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Micheau, C.; 上田 祐生; 元川 竜平; 阿久津 和宏*; 山田 悟史*; 山田 雅子*; Moussaoui, S. A.*; Makombe, E.*; Meyer, D.*; Berthon, L.*; et al.
Journal of Molecular Liquids, 401, p.124372_1 - 124372_12, 2024/05
Supramolecular organization of extractant molecules impacts metal ions separation behavior. Probing bulk and interfacial structures of the relevant systems is expected to provide key insights into the metal ion selectivity and kinetic aspects. The supramolecular features of two solvent extraction systems based on malonamide extractants, N,N,N′,N′-tetrahexylmalonamide (THMA) in toluene and N,N′-dimethyl-N,N′-dibutyl-2-tetradecylmalonamide (DBMA) in n-heptane, were studied using small-angle X-ray scattering for the organic bulk phases, as well as interfacial tension and neutron reflectivity measurements for the interfaces. In the bulk solution, THMA forms dimeric/trimeric associates but no aggregates in toluene, while DBMA forms large aggregates in n-heptane. On the other hand, THMA accumulates in a diffuse layer at the interface at high THMA concentration, whereas DBMA forms a compact but thinner layer. After Pd(II) extraction, the thickness of interfacial layers decreases in the case of THMA, and totally vanishes in the case of DBMA. Based on these new structural information, two mechanisms are proposed for Pd(II) and Nd(III) extraction with malonamides. In toluene, THMA associates slightly accumulate in the vicinity of the interface, then coordinate Pd(II) and diffuse into the organic bulk phase. In n-heptane, DBMA aggregates adsorb at the interface then pick up Nd(III) cations in their polar cores and finally diffuse into the bulk.
-Ga
O
(001)Tsai, Y. H.*; 小畠 雅明; 福田 竜生; 谷田 肇; 小林 徹; 山下 良之*
Applied Physics Letters, 124(11), p.112105_1 - 112105_5, 2024/03
被引用回数：0Recently, gallium oxide (GaO) has attracted much attention as an ultra-wide bandgap semiconductor with a bandgap of about 5 eV. In order to control device properties, it is important to clarify the chemical state of dopants and doping sites. X-ray absorption near edge structure (XANES) and hard X-ray photoemission spectroscopy were used to investigate the dopant sites and chemical states of Sn in Sn-doped -GaO(001) samples. The results show that the chemical state of the Sn dopant is the Sn
oxidation state and that the bond lengths around the Sn dopant atoms are longer due to the relaxation effect after Sn dopant insertion. Comparison of experimental and simulated XANES spectra indicates that the octahedral Ga substitution site in -GaO(001) is the active site of the Sn dopant.
Pt
Al
太田 玖吾*; 渡部 悠貴*; 芳賀 芳範; Iesari, F.*; 岡島 敏浩*; 松本 裕司*
Symmetry (Internet), 15(8), p.1488_1 - 1488_13, 2023/07
被引用回数：1 パーセンタイル：66.09(Multidisciplinary Sciences)Polycrystalline and single crystalline CePtAl samples were synthesized and characterized using EPMA, XRD, XAS and magnetization measurements. The valence of Ce in this compound is trivalent, in agreement with magnetic susceptibility and XAS spectra. The analysis of EXAFS spectra indicates the formation of a honeycomb lattice rather than the disordered hexagonal structure.
X-ray synchrotron diffractionLi, H.*; Liu, Y.*; Zhao, W.*; Liu, B.*; 冨永 亜希; 菖蒲 敬久; Wei, D.*
International Journal of Plasticity, 165, p.103612_1 - 103612_20, 2023/06
被引用回数：3 パーセンタイル：78.7(Engineering, Mechanical)コバルトフリーのマルエージング鋼の強度特性を明らかにするために、高エネルギー放射光X線回折法を利用したその場引張試験を行った。マルテンサイト相とオーステナイト相からの回折プロファイルが得られ、それらの強度及び幅が負荷に伴い変化している様子が観察された。回折プロファイルを解析した結果、時効(as-aged)材では、低応力レベルにてマルテンサイトの含有量が緩やかに減少し、高応力レベルでは急激に減少した。一方、熱処理(as-solution)材では、応力の増加とともにオーステナイト相がマルテンサイト相に著しく転移変態している結果が得られた。これらのことがそれぞれの強度特性に起因していることを明らかにした。
Tsai, T.-H.; 佐々木 新治; 前田 宏治
Journal of Nuclear Science and Technology, 60(6), p.715 - 723, 2023/06
被引用回数：1 パーセンタイル：31.61(Nuclear Science & Technology)A method for processing and visualizing X-ray computed tomography (CT) images of a fuel assembly is developed and applied to a JOYO MK-III fuel assembly. The method provides vertical-section-like images to observe the spatial distribution of CT values in fuel pins and also supplies images that show the relationship between the linear heat rate (LHR) and radial CT-value distribution. In addition, an attempt to analyze the radial cracks in the CT images is proposed, and the results demonstrate the correlation between LHR and the radial cracks.
山崎 泰広*; 篠宮 啓介*; 奥村 忠晴*; 鈴木 賢治*; 菖蒲 敬久; 中村 唯我*
Quantum Beam Science (Internet), 7(2), p.14_1 - 14_12, 2023/05
The suspension plasma spray (SPS) technique has attracted attention because of its various microstructures, which can be achieved by mixing submicron spray particles with a solvent to form a suspension. Thermal barrier coatings (TBCs) with a columnar structure, which might achieve high strain tolerance, can be obtained using the SPS technique. In this study, the internal stress distribution of the SPS-TBC with different columnar structures was evaluated by hybrid measurement using high-energy synchrotron X-ray diffraction analysis and laboratory low-energy X-rays. The effect of microstructure on the internal stress distribution of the SPS-TBC was discussed on the basis of the experimental results. In addition, the in-plane internal stress was decreased by decreasing the column diameter. The thin columnar microstructure of the SPS-TBC has superior strain tolerance. The internal stresses in the column of the SPS-TBC are periodic decrements caused by stress relaxation in porous layers.
吉田 幸彦
IL Nuovo Cimento, 46(2), p.33_1 - 33_8, 2023/03
JAEA is addressing the back-end issues with the steadfast promotion of sustainable measures. The R&D plans are being rationally pursued by considering priorities based on indicators such as bottleneck issues in waste streams, relevance to WAC settings, and effectiveness of cost reduction. In addition, the future vision (JAEA 2050+) has been formulated to promote cross-disciplinary R&D through a new approach that cannot be reached by conventional methods, and active incorporation of information technologies, such as AI technologies. Currently, we are developing intelligent sensing that combines sensing and information processing technologies to realize automatic sorting technology, and non-destructive evaluation technology using high-energy X-ray CT, for legacy wastes. The core technology common to these technologies is image evaluation technology using deep learning models, which was confirmed to perform very well in the evaluation of waste object recognition.
鈴木 智也*; 大坪 右京*; 尾形 剛志*; 塩飽 秀啓; 小林 徹; 矢板 毅; 松岡 光昭*; 村山 憲弘*; 成田 弘一*
Separation and Purification Technology, 308, p.122943_1 - 122943_7, 2023/03
被引用回数：2 パーセンタイル：24.43(Engineering, Chemical)主にAgを含む使用済み製品からPd金属をリサイクルするために硝酸抽出が行われており、ほとんどのPd残留物はAg(I)含有溶液から分離される。しかし、このAg(I)溶液中には少量のPd(II)が残存していることが多い。そのため、硝酸溶液中のPd(II)とAg(I)を分離することは、Pdのリサイクルを効率的に進めるために必要不可欠である。本研究では、アミン(R-Amine),イミノ二酢酸(R-IDA),ピリジン(R-Py),ビスピコリルアミン(R-BPA)で機能化した4種類の窒素ドナー型吸着材を用いて硝酸溶液中のPd(II), Ag(I)を分離する研究を実施した。R-Amine,R-IDA,R-Pyは硝酸溶液からAg(I), Cu(II), Ni(II), Fe(III)を選択的に吸着したが、R-AmineはPdの吸着効率が低いことが判明した。一方、R-BPAはPd(II), Ag(I), Cu(II)を全濃度において90%以上吸着することができた。フーリエ変換赤外分光法及び広域X線吸収微細構造法(EXAFS)による吸着金属イオンの構造解析から、窒素ドナー型吸着剤の分離機構を明らかにした。R-IDA, R-Py, R-BPAへのPd(II)吸着は官能基(それぞれイミノ二酢酸,ピリジン,ビスピコリルアミン)へのPd(II)配位を介して起こり、R-Amineへの吸着はNO
と[Pd(NO)
]
のアニオン交換を介して起こることがわかった。R-IDA,R-Py,R-BPAは、配位性吸着機構により、高いPd(II)吸着挙動を示すことが明らかとなった。塩酸(5.0M)およびチオ尿素(0.1M)溶離液は、それぞれR-IDAから83%およびR-Pyから95%のPd(II)を脱離させた。R-Pyは吸着選択性と脱着効率から最も効果的なPd(II)吸着剤だった。
synchrotron X-ray scattering and nanoindentation testIm, S.*; Jee, H.*; Suh, H.*; 兼松 学*; 諸岡 聡; Choe, H.*; 西尾 悠平*; 町田 晃彦*; Kim, J.*; Lim, S.*; et al.
Construction and Building Materials, 365, p.130034_1 - 130034_18, 2023/02
被引用回数：6 パーセンタイル：70.19(Construction & Building Technology)Nanocrystalline calcium-silicate-hydrate (C-S-H) is a typical heterogeneous material with a multiscale structure spanning a wide length scale from angstrom to micrometer, and whose structure is determined by the Ca/Si ratio. In this study, we directly applied compressive loads on synthetic C-S-H pastes with Ca/Si ratios of 0.6-1.2 and investigated their mechanical properties using the elastic modulus calculated at three length scale levels (i.e., angstrom to nanometer, micrometer, and millimeter) via in-situ synchrotron X-ray scattering, nanoindentation tests, and strain gauges, respectively. Further, 
Si nuclear magnetic resonance spectroscopy was conducted on the C-S-H pastes to elucidate the alterations in the silicate polymerization. The experimental results confirmed the deformation behavior of the C-S-H paste with different Ca/Si ratios under external loading, which was demonstrated to be transferred from the surface of the pastes to particles owing to the presence of multiscale pores.
Wang, Q.*; Hu, Q.*; Zhao, C.*; Yang, X.*; Zhang, T.*; Ilavsky, J.*; Kuzmenko, I.*; Ma, B.*; 舘 幸男
International Journal of Coal Geology, 261, p.104093_1 - 104093_15, 2022/09
被引用回数：5 パーセンタイル：69.58(Energy & Fuels)To understanding the spatial heterogeneity of mineral and pore structure variations in fine-grained shale, microscale X-ray fluorescence (micro-XRF) mapping, (ultra-) small-angle X-ray scattering [(U)SAXS] and wide-angle X-ray scattering were applied for two samples from a piece of Eagle Ford Shale in South Texas. Thin section petrography and field emission-scanning electron microscopy, X-ray diffraction (XRD), total organic carbon, and pyrolysis were also utilized to investigate the potential spatial heterogeneity of pore types, mineral and organic matter compositions for both samples. Overall, the siliceous-carbonate mineral contents in these carbonate-rich Eagle Ford Shale vary between laminations at mm scales. By analyzing six selected sub-samples on each of two samples with X-ray scattering and XRD techniques, nm-sized pores are mainly interparticle ones in the higher calcite regions, where the porosity is also relatively lower, while the lower calcite regions consist of both interparticle and intraparticle pore types with higher porosity. Finally, the micro-XRF and (U)SAXS are combined to generate porosity distribution maps to provide more insights about its heterogeneity related to the laminations and fractures at our observational scales.
and CrUO秋山 大輔*; 日下 良二; 熊谷 友多; 中田 正美; 渡邉 雅之; 岡本 芳浩; 永井 崇之; 佐藤 修彰*; 桐島 陽*
Journal of Nuclear Materials, 568, p.153847_1 - 153847_10, 2022/09
被引用回数：3 パーセンタイル：68.71(Materials Science, Multidisciplinary)ウラン酸鉄,ウラン酸クロム、およびその固溶体を合成し、これらのウラン酸塩が異なる熱的安定性を示すメカニズムを研究した。熱的安定性を評価するため、ウラン酸塩試料の熱重量分析を実施した結果、ウラン酸クロムの分解温度(約1250
C)に対してウラン酸鉄は低温(約800C)で分解するが、クロムを含む固溶体では熱分解に対する安定性が高まることが分かった。この熱的安定性と結晶構造との関係性を調べるため、エックス線結晶構造解析,エックス線吸収微細構造測定,メスバウアー分光測定,ラマン分光分析による詳細な結晶構造と物性の評価を行ったが、本研究で用いたウラン酸塩試料の間に明瞭な差異は観測されなかった。そのため、熱的安定性の違いは結晶構造に起因するものではなく、鉄とクロムとの酸化還元特性の違いによるものと推定した。クロムは3価が極めて安定であるのに対して、鉄の原子価は2価と3価を取ることができる。このため、ウラン酸鉄の場合には結晶中でウランと鉄との酸化還元反応が起こり、低温での分解反応を誘起したものと考えられる。
Im, S.*; Jee, H.*; Suh, H.*; 兼松 学*; 諸岡 聡; 小山 拓*; 西尾 悠平*; 町田 晃彦*; Kim, J.*; Bae, S.*
Journal of the American Ceramic Society, 104(9), p.4803 - 4818, 2021/09
被引用回数：18 パーセンタイル：85.31(Materials Science, Ceramics)This study aims to elucidate the effect of heating on the local atomic arrangements, structure, phase transformation, and mechanical properties of synthesized calcium-silicate-hydrate (C-S-H). The alteration in the atomic arrangement of the synthesized C-S-H (Ca/Si = 0.8) and the formation of crystalline phases that occurred in three distinct transformation stages of dehydration (105-200 C), decomposition (300-600 C), and recrystallization (700-1000 C) were investigated via powder X-ray diffraction, Si nuclear magnetic resonance spectroscopy, and thermogravimetric analysis. Further, the deformation of the local atomic bonding environment and variations in mechanical properties during the three stages were assessed via pair distribution function analysis based on in-situ total X-ray scattering. The results revealed that the C-S-H paste before heating exhibited a lower elastic modulus in real space than that in the reciprocal space in the initial loading stage because water molecules acted as a lubricant in the interlayer. At the dehydration stage, the strain as a function of external loading exhibited irregular deformation owing to the formation of additional pores induced by the evaporation of free moisture. At the decomposition stage, the structural deformation of the main d-spacing (d 
3.0 
) was similar to that of the real space before the propagation of microcracks. At the recrystallization stage, the elastic modulus increased to 48 GPa owing to the thermal phase transformation of C-S-H to crystalline -wollastonite. The results provide direct experimental evidence of the micro- and nanostructural deformation behavior of C-S-H pastes after exposure to high temperature under external loading.
Grazzi, F.*; Cialdai, C.*; Manetti, M.*; Massi, M.*; Morigi, M. P.*; Bettuzzi, M.*; Brancaccio, R.*; Albertin, F.*; 篠原 武尚; 甲斐 哲也; et al.
Rendiconti Lincei. Scienze Fisiche e Naturali, 32(3), p.463 - 477, 2021/09
被引用回数：3 パーセンタイル：22.01(Multidisciplinary Sciences)In this paper, we have studied an additively manufactured metallic component, intended for ultra-high vacuum application, the exit-snout of the MACHINA transportable proton accelerator beam-line. Metal additive manufacturing components can exhibit heterogeneous and anisotropic microstructures. Two non-destructive imaging techniques, X-ray computed tomography and Neutron Tomography, were employed to examine its microstructure. They unveiled the presence of porosity and channels, the size and composition of grains and intergranular precipitates, and the general behavior of the spatial distribution of the solidification lines. While X-ray computed tomography evidenced qualitative details about the surface roughness and internal defects, neutron tomography showed excellent ability in imaging the spatial density distribution within the component. The anisotropy of the density was attributed to the material building orientation during the 3D printing process. Density variations suggest the possibility of defect pathways, which could affect high vacuum performances. In addition, these results highlight the importance of considering building orientation in the design for additive manufacturing for UHV applications.
} polyoxo cluster UO
Cl
(MeO)
(x = 2.3, MeO = methoxide)Fichter, S.*; Radoske, T.*; 池田 篤史
Acta Crystallographica Section E; Crystallographic Communications (Internet), 77(8), p.847 - 852, 2021/08
A new type of polyoxo cluster complex that contains thirteen uranium atoms, {U}, was synthesised and characterised as [U(
-O
)(-O
)(-O)
Cl(O)
] (x = 2.3, MeO = methoxide) (I). The complex crystallises from methanol containing tetravalent uranium (U
) with a basic organic ligand. The characterised {U} polyoxo cluster complex possesses a single cubic uranium polyhedron at the centre of the cluster core. The observed shortening of U-O bonds, together with BVS calculations and the overall negative charge (2-) of (I), suggests that the central uranium atom in (I), that forms the single cubic polyhedron, is presumably oxidised to the pentavalent state (U
) from the original tetravalent state (U). Complex I is, hence, the first example of a polyoxo cluster possessing a single cubic coordination polyhedron of U.
稲見 俊哉*; 菖蒲 敬久; 石井 賢司*
IEEE Transactions on Magnetics, 57(3, Part 2), p.6400105_1 - 6400105_5, 2021/03
被引用回数：0 パーセンタイル：0(Engineering, Electrical & Electronic)Although the observation of magnetic domains well below the surface of a sample appears to be relatively easy, in reality, magnetic domains inside metallic samples have not been investigated in detail due to a lack of adequate techniques. Non-resonant magnetic X-ray diffraction (NRMXRD) is a candidate for such 3-D magnetic microscopy. A relatively small focus size of less than 100 nm and a relatively long attenuation length of more than 100 m can be obtained by using high-energy synchrotron X-rays. However, NRMXRD has a disadvantage in that the magnetic contrast is low. It is known that the magnetic contrast in NRMXRD increases with increasing the total polarization of the incident X-rays. In this feasibility study, we carried out NRMXRD experiments on a metallic iron sample to examine whether the magnetic contrast can be sufficiently enhanced even for high-energy X-rays.
阿部 雄太; 山下 拓哉; 佐藤 一憲; 中桐 俊男; 石見 明洋
Journal of Nuclear Engineering and Radiation Science, 6(2), p.021113_1 - 021113_9, 2020/04
The authors are developing an experimental technology for simulating severe accident (SA) conditions using simulate fuel material (ZrO) that would contribute, not only to Fukushima Daiichi (1F) decommissioning, but also to enhance the safety of worldwide existing and future nuclear power plants through clarification of accident progression behavior. Nontransfer (NTR) type plasma, which has been in practical use with a large torch capacity as high as 2 MW, has the potential to heat subject materials to very high temperatures without selecting the target to be heated. When simulating 1F with SA code, the target of this core-material-melting and relocation (CMMR) experiment was to confirm that NTR plasma has a sufficient heating performance realizing large temperature gradients (
2000 K/m) expected under 1F conditions. The authors selected NTR-type plasma-heating technology that has the advantage of continuous heating in addition to its high-temperature level. The CMMR-2 experiments were carried out in 2017 applying the improved technology (higher heating power and controlled oxygen concentration). The CMMR-2 experiment adopted a 30-min heating period, wherein the power was increased to a level where a large temperature gradient was expected at the lower part of the core under actual 1F accident conditions. Most of the control blade and channel box migrated from the original position. After heating, the simulated fuel assembly was measured by X-ray computed tomography (CT) technology and by electron probe micro-analyzer (EPMA). CT pictures and elemental mapping demonstrated its excellent performance with rather good precision. Based on these results, an excellent perspective, in terms of applicability of the NTR-type plasma-heating technology to the SA experimental study, was obtained.
高橋 宏明*; 舘 幸男
Applied Clay Science, 168, p.211 - 222, 2019/02
被引用回数：9 パーセンタイル：47.52(Chemistry, Physical)異なる膨潤特性をもつNa型及びCs型モンモリロナイトの微細構造と物質移行特性が、ナノフォーカスX線CTによる3次元微細構造分析と重水の拡散実験とを組み合わせて調査された。X線CT観察により、乾燥状態の圧縮Na型モンモリロナイトが飽和膨潤する過程で、連結性マクロ間隙はゲル相によって埋められ、粘土粒子のサイズは小さくなることが確認された。Cs型モンモリロナイトでは、それとは対照的に飽和過程でのゲル相の生成や粒子・間隙サイズの変化は認められなかった。X線CTによって評価された飽和Cs型モンモリロナイトの連結性マクロ間隙の屈曲度及び収れん度を含む幾何学因子は、重水の拡散試験から評価された値と整合した。Na型モンモリロナイトの場合、X線CTと拡散試験から導出された幾何学因子の差異が確認され、これは静電的相互作用による収れん度とX線CTの解像度では観察できないゲル相や層間間隙の屈曲度に起因するものと考えられた。
中村 圭佑; 森下 祐樹; 高崎 浩司; 前畑 京介*; 杉本 哲也*; 木口 優*; 伊豫本 直子*; 満田 和久*
Journal of Low Temperature Physics, 193(3-4), p.314 - 320, 2018/11
被引用回数：0 パーセンタイル：0(Physics, Applied)Spectroscopic measurement of L X-ray is one of important techniques for a non-destructive assay of transuranium (TRU) elements because L X-rays of the energy ranging from 10 to 25 keV are emitted following internal conversion after the alpha-decay of TRU elements. For identification of L X-ray peaks of TRU elements, the energy resolution of the detector is required to be lower than 100 eV of the full width at half maximum (FWHM). In this work, a transition-edge-sensor (TES) microcalorimeter was operated for spectroscopic measurements of L X-rays emitted from a Np-237 and Cm-244 source. Typical L X-ray peaks of Pa, U and Pu elements were clearly identified in the obtained energy spectra. The FWHM energy resolution of the TES microcalorimeter was obtained to be 32.7 eV at Pu L alpha1 X-ray peak of 14.28 keV with natural line width of 12.20 eV. We considered a feasibility of a non-destructive assay of TRU elements with experimental L X-ray spectra obtained by the TES microcalorimeter.
吉田 亨次*; 井上 拓也*; 鳥越 基克*; 山田 武*; 柴田 薫; 山口 敏男*
Journal of Chemical Physics, 149(12), p.124502_1 - 124502_10, 2018/09
被引用回数：4 パーセンタイル：17.83(Chemistry, Physical)異なる幾つかの、グリシン濃度, pH、および充填率(=グリシン溶液の質量/MCM-41の乾燥質量))をパラメーターとして、メソポーラスシリカ(MCM-41)に閉じ込められたグリシン水溶液の示差走査熱量測定、X線回折および準弾性中性子散乱(QENS)を305-180Kの温度範囲で実施して、グリシン水溶液の熱的挙動, 構造、および動的特性に対する閉じ込め効果を検討した。
岡 弘; 丹野 敬嗣; 大塚 智史; 矢野 康英; 皆藤 威二
Nuclear Materials and Energy (Internet), 16, p.230 - 237, 2018/08
被引用回数：4 パーセンタイル：38.58(Nuclear Science & Technology)In determining the nitrogen concentration specifications, nano-structure and high-temperature strength of 9Cr-ODS steel have been investigated as a function of the nitrogen content with the aim of obtaining technical knowledge that makes the specification reasonable. The hardness and tensile strength showed degradation with increasing nitrogen content. For a microstructure, the decrement of residual ferrite phase was confirmed. Since the nitrogen is an austenite stabilizer, the increment of nitrogen enhanced an alpha to 
transformation, resulted in the decrease of the residual ferrite phase. It is considered that the reduction of the strength is due to the decrease of the residual ferrite phase.
