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neutron diffraction study山下 享介*; 古賀 紀光*; Mao, W.*; Gong, W.; 川崎 卓郎; Harjo, S.; 藤井 英俊*; 梅澤 修*
Materials Science and Engineering A, 941, p.148602_1 - 148602_11, 2025/09
Ferrite-austenite duplex stainless steels offer excellent strength and ductility, making them suitable for extreme environments. In this study, 
neutron diffraction during tensile testing at 293 K and 200 K was used to investigate stress partitioning and phase-specific deformation. Phase stress was calculated using a texture-compensated method. At both temperatures, ferrite showed higher phase stress than austenite, acting as the harder phase. At 200 K, both phases exhibited increased strength and work hardening. Austenite showed significant stacking fault formation alongside dislocation migration, while ferrite retained its dislocation-based deformation mode, becoming more effective. Stress contributions from both phases were comparable. No martensitic transformation occurred. Strengthening and enhanced work hardening in both phases led to high strength at 200 K, with ductility similar to that at 293 K.
Cao, T.*; Wei, D.*; Gong, W.; 川崎 卓郎; Harjo, S.; 他10名*
Materials Science and Engineering A, 940, p.148534_1 - 148534_16, 2025/09
The thermal stability of microstructure and mechanical performance is crucial for the industrial application of laser powder bed fusion (LPBF) superalloy components in gas turbines and jet engines. This work investigated the microstructural evolution and strengthening mechanism of LPBF Mar-M509 cobalt-based superalloy before and after thermal exposure at 1200 
C using multi-scale microstructural characterization and in situ neutron diffraction tensile testing. The as-built Mar-M509 superalloy exhibited a heterogeneous microstructural features with coarse columnar and fine equiaxed grains, both containing dendritic and cellular substructures enriched with nanoscale carbides and high-density dislocations. The ultra high strength of the as-built sample was primarily attributed to dislocation-precipitation synergistic strengthening. After thermal exposure at 1200 C for 4 h, the dendritic and cellular substructures disappeared and the dislocation density decreased significantly. This study reveals the microstructural evolution and instability of LPBF Mar-M509 superalloy under high-temperature exposure and the impacts on mechanical properties, which provides critical support for the development of cobalt-based superalloys in high-temperature application fields.
Gu, G. H.*; Jeong, S. G.*; Heo, Y.-U.*; Harjo, S.; Gong, W.; Cho, J.*; Kim, H. S.*; 他4名*
Journal of Materials Science & Technology, 223, p.308 - 324, 2025/07
被引用回数：0 パーセンタイル：0.00(Materials Science, Multidisciplinary)Face-centered cubic (FCC) equi-atomic multi-principal element alloys (MPEAs) exhibit excellent mechanical properties from cryogenic to room temperatures. At room temperature, deformation is dominated by dislocation slip, while at cryogenic temperatures (CTs), reduced stacking fault energy enhances strain hardening with twinning. This study uses in-situ neutron diffraction to analyze the temperature-dependent deformation behavior of Al
(CoNiV)
, a dual-phase (FCC/BCC) medium-entropy alloy (MEA). At liquid nitrogen temperature (LNT), deformation twinning in the FCC matrix leads to additional strain hardening through the dynamic Hall-Petch effect, giving the appearance of improved strengthening at LNT. In contrast, BCC precipitates show dislocation slip at both 77 K and 298 K, with temperature-dependent lattice friction stress playing a significant role in strengthening. The study enhances understanding of deformation behaviors and provides insights for future alloy design.
Mao, W.*; Gong, W.; 川崎 卓郎; Gao, S.*; 伊東 達矢; 山下 享介*; Harjo, S.; Zhao, L.*; Wang, Q.*
Scripta Materialia, 264, p.116726_1 - 116726_6, 2025/07
被引用回数：0An ultrafine-grained 304 austenitic stainless steel exhibited pronounced serrated Luders deformation at 20 K, with stress and temperature oscillations reaching 200 MPa and 20 K. 
neutron diffraction and digital image correlation revealed discontinuous Luders band propagation and burst martensite formation. During deformation, austenite phase stress remained lower than at upper yielding, indicating elastic behavior. Notably, martensite phase stress stayed lower than austenite until fracture, likely due to stress relaxation from burst martensitic transformation at 20 K. The low martensite stress delayed brittle fracture until austenite plastically yielded during uniform deformation.
Park, M.-H.*; 柴田 曉伸*; Harjo, S.; 辻 伸泰*
Acta Materialia, 292, p.121061_1 - 121061_13, 2025/06
被引用回数：1Dual-phase (DP) steel, composed of soft ferrite and hard martensite, offers excellent strength-ductility balance and low cost. This study found that refining the DP microstructure enhanced both yield strength and strain hardening, improving strength and ductility. Digital image correlation (DIC) revealed strain localization in ferrite, but refinement reduced strain differences between ferrite and martensite, suppressing crack initiation. More ferrite/martensite interfaces promoted plasticity in martensite via enhanced deformation constraint. neutron diffraction showed martensite bore higher phase stress, which increased with refinement. By combining 
-DIC and neutron data, individual stress-strain curves for ferrite and martensite were constructed for the first time, explaining the strength-ductility synergy through interphase constraint. These findings offer guidance for designing heterostructured materials to overcome the strength-ductility trade-off.
友田 陽*; Harjo, S.; 徐 平光; 諸岡 聡; Gong, W.; Wang, Y.*
Metals, 15(6), p.610_1 - 610_19, 2025/05
Lattice parameters of product and matrix phases in steels have been measured using in situ X-ray and neutron diffraction during forward and reverse transformations. These parameters are influenced by temperature, transformation-induced internal stresses, alloying element partitioning, crystal defects, and magnetic strains. Disentangling these contributions is essential for understanding lattice behavior. This review explores internal strain (stress) associated with ferrite, pearlite, bainite, martensite, and reverse austenite transformations, emphasizing the distinction between diffusional and displacive mechanisms. It also examines how plastic deformation of austenite affects subsequent bainite or martensite formation. The roles of dislocations and vacancies are identified as critical areas for further research.
Wang, Y.*; Gong, W.; Harjo, S.; 他7名*
Acta Materialia, 288, p.120840_1 - 120840_14, 2025/04
被引用回数：1 パーセンタイル：0.00(Materials Science, Multidisciplinary)Low yield strength and the presence of Luders bands constitute principal impediments to the extensive applications of conventional medium Mn steels with a duplex microstructure of ferrite and austenite. Flash heating and the concept of chemical heterogeneity have been combined to engineer a duplex austenite-martensite microstructure in medium Mn steels, which has proven effective in augmenting the yield strength and mitigating the occurrence of Luders bands. However, the underlying mechanisms remain ambiguous. In the present work, the effect of austenite stability on yielding behavior was systematically investigated in an austenite-martensite duplex medium Mn steel. Austenite stability was identified as the critical factor governing yield strength, where reduced stability promotes early stage deformation induced martensite transformation, thereby decreasing yield strength. Diminished austenite stability may as well induce enhanced work hardening, thereby result in the inclination and eventual elimination of yield plateau, concomitant with the disappearance of Luders bands. These observations expand our current understanding of the yielding behavior in medium Mn steels and offer insights for the design of other advanced high strength steels.
neutron diffraction study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.
Acta Materialia, 287, p.120767_1 - 120767_16, 2025/04
被引用回数：0 パーセンタイル：0.00(Materials Science, Multidisciplinary)Incorporating solute hydrogen into Fe-Cr-Ni-based austenitic stainless steels enhances both strength and ductility, providing a promising solution to hydrogen embrittlement by causing solid-solution strengthening and assisting deformation twinning. However, its impacts on the relevant lattice defects evolution (
, dislocations, stacking faults, and twins) during deformation remains unclear. This study compared the tensile deformation behavior in an Fe-24Cr-19Ni (mass%) austenitic steel with 7600 atom ppm hydrogen-charged (H-charged) and without hydrogen-charged (non-charged) using neutron diffraction. Hydrogen effects on the lattice expansion, solid-solution strengthening, stacking fault probability, stacking fault energy, dislocation density, and strain/stress for twin evolution were quantitatively evaluated to link them with the macroscale mechanical properties. The H-charged sample showed improvements in yield stress, flow stress, and uniform elongation, consistent with earlier findings. However, solute hydrogen exhibited minimal influences on the evolution of dislocation and stacking fault. This fact contradicts the previous reports on hydrogen-enhanced dislocation and stacking fault evolutions, the latter of which can be responsible for the enhancement of twinning. The strain for twin evolution was smaller in the H-charged sample compared to the non-charged one. Nevertheless, when evaluated as the onset stress for twin evolution, there was minimal change between the two samples. These findings suggest that the increase in flow stress due to the solid-solution strengthening by hydrogen is a root cause of accelerated deformation twinning at a smaller strain, leading to an enhanced work-hardening rate and improved uniform elongation.
Naeem, M.*; Rehman, A. U.*; Romero Resendiz, L.*; Salamci, E.*; Aydin, H.*; Ansari, P.*; Harjo, S.; Gong, W.; Wang, X.-L.*; 他3名*
Communications Materials (Internet), 6, p.65_1 - 65_13, 2025/04
The need for lightweight materials with mechanical integrity at ultralow temperatures drives the development of advanced alloys for cryogenic use. Additive manufacturing via laser powder bed fusion (LPBF) offers a scalable way to create alloys with tailored properties. Here, we show that LPBF-processed Al10SiMg exhibits a high ultimate tensile strength (395 MPa) and uniform elongation (25%) at 15 K. These enhancements stem from grain refinement, increased geometrically necessary dislocations, and stress partitioning between the Al matrix and the stiffer Si phase, aiding strain accommodation. neutron diffraction reveals that the Si phase, with its higher yield strength, bears most of the load, while the Al matrix undergoes continuous strain hardening, extending deformation capacity. These results highlight Al10SiMg's promise for cryogenic applications such as hydrogen storage, aerospace, and quantum computing hardware.
Pandian, K.*; Neikter, M.*; Ekh, M.*; Harjo, S.; 川崎 卓郎; Woracek, R.*; Hansson, T.*; Pederson, R.*
JOM, 77(4), p.1803 - 1815, 2025/04
被引用回数：0 パーセンタイル：0.00(Materials Science, Multidisciplinary)To produce dense Ti-6Al-4V components, electron beam powder bed fusion is typically followed by post-heat treatment like hot isostatic pressing (HIP). Standard HIP at 920C/100 MPa for 2 h coarsens the microstructure and reduces yield strength, while low-temp HIP at 800C/200 MPa for 2 h limits coarsening and retains strength comparable to as-built material. A coarser microstructure negatively affects tensile properties. Tensile tests at various temperatures suggest that thermally activated slip systems may influence elongation, requiring further study. In situ neutron time-of-flight diffraction during tensile loading enables analysis of strain evolution and slip plane activity. A two-phase elastic-plastic self-consistent model was used to compare with experiments. Results show basal slip {0002} activated at 20C, pyramidal slip {10-11} at 350C, and 
phase carrying higher stress than 
in the plastic regime.
川崎 卓郎; 福田 竜生; 山中 暁*; 村山 一郎*; 加藤 孝典*; 馬場 将亮*; 橋本 英樹*; Harjo, S.; 相澤 一也; 田中 裕久*; et al.
Journal of Applied Physics, 137(9), p.094101_1 - 094101_7, 2025/03
被引用回数：0 パーセンタイル：0.00(Physics, Applied)Energy harvesting from waste heat can improve energy efficiency in society. This research investigated the structural behaviors of lead zirconate titanate-based ferroelectric ceramics using operando neutron diffraction measurements under the conditions of two energy-harvesting cycles that involve consideration of the temperature changes of automobile exhaust gas for achieving good harvesting efficiencies. Input and output electrical energies and neutron diffraction data were simultaneously collected. The obtained time-resolved neutron-diffraction intensity data indicate that the applied electric fields and temperature changes induced 90 domain rotation and lattice strain. These structural changes and their variations depending on cycle conditions, such as temperature changes, applied electric fields, and circuit switching, provide insight into the origins of the differences in the behaviors of electrical input/output energies in the cycles.
Naeem, M.*; Ma, Y.*; Tian, J.*; Kong, H.*; Romero-Resendiz, L.*; Fan, Z.*; Jiang, F.*; Gong, W.; Harjo, S.; Wu, Z.*; et al.
Materials Science & Engineering A, 924, p.147819_1 - 147819_10, 2025/02
被引用回数：0 パーセンタイル：0.00(Nanoscience & Nanotechnology)Face-centered cubic (fcc) medium-/high-entropy alloys (M/HEAs) typically enhance strength and ductility at cryogenic temperatures via stacking faults, twinning, or martensitic transformation. However, in-situ neutron diffraction on VCoNi MEA at 15 K reveals that strain hardening is driven solely by rapid dislocation accumulation, without these mechanisms. This results in increased yield strength, strain hardening, and fracture strain. The behavior, explained by the Orowan equation, challenges conventional views on cryogenic strengthening in fcc M/HEAs and highlights the role of dislocation-mediated plasticity at low temperatures.
Song, Y.*; Xu, S.*; 佐藤 駿介*; Lee, I.*; Xu, X.*; 大森 俊洋*; 長迫 実*; 川崎 卓郎; 鬼柳 亮嗣; Harjo, S.; et al.
Nature, 638, p.965 - 971, 2025/02
被引用回数：2 パーセンタイル：88.78(Multidisciplinary Sciences)In advanced applications like aerospace and space exploration, materials must balance lightness, functionality, and extreme thermal fluctuation resistance. Shape-memory alloys show promise with strength, toughness, and substantial strain recovery due to superelasticity, but maintaining low mass and effective operation at cryogenic temperatures is challenging. We hereby introduce a novel shape-memory alloy that adheres to these stringent criteria. Predominantly composed of Ti and Al with a chemical composition of Ti
Al
Cr
, this alloy 25 is characterized by a low density (4.36
10
kg/m) and a high specific strength (18510 Pa
m/kg) at room temperature, while exhibiting excellent superelasticity. The superelasticity, owing to a reversible stress-induced phase transformation from an ordered body-centered cubic parent phase to an ordered orthorhombic martensite, allows for a recoverable strain exceeding 7%. Remarkably, this functionality persists across a broad range of temperatures, from deep cryogenic 4.2 K to above room temperature, arising from an unconventional temperature dependence of transformation stresses. Below a certain threshold during cooling, the critical transformation stress inversely correlates with temperature. We interpret this behavior from the perspective of a temperature-dependent anomalous lattice instability of the parent phase. This alloy holds potential in everyday appliances requiring flexible strain accommodations, as well as components designed for extreme environmental conditions such as deep space and liquefied gases.
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*
ISIJ International, 64(14), p.2051 - 2060, 2024/12
An Fe-0.15C-5Mn-0.5Si-0.05Nb steel annealed at 660C and 685C showed L
ders deformation followed by high work hardening, with variations in Lders strain and hardening behavior. neutron diffraction during tensile tests analyzed phase stresses, strength contributions, and austenite orientation. Deformation-induced martensite contributed 
1000 MPa to strength near tensile failure, while austenite mainly enhanced ductility via transformation-induced plasticity. Austenite transformed to martensite during Lders deformation regardless of orientation, though 311-oriented grains tended to remain along the tensile direction.
Sn strands in ITER central solenoid conductors of short and long twist pitch諏訪 友音*; 礒野 高明*; Harjo, S.; 川崎 卓郎; 相澤 一也
Superconductor Science and Technology, 38(1), p.015008_1 - 015008_8, 2024/12
被引用回数：0 パーセンタイル：0.00(Physics, Applied)The ITER central solenoid (CS) conductors are composed of NbSn superconducting cables and stainless steel jackets. Approximately 60,000 electromagnetic loading cycles will be applied to the NbSn strands in the CS conductor over the course of ITER tokamak operation, and the CS conductor is required to maintain the current sharing temperature (
) for these electromagnetic loading cycles. However, in CS conductor prototypes, degradation of was observed after electromagnetic loading cycles. Visual inspections of the tested CS conductors revealed large bending and buckling of the NbSn strands. These strand deformations were considered to be the cause of degradation because even a small amount of strain markedly affects the critical current of NbSn strands. To prevent the strands from bending and buckling, the twist pitch of the cable was shortened to improve stiffness. The stiffer cables did prevent from degrading after electromagnetic loading cycles owing to the shortened twist pitch of the conductors, but a slight increase of was observed. Visual inspections revealed no significant bent or buckled strands, but small deformations cannot be investigated visually. Thus, internal strain was measured by neutron diffraction and the internal strain states of the prototype CS conductors having long twist pitches and the improved short-twist-pitch (STP) CS conductors were evaluated. The results indicated that, after electromagnetic loading cycles, bending of the strands in the STP CS conductor was limited and compressive strain was reduced. Therefore, we determined that this STP is not only effective to prevent degradation caused by bent strands but it also increases by reducing compressive strain.
neutron diffractionNaeem, M.*; Ma, Y.*; Knowles, A. J.*; Gong, W.; Harjo, S.; Wang, X.-L.*; Romero Resendiz, L.*; 他6名*
Materials Science & Engineering A, 916, p.147374_1 - 147374_8, 2024/11
被引用回数：2 パーセンタイル：63.37(Nanoscience & Nanotechnology)Heterostructured materials (HSMs) improve the strength-ductility trade-off of alloys, but their cryogenic performance under real-time deformation is unclear. We studied heterostructured CrCoNi medium-entropy alloy via neutron diffraction at 77 K and 293 K. A significant mechanical mismatch between fine and coarse grains led to an exceptional yield strength of 918 MPa at 293 K, increasing to 1244 MPa at 77 K with a uniform elongation of 34%. This strength-ductility synergy at 77 K is attributed to high dislocation pile-up density, increased planar faults, and martensitic transformation. Compared to homogeneous alloys, HSMs show promise for enhancing cryogenic mechanical performance in medium-/high-entropy alloys.
Harjo, S.; Mao, W.*; Gong, W.; 川崎 卓郎
Proceedings of the 7th International Symposium on Steel Science (ISSS 2024), p.205 - 208, 2024/11
This study aimed to elucidate the effect of grain size on the deformation behavior of TRIP steel. We prepared metastable austenitic Fe-24Ni-0.3C steel samples with average grain sizes of 35 
m (coarse grain: CG) and 0.5 m (ultrafine-grain: UFG) for in situ neutron diffraction studies during tensile deformation at room temperature. Our observations revealed increases in dislocation density in both samples prior to DIMT, indicating that plastic deformation precedes DIMT regardless of grain size. In the UFG sample, a significant rise in dislocation density occurred just around the yielding point with minimal increases in macroscopic plastic strain. Additionally, the dislocations exhibited strong dipole arrangements.
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：12 パーセンタイル：87.44(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.
