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北條 智彦*; 小山 元道*; 熊井 麦弥*; Zhou, Y.*; 柴山 由樹; 城 鮎美*; 菖蒲 敬久; 齋藤 寛之*; 味戸 沙耶*; 秋山 英二*
ISIJ International, 65(2), p.284 - 296, 2025/02
Stress and plastic strain distributions and those partitioning behaviors of ferrite and retained austenite were investigated in the medium manganese (Mn) and the transformation-induced plasticity-aided bainitic ferrite (TBF) steels, and the martensitic transformation behaviors of retained austenite during Luders elongation and work hardening were analyzed using synchrotron X-ray diffraction at SPring-8. The stress and plastic strain of retained austenite and volume fraction of retained austenite were remarkably changed during Luders deformation in the medium Mn steel, implying that the medium Mn steel possessed inhomogeneous deformation at the parallel part of the tensile specimen. On the other hand, the distributions of the stress, plastic strain and volume fraction of retained austenite were homogeneous and the homogeneous deformation occurred at the parallel part of the tensile specimen at the plastic deformation regime with work hardening in the medium Mn and TBF steels. The martensitic transformation of retained austenite at uders deformation in the medium Mn steel was possessed owing to the application of high stress and preferential deformation at retained austenite, resulting in a significant increase in the plastic deformation and reduction of stress in the retained austenite. The martensitic transformation of retained austenite at the plastic deformation regime with work hardening was induced by the high dislocation density and newly applied plastic deformation in retained austenite in the medium Mn steel whereas the TBF steel possessed gradual transformation of retained austenite which is applied high tensile stress and moderate plastic deformation.
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 660
C 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.
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：2 パーセンタイル：47.38(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.
門井 浩太*; 冠野 裕大*; 青木 聡; 井上 裕滋*
ISIJ International, 64(9), p.1450 - 1456, 2024/07
被引用回数：0 パーセンタイル：0.00(Metallurgy & Metallurgical Engineering)オーステナイトステンレス鋼の溶接金属中の孔食に及ぼす化学組成の影響について検討した。クロムおよびモリブデンを多く含む試験片は、再活性化率が低いことが示された。チタンの添加は、耐孔食性を著しく低下させた。クロム欠乏領域はM
C
やTiCのような炭化物の近くに形成された。また、凝固時に生成したTiC相がMC析出の核となった。MCの析出により、クロムの拡散による空乏領域が発生し、耐孔食性の劣化を誘発した。
neutron diffraction during cryogenic cooling山下 享介*; Harjo, S.; 川崎 卓郎; 諸岡 聡; Gong, W.; 藤井 英俊*; 友田 陽*
ISIJ International, 64(2), p.192 - 201, 2024/01
被引用回数：0 パーセンタイル：0.00(Metallurgy & Metallurgical Engineering) neutron diffraction measurements were performed on Fe-33Ni-0.004C alloy (33Ni alloy) and Fe-27Ni-0.5C alloy (27Ni-0.5C alloy) during cooling from room temperature to the cryogenic temperature (4 K) to evaluate changes in the lattice constants of austenite and martensite, and changes in the tetragonality of martensite due to thermally induced martensitic transformation. As the martensitic transformation progressed, the lattice constants of austenite in both alloys deviated to smaller values than those predicted considering the thermal shrinkage, accompanied by an increase in the full width at half maximum of austenite. The fresh martensite formed in both alloys had a body-centered tetragonal (BCT) structure, regardless of the carbon content. The tetragonality of martensite decreased with progressive martensitic transformation during cooling in the 33Ni alloy, but was almost constant in the 27Ni-0.5C alloy. This suggests that carbon is necessary to maintain the tetragonality of martensite during cooling. The tetragonality of martensite in the 27Ni-0.5C alloy decreased during room temperature aging because of carbon mobility.
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：1 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.
土田 紀之*; Kuramoto, Shota*; 上路 林太郎*; Gong, W.; Harjo, S.; 廣井 孝介; 河村 幸彦*
ISIJ International, 64(2), p.354 - 360, 2024/01
被引用回数：0 パーセンタイル：0.00(Metallurgy & Metallurgical Engineering)The effects of pre-strain on the mechanical properties of high strength martensitic steels were investigated using either strain tempering (ST) or quenching and tempering (QT) samples. In the tensile tests at deformation temperatures between 296 and 573 K, the ST sample exhibited an increase in both the tensile strength (TS) and uniform elongation (U El) at 473 to 523 K, whereas the QT sample showed an increase in U El with little change in the TS and yield strength (YS). The results of in situ neutron diffraction experiments revealed an increase in the stress partitioning to the bcc phase with an increase in the deformation temperature from 296 to 523 K. The difference in the phase stress between the bcc and cementite phases decreased with an increase in the temperature due to the decrease in the cementite strength. Pre-strain of 0.5% increased the YS at 296 K with a slight work hardening; the initial dislocation density (
) decreased at 523 K, but increased significantly after yielding, leading to a better combination of TS and U.El. The combination of pre-strain, tempering, and deformation temperatures caused the change in before deformation and the increase in after yielding of the martensitic steel.
Zhang, Y.*; 丸澤 賢人*; 工藤 航平*; 諸岡 聡; Harjo, S.; 宮本 吾郎*; 古原 忠*
ISIJ International, 64(2), p.245 - 256, 2024/01
被引用回数：2 パーセンタイル：67.89(Metallurgy & Metallurgical Engineering)As-quenched martensite in carbon steels needs to be tempered to restore its ductility and toughness for practical applications. During tempering of martensite, microstructural evolutions induced by a series of reactions relevant to carbon diffusion is known to occur. In this study, multi-aspect characterization using advanced techniques such as in-situ neutron diffraction, transmission electron microscopy and three-dimensional atom probe tomography, was performed to investigate the changes in tetragonality, physical properties, microstructure and solute carbon content in high-carbon martensite, with an aim to clarify its low-temperature tempering behaviors. A binary alloy with a chemical composition of Fe-0.78 mass%C was austenitized and quenched to prepare the as-quenched martensite, followed by tempering in continuous heating at different heating rates. It was found that various reactions occurred sequentially during tempering, starting from the structure modulation generated by carbon clustering in the 0th stage, then followed by the precipitation of metastable 
-carbide particles on linear features in the 1st stage, towards the later decomposition of retained austenite and precipitation of cementite in the 2nd and 3rd stages, respectively. After analyzing the experimental results, the solute carbon content in martensite tempered under various conditions was found to be in good agreement with that estimated from the lattice volume expansion, whereas the evaluation based on the tetragonality might lead to some underestimation of the solute carbon content in martensite tempered at high temperatures.
ders band propagation in an Fe-5Mn-0.1C medium Mn steel clarified through scanning electron microscopy小山 元道*; 山下 享介*; 諸岡 聡; Yang, Z.*; Varanasi, R. S.*; 北條 智彦*; 川崎 卓郎; Harjo, S.
ISIJ International, 62(10), p.2043 - 2053, 2022/10
被引用回数：10 パーセンタイル：64.75(Metallurgy & Metallurgical Engineering) deformation experiments with cold-rolled and intercritically annealed Fe-5Mn-0.1C steel were carried out at ambient temperature to characterize the deformation heterogeneity during Lders band propagation. Deformation band formation, which is a precursor phenomenon of Lders band propagation, occurred even in the macroscopically elastic deformation stage. The deformation bands in the Lders front grew from both the side edges to the center of the specimen. After macroscopic yielding, the thin deformation bands grew via band branching, thickening, multiple band initiation, and their coalescence, the behavior of which was heterogeneous. Thick deformation bands formed irregularly in front of the region where the thin deformation bands were densified. The thin deformation bands were not further densified when the spacing of the bands was below 10 
m. Instead, the regions between the deformation bands showed a homogeneous plasticity evolution. The growth of the thin deformation bands was discontinuous, which may be due to the presence of ferrite groups in the propagation path of the deformation bands. Based on these observations, a model for discontinuous Lders band propagation has been proposed.
ders deformation in an Fe-5Mn-0.1C medium-Mn steel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.
ISIJ International, 62(10), p.2036 - 2042, 2022/10
被引用回数：20 パーセンタイル：83.63(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 Lders 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.
Harjo, S.; Gong, W.; 川崎 卓郎; 諸岡 聡; 山下 享介*
ISIJ International, 62(10), p.1990 - 1999, 2022/10
被引用回数：1 パーセンタイル：7.93(Metallurgy & Metallurgical Engineering)Two mechanisms inconsistent each other, a relaxation of type II internal stress and a presence of mobile dislocation, were previously proposed to describe the low elastic limit of as-quenched lath martensite steels. In this study, neutron diffraction experiments were performed to revisit the deformation behavior of lath martensite steel. The highly dense random arrangement dislocations easily moved at the beginning of deformation, then accumulated, annihilated and changed the arrangement differently depending on the orientation of the packet with respect to the deformation direction. The movement of highly dense random arrangement dislocations played an important role as a mechanism at the beginning of deformation, and can be a true feature of mobile dislocations.
岩本 ちひろ*; 高村 正人*; 上野 孝太*; 片岡 美波*; 栗原 諒*; 徐 平光; 大竹 淑恵*
ISIJ International, 62(5), p.1013 - 1022, 2022/05
被引用回数：3 パーセンタイル：24.31(Metallurgy & Metallurgical Engineering)Neutron diffraction is a powerful non-destructive method for evaluating the microscopic structure and internal stress of metal plates as a bulk average. Precise neutron diffraction measurements with a high intensity neutron beam have already been carried out at large-scale neutron facilities. However, it is not easy to provide users with enough experimental opportunities. We are working on upgrading the neutron diffractometer with techniques of time-of-flight to enable stress measurements at RIKEN accelerator-driven compact neutron source (RANS). To improve neutron diffraction resolution, delayed neutrons, which expand neutron beam pulse width, should be suppressed. However, it is difficult to separate the delayed neutrons experimentally. In this study, a new analysis method has been proposed to deconvolute the diffraction peak from the delayed neutron component. Moreover, a new collimator system, called decoupled collimator system, has been developed to reduce the number of delayed neutrons. The diffraction patterns from a powder sample of pure body-centered cubic iron were measured with the decoupled collimator and the diffraction peak of {211} reflection was analyzed by the new analysis method using a model function of a single exponential decay function convoluted with a Gaussian function. By this method, the decoupled collimator system has been confirmed to achieve a smaller measurement limit of lattice strain 
than a small-aperture polyethylene collimator system and a non-collimator system. The currently available was 6.7
10
, this means that the internal stress up to 130 MPa can be well evaluated for steel materials with a Young's modulus of 200 GPa at RANS.
雨宮 雄太郎*; 中田 伸生*; 諸岡 聡; 小坂 誠*; 加藤 雅治*
ISIJ International, 62(2), p.282 - 290, 2022/02
被引用回数：3 パーセンタイル：24.31(Metallurgy & Metallurgical Engineering)To gain a deeper understanding of the dynamic accommodation mechanism of the internal stress in pearlite originating from the lattice misfit between ferrite and cementite phases, the lattice parameter ratios of cementite, b
/a and c/a, were locally analyzed in detail using the electron backscatter diffraction (EBSD) technique. The EBSD analysis revealed that the lattice parameter ratios of the cementite lamellae clearly differed from those of the spheroidized cementite particles, indicating that pearlite has a certain amount of internal stress as long as it maintains a lamellar structure. The internal stress in pearlite gradually decreased during the isothermal holding at 923 K after the pearlitic transformation due to the interfacial atomic diffusion of Fe atoms. However, a comparison with the theoretical values obtained from the Pitsch-Petch orientation relationship revealed that a large amount of internal stress had been already accommodated during the pearlitic transformation by the introduction of misfit dislocations and structural ledges on ferrite/cementite lamellar interfaces, i.e., the internal stress of pearlite is dynamically reduced by two different processes; built-in accommodation upon pearlitic transformation and additional time-dependent relaxation after pearlitic transformation. On the other hand, the analysis of the EBSD and neutron diffraction results yielded intriguingly different lattice parameters of cementite, indicating that various crystallographic orientation relationships between ferrite and cementite coexist in pearlite. Furthermore, the elastic strain energy analysis suggests that the invariant-line criterion on the ferrite/cementite interface plays an important role for the selection of orientation relationships in pearlite.
大場 洋次郎; 諸岡 聡; 大石 一城*; 鈴木 淳市*; 土山 聡宏*
ISIJ International, 62(1), p.173 - 178, 2022/01
被引用回数：3 パーセンタイル：24.31(Metallurgy & Metallurgical Engineering)Neutron transmission spectra of Cu steel were measured to characterize the change of microstructures by cold rolling. Bragg edges in neutron attenuation coefficients indicate the rotation of {110} planes of ferrite grains and is useful to characterize the evolution of preferred orientations with the cold rolling. In addition, SANS contribution in the neutron attenuation coefficients provides the nanostructural information about the deformation of the Cu precipitates. These results demonstrate that the neutron transmission analysis is beneficial for microstructural characterization in steels.
足立 望*; 上野 春喜*; 尾上 勝彦*; 諸岡 聡; 戸高 義一*
ISIJ International, 61(8), p.2320 - 2322, 2021/08
被引用回数：5 パーセンタイル：28.30(Metallurgy & Metallurgical Engineering)This study investigated the hydrogen permeation property of cementite by fabricating bulk cementite sample using the process combining the mechanical ball milling and subsequent pulse current sintering. The bulk cementite sample having a 96 vol% of cementite was successfully fabricated. The prepared bulk cementite showed no signal of hydrogen permeation during the 3.5 day of electrochemical hydrogen permeation test. The morphology of blister formed in the sample indicated that diffusion coefficient of hydrogen in cementite is very small.
中山 雄太*; 小川 文男*; 旭吉 雅健*; 橋立 竜太; 若井 隆純; 伊藤 隆基*
ISIJ International, 61(8), p.2299 - 2304, 2021/08
被引用回数：5 パーセンタイル：28.30(Metallurgy & Metallurgical Engineering)高温において多軸負荷を受ける改良9Cr-1Mo鋼のクリープ疲労強度について述べる。中空円筒試験片を用いて、さまざまなひずみ波形での低サイクル疲労試験を実施した。低サイクル疲労試験は、軸ひずみを固定した比例負荷と、軸ひずみとせん断ひずみの位相差が90度の非比例負荷の下で実施した。応力緩和とひずみ保持が破壊寿命に及ぼす影響を検討するために、さまざまなひずみ速度での低サイクル疲労試験とさまざまな保持時間でのクリープ疲労試験も実施した。2種類の多軸クリープ疲労寿命評価方法を提案した。第一の方法は、非比例負荷係数とクリープ損傷を考慮したマンソンのユニバーサルスロープ法を使用してひずみ範囲を計算する。第二の方法は、線形損傷則を用いて非比例負荷係数を考慮して疲労損傷を計算し、修正延性損耗則からクリープ損傷を計算する。第二の方法は精度が優れ、第一の方法はそれより精度は劣るが、実用性が高い。
西村 隼杜*; 北條 智彦*; 味戸 沙耶*; 柴山 由樹*; 小山 元道*; 齋藤 寛之*; 城 鮎美*; 安田 良*; 菖蒲 敬久; 秋山 英二*
ISIJ International, 61(4), p.1170 - 1178, 2021/04
被引用回数：7 パーセンタイル：38.80(Metallurgy & Metallurgical Engineering)The effects of residual stress on the hydrogen embrittlement behavior of a tempered martensitic steel sheet with 1-GPa-class tensile strength stretch-formed by a hemisphere punch simulating press-formed automotive structural parts were investigated. Cracking on the stretch-formed specimen induced by potentiostatic hydrogen charging was initiated in the foot of the impression of the specimen and propagated to the radial direction both toward the hillside and the plain. The mixture of quasi cleavage and intergranular fractures were observed whole through the fracture surface. Residual stress in the stretch-formed specimens was analyzed by using energy-dispersive X-ray diffraction method utilizing the synchrotron X-ray radiation at SPring-8. In addition, stress and plastic strain distributions in the specimen were analyzed by using Finite Element Method (FEM). These analyses depicted that the high tensile stress in the circumferential direction was in the foot of the impression, corresponding to the direction of the crack growth. The FEM analysis revealed that the high triaxial stress was in the foot suggesting accumulation of hydrogen. It was considered that the preferential crack initiation at the foot was promoted by the high residual stress in the circumferential direction and the hydrogen accumulation due to stress-induced diffusion.
五十嵐 誉廣; 大谷 恭平; 加藤 千明; 坂入 正敏*; 富樫 侑介*; 馬場 和彦*; 高木 周作*
ISIJ International, 61(4), p.1085 - 1090, 2021/04
被引用回数：2 パーセンタイル：10.70(Metallurgy & Metallurgical Engineering)水溶液中の金属カチオン(Zn
, Mg, Na
)が鉄への水素透過に及ぼす影響を明らかにするために、鉄表面からの水素透過量をレーザーアブレーションを用いた電気化学試験により測定した。また、金属カチオンによる水素透過の基本的なメカニズムを得るために、第一原理計算を使用して金属カチオンの吸着ポテンシャルと鉄表面周辺の電子状態を取得した。実験解析から、溶液中のZnによって鉄表面の陽極反応が抑制されることがわかった。また量子解析から、ZnイオンはNa, Mgイオンよりも鉄表面に強く結合することがわかった。これより、鉄の溶解反応はZn層の形成により抑制され鉄への水素透過の抑制につながることが示唆された。
柴山 由樹; 北條 智彦*; 小山 元道*; 齋藤 寛之*; 城 鮎美*; 安田 良*; 菖蒲 敬久; 松野 崇*; 秋山 英二*
ISIJ International, 61(4), p.1322 - 1329, 2021/04
被引用回数：7 パーセンタイル：38.80(Metallurgy & Metallurgical Engineering)The effects of stress and plastic strain distributions on the hydrogen embrittlement fracture of the U-bent martensitic steel sheet specimen were investigated. The hydrogen embrittlement testing of the U-bent specimen was performed. Fracture morphology mainly consisting of intergranular fracture was found inside the hydrogen charged U-bent specimen, which indicated that the crack initiation took place in the interior, and shear lips were found near both surfaces of the U-bent sheet. The synchrotron X-ray diffraction measurement and the finite element simulation were utilized to analyze the stress and plastic strain distributions in the thickness direction of the U-bent specimen. The elastic strain distributions obtained by the measurement showed a good agreement with the simulation. The crack initiation site of the hydrogen-charged U-bent specimen was considered to be correspondent with the region where the tensile stress was the highest, suggesting that the maximum tensile stress predominantly determine the crack initiation.
Harjo, S.; 川崎 卓郎; 土田 紀之*; 諸岡 聡; Gong, W.*
ISIJ International, 61(2), p.648 - 656, 2021/02
被引用回数：9 パーセンタイル：47.50(Metallurgy & Metallurgical Engineering) neutron diffraction measurements of two low-alloy steels and a 304-type stainless steel during tensile and creep tests were performed at room temperature. Changes in the diffraction pattern, the integrated peak intensities of austenite (), and the peak positions of were analyzed and discussed to elucidate the relationship between intergranular stress in and the occurrence of martensitic transformation during deformation. Tensile loading experiments revealed that the susceptibility to martensitic transformation depended on the -(hkl) grains, where -(111) grains underwent martensitic transformation at the latest. The -hkl dependence of the susceptibility to martensitic transformation was found to be controlled by the shear stress levels in -(hkl) grains, which were affected by the intergranular stress partitioning during deformation.
