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物質科学研究センター
JAEA-Review 2024-037, 141 Pages, 2024/11
JAEA-Review-2024-037.pdf:13.08MB
JRR-3(Japan Research Reactor No.3)には、日本原子力研究開発機構(原子力機構)が所管する15台の中性子ビーム利用実験装置が設置されており、装置高度化を含めた原子力機構の独自利用を行うとともに施設供用装置として外部利用者に供し、様々な研究成果を創出している。本報告書は、運転再開後の令和3年度、令和4年度の独自利用研究および中性子ビーム利用実験装置の高度化などの技術開発の進捗状況を取りまとめたものである。
neutron diffraction study to elucidate hydrogen effect on the deformation mechanism in Type 310S austenitic stainless steel伊東 達矢; 小川 祐平*; Gong, W.; Mao, W.*; 川崎 卓郎; 岡田 和歩*; 柴田 曉伸*; Harjo, S.
Proceedings of the 7th International Symposium on Steel Science (ISSS 2024), p.237 - 240, 2024/11
Hydrogen embrittlement has long been an obstacle to the development of safe infrastructure. However, in contrast to hydrogen's embrittling effect, recent research has revealed that the addition of hydrogen improves both the strength and uniform elongation of AISI Type 310S austenitic stainless steel. A detailed understanding of how hydrogen affects the deformation mechanism of this steel could pave the way for the development of more advanced materials with superior properties. In the present study, 
neutron diffraction experiments were conducted on Type 310S steel with and without hydrogen-charged to investigate the effect of hydrogen on the deformation mechanism. In addition to the effect of solid-solution strengthening by hydrogen, the q-value, a parameter representing the proportion of edge and screw dislocations in the accumulated dislocations, was quantitatively evaluated using CMWP analysis on neutron diffraction patterns. The comparison of q-values between the hydrogen-charged and non-charged samples reveals that hydrogen has minimal effect on dislocation character in Type 310S steel.
Mao, W.*; Gao, S.*; Gong, W.; 川崎 卓郎; 伊東 達矢; Harjo, S.; 辻 伸泰*
Acta Materialia, 278, p.120233_1 - 120233_13, 2024/10
被引用回数：1 パーセンタイル：65.10(Materials Science, Multidisciplinary)Using a hybrid method of in situ neutron diffraction and digital image correlation, we found that ultrafine-grained 304 stainless steel exhibits Luders deformation after yielding, in which the deformation behavior changes from a cooperation mechanism involving dislocation slip and martensitic transformation to one primarily governed by martensitic transformation, as the temperature decreases from 295 K to 77 K. Such martensitic transformation-governed Luders deformation delays the activation of plastic deformation in both the austenite parent and martensite product, resulting in delayed strain hardening. This preserves the strain-hardening capability for the later stage of deformation, thereby maintaining a remarkable elongation of 29% while achieving a high tensile strength of 1.87 GPa at 77 K.
Zhang, Y.-J.*; 梅田 岳昌*; 諸岡 聡; Harjo, S.; 宮本 吾郎*; 古原 忠*
Metallurgical and Materials Transactions A, 55(10), p.3921 - 3936, 2024/10
被引用回数：0 パーセンタイル：0.00(Materials Science, Multidisciplinary)In this study, a series of eutectoid steels with Mn addition up to 2 mass% were isothermally transformed at various temperatures from 873 K to 973 K to clarify the pearlite growth kinetics and the underlying thermodynamics at its growth front. The microscopic observation indicates the acceleration in pearlite growth rate and refinement in lamellar spacing by decreasing the transformation temperature or the amount of Mn addition. After analyzing the solute distribution at pearlite growth front via three-dimensional atom probe, no macroscopic Mn partitioning across pearlite/austenite interface is detected, whereas Mn segregation is only observed at ferrite/austenite interface. Furthermore, in-situ neutron diffraction measurements performed at elevated temperatures reveals that the magnitude of elastic strain generated during pearlite transformation is very small.
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
被引用回数：1 パーセンタイル：65.10(Nanoscience & Nanotechnology)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.
渡邊 未来*; 宮本 吾郎*; Zhang, Y.*; 諸岡 聡; Harjo, S.; 小林 康浩*; 古原 忠*
ISIJ International, 64(9), p.1464 - 1476, 2024/07
被引用回数：0 パーセンタイル：0.00(Metallurgy & Metallurgical Engineering)The mechanical properties of TRIP steels depend on heterogeneities of chemical composition and grain size in the retained 
structure, although these heterogeneities have not been characterized in detail. Therefore, in this study, we quantitatively investigate the inhomogeneous carbon concentration and grain size distribution, and its effects on the thermal stability of the retained in Fe-2Mn-1.5Si-0.4C (mass%) TRIP steel using FE-EPMA, EBSD, M
ssbauer spectroscopy, and in-situ neutron diffraction during bainitic transformation at 673 K. In-situ neutron diffraction experiments detects high-carbon evolving during bainite transformation, in addition to the original , and the time variation of the volume fraction of highcarbon agrees well with the fraction of retained at room temperature. Williamson-Hall analysis based on peak width suggests that heterogeneity of carbon content exists even within the high-carbon . Compositional analysis using FE-EPMA and three-dimensional atom probe directly revealed that fine filmy was highly enriched with carbon compared to larger blocky , and the carbon content in blocky decreases with increasing blocky size. DICTRA simulation qualitatively reproduces the size dependency of carbon enrichment into . It was also found that tends to be retained at higher carbon content and smaller grain size since the smaller grain size directly improves thermal stability and the smaller size further contributes to the thermal stability via enhanced carbon enrichment.
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, 33(13), p.6352 - 6361, 2024/07
被引用回数：0 パーセンタイル：0.00(Materials Science, Multidisciplinary)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 (
-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
showed a low yield strength (YS) and TS, but a better U.El and -value. The neutron diffraction results are discussed to explain the mechanical properties.
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
被引用回数：0 パーセンタイル：0.00(Materials Science, Multidisciplinary)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.
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.
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
Zn
Y
alloy, initially comprised two phases: the HCP 
matrix (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 Mg phase, resulting in a bimodal microstructure. This microstructure consisted of a deformed Mg component and a recrystallized Mg component. An analysis employing Electron Backscatter Diffraction (EBSD) data facilitated multimodal characterization, enabling successful determination of stresses within the individual Mg components, as well as the LPSO phase stress.
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。
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：2 パーセンタイル：36.02(Materials Science, Multidisciplinary)Dynamic transformation (DT) of austenite () to ferrite () 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 + duplex microstructure in equilibrium was prepared and isothermally compressed in + two-phase region to achieve quantitative analysis of microstructure evolution, stress partitioning and thermodynamics during DT. to DT during isothermal compression and to 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 and 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 phase in Fe-14Ni alloy by deformation was rationalized since the to transformation decreased the total Helmholtz free energy by decreasing the elastic and dislocation energies.
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
被引用回数：2 パーセンタイル：82.74(Materials Science, Multidisciplinary)We report an in situ neutron diffraction study of 316 L that reveals an extraordinary work-hardening rate (WHR) of 
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 (-to-') 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 '-martensite increase significantly. The neutron diffraction data further suggest that the -to-' phase transformation was mediated by the 
-martensite, as evidenced by the concurrent decline of the phase with the phase.
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
被引用回数：1 パーセンタイル：65.10(Nanoscience & Nanotechnology)This work focused on the mechanical properties and serration-involved deformation behavior of advanced alloys at 15 K. Evolution of stacking faults and -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.
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
被引用回数：4 パーセンタイル：60.41(Materials Science, Multidisciplinary)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.
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
被引用回数：7 パーセンタイル：96.45(Engineering, Mechanical)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.
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：0.00(Materials Science, Multidisciplinary)FeTiO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
は圧縮され、TiO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
(3
)の電子配置はTi
(3
)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。
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：1 パーセンタイル：65.10(Metallurgy & Metallurgical Engineering)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
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 Lders 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.
neutron diffraction measurement during tensile deformation山下 享介*; 諸岡 聡; Gong, W.; 川崎 卓郎; Harjo, S.; 北條 智彦*; 興津 貴隆*; 藤井 英俊*
鉄と鋼, 110(3), p.241 - 251, 2024/02
被引用回数：0 パーセンタイル：0.00(Metallurgy & Metallurgical Engineering)A Fe-0.15C-5Mn-0.5Si-0.05Nb medium Mn steel annealed at 660C and 685C both exhibited inhomogeneous deformation with Luders deformation and extremely high work hardening rates, but with different Luders strain and work hardening behavior. 
neutron diffraction measurements during tensile test were performed to investigate changes in the phase stresses and in the contributed stresses to the strength of the constituent phases, and crystal orientation of austenite. The role of each constituent phase in the deformation and the effect of crystallographic orientation on austenite stability were discussed. Deformation induced martensite showed excellent phase stress and contributed to the strength approximately 1000 MPa, which is close to macroscopic tensile strength.
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
被引用回数：0 パーセンタイル：0.00(Metallurgy & Metallurgical Engineering)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.
