hydrogenated particles smaller than 2 nm. The f.c.c. structure was maintained in larger particles after hydrogenation in cases where the M–H interaction is weak. Lattice deformation was induced in cases of strong M–H interaction. A shift of critical size for icosahedral–cubic transition by hydrogenation was also inferred. The number of absorbed H atoms increased concomitantly with increasing particle size and M–H interaction. Most absorbed H atoms located at O-sites when M–H interaction was weak. The T-site occupancy increased with M–H interaction. Analysis using local atomic configuration revealed that structural variation in nanoparticles results from three factors: surface effects, icosahedral transformation, and lattice deformation attributable to M–H interaction.
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Synthesis and Hydrogen Storage Behaviour of Pure Mg₂FeH₆ at Nanoscale

Xuanzhou Zhang, Wenhuai Tian, Junzhi Yang, Rong Yang, Jie Zheng, Xingguo Li

pp. 618-622

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Synthesis and Hydrogen Storage Behaviour of Pure Mg₂FeH₆ at Nanoscale

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DOI:10.2320/matertrans.MA201008

Abstract

Pure Mg₂FeH₆ compounds with two different morphologies have been successfully synthesized directly by mechanical milling (MM) and sintering of a mixture of 2Mg+Fe nanoparticles under an H₂ atmosphere, respectively. The successful preparation of pure Mg₂FeH₆ can be attributed to the small particle sizes of Mg and Fe nanoparticles prepared by hydrogen plasma-metal reaction (HPMR), which provides shorter diffusion distance for hydrogen and the metals. The X-ray diffraction (XRD) and scanning electron microscopy (SEM) results show that the Mg₂FeH₆ synthesized by mechanical milling has larger particle size but smaller crystallite size compared with the Mg₂FeH₆ synthesized by sintering. The Mg₂FeH₆ synthesized by mechanical milling can desorb more than 4.5 mass% hydrogen in 10 min under an initial hydrogen pressure of 0.001 bar at 573 K. Compared with the Mg₂FeH₆ synthesized by sintering under the same conditions as the Mg₂FeH₆ synthesized by mechanical milling, it is suggested that decrease of crystallite size is beneficial for enhancing desorption property of Mg₂FeH₆.
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Cyclic Hydrogenation and Dehydrogenation Property of LiNH₂ Impregnated into Ni Foam

Masaharu Menjo, Yoshihiro Hyodo, Satoko Moriyama, Hai-Wen Li, Motoaki Matsuo, Satoshi Semboshi, Shin-ichi Orimo

pp. 623-626

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Cyclic Hydrogenation and Dehydrogenation Property of LiNH₂ Impregnated into Ni Foam

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DOI:10.2320/matertrans.MA201012

Abstract

Cyclic hydrogenation and dehydrogenation property of LiNH₂ impregnated into the Ni foam was experimentally investigated, comparing with that of conventional LiNH₂ powder. The amount of dehydrogenation from the impregnated sample after activating was 4.3 mass% (without the weight of the Ni foam), and remained 3.3 mass% after the 49th cycle of hydrogenation and dehydrogenation, while the amount from the powder sample drastically decreased down to 0.5 mass% until only the 11th cycle. The main origin of the superior cyclic property of the impregnated sample was attributed to the suppression of sintering, mainly due to release of the exothermic heat during the hydrogenation supported by the frames of the Ni foam.
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Hydrogen Storage Properties of the Mg(NH₃)₆Cl₂-LiH Combined System

Yongfeng Liu, Ruijun Ma, Runlai Luo, Kun Luo, Mingxia Gao, Hongge Pan

pp. 627-634

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Hydrogen Storage Properties of the Mg(NH₃)₆Cl₂-LiH Combined System

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DOI:10.2320/matertrans.MA201013

Abstract

Metal ammine complexes (MACs) were recently regarded as one of promising materials for reversible hydrogen storage due to their high hydrogen content. In this work, a first attempt is conducted to elucidate the hydrogen storage reversibility by combining Mg(NH₃)₆Cl₂ with LiH. It is found that hydrogen is gradually evolved from the combined system during ball milling. After 24 h of milling, approximate 3.5 mass% of hydrogen, equivalent to 6 mol of H₂ molecules, is released from the Mg(NH₃)₆Cl₂-18LiH mixture. Additional 3.4 mass% of hydrogen is further desorbed from the combined system milled for 24 h with a two-step reaction in heating process. Totally ∼12 mol of H₂ molecules are librated from the Mg(NH₃)₆Cl₂-18LiH mixture along with the formation and consumption of Mg(NH₂)₂ and LiNH₂ in the ball milling and subsequent heating process. The resultant products consist of Li₂Mg(NH)₂, Li₂NH, LiH and LiCl after dehydrogenation at 310°C. Further hydrogenation experiment indicates that ∼6 mol of H₂ molecules are reversibly stored in the Mg(NH₃)₆Cl₂-12LiH mixture.
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Correlation between Structure of Titanium Additives and Dehydrogenation Reaction of Magnesium Borohydride Studied by Continuous Observation of X-Ray Absorption Spectroscopy

Daiju Matsumura, Takahiro Ohyama, Yuka Okajima, Yasuo Nishihata, Hai-Wen Li, Shin-ichi Orimo

pp. 635-640

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Correlation between Structure of Titanium Additives and Dehydrogenation Reaction of Magnesium Borohydride Studied by Continuous Observation of X-Ray Absorption Spectroscopy

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DOI:10.2320/matertrans.MA201018

Abstract

Local structure of Ti-based additives in Mg(BH₄)₂ was studied by X-ray absorption fine structure spectroscopy with conventional and dispersive mode in order to understand the correlation between the structure of the additives and dehydrogenation property of Mg(BH₄)₂. Simultaneous measurement of the dehydrogenation curve and the X-ray absorption spectroscopy by the dispersive optics revealed that a part of TiCl₃ additive is converted to Ti_xMg_1−3x⁄2(BH₄)₂ (x=0∼0.67) just after ball milling mixture and then promptly resolved to TiB₂ at 100–150°C with the first dehydrogenation peak. TiO₂ additive is slowly converted to lower oxidation state in wide temperature range around the second dehydrogenation peak at 350°C where the main dehydrogenation reaction of Mg(BH₄)₂ occurs.
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Promotional Effect of Aluminum on MgH₂+LiBH₄ Hydrogen Storage Materials

Young Li, Toshihisa Izuhara, Hiroyuki T. Takeshita

pp. 641-646

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Promotional Effect of Aluminum on MgH₂+LiBH₄ Hydrogen Storage Materials

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DOI:10.2320/matertrans.MA201005

Abstract

The effect of Al addition on the reversibility of a MgH₂+2LiBH₄ hydrogen storage mixture was examined in order to improve the mixture’s requirement for a hydrogen atmosphere even in dehydrogenation. The experiments using high pressure differential scanning calorimetry and X-ray powder diffraction confirmed that a MgH₂+Al+4LiBH₄ mixture can reversibly dehydrogenate and rehydrogenate below 773 K under mild conditions of 0.1 MPa H₂ for dehydrogenation and 4.0 MPa H₂ for rehydrogenation. Moreover, thermogravimetry tests revealed that this mixture starts hydrogen desorption at about 530 K, which is 80 K lower than the corresponding temperature for the MgH₂+2LiBH₄ mixture, and desorbs 9.5 mass% of hydrogen below 773 K. Thus, the addition of Al improves not only the reversibility of the reaction but also dehydrogenation kinetics. The hydrogen desorption of the mixture occurs by three steps, which includes the formation of Mg-Al alloys by the reaction of MgH₂ and metallic Al followed by the formation of Mg_1−xAl_xB₂ by the reaction of the Mg-Al alloys and LiBH₄. Al in this mixture suppresses the formation of metallic Mg and accelerates the formation of Mg_1−xAl_xB₂ from B produced by dehydrogenation of LiBH₄. Mg_1−xAl_xB₂ is derived from partial substitution of Al for Mg in MgB₂, which contributes to reversible hydrogenation and dehydrogenation of MgH₂+2LiBH₄.
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Cooperative Catalysis on the Dehydrogenation of NdCl₃ Doped LiBH₄-MgH₂ Composites

H. Wang, H. L. Zhang, C. Luo, T. Sun, M. Zhu

pp. 647-650

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Cooperative Catalysis on the Dehydrogenation of NdCl₃ Doped LiBH₄-MgH₂ Composites

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DOI:10.2320/matertrans.MA201016

Abstract

To improve the dehydrogenation properties of LiBH₄, the MgH₂ and NdCl₃ were added with different modes by ball-milling, and their influences on the decomposition of LiBH₄ were investigated by performing X-ray diffraction (XRD) analysis and dehydriding kinetic measurements. The results show that adding either NdCl₃ or MgH₂ alone could not promote the decomposition of LiBH₄. But for the NdCl₃ doped LiBH₄-MgH₂ composites, not only the decomposition of MgH₂ is accelerated, but also the dehydrogenation rate and capacity of LiBH₄ are greatly enhanced. The kinetic improvement is attributed to a cooperative catalytic role arising from dual addition of MgH₂ and NdCl₃. The NdH₂ phase, resulting from reaction between MgH₂ and NdCl₃, might be responsible for the enhanced dehydrogenation of LiBH₄.
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Hydrogen Releasing of Lithium Amidoborane-LiNH₂BH₃

Zaixing Yang, Yan Wang, Jing Liang, Jun Chen

pp. 651-653

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Hydrogen Releasing of Lithium Amidoborane-LiNH₂BH₃

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DOI:10.2320/matertrans.MA201015

Abstract

This paper reports on the preparation and hydrogen releasing of lithium amidoborane (LiNH₂BH₃, LiAB). LiAB is synthesized by a wet-chemical route through the direct interaction of LiH with NH₃BH₃ in tetrahydrofuran (THF) at room temperature. The structure of the as-prepared sample is investigated using X-ray diffraction (XRD) and Fourier Transform Infrared (FTIR) spectroscopy. The thermal decomposition process is determined by temperature programmed desorption/mass spectrometer (TPD/MS). The results show that the as-prepared LiAB starts to release H₂ at the temperature of 70.9°C, which is much lower than that of pure AB, while detectable NH₃ releasing should be controlled.
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Enhanced Electrical Conductivities of Complex Hydrides Li₂(BH₄)(NH₂) and Li₄(BH₄)(NH₂)₃ by Melting

Yu Zhou, Motoaki Matsuo, Yohei Miura, Hitoshi Takamura, Hideki Maekawa, Arndt Remhof, Andreas Borgschulte, Andreas Züttel, Toshiya Otomo, Shin-ichi Orimo

pp. 654-657

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Enhanced Electrical Conductivities of Complex Hydrides Li₂(BH₄)(NH₂) and Li₄(BH₄)(NH₂)₃ by Melting

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DOI:10.2320/matertrans.MA201003

Abstract

The electrical conductivities of complex hydrides Li₂(BH₄)(NH₂) and Li₄(BH₄)(NH₂)₃ consisting of (BH₄)⁻ and (NH₂)⁻ anions are investigated focusing on their low melting temperatures (365 K for Li₂(BH₄)(NH₂) and 490 K for Li₄(BH₄)(NH₂)₃). The two hydrides show lithium fast-ion conductivities of about 1×10⁻⁴ S·cm⁻¹ at room temperature. After melting, the total ion conductivities of Li₂(BH₄)(NH₂) and Li₄(BH₄)(NH₂)₃ reach 6×10⁻² S·cm⁻¹ (378 K) and 2×10⁻¹ S·cm⁻¹ (513 K), respectively. The crystal structure and local atomistic structures closely correlated with the lithium ion conduction before and after melting are also discussed.
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Design of Gas Controllable H₂ | H⁺electrolyte | Pt Cell and the Evaluation Method of a Dilute Hydrogen and Oxygen Gas in the Electrolyte

Shuji Harada, Yuki Nagai, Kazuya Kazama

pp. 658-662

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Design of Gas Controllable H₂ | H⁺electrolyte | Pt Cell and the Evaluation Method of a Dilute Hydrogen and Oxygen Gas in the Electrolyte

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DOI:10.2320/matertrans.M2010230

Abstract

A gas handling technique of the gas controllable H₂ | H⁺electrolyte | Pt cell has been reported in order to obtain the reproducible gas environmental condition. The small amount of dissolved hydrogen and oxygen gas in the electrolyte has been evaluated by measurements of the temperature dependence of electromotive force (EMF) of the cell. The gas controllable technique and the evaluation method of a dilute H and O gas dissolved in an electrolyte should contribute to clarify the interfacial phenomena on electrode materials.
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3. Enhanced Electrical Conductivities of Complex Hydrides Li₂(BH₄)(NH₂) and Li₄(BH₄)(NH₂)₃ by Melting MATERIALS TRANSACTIONS Vol.52(2011), No.4
Alloying Behavior of Ni₃M-Type Compounds with D0_a Structure

H. Sugimura, Y. Kaneno, T. Takasugi

pp. 663-671

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Alloying Behavior of Ni₃M-Type Compounds with D0_a Structure

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DOI:10.2320/matertrans.M2010386

Abstract

The atom substitution preference of ternary additions in Ni₃M-type GCP (geometrically close-packed) compounds with D0_a structure was determined from the direction of single-phase region of the GCP phase on the reported ternary phase diagrams. In Ni₃Nb, Co and Cu preferred the substitution for Ni-site, Hf, Ta, Ti, V and W the substitution for Nb-site, and Fe the substitution for both sites. In Ni₃Ta, Co, Cu, Fe, Ir, Mn and Re preferred the substitution for Ni-site, Mo and Nb the substitution for Ta-site, and Al and Cr the substitution for both sites. In Ni₃Mo, Pd and W preferred the substitution for Ni-site, and Al, Nb, Ta, Ti and Zr the substitution for Mo-site. The thermodynamic model, which was based on the change in heat of formation of the host compound by a small addition of ternary solute, was applied to predict the atom substitution preference of ternary additions. The heat of compound formation used in the thermodynamic calculation was derived from Miedema’s formula. Good agreement was obtained between the thermodynamic model and the result of the literature search. For Ni₃Mo, with a small negative heat of formation, a weak binding force between the constituent elements is often enhanced by the addition of the ternary elements that substitute for Mo-site.
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Structures and Local Electronic States of Dislocation Loop in 4H-SiC via a Linear-Scaling Tight-Binding Study

Fusanori Hamasaki, Kenji Tsuruta

pp. 672-676

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Structures and Local Electronic States of Dislocation Loop in 4H-SiC via a Linear-Scaling Tight-Binding Study

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DOI:10.2320/matertrans.MBW201024

Abstract

The atomic- and electronic-level structures of a dislocation loop and a stacking fault in 4H-SiC crystal are investigated by using large-scale tight-binding (TB) molecular-dynamics simulation. We employ a linear-scaling TB method implemented on a parallel computer in order to accelerate the 9,600-atoms calculation which is required for such a nanoscale simulation. We find that the initial configuration that involves unstable C-C networks around the dislocation loop is relaxed to a structure having six-membered rings, and that the distribution of electron populations is inhomogeneous on the loop. The local electronic density of states shows two peaks in the bulk band gap, where one of these peaks may correspond to the defect state observed in EBIC and CL experiments.
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Kinetics of Solid-State Reactive Diffusion between Au and Al

Minho O, Masanori Kajihara

pp. 677-684

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Kinetics of Solid-State Reactive Diffusion between Au and Al

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DOI:10.2320/matertrans.M2010433

Abstract

In the wire bonding technique, a thin Au wire is interconnected with an Al layer on a Si chip. During energization heating at solid-state temperatures, however, brittle Au-Al compounds with high electrical resistivities are formed at the interconnection by the reactive diffusion between Au and Al. In order to examine the growth behavior of the Au-Al compounds, the kinetics of the reactive diffusion was experimentally observed using sandwich Al/Au/Al diffusion couples. The diffusion couple was prepared by a diffusion bonding technique and then isothermally annealed at temperatures of 623–723 K for various times up to 103 h. Under such annealing conditions, the diffusion couple is practically considered semi-infinite. Owing to annealing, compound layers consisting of AuAl₂, AuAl and Au₈Al₃ are produced at the initial Au/Al interface in the diffusion couple. The volume fraction in the compound layers is larger for Au₈Al₃ than for AuAl and AuAl₂ in the early stages but becomes smaller for Au₈Al₃ than for AuAl and AuAl₂ in the late stages. However, there are no systematic dependencies of the volume fraction on the annealing time and temperature. The total thickness of the compound layers is proportional to a power function of the annealing time. The exponent of the power function is smaller than 0.5 at 673–723 K. The exponent smaller than 0.5 means that the interdiffusion across the compound layers governs the layer growth and boundary diffusion predominantly contributes to the interdiffusion. On the other hand, at 623 K, the exponent is equal to unity for annealing times shorter than 8 h but smaller than 0.5 for those longer than 8 h. The exponent of unity indicates that the layer growth is controlled by the interface reaction at the migrating interface. Thus, at T=623 K, the transition of the rate-controlling process occurs at a critical annealing time of 8 h.
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Microstructural Aspects during the Preparation of Y₃Al₅O₁₂ by Combustion Synthesis and Temperature Field Simulation

Yuepeng Song, Jiangtao Li, Yixiang Chen, Wenwen Ji, Chong Soo Lee, Hyoung Seop Kim

pp. 685-690

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Microstructural Aspects during the Preparation of Y₃Al₅O₁₂ by Combustion Synthesis and Temperature Field Simulation

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DOI:10.2320/matertrans.M2010295

Abstract

The combustion front quenching method (CFQM) combined with the temperature field simulated using the finite element method was used to investigate the microstructural aspects of the fabrication of transparent Y₃Al₅O₁₂ via combustion synthesis. The simulated results indicate that there are three regions corresponding with the temperature distribution whose microstructural aspects were studied. The composite mixtures of the products cannot be separated depending only on their gravities. The filamentous profile of aluminum along with many aluminous intermediate products are detected by XRD, SEM and EDS analysis in the preheat region, which indicates that the heat-transfer can affect the mass-transfer process and the subsequent reaction process. The microstructural aspects show that the combustion reaction of the Al/NiO/Y₂O₃ powder mixture was initiated by the melting of Al particles.
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Effect of Martensitizing Temperature on Creep Strength of Modified 9Cr Steel

Manabu Tamura, Takuya Kumagai, Nobuhiro Miura, Yoshihiro Kondo, Kei Shinozuka, Hisao Esaka

pp. 691-698

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Effect of Martensitizing Temperature on Creep Strength of Modified 9Cr Steel

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DOI:10.2320/matertrans.H-M2011802

Abstract

A modified 9Cr-1Mo steel was cooled to a temperature between the M_s point and room temperature from the normalizing temperature and then directly heated to the tempering temperature. It was found that the time to rupture at 650 and 700°C of the steel heat-treated by the new heat treatment increased 2–3 times longer than that of the steel conventionally normalized and tempered. The microstructure of the improved steel was tempered martensite and the size of martensite blocks was larger than for the conventional heat treatment. The hardness of the improved steel was fully recovered after tempering. This strengthening is not caused by fresh martensite, but caused by the refining of M₂₃C₆ and V(C,N) particles in addition to the increase in the martesite block size, where M denotes metallic elements.
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Hardening and Toughening Mechanisms of Cemented Carbides with Plate-Like WC Grains Prepared by Seeding

Kun Liu, Lihui Zhu, Ranran Tu

pp. 699-703

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Hardening and Toughening Mechanisms of Cemented Carbides with Plate-Like WC Grains Prepared by Seeding

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DOI:10.2320/matertrans.M2010380

Abstract

WC-10Co (mass pct.) cemented carbides containing plate-like WC grains were prepared by using plate-like WC single crystals as seeds. With the increase of seed addition amount, more and bigger plate-like WC grains are formed, the hardness and transverse rupture strength (TRS) increase first and then decrease. When 2.5 mass% seeds are added in WC-10Co, the density is hardly affected, whereas the hardness and TRS increase simultaneously, especially TRS increases by 12.8%. The hardening and toughening mechanisms of WC-10Co cemented carbides with plate-like WC grains were discussed.
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2. The Effect of Preheating on Notched Tensile Strength and Impact Toughness of Ti-6Al-6V-2Sn Laser Welds MATERIALS TRANSACTIONS Vol.52(2011), No.3
3. Effect of Internal Strain on Martensitic Transformations in NiTi Shape Memory Alloys MATERIALS TRANSACTIONS Vol.52(2011), No.3
Activity Measurement of Titanium-Tin Alloys by Knudsen Effusion Method

Satoshi Itoh, Yosuke Inoue

pp. 704-708

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Activity Measurement of Titanium-Tin Alloys by Knudsen Effusion Method

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DOI:10.2320/matertrans.M-M2011801

Abstract

The activity of tin in Ti-Sn alloy has been determined at 1400 K by Knudsen effusion method with electrobalance. The activity of titanium was calculated by applying the Gibbs-Duhem relation to the Ti-Sn binary system. The standard Gibbs energy of the formation of intermetallic compound such as Ti₃Sn, Ti₂Sn, Ti₅Sn₃ and Ti₆Sn₅ was calculated at 1400 K by using the activities of components. X-ray diffraction studies were additionally conducted for some samples after the activity measurement. The identified phases were consistent with the phase diagram reported in the literature.
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3. Electron Microscopy Studies of Non-Local Effects’ Impact on Cathodoluminescence of Semiconductor Laser Structures MATERIALS TRANSACTIONS Vol.52(2011), No.3
Production of Ni-P Amorphous Alloy-Coated Bipolar Plate for PEM Fuel Cell by Electro-Less Plating

Sung-chul Kim, Shin-ichi Yamaura, Akihiro Makino, Akihisa Inoue

pp. 709-713

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Production of Ni-P Amorphous Alloy-Coated Bipolar Plate for PEM Fuel Cell by Electro-Less Plating

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DOI:10.2320/matertrans.MBW201007

Abstract

In this work, electro-less plating was adopted to produce a new metallic bipolar plate coated with amorphous alloy. The Ni-P amorphous alloy thin film was deposited on Al plate with a bipolar plate flow field and its corrosion resistance and contact electrical resistance were measured. As results, it was found that the electro-less plated Ni-P amorphous thin film showed much lower corrosion resistance than the Ni-Cr-P-B metallic glass because of its lack of Cr content and also found that the Ni-P film showed lower contact electrical resistance than the stainless steel SUS316L plate.
The electricity generation tests with the single cell having the Ni-P amorphous alloy-coated bipolar plates produced in this study revealed that the single cell with the Ni-P amorphous alloy-coated bipolar plates showed excellent I-V performance as well as the cell with the carbon bipolar plates after 39th repetition. However, the I-V performance degraded gradually and was found to be much lower than that with the carbon bipolar plates after 50th repetition. Then the long time durability tests for 24 h were also conducted at the constant current density of 200 mA·cm⁻². It was found that the cell voltage of the single cell with the Ni-P amorphous alloy-coated bipolar plates decreased gradually with time.
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3. Effect of Internal Strain on Martensitic Transformations in NiTi Shape Memory Alloys MATERIALS TRANSACTIONS Vol.52(2011), No.3
Surface Age Hardening and Wear Properties of Beta-Type Titanium Alloy by Laser Surface Solution Treatment

Yasuhiro Michiyama, Kei Demizu

pp. 714-718

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Surface Age Hardening and Wear Properties of Beta-Type Titanium Alloy by Laser Surface Solution Treatment

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DOI:10.2320/matertrans.MBW201003

Abstract

This paper describes the creation of a surface-hardened layer with a minimum thickness of 1.0 mm on a titanium alloy. Two layers, a soft layer and a thick surface-hardened layer, were created on the titanium alloy specimens by using different age hardening speeds caused by different conditions of solution treatment. The solution treatment used furnace heating and laser heating as heating methods. Our accelerated aging treatment was conducted at temperature 300°C for aging times 86.4–432.0 ks after the solution treatment. Changes in the titanium alloy specimens after the aging treatment were examined by hardness and wear tests and microstructure observation.
The results revealed that the laser-heated part hardened at an early stage in aging time. Because of the difference in hardening speed, a hardened layer was formed. Except for the case of furnace heating at 700°C, the grain diameter of the laser-heated parts barely changed after furnace heating. The wear amount of the titanium alloy decreased with hardness; this decrease was remarkable especially at 450 HV and higher. For the specimens of both furnace- and laser-heated parts having the same hardness, the wear amounts were the same. The specimen that was laser heated for 259.2 ks after furnace heating at 800°C had an effective hardened layer with hardness 490–500 HV, ranging from the surface to a thickness of about 1.0 mm. The hardness of the internal unhardened layer for this specimen was 260 HV.
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3. Effect of Internal Strain on Martensitic Transformations in NiTi Shape Memory Alloys MATERIALS TRANSACTIONS Vol.52(2011), No.3
Reactions of Ti, V, Nb and Ta with N₂ Gas at 2000°C under Concentrated Solar Beam in a Solar Furnace at PROMES-CNRS

Nobumitsu Shohoji, Fernando Almeida Costa Oliveira, Luís Guerra Rosa, Gilles Peraudeau, Bernard Granier, Teresa Magalhães, Jorge Cruz Fernandes

pp. 719-727

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Reactions of Ti, V, Nb and Ta with N₂ Gas at 2000°C under Concentrated Solar Beam in a Solar Furnace at PROMES-CNRS

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DOI:10.2320/matertrans.M2010314

Abstract

Reactions of d-group transition metals including Ti, V, Nb and Ta with N₂ gas were investigated at target temperature of 2000°C under heating with concentrated solar beam at PROMES-CNRS in Odeillo (France). In the typical experimental setup using graphite crucible as the sample holder, synthesis of pure nitride with fcc (face centred cubic) structure was proved to be difficult on account of inevitable C₂ radical plume with high carbon activity a(C) from the graphite components and the majority of reaction products were carbo-nitride. By insertion of Sky blue filter in the solar beam path before entering into the parabolic concentrator, C₂ radical formation appeared to be efficiently suppressed and phases with high N content were synthesized. However, under conditions in which C₂ radical plume yield was considerable, nitrogen content in the reaction products became suppressed and tetragonal Nb₄N₃ yielded in place of fcc NbN from Nb or N-deficit sub-nitride Ta₂N in place of mono-nitride TaN formed.
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3. Effect of Internal Strain on Martensitic Transformations in NiTi Shape Memory Alloys MATERIALS TRANSACTIONS Vol.52(2011), No.3
Foaming Agents for Powder Metallurgy Production of Aluminum Foam

Takuya Koizumi, Kota Kido, Kazuhiko Kita, Koichi Mikado, Svyatoslav Gnyloskurenko, Takashi Nakamura

pp. 728-733

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Foaming Agents for Powder Metallurgy Production of Aluminum Foam

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DOI:10.2320/matertrans.M2010401

Abstract

Metallic foams are commonly produced using hydride foaming agents. Carbonates are safer to handle than hydrides; however, their use in the powder metallurgy (PM) route to obtaining a fine and homogenous cell structure has not been evaluated. In this study, carbonates and hydroxides were investigated as foaming agents for the production of Al-Si-Cu alloy foams by the PM route. The thermal decomposition behavior of the foaming agents was evaluated in conjunction with the cell structure of the aluminum foams produced. From the results, it was clarified that a foaming agent that began decomposing after the matrix melted is required to obtain a fine and homogenous cell structure. The TiH₂ foam formed under similar conditions was obviously different and had a coarse and rounded cell structure. MgCO₃ and CaMg(CO₃)₂ were selected as suitable foaming agents for the Al-Si-Cu alloy. Once expanded, the CaMg(CO₃)₂ foam had a specific gravity of 1.19 and a homogeneous, fine and spherical cell structure.
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3. Effect of Internal Strain on Martensitic Transformations in NiTi Shape Memory Alloys MATERIALS TRANSACTIONS Vol.52(2011), No.3
Effects of Electron Beam Irradiation on Elasticity of CFRTP (CF/PEEK)

Hiroaki Takei, Michelle Salvia, Alain Vautrin, Akira Tonegawa, Yoshitake Nishi

pp. 734-739

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Effects of Electron Beam Irradiation on Elasticity of CFRTP (CF/PEEK)

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DOI:10.2320/matertrans.MBW201005

Abstract

Homogeneous low voltage electron beam irradiation (HLEBI) improved the elasticity indicated by both flexural modulus (E_f) and the maximum slope value ((dσ⁄dε)_max) of the bending stress–strain curve of carbon fiber reinforced thermoplastic polyetheretherketone (CFRTP) composite sheets with 0.50 mm thickness, although the penetration depth estimated was from 0.14 to 0.21 mm on both side surfaces. HLEBI remarkably enhanced both E_f and (dσ⁄dε)_max. The E_f at middle cumulative probability (P_E) of 0.50 for CFRTP irradiated at 0.30 MGy (kJg⁻¹) was 3.3 GPa, which was 27% higher (2.6 GPa) than for CFRTP before irradiation. Moreover, (dσ⁄dε)_max at middle cumulative probability (P_E=0.50) was more than 4.9 GPa for CFRTP irradiated at 0.30 MGy. The interfacial friction force, as well as the strengthening of both carbon fiber and polyetheretherketone probably contributed to the HLEBI effects to enhance both E_f and (dσ⁄dε)_max in the CFRTP.
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3. Effect of Internal Strain on Martensitic Transformations in NiTi Shape Memory Alloys MATERIALS TRANSACTIONS Vol.52(2011), No.3
Microwave Absorption Properties of Polymer Modified Ni-Zn Ferrite Nanoparticles

Kazuaki Shimba, Kiyotaka Furuta, Nobuyuki Morimoto, Nobuki Tezuka, Satoshi Sugimoto

pp. 740-745

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Microwave Absorption Properties of Polymer Modified Ni-Zn Ferrite Nanoparticles

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DOI:10.2320/matertrans.MBW201013

Abstract

Polymer composites of magnetic particles are widely used as microwave absorbers. An effective method for obtaining thinner microwave absorbers for device design is increasing the volume fraction of magnetic nanoparticles by enhancing the permeability of composites. In this study, composites were prepared using Ni-Zn ferrite nanoparticles surface-modified with 4-META (4-methacryloylioxyethyl trimellitate anhydride) and cross-linked with PEG-4SH (pentaerythritol tetra-polyethylene glycol ether with four thiol-modified terminals). These composites have a high volume fraction of nanoparticles (up to 72 vol%) and permeability (μ_{r max}″=5.9). In addition, the prepared composites showed good microwave absorption properties (R.L.<−20 dB) with a smaller matching thickness than conventional microwave absorber using spinel-type ferrite.
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3. Effect of Internal Strain on Martensitic Transformations in NiTi Shape Memory Alloys MATERIALS TRANSACTIONS Vol.52(2011), No.3
Investigation of a Flotation Process with De-Sliming and Attrition to Upgrade and Recover Cu and Mo from a Cu-Mo Flotation Tailing

Jan Pana Rabatho, William Tongamp, Atsushi Shibayama, Yasushi Takasaki, Sachihito Nitta, Tetsuo Imai

pp. 746-752

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Investigation of a Flotation Process with De-Sliming and Attrition to Upgrade and Recover Cu and Mo from a Cu-Mo Flotation Tailing

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DOI:10.2320/matertrans.M-M2011803

Abstract

In some (Cu-Mo) mines around the world, Mo recovery is low due to poor liberation, fine dissemination in gangue minerals, and losses of Cu and Mo to tailing streams. Studies to recover these materials as a new resource will increasingly become an attractive option. In the current study, a flotation tailing sample obtained from a mine recovering only 40% Mo was re-floated to upgrade Cu and Mo. The sample containing 0.07% Cu and 0.01% Mo, was used in the study and the goal was to improve the grades to over 2.0% Cu and 0.5% Mo, to obtain an additional feed for the flotation process. Sodium aluminium silicate (NaAlSi₃O₈) and quartz (SiO₂) were observed as the dominant mineral phases. The original samples were milled and screened to pass 105 μm screen to be used in the subsequent tests. To evaluate the efficiency of the process, both single and multi-stage flotation steps including de-sliming for the removal of fines and attrition for surface activation, together with other parameters (pH, PAX concentration, time) were performed. Based on the experimental results, a four-stage flotation process allowed the improvement of Cu and Mo grades to 1.63% and 0.24% respectively. A single-stage flotation process with de-sliming and attrition stages before flotation with PAX and MIBC concentrations of 40 g/t improved Cu and Mo grades to 2.07% and 0.64%, with a recovery of 48.60% and 65.97% respectively.
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Long Time Stability of Pb-Free Sn-9Zn Elements for AC-Low Voltage Fuse Performance

Kazuhiro Matsugi, Yasuhiro Iwashita, Yong-Bum Choi, Gen Sasaki, Koji Fujii

pp. 753-758

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Long Time Stability of Pb-Free Sn-9Zn Elements for AC-Low Voltage Fuse Performance

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DOI:10.2320/matertrans.M2010389

Abstract

In order to evaluate the stability in long time for the performance of AC-low voltage fuses, this study aimed to measure the changes of the specific resistivity, specific heat and thermal conductivity due to the microstructure-change, using a diffusion couple consisting of the Sn-9Zn fuse element and Cu-connector which are exposed at 443 K for 7.2 ks. The reaction area with the thickness of 5 μm consisting of Sn, Cu and Zn phases, was formed at its interface. The values in their properties were increased due to microstructure-change caused by the diffusion. The equations for the estimation of their values could be represented as a function of temperature. The good stability in long time for the un-melt down performance at 210 A of electric current, was confirmed by three-dimensional voltage and temperature calculations on fuse elements after diffusion.
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2. The Effect of Preheating on Notched Tensile Strength and Impact Toughness of Ti-6Al-6V-2Sn Laser Welds MATERIALS TRANSACTIONS Vol.52(2011), No.3
3. Effect of Internal Strain on Martensitic Transformations in NiTi Shape Memory Alloys MATERIALS TRANSACTIONS Vol.52(2011), No.3
Sintering Behavior of Tungsten Heavy Alloy Products Made by Plasma Spray Forming

Yueming Wang, Xiang Xiong, Lu Xie, Xuan Xu, Xiaobing Min, Feng Zheng

pp. 759-767

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Sintering Behavior of Tungsten Heavy Alloy Products Made by Plasma Spray Forming

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DOI:10.2320/matertrans.M2010391

Abstract

Refractory metallic thin-walled products of 95W–3.5Ni–1.5Fe (in mass%) were fabricated by plasma spray forming (PSF) in argon atmosphere at 1.01×10⁵ Pa followed by high temperature sintering (1200, 1300, 1400 and 1465°C). Scanning electron microscope (SEM), energy dispersive X-ray spectroscopy (EDS), Archimedes method, differential scanning calorimetry (DSC) and X-ray diffractometer (XRD) have been employed to study microstructure, solubilities, density, solidus and liquidus temperatures and phases of the parts. Lamellar structure consisting of vertical columnar grains and fine particles was found in PSF deposits. Supersaturated solid solutions were formed in the deposits with the relative density of 88±2%. Solidus and liquidus temperatures of γ phase were measured to be 1392 and 1412±5°C, respectively. Initial lamellar structure was remained in the tested samples after sintering at lower temperatures (1200°C/90 min, 1300°C/90 min and 1400°C/15, 90 min) and turned into granular structure at 1465°C/5, 15, 30, 90 min. In addition, the relative densities of deposits, after sintering at 1200, 1300, 1400 and 1465°C for 90 min, were increased from 88 to 90, 92, 94 and 98±2%, respectively. A five-stage sintering mechanism proposed by us previously has been re-validated and double checked by experimental results.
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Laser-Induced Synthesis of CaMoO₄ Nanocolloidal Suspension and Its Optical Properties

Jong-Won Yoon, Chel-Jong Choi, Daewon Kim

pp. 768-771

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Laser-Induced Synthesis of CaMoO₄ Nanocolloidal Suspension and Its Optical Properties

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DOI:10.2320/matertrans.M2010407

Abstract

Pulsed laser ablation in a liquid phase was employed successfully to synthesize a calcium molybdate (CaMoO₄) nanocolloidal suspension. The crystalline phase, particle morphology, particle size distribution, absorbance, optical band-gap and photoluminescence (PL) were examined. Stable colloidal suspensions consisting of well-dispersed CaMoO₄ nanoparticles with a narrow size distribution could be obtained without a surfactant. The optical absorption edge located near 270 nm was blue-shifted by approximately 70 nm compared to that reported for bulk crystals. The estimated optical energy band-gap was 4.7 eV and the PL spectrum was blue-shifted at approximately 430 nm compared to the emission of bulk CaMoO₄ target (525 nm). The observed band-gap widening and blue-shift of PL emission was attributed to the quantum-size effect due to the very small size of the CaMoO₄ nanoparticles prepared by pulsed laser ablation in deionized water.
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3. Effect of Internal Strain on Martensitic Transformations in NiTi Shape Memory Alloys MATERIALS TRANSACTIONS Vol.52(2011), No.3
Parallel Receiving Needle Beam Ultrasonic Testing Technique

Hajime Takada, Takafumi Ozeki

pp. 772-779

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Parallel Receiving Needle Beam Ultrasonic Testing Technique

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DOI:10.2320/matertrans.M2010335

Abstract

A new ultrasonic testing technique and a new test system using a transducer array have been developed. The test system works as follows: (1) Ultrasonic waves are transmitted from all the ultrasonic transducer elements in the array at the same time; and (2) By additively synthesizing time-converted ultrasound signals transformed from echo signals received by all the ultrasonic transducer elements in the array at the same time, lines of continuously focused receiving beam (receiving needle beam) are closely formed under the transducer array (parallel receiving needle beam). Also, internal flaws in a cross-section are detected at once using the parallel receiving needle beam. The results of experiments using a 50-MHz transducer array and the developed system have proven that ultra-minute internal flaws 20 μm in diameter can be detected at a scan speed of 1000 mm/s. In addition, the focal zone formed is very long as compared with conventional point-focused beam forming. It is concluded that the system is suitable for simultaneous testing of a cross-section of a test object at high scanning speed.
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Construction of Processing Map for Biomedical Co-29Cr-6Mo-0.23C-0.14N Alloy by Using Compression Tests

Yui Yamashita, Yunping Li, Hiroaki Matsumoto, Yuichiro Koizumi, Akihiko Chiba

pp. 780-786

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Construction of Processing Map for Biomedical Co-29Cr-6Mo-0.23C-0.14N Alloy by Using Compression Tests

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DOI:10.2320/matertrans.M2010388

Abstract

The high-temperature deformation behavior of Co-29Cr-6Mo-0.23C-0.14N alloy was investigated by carrying out compression tests; the tests were carried out in the temperature range of 1000–1200°C and strain rates ranging from 0.01 to 30 s⁻¹ with a height reduction of approximately 65%. The optimum hot-working conditions were determined from the processing map based on the dynamic materials model. Dynamic recrystallization was observed to occur over the entire temperature and strain rate range. However, uniformly sized grains were formed for strain rates higher than 1 s⁻¹, which is considered to be the optimum hot-working condition. In addition, authors suggested that in extremely low stacking fault energy alloy, explosive and homogeneous formation of mechanical twinning should be considered to be stable state, and new processing map with more detailed description of deformation mechanism seems necessary in future.
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A Three Dimensional Cellular Automaton Model for the Prediction of Solidification Morphologies of Brass Alloy by Horizontal Continuous Casting and Its Experimental Verification

De-Chang Tsai, Weng-Sing Hwang

pp. 787-794

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A Three Dimensional Cellular Automaton Model for the Prediction of Solidification Morphologies of Brass Alloy by Horizontal Continuous Casting and Its Experimental Verification

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DOI:10.2320/matertrans.M2010402

Abstract

The purpose of this study is to predict the morphologies of the solidification process for brass alloys (Cu70Zn30 and Cu65Zn35) by horizontal continuous casting (HCC) and to verify its accuracy by the observed experimental results. This study was extended from previous study (predict the solidification microstructure of pure copper rod by vertical continuous casting process). In numerical simulation aspect, finite difference method (FDM) and cellular automaton (CA) model were utilized to solve the macro-temperature field and micro-nucleation and grain growth of brass alloy respectively. From the observed casting experiment, the unidirectionally solidified brass rod could be fabricated by the HCC process with using cooled mold. The cast grain morphology by CAFD model was corresponding to the result of actual casting experiment well.
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Thermoelectric Properties of Fine-Grained PbTe Bulk Materials Fabricated by Cryomilling and Spark Plasma Sintering

Chia-Hung Kuo, Hsiu-Shan Chien, Chii-Shyang Hwang, Ya-Wen Chou, Ming-Shan Jeng, Masahiro Yoshimura

pp. 795-801

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Thermoelectric Properties of Fine-Grained PbTe Bulk Materials Fabricated by Cryomilling and Spark Plasma Sintering

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DOI:10.2320/matertrans.M2010331

Abstract

Dense fine-grained PbTe bulk materials without oxide phases are fabricated using a process that combines cryomilling (mechanical milling at cryogenic temperature) and spark plasma sintering (SPS). In the process, micro-grained PbTe powder is cryomilled into nanocrystalline powders, which are then rapidly densified into dense bulk samples with fine grains by SPS at 573 K. The effect of cryomilling on the composition ratio, microstructure, and thermoelectric properties of sintered PbTe samples is investigated. Experimental results indicate that when the grain size decreases to the nano-scale, the Seebeck coefficient increases, the thermal conductivity decreases, and the electrical conductivity only slightly changes for all sintered samples. According to the results, the combination of cryomilling and spark plasma sintering can improve the thermoelectric transport properties of PbTe bulk materials.
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Microstructure Evaluation of Friction Stir Welded AZ91 with CaO Mg Alloy

Don Hyun Choi, Byung Wook Ahn, Shae Kwang Kim, Yun Mo Yeon, Young Jik Kim, Sun-Kyu Park, Seung Boo Jung

pp. 802-805

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Microstructure Evaluation of Friction Stir Welded AZ91 with CaO Mg Alloy

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DOI:10.2320/matertrans.M2010271

Abstract

The present study was carried out to evaluate the microstructural properties of a friction stir welded AZ91 with CaO Mg alloy. For this work, friction stir welding (FSW) was performed at a tool rotation speed of 1250 rpm and a traveling speed of 32 mm·min⁻¹. A network of intermetallic compounds (Al₂Ca) was observed in the base metal (BM). In the stir zone (SZ), fine grains and intermetallic compound particles were formed due to dynamic recrystalization and mechanical stirring. The hardness profile showed that the hardness of the SZ was higher than that of the BM, probably due to the presence of fine grains and thermally stable intermetallic compounds.
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Abnormal Hydrogen Absorption/Desorption Properties of Nanoporous Pt with Large Lattice Strains

Masataka Hakamada, Toshiyuki Furukawa, Tao Yamamoto, Masaki Takahashi, Mamoru Mabuchi

pp. 806-809

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Abnormal Hydrogen Absorption/Desorption Properties of Nanoporous Pt with Large Lattice Strains

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DOI:10.2320/matertrans.M2010403

Abstract

Hydrogen absorption/desorption properties of nanoporous Pt fabricated by dealloying were investigated. At high pressure (>1.3 MPa), the nanoporous Pt released hydrogen during hydrogen pressurization; in contrast, it absorbed hydrogen up to 3.5 atom% during hydrogen depressurization, which have not been seen in current metal/hydride systems including nanoparticles. First-principles calculations suggested that the abnormal hydrogen absorption/desorption properties are due to the relaxation/preservation of the lattice strain in Pt hydride.
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Laser Forming of Zr-Based Coatings on AZ91D Magnesium Alloy Substrates for Wear and Corrosion Resistance Improvement

T. M. Yue, K. J. Huang

pp. 810-813

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Laser Forming of Zr-Based Coatings on AZ91D Magnesium Alloy Substrates for Wear and Corrosion Resistance Improvement

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DOI:10.2320/matertrans.M2010274

Abstract

To improve the wear and corrosion resistance of AZ91D magnesium alloy, Zr-based coatings were fabricated on the alloy substrate using laser forming. They were prepared from (i) Zr+Mg powders (5:1 mass%), and (ii) an undercoating of Zr+Mg powders (5:1 mass%) with a top layer of Zr powder. The Zr+Mg powder coating was found to consist primarily of Zr particles with some Zr-based intermetallic compounds in a Mg-Al matrix; while that with an extra top coating of Zr powder had an outer layer composed of Zr oxides and Zr aluminides. With regard to wear and corrosion resistance, the highest improvement was obtained for the specimen that was clad with a top layer of Zr powder. Compared to the AZ91D specimen without a laser formed coating, a fivefold decrease in weight loss and around three orders of magnitude decrease in corrosion current density respectively were obtained.
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Comments on “the Papers on Zr-Ti-Al-Ni-Cu Amorphous Alloy Sheets and Zr-Al-Ni-Cu Amorphous Alloy Wires Published in Materials Transaction JIM Vol. 39, No. 8 and No. 12 (1998) and Vol. 41, No. 11 (2000)” by Tao Zhang and Akihisa Inoue as well as the Relevance to the Errata Given in Materials Transactions Vol. 51, No. 8 (2010)

Hiroshi Oikawa, Yoshio Waseda

pp. 814-815

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Comments on “the Papers on Zr-Ti-Al-Ni-Cu Amorphous Alloy Sheets and Zr-Al-Ni-Cu Amorphous Alloy Wires Published in Materials Transaction JIM Vol. 39, No. 8 and No. 12 (1998) and Vol. 41, No. 11 (2000)” by Tao Zhang and Akihisa Inoue as well as the Relevance to the Errata Given in Materials Transactions Vol. 51, No. 8 (2010)

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DOI:10.2320/matertrans.M2010366

Abstract

The authors of three papers on Zr-Ti-Al-Ni-Cu amorphous alloy sheets and Zr-Al-Ni-Cu amorphous alloy wires, previously published in Materials Transaction JIM Vol. 39, No. 8 and No. 12 (1998) and Vol. 41, No. 11 (2000), are requested to explain explicitly the reason for the late corrections after more than a decade published in Materials Transaction Vol. 51, No. 8 (2010).
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MATERIALS TRANSACTIONS Vol. 52 (2011), No. 4

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