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Synthesis, crystal structure, local structure, and magnetic properties of polycrystalline and single-crystalline Ce$$_2$$Pt$$_6$$Al$$_{15}$$

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

Polycrystalline and single crystalline Ce$$_2$$Pt$$_6$$Al$$_{15}$$ 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.


Deformation mechanism of a strong and ductile maraging steel investigated using ${it in situ}$ X-ray synchrotron diffraction

Li, 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:0 パーセンタイル:81.79(Engineering, Mechanical)



Data processing and visualization of X-ray computed tomography images of a JOYO MK-III fuel assembly

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:33.72(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.


Relationship between internal stress distribution and microstructure in a suspension-sprayed thermal barrier coating with a columnar structure

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.


Selective adsorption of Pd(II) over Ag(I) in nitric acid solutions using nitrogen-donor-type adsorbents

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:1 パーセンタイル:26.5(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$$_{3}$$$$^{-}$$と[Pd(NO$$_{3}$$)$$_{4}$$]$$^{2-}$$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。


Insight on the mechanical properties of hierarchical porous calcium-silicate-hydrate pastes according to the Ca/Si molar ratio using ${it in situ}$ synchrotron X-ray scattering and nanoindentation test

Im, 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:3 パーセンタイル:58.24(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, $$^{29}$$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.


Micro- to nano-scale areal heterogeneity in pore structure and mineral compositions of a sub-decimeter-sized Eagle Ford Shale

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:3 パーセンタイル:72.03(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.


Study on the relation between the crystal structure and thermal stability of FeUO$$_{4}$$ and CrUO$$_{4}$$

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:2 パーセンタイル:71.05(Materials Science, Multidisciplinary)



Temperature effects on local structure, phase transformation, and mechanical properties of calcium silicate hydrates

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:8 パーセンタイル:84.8(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 $$^{circ}$$C), decomposition (300-600 $$^{circ}$$C), and recrystallization (700-1000 $$^{circ}$$C) were investigated via powder X-ray diffraction, $$^{29}$$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 $$approx$$ 3.0 ${AA}$) 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 $$beta$$-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.


A Multi-technique tomography-based approach for non-invasive characterization of additive manufacturing components in view of vacuum/UHV applications; Preliminary results

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:2 パーセンタイル:22.98(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.


Structure of the {U$$_{13}$$} polyoxo cluster U$$_{13}$$O$$_{8}$$Cl$$_{x}$$(MeO)$$_{38-x}$$ (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$$_{13}$$}, was synthesised and characterised as [U$$_{13}$$($$mu$$$$_{4}$$-O$$_{rm oxo}$$)$$_{8}$$($$mu$$$$_{4}$$-O$$_{rm MeO}$$)$$_{2}$$($$mu$$$$_{2}$$-O$$_{rm MeO}$$)$$_{24}$$Cl$$_{x}$$(O$$_{rm MeO}$$)$$_{12-x}$$] (x = 2.3, MeO = methoxide) (I). The complex crystallises from methanol containing tetravalent uranium (U$$^{rm IV}$$) with a basic organic ligand. The characterised {U$$_{13}$$} 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$$^{rm V}$$) from the original tetravalent state (U$$^{rm IV}$$). Complex I is, hence, the first example of a polyoxo cluster possessing a single cubic coordination polyhedron of U$$^{rm V}$$.


Feasibility study of magnetic-domain observation by means of non-resonant magnetic X-ray diffraction

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 $$mu$$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.


Development of experimental technology for simulated fuel-assembly heating to address core-material-relocation behavior during severe accident

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$$_{2}$$) 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.


3D-microstructure analysis of compacted Na- and Cs-montmorillonites with nanofocus X-ray computed tomography and correlation with macroscopic transport properties

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:48.17(Chemistry, Physical)



Spectroscopic measurements of L X-rays with a TES microcalorimeter for a non-destructive assay of transuranium elements

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.


Thermal behavior, structure, dynamic properties of aqueous glycine solutions confined in mesoporous silica MCM-41 investigated by X-ray diffraction and quasi-elastic neutron scattering

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:3 パーセンタイル:12.78(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。


Effect of nitrogen concentration on nano-structure and high-temperature strength of 9Cr-ODS steel

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:39.03(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 $$gamma$$ 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.


Development of experimental technology for simulated fuel-assembly heating to address core-material-relocation behavior during severe accident

阿部 雄太; 山下 拓哉; 佐藤 一憲; 中桐 俊男; 石見 明洋; 永江 勇二

Proceedings of 26th International Conference on Nuclear Engineering (ICONE-26) (Internet), 9 Pages, 2018/07

Authors are developing an experimental technology to realize experiments simulating Severe Accident (SA) conditions using simulant fuel material (ZrO$$_{2}$$ with slight addition of MgO for stabilization) 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 the accident progression behavior. Based on the results of the prototype test, improvement of plasma heating technology was conducted. The Core Material Melting and Relocation (CMMR)-1/-2 experiments were carried out in 2017 with the large-scale simulated fuel assembly (1 m $$times$$ 0.3 m $$phi$$) applying the improved technology (higher heating power and controlled oxygen concentration). In these two tests, heating history was different resulting basically in similar physical responses with more pronounced material melting and relocation in the CMMR-2 experiment. The CMMR-2 experiment is selected here from the viewpoint of establishing an experimental technology. The CMMR-2 experiment adopted 30-min heating period, the power was increased up to a level so that a large temperature gradient ($$>$$ 2,000 K/m) expected at the lower part of the core in the actual 1F accident conditions. Most of the control blade and the channel box migrated from the original position. After the heating, the simulated fuel assembly was measured by the 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 non-transfer type plasma heating technology to the SA experimental study was obtained.



佐藤 成男*; 黒田 あす美*; 佐藤 こずえ*; 熊谷 正芳*; Harjo, S.; 友田 陽*; 齋藤 洋一*; 轟 秀和*; 小貫 祐介*; 鈴木 茂*

鉄と鋼, 104(4), p.201 - 207, 2018/00

 被引用回数:8 パーセンタイル:44.73(Metallurgy & Metallurgical Engineering)

To investigate the characteristics of dislocation evolution in ferritic and austenitic stainless steels under tensile deformation, neutron diffraction line-profile analysis was carried out. The austenitic steel exhibited higher work hardening than the ferritic steel. The difference in the work hardening ability between the two steels was explained with the dislocation density estimated by the line-profile analysis. The higher dislocation density of the austenitic steel would originate from its lower stacking fault energy. Dislocation arrangement parameters indicated that the strength of interaction between dislocations in the austenitic steel was stronger than that in the ferritic steel.


Development of non-transfer type plasma heating technology to address CMR behavior during severe accident with BWR design conditions

阿部 雄太; 佐藤 一憲; 中桐 俊男; 石見 明洋; 永江 勇二

Proceedings of 2017 International Congress on Advances in Nuclear Power Plants (ICAPP 2017) (CD-ROM), 7 Pages, 2017/04

Authors are developing an experimental technology to realize experiments simulating severe accident conditions that would contribute not only to Fukushima Daiichi (1F) decommissioning but also to enhance safety of worldwide existing and future nuclear power plants through clarification of the accident progression behavior. In the first part of this program, called Phase I hereafter, a series of small-scale experiments (10 cm $$times$$ 10 cm $$times$$ 25 cmh) were performed in March 2015 and it was demonstrated that non-transfer (NTR) type plasma heating is capable of successfully melting the high melting-point ceramics. In order to confirm applicability of this heating technology to larger scale test specimens to address the experimental needs, authors performed a second series plasma heating tests in 2016, called Phase II hereafter, using a simulated fuel assembly with a larger size (100 cm $$times$$ 30 cm phi). In the phase II part of the program, the power was increased up to a level so that a large temperature gradient (2,000 K/m - 4,000 K/m) expected at the lower part of the core in the actual 1F accident conditions. After the heating, these test pieces were measured by the X-ray Computed Tomography (CT) technology. CT pictures demonstrated its excellent performance with rather good precision. Based on these results, basic applicability of the NTR plasma heating for the SA experimental study was confirmed. With the Phase II-type 100 cm-high test geometry, core material relocation (CMR) behavior within the active core region and its access to the core support structure region would be addressed. JAEA is also preparing for the next step large-scale tests using up to four simulated fuel assemblies covering the lower part of the active fuel and fully simulating the upper part of the lower core support structures addressing CMR behavior including core material relocation into the lower plenum.

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