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論文

Anomalous dislocation response to deformation strain in CrFeCoNiPd high-entropy alloys with nanoscale chemical fluctuations

Ying, H.*; Yang, X.*; He, H.*; Yan, A.*; An, K.*; Ke, Y.*; Wu, Z.*; Tang, S.*; Zhang, Z.*; Dong, H.*; et al.

Scripta Materialia, 250, p.116181_1 - 116181_7, 2024/09

Nanoscale chemical fluctuations and their effect on the deformation behavior of CrFeCoNi-based high-entropy alloys (HEAs) were investigated using small-angle scattering and in situ neutron diffraction measurements. Small-angle scattering results demonstrated the presence of nano ($$>$$10 nm) chemical fluctuations in the as-prepared CrFeCoNiPd HEAs, which was attributed to the negative mixing of enthalpy and the significant atomic radius difference between Pd and the constituent elements in the CrFeCoNi-based alloys. Subsequent tensile tests demonstrated that the yield and tensile strengths of the as-prepared CrFeCoNiPd HEA surpass those of the as-prepared CrMnFeCoNi HEA. Neutron diffraction data analysis revealed an anomalous response of dislocation evolution with the strain.

論文

Mechanical properties of base metal and heat-affected zone in friction-stir-welded AA6061-T6 at ultra-low temperature of 20 K

Nguyen, T.-D.*; Singh, C.*; Kim, Y. S.*; Han, J. H. *; Lee, D.-H.*; Lee, K.*; Harjo, S.; Lee, S. Y.*

Journal of Materials Research and Technology, 31, p.1547 - 1556, 2024/07

This study investigates the mechanical properties of a friction-stir-welded (FSW) AA6061-T6 aluminum alloy at ultra-low temperature (ULT) of 20 K. In-situ neutron diffraction and orientation imaging microscopy were employed to compare the tensile deformation behavior of the base metal (BM) and heat-affected zone (HAZ) in the FSW aluminum plate. The results demonstrate that compared to room-temperature (RT), ULT induces a significant improvement in tensile strength and ductility in both the BM and HAZ. The enhanced mechanical properties in BM at ULT result from a more homogeneous deformation than occurs at RT. On the other hand, HAZ at ULT exhibits an even lower yield strength than at RT, but the strain hardening rate (SHR) is the most significant among the alloys, leading to a tensile strength of 346 MPa and the highest ductility of 46.8%. The lowest yield strength corresponds to the lowest-hardness zones in HAZ, caused by dissolved/coarsened precipitates during the FSW process.

論文

マルチピークを用いた応力評価

Harjo, S.; Gong, W.; 川崎 卓郎

日本材料学会第58回X線材料強度に関するシンポジウム講演論文集, p.51 - 54, 2024/07

In-situ neutron diffraction was used to study tensile deformation in an extruded AZ31 alloy. The aim was to validate existing methods and develop new ones for stress evaluation in magnesium alloys. Results showed varied increases in lattice strains among grains, posing challenges for conventional procedures. A new method, considering grain volume fraction and multiple orientations, proved highly accurate. When simultaneous hk.l peaks weren't available, the 12.1 peak was recommended for stress evaluation, showing a linear relationship with applied stress throughout deformation.

論文

マルチモーダル化したマグネシウム合金の変形中の構成相・組織の挙動

Harjo, S.; Gong, W.; 相澤 一也; 山崎 倫昭*; 川崎 卓郎

日本材料学会第58回X線材料強度に関するシンポジウム講演論文集, p.58 - 60, 2024/07

The experiment and analysis procedures for a sample exhibiting multimodal structures were outlined. The sample, a Mg$$_{97}$$Zn$$_1$$Y$$_2$$ alloy, initially comprised two phases: the HCP $$alpha$$ matrix ($$alpha$$Mg) and the long-period stacking ordered phase (LPSO), constituting approximately 25% of the volume. Through hot extrusion at 623 K with an extrusion ratio (R) of 5.0, the alloy was rendered multimodal. Specifically, at an R value of 5.0, dynamic recrystallization occurred partially within the $$alpha$$Mg phase, resulting in a bimodal microstructure. This microstructure consisted of a deformed $$alpha$$Mg component and a recrystallized $$alpha$$Mg component. An analysis employing Electron Backscatter Diffraction (EBSD) data facilitated multimodal characterization, enabling successful determination of stresses within the individual $$alpha$$Mg components, as well as the LPSO phase stress.

論文

変形その場パルス中性子回折実験により高強度マグネシウム合金の強度増加機構を解明

Harjo, S.

Isotope News, (793), p.13 - 16, 2024/06

高強度マグネシウム(Mg)合金の高温押出加工による大幅な強度増加の機構を引張変形その場中性子回折実験によってどのように解明したかについて紹介する。高温押出加工の条件により組織が複雑化し、構成相それぞれの組織からの強度への寄与について解説する。

論文

Quantitative analysis of microstructure evolution, stress partitioning and thermodynamics in the dynamic transformation of Fe-14Ni alloy

Li, L.*; 宮本 吾郎*; Zhang, Y.*; Li, M.*; 諸岡 聡; 及川 勝成*; 友田 陽*; 古原 忠*

Journal of Materials Science & Technology, 184, p.221 - 234, 2024/06

 被引用回数:0 パーセンタイル:0.00(Materials Science, Multidisciplinary)

Dynamic transformation (DT) of austenite ($$gamma$$) to ferrite ($$alpha$$) in the hot deformation of various carbon steels was widely investigated. However, the nature of DT remains unclear due to the lack of quantitative analysis of stress partitioning between two phases and the uncertainty of local distribution of substitutional elements at the interface in multi-component carbon steels used in the previous studies. Therefore, in the present study, a binary Fe-Ni alloy with $$alpha$$+$$gamma$$ duplex microstructure in equilibrium was prepared and isothermally compressed in $$alpha$$+$$gamma$$ two-phase region to achieve quantitative analysis of microstructure evolution, stress partitioning and thermodynamics during DT. $$gamma$$ to $$alpha$$ DT during isothermal compression and $$alpha$$ to $$gamma$$ reverse transformation on isothermal annealing under unloaded condition after deformation were accompanied by Ni partitioning. The lattice strains during thermomechanical processing were obtained via in-situ neutron diffraction measurement, based on which the stress partitioning behavior between $$gamma$$ and $$alpha$$ was discussed by using the generalized Hooke's law. A thermodynamic framework for the isothermal deformation in solids was established based on the basic laws of thermodynamics, and it was shown that the total Helmholtz free energy change in the deformable material during the isothermal process should be smaller than the work done to the deformable material. Under the present thermodynamic framework, the microstructure evolution in the isothermal compression of Fe-14Ni alloy was well explained by considering the changes in chemical free energy, plastic and elastic energies and the work done to the material. In addition, the stabilization of the soft $$alpha$$ phase in Fe-14Ni alloy by deformation was rationalized since the $$gamma$$ to $$alpha$$ transformation decreased the total Helmholtz free energy by decreasing the elastic and dislocation energies.

論文

Microscopic insights of the extraordinary work-hardening due to phase transformation

Ma, Y.*; Naeem, M.*; Zhu, L.*; He, H.*; Sun, X.*; Yang, Z.*; He, F.*; Harjo, S.; 川崎 卓郎; Wang, X.-L.*

Acta Materialia, 270, p.119822_1 - 119822_13, 2024/05

We report an in situ neutron diffraction study of 316 L that reveals an extraordinary work-hardening rate (WHR) of $$sim$$7 GPa at 15 K. Detailed analyses show that the major contribution to the excellent strength and ductility comes from the transformation-induced plasticity (TRIP) effect, introduced by the austenite-to-martensite ($$gamma$$-to-$$alpha$$') phase transition. A dramatic increase in the WHR is observed along with the transformation; the WHR declined when the austenite phase is exhausted. During plastic deformation, the volume-fraction weighted phase stress and stress contribution from the $$alpha$$'-martensite increase significantly. The neutron diffraction data further suggest that the $$gamma$$-to-$$alpha$$' phase transformation was mediated by the $$varepsilon$$-martensite, as evidenced by the concurrent decline of the $$varepsilon$$ phase with the $$gamma$$ phase.

論文

In-situ neutron diffraction study of serration-involved ultra-cryogenic deformation behavior at 15 K

Kim, Y. S.*; Chae, H.*; Lee, D.-Y.*; Han, J. H. *; Hong, S.-K.*; Na, Y. S.*; Harjo, S.; 川崎 卓郎; Woo, W.*; Lee, S.-Y.*

Materials Science & Engineering A, 899, p.146453_1 - 146453_7, 2024/05

This work focused on the mechanical properties and serration-involved deformation behavior of advanced alloys at 15 K. Evolution of stacking faults and $$varepsilon$$-martensite improved the mechanical performance of CoCrNi alloys, and significant strain-induced martensite transformation of DED-SS316L led to superior strength and strain hardening. A magnitude in stress drop was governed by dislocation density, phase type, and lattice defects, irrespective of processing method. FCC {200} notably was influenced recovery behavior after stress drop, and the contribution of strain energy density by serration on tensile toughness was the greatest for HR-CoCrNi.

論文

Mechanical stability of retained austenite and texture evolution in additively manufactured stainless steel

Chae, H.*; Huang, E.-W.*; Jain, J.*; Lee, D.-H.*; Harjo, S.; 川崎 卓郎; Lee, S. Y.*

Metals and Materials International, 30(5), p.1321 - 1330, 2024/05

In situ neutron diffraction during tensile deformation was performed for the stainless steels prepared by the additive manufacturing (AM) processes with two strategies: vertically built and horizontally built. The AM steels were further aged without solid solution treatment. As the results, the retained austenite was found to be more stable because the chemical composition became homogeneous by aging, and the onset of deformation induced martensitic transformation was delayed.

論文

Contributions of multimodal microstructure in the deformation behavior of extruded Mg alloys containing LPSO phase

萩原 幸司*; 眞山 剛*; 山崎 倫昭*; Harjo, S.; 徳永 透子*; 山本 和輝*; 杉田 三佳*; 青山 海琳*; Gong, W.; 西本 宗矢*

International Journal of Plasticity, 173, p.103865_1 - 103865_21, 2024/02

The unique control mechanisms of the plastic deformation of two-phase extruded alloy composed of Mg and long-period stacking ordered (LPSO) phase were clarified by comparison with those of other Mg solid-solution alloys, focusing on the question of why do the Mg/LPSO two-phase alloys exhibit both large elongation and high strength? The stress-strain curves for each grain in the alloys could be imaginary estimated using neutron diffraction analysis during the tensile test. The results demonstrate that the deformation behaviors of the worked and recrystallized grains are significantly different in all the Mg-extruded alloys owing to the strong plastic anisotropy in Mg with hexagonal close-packed (hcp) structure. Therefore, the deformation behavior is controlled by a composite-like deformation mechanism, even in single-phase Mg solid-solution alloys.

論文

Anisotropic electrical conductivity changes in FeTiO$$_3$$ structure transition under high pressure

山中 高光*; 中本 有紀*; 坂田 雅文*; 清水 克哉*; 服部 高典

Physics and Chemistry of Minerals, 51(1), p.4_1 - 4_10, 2024/02

 被引用回数:0 パーセンタイル:0.10(Materials Science, Multidisciplinary)

FeTiO$$_3$$イルメナイトの中性子及び放射光X線回折と電気伝導度測定を高圧下で行った。イルメナイトの構造は28GPaまで保持された。構造解析の結果、8GPa以下ではFeO$$_6$$は圧縮され、TiO$$_6$$はほとんど圧縮されないことが分かった。抵抗率は、金属イオン対の中で原子間距離が最も短いFe-Ti方向で最も小さかった。c軸に垂直な方向の抵抗率は圧力とともに単調減少するが、c軸に沿った抵抗率は圧力とともに山なりとなった。最大エントロピー解析の結果、Fe$$^{2+}$$(3$$d^6$$)の電子配置はTi$$^{4+}$$(3$$d^0$$)よりも圧縮下で大きく変化することがわかった。異方的な電気伝導度とFe-Ti原子間距離の非一様な圧縮は、Feイオンの高スピン状態から中間スピン状態へのスピン転移によって説明できるかもしれない。

論文

Fe-5Mn-0.1C中Mn鋼におけるリューダース変形中の微視組織および塑性の発達

小山 元道*; 山下 享介*; 諸岡 聡; 澤口 孝宏*; Yang, Z.*; 北條 智彦*; 川崎 卓郎; Harjo, S.

鉄と鋼, 110(3), p.197 - 204, 2024/02

 被引用回数:0 パーセンタイル:0.02

The local plasticity and associated microstructure evolution in Fe-5Mn-0.1C medium-Mn steel (wt.%) were investigated in this study. Specifically, the micro-deformation mechanism during L$"u$ders banding was characterized based on multi-scale electron backscatter diffraction measurements and electron channeling contrast imaging. Similar to other medium-Mn steels, the Fe-5Mn-0.1C steel showed discontinuous macroscopic deformation, preferential plastic deformation in austenite, and deformation-induced martensitic transformation during L$"u$ders deformation. Hexagonal close-packed martensite was also observed as an intermediate phase. Furthermore, an in-situ neutron diffraction experiment revealed that the pre-existing body- centered cubic phase, which was mainly ferrite, was a minor deformation path, although ferrite was the major constituent phase.

論文

Deformation-induced martensitic transformation at tensile and compressive deformations of bainitic steels with different carbon contents

上路 林太郎*; Gong, W.; Harjo, S.; 川崎 卓郎; 柴田 曉伸*; 木村 勇次*; 井上 忠信*; 土田 紀之*

ISIJ International, 64(2), p.459 - 465, 2024/01

Deformation-induced martensitic transformation (DIMT) during tensile or compressive deformations of the bainitic steels with various carbon content (0.15%C, 0.25%C, 0.62%C) was studied. In all of the bainitic steels, the tensile deformation exhibited larger work hardening than the compression. This difference indicates the suppression of the DIMT at the compression, and actually the measurements of electron back scattering diffraction (EBSD) confirmed the less reduction of retained austenite at the compression of all the bainitic steels. Additionally, the steel with the highest carbon content was examined by in situ neutron diffraction and clarified the difference similar to that obtained by the EBSD measurement. The regression of the relation between the fraction of austenite and applied strain with the conventional empirical equation revealed that the kinetic of DIMT is strongly dependent with the stress polarity, but not significantly changed by the carbon content.

論文

Probing deformation behavior of a refractory high-entropy alloy using ${it in situ}$ neutron diffraction

Zhou, Y.*; Song, W.*; Zhang, F.*; Wu, Y.*; Lei, Z.*; Jiao, M.*; Zhang, X.*; Dong, J.*; Zhang, Y.*; Yang, M.*; et al.

Journal of Alloys and Compounds, 971, p.172635_1 - 172635_7, 2024/01

 被引用回数:0 パーセンタイル:0.00(Chemistry, Physical)

The grain orientation-dependent lattice strain evolution of a (TiZrHfNb)$$_{98}$$$$N_2$$ refractory high-entropy alloy (HEA) during tensile loading has been investigated using ${it in situ}$ neutron diffraction. The equivalent strain-hardening rate of each of the primary $$<hkl>$$-oriented grain families was found to be relatively low, manifesting the macroscopically weak work-hardening ability of such a body-centered cubic (BCC)-structured HEA. This finding is indicative of a dislocation planar slip mode that is confined in a few single-slip planes and leads to in-plane softening by high pile-up stresses.

論文

Stress evaluation method by neutron diffraction for HCP-structured magnesium alloy

Harjo, S.; Gong, W.; 川崎 卓郎

Quantum Beam Science (Internet), 7(4), p.32_1 - 32_13, 2023/12

Tensile deformation in situ neutron diffraction of an extruded AZ31 alloy was performed to validate conventional procedures and to develop new procedures for stress evaluation from lattice strains by diffraction measurements of HCP-structured magnesium alloys. Increases in the lattice strains with respect to the applied true stress after yielding largely vary among [${it hk.l}$] grains. The newly proposed procedure of stress evaluation from the lattice strains shows very high accuracy and reliability by weighting the volume fraction of [${it hk.l}$] grains and evaluating them in many [${it hk.l}$] orientations in addition to multiplication by the diffraction elastic constant. When multiple ${it hk.l}$ peaks cannot be obtained simultaneously, we recommend to use the 12.1 peak for stress evaluation.

論文

Measurement of mechanical behavior of $$^{11}$$B-enriched MgB$$_{2}$$ wire using a pulsed neutron source

町屋 修太郎*; 長村 光造*; 菱沼 良光*; 谷口 博康*; Harjo, S.; 川崎 卓郎

Quantum Beam Science (Internet), 7(4), p.34_1 - 34_17, 2023/10

Measuring the actual strain on the MgB$$_2$$ filaments are of paramount importance, since tensile stress and strain diminish the critical current. In this study, the strain measurement using neutron diffraction during tensile loading was established. We fabricated a MgB$$_2$$ wire enriched with boron-11, an isotope having a smaller neutron absorption cross- section than natural boron, and succeeded in obtaining changes in the lattice constant under tensile loading through Rietveld analysis.

論文

中性子回折によるハイエントロピー合金の変形挙動のその場観察

Harjo, S.

日本結晶学会誌, 65(3), p.178 - 182, 2023/08

Observations of deformation behavior of high entropy alloys using ${it in situ}$ neutron diffraction measurements during deformation at various temperatures are reviewed. Neutrons are used to investigate stresses and crystallographic microstructures inside engineering materials, taking advantage of their large penetrating power and the ability to see the arrangement of atoms by diffraction methods. The important structural details of high entropy alloys such as internal stresses, phase conditions, dislocations, texture etc. are discussed in relation to the deformation conditions. Some highlights are introduced: (a) Cooperative deformation in CrMnFeCoNi alloy at ultralow temperatures, (b) Stacking fault energies in CrFeCoNi and CrCoNi alloys, and (c) Load redistribution in eutectic high entropy alloy AlCoCrFeNi$$_{2.1}$$ during high temperature deformation.

論文

Spontaneous topological Hall effect induced by non-coplanar antiferromagnetic order in intercalated van der Waals materials

高木 寛貴*; 高木 里奈*; 見波 将*; 野本 拓也*; 大石 一城*; 鈴木 通人*; 柳 有起*; 平山 元昭*; Khanh, N.*; 軽部 皓介*; et al.

Nature Physics, 19(7), p.961 - 968, 2023/07

 被引用回数:8 パーセンタイル:95.84(Physics, Multidisciplinary)

In ferromagnets, electric current generally induces a transverse Hall voltage in proportion to the internal magnetization. This effect is frequently used for electrical readout of the spin up and down states. While these properties are usually not expected in antiferromagnets, recent theoretical studies predicted that non-coplanar antiferromagnetic order with finite scalar spin chirality - meaning a solid angle spanned by neighboring spins - can induce a large spontaneous Hall effect even without net magnetization or external magnetic field. This phenomenon, the spontaneous topological Hall effect, can potentially be used for the efficient electrical readout of the antiferromagnetic states, but it has not been experimentally verified due to a lack of appropriate materials hosting such magnetism. Here, we report the discovery of all-in-all-out type non-coplanar antiferromagnetic order in triangular lattice compounds CoTa$$_{3}$$S$$_{6}$$ and CoNb$$_{3}$$S$$_{6}$$. These compounds are reported to host unconventionally large spontaneous Hall effect despite their vanishingly small net magnetization, and our analysis reveals that it can be explained in terms of the topological Hall effect that originates from the fictitious magnetic field associated with scalar spin chirality. These results indicate that the scalar spin chirality mechanism offers a promising route to the realisation of giant spontaneous Hall response even in compensated antiferromagnets, and highlight intercalated van der Waals magnets as a promising quasi-two-dimensional material platform to enable various nontrivial ways of electrical reading and possible writing of non-coplanar antiferromagnetic domains.

論文

Effects of loading direction on the anisotropic tensile properties of duplex stainless steels based on phase strains obtained by in situ neutron diffraction experiments

松下 慧*; 土田 紀之*; 石丸 詠一郎*; 平川 直樹*; Gong, W.; Harjo, S.

Journal of Materials Engineering and Performance, 10 Pages, 2023/06

This study investigated the anisotropy of the tensile properties in a duplex stainless steel of 24Cr-5Ni-0.18N based on in situ neutron diffraction experiments. The 24Cr-5Ni-0.18N steel showed a better balance of tensile strength (TS) and uniform elongation (U.El) compared with 329J4L and 329J1 steels. The Lankford value ($$r$$-value) of the 24Cr-5Ni-0.18N steel was comparable to other duplex stainless steels while showing a larger TS. Regarding the anisotropy of the mechanical properties, the results for a test specimen oriented at 45$$^{circ}$$ showed a low yield strength (YS) and TS, but a better U.El and $$r$$-value. The neutron diffraction results are discussed to explain the mechanical properties.

論文

Accuracy of measuring rebar strain in concrete using a diffractometer for residual stress analysis

安江 歩夢*; 川上 真由*; 小林 謙祐*; Kim, J.; 宮津 裕次*; 西尾 悠平*; 向井 智久*; 諸岡 聡; 兼松 学*

Quantum Beam Science (Internet), 7(2), p.15_1 - 15_14, 2023/05

Neutron diffraction is a noncontact method that can measure the rebar strain inside concrete. In this method, rebar strain and stress are calculated using the diffraction profile of neutrons irradiated during a specific time period. In general, measurement accuracy improves with the length of the measurement time. However, in previous studies, the measurement time was determined empirically, which makes the accuracy and reliability of the measurement results unclear. In this study, the relationship between the measurement time and the measurement standard deviation was examined for reinforced concrete specimens under different conditions. The aim was to clarify the accuracy of the measurement of rebar stress using the neutron diffraction method. It was found that if the optical setup of the neutron diffractometer and the conditions of the specimen are the same, there is a unique relationship between the diffraction intensity and the rebar stress standard deviation. Furthermore, using this unique relationship, this paper proposes a method for determining the measurement time from the allowable accuracy of the rebar stress, which ensures the accuracy of the neutron diffraction method.

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