DOI： 10.2320/matertrans.MT-N2022004]

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Language：English   Publishing type：Research paper (scientific journal)   Publisher：Journal of the Ceramic Society of Japan  

Shrinkage-rate controlled flash (SCF) sintering using alternative current electric field was systematically performed for 310 mol% Y2O3-doped ZrO2. As results, the uniformly densified compacts with about 99% relative densities could be produced at furnace temperatures of about 754781 °C for about 30 min as SCF-regime irrespective of Y concentration, while the achieved densities were limited by conventional flash sintering. The shrinkage-rates during SCF-sintering were found to be enhanced in lower temperature range comparing those during thermal-sintering. The enhancement of shrinkage-rates in lower temperature range observed in SCFsintering is possibly related to the reduction of apparent activation energy of sintering under electric fields.

DOI： 10.2109/jcersj2.22114

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Language：English   Publishing type：Research paper (scientific journal)   Publisher：Journal of the Ceramic Society of Japan  

A phenomenon often appears that the final achieved density is limited during conventional flash sintering even under alternative current electric field. By observing the cross-sectional microstructure of the flash sintered 8 mol %Y2O3-doped ZrO2 at this state, we found that a thin surface portion with near full density surrounds a porous inside with lower density. The densified thin surface portion is shell-like structure covering a whole of the sintered compact. The formation of this characteristic shell-like structure in the early stage of flash sintering greatly restricts subsequent densification of porous inside. In order to suppress the formation of the shell that inhibit densification, a technique of controlling a steep power spike at a flash event must be necessary to be appropriately transitioned.

DOI： 10.2109/jcersj2.22109

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Language：English   Publishing type：Research paper (scientific journal)   Publisher：Journal of the Ceramic Society of Japan  

Shrinkage-rate control flash (SCF) sintering is an attractive flash sintering that is modified to densify ceramic green compacts up to high density, which controls electric current to keep shrinkage-rate constant by feedback from shrinkage behavior during a flash state. To build up easier sintering protocol and to realize faster shrinkage-rate, we attempted automated SCF-sintering using the predicted current profile without feedback of the shrinkage behavior. As results, 8YSZ polycrystal with a density of 5.83 g/cm3 and a grain size of 1.84.5 μm could be produced within 10 min during SCF and soaking regimes at the furnace temperature of 870 °C, although the linearity of shrinkage-rate during automated SCF-sintering is degraded from the assumed shrinkage-rate. In order to improve automated SCF-sintering further, a more accurate method of approximating the current profile would be necessary to realize the higher linearity of shrinkage-rate.

DOI： 10.2109/jcersj2.22009

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Language：English   Publishing type：Research paper (scientific journal)  

DOI： 10.1039/d1ta03307g

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Language：English   Publishing type：Research paper (scientific journal)  

DOI： 10.1111/jace.17912

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Language：English   Publishing type：Research paper (scientific journal)  

DOI： 10.2109/jcersj2.21066

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Language：English  

DOI： 10.1016/j.jeurceramsoc.2021.03.005

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Language：English   Publishing type：Research paper (scientific journal)  

DOI： 10.2109/jcersj2.20192

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Publisher：Funtai Oyobi Fummatsu Yakin/Journal of the Japan Society of Powder and Powder Metallurgy  

Shrinkage behaviors during shrinkage rate-controlled flash (SCF) sintering were investigated for 8 mol% Y2O3–ZrO2 (8YSZ) when shrinkage rates were varied between 60 and 300 μm/min under alternating current fields of 50 Vrms/cm, 1200 mArms, and 1000 Hz at a furnace temperature of approximately 870°C. Volumetric power dissipation and electrical conductivity were shown to exhibit similar dependencies against linear shrinkages even if the shrinkage rates were changed. The 8YSZ polycrystals, with similar microstructure and density, could be produced under all SCF conditions used in this study, which was confirmed as a characteristic feature of SCF sintering. Finally, the 8YSZ polycrystals with a density of 5.91–5.93 g/cm3 and a grain size of 2.2–2.6 μm could be produced with a shrinkage process period of 15–65 min at a furnace temperature of approximately 870°C.

DOI： 10.2497/jjspm.68.482

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Publisher：Funtai Oyobi Fummatsu Yakin/Journal of the Japan Society of Powder and Powder Metallurgy  

The uniformity of shrinkages and the distribution of grain sizes were investigated for flash-sintered 3 mol%Y2O3-ZrO2 compacts in direct current and alternating current (AC) electric fields using rectangular-shaped and circular truncated cone-shaped green compacts. The use of a high-frequency AC electric field enough to suppress electrode overvoltage was confirmed to be advantageous for uniform shrinkages, regardless of the shapes of the green compacts. However, the grain size distribution became larger in cone-shaped green compacts, the cross-sectional areas of which varied along the compact. The grain sizes in flashed cone-shaped green compacts were found to exhibit a near linear relation to current density, which provides a means for determining the grain size distribution upon the flash sintering of green compacts with different cross-sectional areas along an electric field.

DOI： 10.2497/jjspm.68.487

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Language：Japanese   Publisher：Cancer Medicine  

Epstein-Barr virus (EBV)-positive B cells have been detected in 66%-86% of patients with angioimmunoblastic T-cell lymphoma (AITL). However, it remains controversial whether EBV status has an impact on the survival of patients with AITL. In this study, we aimed to reevaluate the impact of EBV on the clinicopathological characteristics of AITL. In particular, we focused on the impact of EBV in younger patients with AITL. In total, 270 cases of AITL were studied. Epstein-Barr virus-positive B cells were detected in 191 (71%) cases (EBER+ group). Among the patients who received anthracycline-based therapy, the EBER status did not affect the overall survival (OS) or progression-free survival (PFS). In the younger group of AITL (≤60 years), PFS was significantly worse in the EBER− group compared to the EBER+ group (P =.0013). Furthermore, the multivariate analysis identified EBER-negative status, thrombocytopenia, and elevated serum IgA level as significant adverse prognostic factors for PFS (P <.001, P <.001, and P =.002). Based on these findings, we constructed new prognostic model for the younger group, based on three adverse factors. We classified the patients into two risk groups: low risk (no or 1 adverse factor) and high risk (2 or 3 adverse factors). This new model for younger patients with AITL showed that both OS and PFS were significantly related to the level of risk (P <.0001). In summary, this study showed that, among younger patients with AITL, an EBER+ status significantly improved prognosis compared to an EBER− status. Our new prognostic model should be applicable to younger patients with AITL.

DOI： 10.1002/cam4.2742

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Language：Japanese   Publisher：Reproduction, Fertility and Development  

In order to help elucidate the process of epiblast and trophoblast cell differentiation in bovine embryos in vitro, we attempted to develop a suitable culture medium to allow extended embryo culture. Day 7 bovine blastocysts developed in conventional medium were cultured further in embryonic stem cell medium with or without leukaemia inhibitory factor (LIF) until Day 23. At Day 14, the expression of octamer-binding transcription factor 3/4 (OCT3/4) and VIMENTIN was significantly higher in embryos cultured with than without LIF, but embryonic disc formation was not observed. Although expression of SRY (sex determining region Y)-box 17 (SOX17) mRNA was significantly lower in Day 14 embryos cultured with and without LIF than in in vivo embryos, hypoblast cells formed just inside the trophoblast cells of the in vitro-cultured embryos. On Day 23, expression of placental lactogen (PL) and prolactin-related protein 1 (PRP1) was not affected by LIF in in vitro-cultured embryos, levels of both genes were significantly lower in the in vitro than in vivo embryos. Similar to in vivo embryos, binucleate cell clusters seen in Day 23 in vitro-cultured embryos were composed of PL-negative and -positive cells. These results suggest that our culture system partially reproduced the differentiation process of trophoblast cells in vivo.

DOI： 10.1071/RD18343

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Language：English   Publishing type：Research paper (scientific journal)  

DOI： 10.1111/jmi.12759

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Language：Japanese   Publisher：Conference Program Digest - 7th International Conference on Manipulation, Manufacturing and Measurement on the Nanoscale, IEEE 3M-NANO 2017  

This paper presents a growth and characterization of vertically aligned PdxCoi-x alloy encapsulated inside Multi-Walled Carbon Nanotube (MWCNT) arrays on Pd/Co thin layers coated on Si substrate by a dc bias-enhanced plasma chemical vapor deposition (CVD) method. The Metal Alloy Encapsulated within MWCNTs (MAE-MWCNTs) were characterized by a scanning electron microscope (SEM) and a transmission electron microscopy (TEM). The SEM images show the teardrop-shape particles encapsulated within the tube top of MWCNTs. A vibrating sample magnetometer was used to study the magnetism of a large number of MAE-MWCNTs on Si substrate at room temperature. The hysteresis loop of the ME-MWCNTs shows clear ferromagnetic behavior and the easy axis of magnetization is parallel to the MEA-MWCNT tube axis, as can be elucidated from the large coercive fields and remanence values. Moreover, TEM off-axis electron holograms were used to study the magnetism of the individual MAE-MWCNT or the two pair of MAE-MWCNTs. Based on electron holography, we have successfully obtained the saturation magnetization of 0.7 T and 1.12 T for the individual MAE-MWCNT with diameters of 41 nm and 83 nm, respectively.

DOI： 10.1109/3M-NANO.2017.8286262

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Publishing type：Research paper (scientific journal)   Publisher：Elsevier BV  

DOI： 10.1016/j.jeurceramsoc.2023.12.046

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Publishing type：Research paper (scientific journal)   Publisher：Elsevier BV  

DOI： 10.1016/j.jeurceramsoc.2023.06.001

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Publishing type：Research paper (scientific journal)  

The development of a high-speed sintering method that can shorten the entire sintering time while guaranteeing the mechanical properties is very attractive as a sintering process for structural ceramic polycrystals. For this purpose, a sintering protocol that combines shrinkage-rate-controlled flash sintering, which controls the shrinkage rate to be constant with the use of an alternative current electric field, and a rapid furnace ramp were applied to 3-mol % Y2O3-doped ZrO2 (3YSZ). As a result, a 3YSZ sintered polycrystal with about the relative density of 99.5 % (6.06 g/cm3) could be successfully fabricated within 30 min as the entire sintering time, which includes the furnace-heating regime. The sintered 3YSZ polycrystal is confirmed to exhibit a Vickers hardness of approximately 1290 HV and a fracture toughness (KIC) of approximately 5.2 MPa m1/2, which are similar values to those obtained from a typical thermally sintered 3YSZ polycrystal.

DOI： 10.2109/jcersj2.23041

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Publishing type：Research paper (scientific journal)  

DOI： 10.1021/acs.jpcc.3c01679

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Publishing type：Research paper (scientific journal)   Publisher：Elsevier BV  

DOI： 10.1016/j.apt.2023.103970

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Language：English   Publishing type：Research paper (scientific journal)   Publisher：Wiley  

In this study, flash joining experiments were conducted using an AC field on 3 mol% Y2O3‐stabilized tetragonal ZrO2 polycrystal (Y‐TZP) bodies. Furthermore, the necessary conditions to obtain an almost complete self‐joining of Y‐TZP bodies were clarified. The specimens were successfully joined by applying an AC field at 60 mA·mm−2 for 80 s at a furnace temperature of 1000°C, thus resulting in a successfully joined specimen with 92% of the flexural strength of the as‐sintered Y‐TZP body. Almost complete self‐joining of Y‐TZP was achieved at current densities above 30 mA·mm−2, and input energy densities of >24 J·mm−3. Both the input energy density and electric current were critical factors for producing the reliable joining of ceramics.

DOI： 10.1111/jace.18889

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Publishing type：Research paper (scientific journal)   Publisher：Elsevier BV  

DOI： 10.1016/j.jeurceramsoc.2022.10.065

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Language：English   Publishing type：Research paper (scientific journal)   Publisher：Elsevier BV  

DOI： 10.1016/j.jlumin.2022.119508

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Publishing type：Research paper (scientific journal)   Publisher：Japan Institute of Metals  

DOI： 10.2320/matertrans.mt-n2022004

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Publishing type：Research paper (scientific journal)  

The apparent activation energy of sintering for 8-mol%-Y2O3-doped ZrO2 during shrinkage-rate-controlled flash sintering was determined using a master sintering curve. The activation energy during SCF sintering was found to decrease from approximately 700 to 430 kJ/mol with density. The activation energy in a high-density region is approximately similar value of lattice diffusion, 460 kJ/mol. The relative density range over which the decrease in activation energy occurred during SCF sintering was smaller than during thermal sintering and further moved to a lower temperature range. The increase in shrinkage rate at lower temperatures that occurs during SCF sintering could be considered to be related to this decrease in activation energy.

DOI： 10.2320/matertrans.MT-T2023002

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Publishing type：Research paper (scientific journal)   Publisher：Japan Institute of Metals  

DOI： 10.2320/matertrans.MT-M2023048

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Language：English   Publishing type：Research paper (scientific journal)   Publisher：Elsevier BV  

DOI： 10.1016/j.ceramint.2022.06.185

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Language：English   Publishing type：Research paper (scientific journal)   Publisher：American Chemical Society (ACS)  

DOI： 10.1021/acsaelm.2c00691

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Language：English   Publishing type：Research paper (scientific journal)   Publisher：Royal Society of Chemistry ({RSC})  

DOI： 10.1039/d2cc02510h

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Language：English   Publishing type：Research paper (scientific journal)   Publisher：Elsevier BV  

DOI： 10.1016/j.micron.2022.103289

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Publishing type：Research paper (scientific journal)   Publisher：Royal Society of Chemistry (RSC)  

1-Hexanoic acid stabilised copper nanoparticles were obtained. Cu₆₄O phase could be found on the particle surface. During sintering, the stabilising molecule, 1-hexanoic acid, reduced Cu₆₄O to Cu and it introduced neckings between the particles.

DOI： 10.1039/d1ma01242h

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Language：English   Publishing type：Research paper (scientific journal)   Publisher：Elsevier BV  

DOI： 10.1016/j.ceramint.2022.01.069

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Language：English   Publishing type：Research paper (scientific journal)   Publisher：Elsevier BV  

DOI： 10.1016/j.actamat.2022.117704

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Language：English   Publishing type：Research paper (scientific journal)   Publisher：American Chemical Society (ACS)  

DOI： 10.1021/acsomega.2c00359

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Language：English   Publishing type：Research paper (scientific journal)   Publisher：Wiley  

Herein, we investigated the surface of an (La_0.3Sr_0.7)(Al_0.65Ta_0.35)O₃ (LSAT) single crystal via scanning transmission electron microscopy (STEM) after annealing in air. We found amorphous mounds and atomically flat surfaces formed on the surface of the (100) LSAT single crystal subsequent to heat treatment. These surface mounds mainly constituted SrO, including ~50 at.% Al. The atomically flat surface showed a B‐site termination determined by the direct surface observation at the atomic scale through HAADF‐STEM. The atomic arrangements on the surface were accommodated by surface‐mound formation and La evaporation. Consequently, the ordered structure disappeared because of the increase in the Ta content at the terminated B‐site layer.

DOI： 10.1002/sia.7043

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Other Link： https://onlinelibrary.wiley.com/doi/full-xml/10.1002/sia.7043

Language：English   Publishing type：Research paper (scientific journal)   Publisher：American Chemical Society ({ACS})  

DOI： 10.1021/acsomega.1c06769

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Language：English   Publishing type：Research paper (scientific journal)   Publisher：Royal Society of Chemistry (RSC)  

Nanoporous ultra-high-entropy alloys containing 14 elements (Al, Ag, Au, Co, Cu, Fe, Ir, Mo, Ni, Pd, Pt, Rh, Ru, and Ti) were obtained by dealloying. The products showed excellent electrocatalytic performance for water splitting in acidic media.

DOI： 10.1039/d1sc01981c

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Language：Japanese   Publishing type：Research paper (scientific journal)  

The shrinkage behavior of barium titanate (BaTiO3) green compacts during flash sintering with a square alternating current (AC) field including a zero-field duration (AC-pulse wave) was investigated. It was found that an AC-pulse wave is effective for the densification of BaTiO3 green compacts without reduction and discharge, which is confirmed by transmission electron microscopy and electron energy loss spectroscopy. BaTiO3 sintered polycrystal was obtained at a furnace temperature of 1000 °C by the optimal AC-pulse conditions of 285 V/cm at 250 Hz and a duty ratio of 30 %. A waveform with alternating polarity and the inclusion of a zero-field duration is shown to be possibly useful for flash sintering of oxide materials including altervalent cations.

DOI： 10.2109/jcersj2.20181

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Language：English   Publishing type：Research paper (scientific journal)   Publisher：PERGAMON-ELSEVIER SCIENCE LTD  

Carbon materials have previously been reported to work as catalysts for hydrogen (H-2) production from hydrocarbons. Mechanisms of the catalytic behavior of graphite and carbon black (CB) have often been discussed in literature. Graphite and CB is constructed from mainly 6-membered rings with sp(2) bonds. To understand the catalytic behavior of carbon materials for H-2 production by methane (CH4) decomposition, the catalytic behavior of fullerenes with 6-membered rings and also those comprising 5- and 7-membered rings with sp(2) bonds and their associated mechanisms should be investigated. In this study, the fullerene catalyst activity has been investigated using gas chromatography and the electronic states and nanoscale structures have been analyzed.H-2 production started at 400 degrees C and the H-2 production rate gradually increased with time, and the activation energy of the fullerene for H-2 production by CH4 decomposition was found to be 166 kJ/mol. Moreover, in situ heating X-ray photon spectroscopy (XPS) measurements showed that the pi-pi* transition signal becomes stronger with increasing temperature above the threshold of 300 degrees C. The transition of the pi. electrons to pi* orbitals upon heating is expected to decompose CH 4 absorbed on fullerene. Moreover, transmission electron microscopy (TEM) analysis revealed that the generated carbon atoms from the CH4 decomposition were deposited onto the surfaces of the fullerenes, forming amorphous and layered concentric sphere carbon. Amorphous carbon is reported to not work as a catalyst for CH4 decomposition at around 400 degrees C. From XPS analysis and TEM observations of these two structures, it is anticipated that the ring structures without 6-membered rings in carbon materials with sp(2) bonding contribute to this catalytic behavior for CH4 decomposition at a low temperature of 400 degrees C. (C) 2020 Hydrogen Energy Publications LLC. Published by Elsevier Ltd. All rights reserved.

DOI： 10.1016/j.ijhydene.2020.03.178

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Language：English   Publishing type：Research paper (scientific journal)   Publisher：ELSEVIER SCI LTD  

We investigated the photoluminescence (PL) properties of 3 mol%Y2O3-ZrO2 (3YSZ) polycrystals. The 3YSZ polycrystals were prepared by an isothermal flash sintering technique in which an alternating electric field was applied at a predetermined furnace temperature. After flash sintering, clear, visibly blue PL at 2.82 eV (440 nm) was confirmed under an ultraviolet light (3.4 eV (365 nm)); however, no visible PL was observed from 3YSZ polycrystals conventionally sintered using the same raw powders. Thus, the emission of blue PL was induced by the electric field applied during sintering. The obtained PL band was related to excitation at 3.87 eV (320 nm), which is possibly assigned to the singly ionized associated oxygen vacancy defects (AOD + centers). Furthermore, the blue emission was stable after high temperature annealing at 1400 degrees C for 1 h in air. We possibly attribute the emission of this PL to the stabilization of AOD + centers by the electric field loading during flash sintering.

DOI： 10.1016/j.jeurceramsoc.2019.12.060

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Language：English   Publishing type：Research paper (scientific journal)   Publisher：WILEY  

The effect of direct current (DC) and alternating current (AC) on nitridation of 3 mol% Y2O3-doped ZrO2 (3YSZ) after keeping in a flash state for 1 hour was investigated. The inside of the DC-flashed compact was confirmed to exhibit blacking. Scanning transmission electron microscopy, electron energy loss spectroscopy, and X-ray diffraction analysis revealed that zirconium nitrides formed in the blackened area. In contrast, a uniformly densified compact without blackening was obtained by AC fields. No zirconium nitrides formed in the compacts exposed to AC fields even when the flash state was maintained for 1 hour. Therefore, AC fields are effective to suppress nitridation of 3YSZ during flash sintering.

DOI： 10.1111/jace.16990

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Language：English   Publishing type：Research paper (scientific journal)   Publisher：ROYAL SOC CHEMISTRY  

Precise design of hollow nanostructures can be realized via various approaches developed in the last two decades, endowing nanomaterials with unique structures and outstanding performances, showing their usefulness in a broad range of fields. Herein, we demonstrate the formation of SnO2@SiO2 hollow nanostructures, for the first time, by interaction between liquid state Sn cores and SiO2 shell structures inside Sn@SiO2 core-shell nanoparticles with real-time observation via in situ transmission electron microscopy (TEM). Based on the in situ results, designed transformation of the nanoparticle structure from core-shell Sn@SiO2 to yolk-shell Sn@SiO2 and hollow SnO2@SiO2 is demonstrated, showing the controllable structure of core-shell Sn@SiO2 nanoparticles via fixing liquid-state Sn inside a SiO2 shell which has a certain Sn containing capacity. The present approach expands the toolbox for the design and preparation of yolk-shell and hollow nanostructures, thus providing us with a new strategy for fabrication of more complicated nanostructures.

DOI： 10.1039/c9na00782b

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Language：English  

Pt/Au alloy nanoparticles (NPs) in a wide composition range have been synthesized by room-temperature simultaneous sputter deposition from two independent magnetron sources onto liquid PEG (MW = 600). The prepared NPs were alloyed with the face-centered cubic (fcc) structure. In addition, the particle sizes, composition, and shape are strongly correlated but can be tailored by an appropriate variation of the sputtering parameters. No individual particle but large agglomerates with partial alloy structure formed at Pt content of less than 16 atom %. Highly dispersed NPs with no agglomeration were observed in PEG when the quantity of Pt is more than 26 atom %. On the other hand, a small amount of Pt could terminate the agglomeration of Au when sputtering on the grids for transmission electron microscope observation. Our experiment and computer simulation carried out by two different methods indicate that the composition-dependent particle size of Pt/Au can be explained by the atomic concentration, formation energy of the cluster, and interaction between different metal atoms and the PEG molecule.

DOI： 10.1021/acs.langmuir.0c00152

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Language：Japanese   Publishing type：Research paper (scientific journal)   Publisher：Royal Society of Chemistry (RSC)  

<p>In this work, we introduce a green synthesis technique, double-target sputtering into a liquid polymer – polyethylene glycol (PEG, M. W. = 600), to synthesize palladium–copper (Pd–Cu) alloy nanoparticles (NPs) dispersed in PEG.</p>

DOI： 10.1039/d0nj00288g

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Language：Japanese   Publishing type：Research paper (scientific journal)  

© 2020 The Japan Society of Applied Physics. Photoluminescence band variation of Y2O3-doped ZrO2 (YSZ) polycrystals was investigated for flash-sintered YSZ polycrystals. Nearly full density could be obtained by flash sintering under an alternating current field of 100 V cm-1, 100 Hz, limiting current of 1000 mA and at 1200 °C for 5 min. The flash-sintered YSZ polycrystals emitted blue photoluminescence even at room temperature under excitation of a handheld ultraviolet light, which could be observed with the naked eye. By contrast, conventionally sintered YSZ polycrystals emitted no photoluminescence despite using the same raw powders. In addition, the photoluminescence bands were tunable by varying the Y2O3 content.

DOI： 10.35848/1882-0786/ab7710

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Language：English   Publishing type：Research paper (scientific journal)   Publisher：AMER CHEMICAL SOC  

This research is devoted for the synthesis of Fe oxide and Fe nanoparticles (NPs) via, respectively, thermal decomposition of iron(III) oleate and H-2 reduction of either iron(III) oleate or iron oxide NPs in a NaCl matrix. Lowering the weight ratios of metal precursor to NaCl and synthesis temperature results in smaller particle sizes. A higher uniformity of Fe NPs can be achieved with a two-step synthesis, that is, thermal decomposition of iron oleate followed by H-2 reduction of iron oxides, with the milling of iron oxides and NaCl prior to the reduction step. Fe NPs obtained in this study are stable in the air for long-time storage. It is found that thin oxide and C layers on the particle surface are responsible for their stability.

DOI： 10.1021/acssuschemeng.9b03950

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Language：English   Publishing type：Research paper (scientific journal)   Publisher：CERAMIC SOC JAPAN-NIPPON SERAMIKKUSU KYOKAI  

A simple technique to control the specimen electric current during flash sintering was developed using AC electric fields in 3 mol% Y2O3-doped ZrO2. Flash sintering is characterized by the occurrence of a flash event, i.e., a spike in the specimen electric current, which makes it difficult to control the specimen electric current at/after the flash event for AC electric fields. However, AC electric fields are very attractive from the viewpoint of a suppression of the severe reduction arising from the unidirectional ionic flow during the flash event, which is a fatal phenomenon with DC electric fields. In this study, we develop a simple technique to control the AC electric fields at/after the flash event by limiting the AC electric fields under certain values. As a result, the flash state after the flash event is successfully maintained. Further, it is found that 3 mot% Y2O3-doped ZrO2 compacts prepared by DC- and AC-flash sintering emit blue fluorescence (FL) under 254 nm ultraviolet tight. The blue FL is not obtained in the compacts prepared by conventionally-sintering. The application of electric fields is confirmed to result in the blue florescent properties of 3 mot% Y2O3-doped ZrO2 compacts. (C) 2019 The Ceramic Society of Japan. All rights reserved.

DOI： 10.2109/jcersj2.19144

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Language：Japanese   Publishing type：Research paper (scientific journal)   Publisher：American Chemical Society (ACS)  

DOI： 10.1021/acsaem.9b01736

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Language：English   Publishing type：Research paper (scientific journal)  

A two-dimensional nanocarbon, graphene, has attracted substantial interest due to its excellent properties. The reduction of graphene oxide (GO) has been investigated for the mass production of graphene used in practical applications. Different reduction processes produce different properties in graphene, affecting the performance of the final materials or devices. Therefore, an understanding of the mechanisms of GO reduction is important for controlling the properties of functional two-dimensional systems. Here, we determined the average structure of reduced GO prepared via heating and photoexcitation and clearly distinguished their reduction mechanisms using ultrafast time-resolved electron diffraction, time-resolved infrared vibrational spectroscopy, and time-dependent density functional theory calculations. The oxygen atoms of epoxy groups are selectively removed from the basal plane of GO by photoexcitation (photon mode), in stark contrast to the behavior observed for the thermal reduction of hydroxyl and epoxy groups (thermal mode). The difference originates from the selective excitation of epoxy bonds via an electronic transition due to their antibonding character. This work will enable the preparation of the optimum GO for the intended applications and expands the application scope of two-dimensional systems.

DOI： 10.1021/acsnano.9b03060

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Language：Japanese   Publisher：American Chemical Society ({ACS})  

DOI： 10.1021/acsanm.9b00703

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Language：English  

We use a green sputtering technique to deposit a Pt/Cu alloy target on liquid polyethylene glycol (PEG) to obtain well-dispersed and stable Pt29Cu71 alloy nanoparticles (NPs). The effects of sputtering current, rotation speed of the stirrer, sputtering time, sputtering period, and temperature of PEG on the particle size are studied systematically. Our key results demonstrate that the aggregation and growth of Pt/Cu alloy NPs occurred at the surface as well as inside the liquid polymer after the particles landed on the liquid surface. According to particle size analysis, a low sputtering current, high rotation speed for the stirrer, short sputtering period, and short sputtering time are found to be favorable for producing small-sized single crystalline alloy NPs. On the other hand, varying the temperature of the liquid PEG does not have any significant impact on the particle size. Thus, our findings shed light on controlling NP growth using the newly developed green sputtering deposition technique.

DOI： 10.1021/acs.langmuir.9b01112

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Language：English   Publishing type：Research paper (scientific journal)   Publisher：AMER CHEMICAL SOC  

The most commonly used phase change materials (PCMs), like organic compounds and inorganic salts, were limited in application by their low thermal conductivity. Herein, for the first time, alumina-encapsulated metallic Sn-based PCMs, named Sn@Al2O3, were successfully fabricated with tunable size (60-2000 nm) by a facile process from low-cost chemicals. The robust fabrication process consists of a surfactant-free solvothermal synthesis of SnO2 spheres, boehmite treatment on SnO2 spheres, calcination in the air, and the final hydrogen reduction to transform SnO2 to metallic Sn, endowing the PCMs with high potential for mass production. The as-obtained Sn@Al2O3 showed a core-shell structure, in which a main metallic Sn core located in the center covered with an Al2O3 shell with small Sn nanoparticles distributed inside. The boehmite treatment, in which the penetration of aluminum species into SnO2 spheres played an important role, was found to be responsible for the unique structure formation of final Sn@Al2O3. The understanding of structure formation mechanism gives the possibilities of a new facile way for the synthesis of metal nanoparticles and particle-distributed nanostructures. The obtained Sn@Al2O3 particles not only have high PCM content (92.37 wt %) but also show a stable thermal behavior and morphology during 100 melt freeze cycles in the air atmosphere. Furthermore, the low melting temperature of the PCM core, combined with high thermal conductivity of both core material (Sn, 66.8 W m(-1) K-1) and shell material (Al2O3, 35 W m(-1) K-1), makes Sn@Al2O3 potentially suitable for rapid thermal energy storage in the range 100-300 degrees C.

DOI： 10.1021/acsanm.9b00649

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Language：English   Publishing type：Research paper (scientific journal)   Publisher：ROYAL SOC CHEMISTRY  

Methane reforming at low temperatures is of growing importance to mitigate the environmental impact of the production of synthesis gas, but it suffers from short catalyst lifetimes due to the severe deposition of carbon byproducts. Herein, we introduce a new class of topology-tailored catalyst in which tens-of-nanometer-thick fibrous networks of Ni metal and oxygen-deficient Y2O3 are entangled with each other to form a rooted structure, i.e., Ni#Y2O3. We demonstrate that the rooted Ni#Y2O3 catalyst stably promotes the carbon-dioxide reforming of methane at 723 K for over 1000 h, where the performance of traditional supported catalysts such as Ni/Y2O3 diminishes within 100 h due to the precluded mass transport by accumulated carbon byproducts. In situ TEM demonstrates that the supported Ni nanoparticles are readily detached from the support surface in the reaction atmosphere, and migrate around to result in widespread accumulation of the carbon byproducts. The long-term stable methane reforming over the rooted catalyst is ultimately attributed to the topologically immobilized Ni catalysis centre and the synergistic function of the oxygen-deficient Y2O3 matrix, which successfully inhibits the accumulation of byproducts.

DOI： 10.1039/c8sc04965c

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Scopus

PubMed

Language：English  

The development of efficient catalysts with high activities and durabilities for use in the dry reforming of methane (DRM) is desirable but challenging. We report the development of a nanoporous nickel composite (nanoporous Ni/Y2O3) via a facile one-step dealloying technique, for use in the DRM. Focusing on the low-temperature DRM, our composite possessed remarkable activity and durability against coking compared with conventional particle-based Ni catalysts. This was attributed to the aluminum oxides present on the Ni surface, which suppress pore coarsening. In addition, the inert bundled Y2O3 nanowires are suitable for use as substrates for nanoporous Ni.

DOI： 10.1021/acsomega.8b02023

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Scopus

PubMed

Language：English   Publishing type：Research paper (scientific journal)   Publisher：WILEY  

It is difficult to obtain pure ZrO2 sintered compacts with a bulk style at room temperature because a large volumetric expansion from tetragonal to monoclinic phase (t/m) transformation occurs at around 1000 degrees C, which is lower than the sintering temperature. In contrast, pure monoclinic ZrO2 can be consolidated without shattering using flash-sintering at 1350 degrees C for 5minutes under an applied DC electric field of 175V/cm. High-resolution transmission electron microscopy and electron energy loss spectroscopy have revealed that amorphous films are formed along grain boundaries after flash-sintering at 1350 degrees C for 5minutes. Monoclinic ZrO2 flash-sintered compact including the amorphous films are able to survive without shattering through the t/m transformation, as the amorphous films partially absorb the large volumetric expansion arising from the t/m transformation. The formation of the amorphous films results from the severe reducing condition due to the applied DC electric fields during flash-sintering.

DOI： 10.1111/jace.15485

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Scopus

Language：English   Publishing type：Research paper (scientific journal)   Publisher：Royal Society of Chemistry  

Au/Ag alloy nanoparticles (NPs) were successfully prepared by a one step synthesis using HAuCl4 and [Ag(NH3)2]+ as the corresponding precursors in a microwave-induced plasma in liquid process (MWPLP) without the addition of any organic protecting or reducing agents. The time dependent reduction and particle formation during the 140 min plasma discharge were studied with TEM, UV-vis extinction spectra, and ICP-OES. After 140 min, the HAADF-STEM and EDX results indicated that the obtained Au/Ag NPs were alloy NPs. Varying the input molar ratios of the metal precursors allowed for control of the composition of the Au/Ag alloy NPs.

DOI： 10.1039/c7nj05154a

Web of Science

Scopus

Language：English   Publishing type：Research paper (scientific journal)   Publisher：AMER CHEMICAL SOC  

We herein present the preparation of short, bulky cationic thiolate (thiocholine)-protected fluorescent Au nanoclusters via sputter deposition over a liquid polymer matrix. The obtained Au nanoclusters showed near-infrared fluorescence and had an average core diameter of 1.7 +/- 0.6 nm, which is too large compared to that of the reported fluorescent Au nanoclusters prepared via chemical means. We revealed the mechanism of formation of this unique material using single particle electron microscopy, optical measurements, X-ray photoelectron spectroscopy (XPS), and high-performance liquid chromatography fractionations. The noncrystallized image was observed via single-particle high-angle annular dark-field scanning transmission electron microscopy observations and compared with chemically synthesized crystalline Au nanoparticle with the same diameter, which demonstrated the unique structural characteristic speculated via XPS. The size fractionation and size-dependent fluorescence measurement, together with other observations, indicated that the nanoclusters most probably contained a mixture of very small fluorescent species in their aggregated form and were derived from the sputtering process itself and not from the interaction between thiol ligands.

DOI： 10.1021/acs.langmuir.8b00067

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PubMed

Language：English   Publishing type：Research paper (scientific journal)   Publisher：AMER CHEMICAL SOC  

Alloy nanoparticles (NPs) of a bimetal system, Au/Cu, that form intermetallic compounds in a bulk state have been successfully produced using a double-target sputtering technique onto a low-cost and biocompatible liquid polymer (polyethylene glycol, PEG). The formation of an Au/Cu solid solution alloy in individual NPs was revealed by scanning transmission electron microscopy-energy-dispersive X-ray elemental mapping analysis. Altering the sputter currents for Au and Cu targets resulted in a tailored NP composition, but the particle sizes did not significantly vary. We found similar structures, sizes, and optical properties of Au/Cu NPs obtained by double-head sputtering on carbon-coated transmission electron microscopy grids or PEG and by Au/Cu alloy target sputtering. Random alloy formation occurred in matrix sputtering using double-target heads. This method is advantageous for manipulating the alloy composition through highly independent control of sputter parameters for each metal target.

DOI： 10.1021/acs.langmuir.7b03194

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PubMed

Language：English   Publishing type：Research paper (scientific journal)   Publisher：MDPI AG  

We performed in-situ transmission electron microscopy (TEM) on a dealloyed nanoporous NiCo catalyst used for the dry reforming of methane (DRM) to investigate the origin of the catalytic activity and structural durability. The in-situ observations and local chemical analysis indicated that the DRM induced chemical demixing of Ni and Co accompanied by grain refinement, implying possible synergic effects in a general bimetallic NiCo catalyst when used for the DRM.

DOI： 10.3390/met7100406

Web of Science

Scopus

Language：English   Publishing type：Research paper (scientific journal)   Publisher：WILEY  

Consolidated, monoclinic ZrO2 polycrystal was produced from undoped ZrO2 powders in air by flash sintering at the sintering temperature of 1350 degrees C for 5minutes or 3hours under an applied DC electric field of 175V/cm. When the ZrO2 was heated under the applied DC field, the electric current of the specimen steeply increased at the furnace temperature of 1335 degrees C below the sintering temperature of 1350 degrees C. When the furnace temperature was decreased from the sintering temperature of 1350 degrees C to room temperature, volumetric expansion associated with tetragonal-to-monoclinic phase transformation gradually took place at the furnace temperature from 1000 degrees C to 750 degrees C, and monoclinic ZrO2 body was remained consolidated even at room temperature in both specimens. In contrast, conventionally sintered ZrO2 without applying DC field exhibited the abrupt volumetric expansion at about 1000 degrees C, and shattered. SEM observation revealed the presence of grain-boundary second phase in the flash-sintered specimen for 3hours, which is a possible origin of keeping a bulk body at room temperature. The thinner second phase is considered to be formed also in the flash-sintered specimen for 5minutes, although the formation of the phase could not be observed clearly by SEM observation. On the other hand, XRD measurements showed that <001> directions of the monoclinic ZrO2 grains were oriented along the applied DC field after the isothermal flash sintering for 3hours while the grain alignment could not be observed in flash-sintered specimen for 5minutes. The alignment of ZrO2 grains observed in the isothermal flash sintering is considered to be closely related to the preferential direction of oxygen ionic conduction and the second phase formed along grain boundaries.

DOI： 10.1111/jace.14954

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Scopus

Language：English   Publishing type：Research paper (scientific journal)   Publisher：WILEY  

In BaTiO3, flash-sintering associated with a surge of the specimen electric current sometimes results in an inhomogeneous microstructure including Ti-excess secondary phases because of discharging. We applied field-assisted sintering technique (FAST) under precisely controlled specimen current that was set just below the threshold value for the occurrence of flash event for BaTiO3, to avoid the occurrence of the discharging. As a result, uniform and fine-grained compacts were obtained without any secondary phases. A relative density of approximately 92% was achieved under FAST condition of 100 V/cm with a limiting current of 72 mA and soaking time of 3 hours at 1070 degrees C. The voltages during sintering under a constant current of 72 mA were found to decrease during the soaking process. Electron energy loss spectroscopy revealed the generation of excess oxygen vacancies at/near grain boundaries. The excess oxygen vacancies induced by application of DC electric fields were confirmed to reduce the voltages and to retard the shrinkage rate in a final sintering stage.

DOI： 10.1111/jace.14938

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Scopus

Language：English   Publishing type：Research paper (scientific journal)   Publisher：AMER CHEMICAL SOC  

For the first time, investigation on the effect of lowering the synthesis temperature below room temperature (10 to -10 degrees C) and increasing the viscosity of the reaction solution at certain temperatures has been used to trigger the formation of single-crystalline ss-Sn nanorods (NRs) in a chemical synthesis using an organic solvent. These two parameters govern the energy of the particles in the solution, thereby mediating the selective attachment to the nuclei and the preferential growth of Sn along the c-axis. The length and aspect ratio of the NRs were inversely proportional to the synthesis temperature and directly proportional to the viscosity of the reaction solution. In addition, we found that poly(vinylpyrrolidone) with a high molecular weight aided the formation of longer and higher aspect ratio NRs via the bridge flocculation effect.

DOI： 10.1021/acs.cgd.7b00227

Web of Science

Language：English   Publishing type：Research paper (scientific journal)   Publisher：AMER CHEMICAL SOC  

Production of oxygen-deficient tungsten oxide nanoparticles with a diameter of around 10 nm have been successfully developed using a microwave-induced plasma in liquid technique. The prepared blue-green nanoparticles exhibit strong absorption in the visible region; thus, these could be efficient visible-light photocatalysts. The high-angle annular dark-field images revealed the dislocation of tungsten, which causes oxygen deficiencies.

DOI： 10.1021/acsomega.7b00986

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PubMed

Language：English   Publishing type：Research paper (scientific journal)   Publisher：PERGAMON-ELSEVIER SCIENCE LTD  

Nanofluidics in CNTs is argumentative though it is theoretically calculated by various reports. It is because only a few of experimental reports are available, and the measured permeability is not so large as that suggested from the theoretical calculations. Also, water motion suppression in the confined space has not been exhibited by flux measurement. The present work explores these yet-unsolved discrepancies using the measurable size membrane of vertically aligned double-walled carbon nanotube array, which is borne with durability and flexibility, and a conventional measurement method is applied to the membranes. Water motion suppression occurs in the CNT confined space significantly, depending on temperature. Additionally, it is confirmed that the obtained permeability correlates to the reported experimental results with regard to the relationship between CNT length and permeability, and the correlation does not agree with permeability calculated from the Hagen-Poiseuille law. These results pose an insight into the inherent water transport characteristics in the CNT confined space. (C) 2017 Elsevier Ltd. All rights reserved.

DOI： 10.1016/j.carbon.2017.05.034

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Scopus

Language：English   Publishing type：Research paper (scientific journal)   Publisher：ROYAL SOC CHEMISTRY  

Catalytic remediation of automobile exhaust has relied on precious metals (PMs) including platinum (Pt). Herein, we report that an intermetallic phase of Ni and niobium (Nb) (i.e., Ni3Nb) exhibits a significantly higher activity than that of Pt for the remediation of the most toxic gas in exhaust (i.e., nitrogen monoxide (NO)) in the presence of carbon monoxide (CO). When subjected to the exhaust-remediation atmosphere, Ni3Nb spontaneously evolves into a catalytically active nanophase-separated structure consisting of filamentous Ni networks (thickness < 10 nm) that are incorporated in a niobium oxide matrix (i.e., NbOx (x < 5/2)). The exposure of the filamentous Ni promotes NO dissociation, CO oxidation and N-2 generation, and the NbOx matrix absorbs excessive nitrogen adatoms to retain the active Ni-0 sites at the metal/oxide interface. Furthermore, the NbOx matrix immobilizes the filamentous Ni at elevated temperatures to produce long-term and stable catalytic performance over hundreds of hours.

DOI： 10.1039/c6sc05473k

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PubMed

Language：English   Publishing type：Research paper (scientific journal)   Publisher：CERAMIC SOC JAPAN-NIPPON SERAMIKKUSU KYOKAI  

Recently, carbon materials were reported to work as catalysts for the production of H-2 from hydrocarbons. However, the hydrogen production rate is extremely low. To broaden the scope of carbon materials as catalysts for the decomposition of hydrocarbons, a higher H-2 production rate is required. Thus, the hydrogen production rate under conditions employing a low flow rate of hydrocarbon per unit area and a large quantity of carbon materials as the catalyst should be evaluated, and the influence of these conditions on the rate of H-2 production by carbon materials should be discussed. Herein, the H-2 production rate was measured under conditions employing a low flow rate of CH4 and a large quantity of carbon black (CB) as a catalyst. H-2 production started at 600 degrees C and the production rate was less than 0.1%. The transmission electron microscope image of CB heated in CH4 atmosphere demonstrated that a low flow rate of CH4 does not affect the reaction site (i.e., graphite edges) of CB. However, the H-2 production rate was extremely low compared to that achieved with a high flow rate. It is proposed that there is an optimal flow rate for maintaining the catalytic activity at the graphite edge of CB for decomposition of CH4. (C) 2017 The Ceramic Society of Japan. All rights reserved.

DOI： 10.2109/jcersj2.16246

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Scopus

Language：English   Publishing type：Research paper (scientific journal)   Publisher：CHEMICAL SOC JAPAN  

Au/Pd alloy nanoparticles (NPs) were successfully synthesized using HAuCl4, H2PdCl4, and alpha-thioglycerol as precursors and a stabilizer, respectively, by microwave-induced plasma in liquid process (MWPLP). After only several minutes of microwave irradiation, metallic NPs were obtained in aqueous environment without any reducing agent. The reduction mechanism of metal ions was confirmed by UV-vis spectral changes. The results from HAADF-STEM and EDS indicated that synthesized NPs were bimetallic Au/Pd. Moreover, XRD patterns of synthesized NPs implied that the composition of bimetallic NPs could be controlled by changing the initial ratio of metal precursors.

DOI： 10.1246/bcsj.20160333

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Scopus

Language：English   Publishing type：Research paper (scientific journal)   Publisher：ELSEVIER SCI LTD  

WC grains in WC-Co alloys are shaped as truncated triangular prisms, each with a basal plane of a (0001) truncated triangle and two {1 (1) over bar 00} prismatic planes, one narrower and one wider. This anisotropic shape is related to the polarity of the WC lattice, which comes from the difference in the spacing of the W and C layers in the &lt;0001&gt; projection. We directly determined the relationship between the two {1 (1) over bar 00} prismatic planes and the polarity of the WC lattice by using high-resolution scanning transmission electron microscopy (STEM). High-angle annular dark-field STEM and annular bright-field STEM revealed that the wider prismatic plane had W and C atomic layers with a shorter spacing, while the narrower plane had a longer spacing. The WC/Co interface on the wider prismatic side was atomically flat, while many steps formed on the surface of the narrower prismatic side. This difference in step formation at these interfaces could have come from the difference in how their W-C bonds formed. (C) 2016 Elsevier Ltd. All rights reserved.

DOI： 10.1016/j.ijrmhm.2016.10.013

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Language：English   Publishing type：Research paper (scientific journal)  

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Web of Science

Language：English   Publishing type：Research paper (international conference proceedings)   Publisher：IEEE  

This paper presents a growth and characterization of vertically aligned PdxCo1-x alloy encapsulated inside Multi-Walled Carbon Nanotube (MWCNT) arrays on Pd/Co thin layers coated on Si substrate by a dc bias-enhanced plasma chemical vapor deposition (CVD) method. The Metal Alloy Encapsulated within MWCNTs (MAE-MWCNTs) were characterized by a scanning electron microscope (SEM) and a transmission electron microscopy (TEM). The SEM images show the teardrop-shape particles encapsulated within the tube top of MWCNTs. A vibrating sample magnetometer was used to study the magnetism of a large number of MAE-MWCNTs on Si substrate at room temperature. The hysteresis loop of the ME-MWCNTs shows clear ferromagnetic behavior and the easy axis of magnetization is parallel to the MEA-MWCNT tube axis, as can be elucidated from the large coercive fields and remanence values. Moreover, TEM off-axis electron holograms were used to study the magnetism of the individual MAE-MWCNT or the two pair of MAE-MWCNTs. Based on electron holography, we have successfully obtained the saturation magnetization of 0.7 T and 1.12 T for the individual MAE-MWCNT with diameters of 41 nm and 83 nm, respectively.

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Event date： 2021.5

Language：Japanese   Presentation type：Oral presentation (general)  

Venue：オンライン   Country：Japan  

Event date： 2020.11

Language：Japanese   Presentation type：Poster presentation  

Event date： 2020.11

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Event date： 2020.6

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Venue：愛知，分子科学研究所 明大寺キャンパス   Country：Japan  

Event date： 2016.9

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Venue：北海道大学   Country：Japan  

Event date： 2013.10

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Event date： 2013.10

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Event date： 2013.10

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Country：Taiwan, Province of China  

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Event date： 2011.6 - 2011.7

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Event date： 2004.7

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Event date： 2004.1

Language：Japanese   Presentation type：Poster presentation  

Country：Japan  

徳永智春, 渡邉 啓, 加藤 理, 林 靖彦, 藤 昇一, 金子賢治

Event date： 2003.9

Language：Japanese   Presentation type：Oral presentation (general)  

Country：Japan