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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
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.
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
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.
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：5 パーセンタイル：64.46(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.
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：2 パーセンタイル：32.54(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.
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：0 パーセンタイル：0(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：2 パーセンタイル：32.54(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：2 パーセンタイル：32.54(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：2 パーセンタイル：32.54(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.
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：4 パーセンタイル：33.99(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。
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：3 パーセンタイル：25.78(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.
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：1 パーセンタイル：8.06(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：3 パーセンタイル：25.78(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.
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：3 パーセンタイル：25.78(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.
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：5 パーセンタイル：41.35(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.
細谷 佳弘*; 松村 雄太*; 友田 陽*; 小貫 祐介*; Harjo, S.
ISIJ International, 60(9), p.2097 - 2106, 2020/09
被引用回数：5 パーセンタイル：31.59(Metallurgy & Metallurgical Engineering)In this paper, the microstructure formation during the R&P process and the deformation mechanism that would bring about the excellent strength-ductility balance are discussed based on the results obtained from the in situ neutron diffraction measurement. The results have revealed that the typical Luders-like stress-strain curve of R&P steel is caused by competitive plastic flow between austenite and martensite, and an effective transformation induced plasticity phenomenon.
Islam, M. S.*; 大谷 恭平; 坂入 正敏*
ISIJ International, 58(9), p.1616 - 1622, 2018/09
被引用回数：5 パーセンタイル：27.74(Metallurgy & Metallurgical Engineering)亜鉛めっき鋼板の腐食挙動には溶出した亜鉛イオンが寄与していると考えられるため、炭素鋼の腐食に及ぼす亜鉛イオンの影響および他の金属カチオンの影響を浸漬腐食試験および電気化学的手法を用いて調査した。浸漬腐食試験で得られた外観写真や質量変化から実験に用いたNa, Mg, Zn, Al
のなかで亜鉛は最も炭素鋼の防食に寄与することがわかった。XPS測定より亜鉛イオンは鋼の表面に結合していることが分かり、更に電気化学インピーダンス測定から亜鉛イオンが溶液に存在していると炭素鋼の腐食抵抗が大きくなるため耐食性の高い表面状態になっていることがわかった。実験結果より、亜鉛イオンは炭素鋼表面に亜鉛の金属カチオン層を形成して塩化物イオンによる攻撃を防いでいたと推察できる。すなわち、亜鉛めっき鋼板の防食作用は犠牲防食だけでなく溶出した亜鉛イオンによる防食作用も大きく寄与していると考えられる。
佐藤 成男*; 菖蒲 敬久; 佐藤 こずえ*; 小川 博美*; 我妻 一昭*; 熊谷 正芳*; 今福 宗行*; 田代 仁*; 鈴木 茂*
ISIJ International, 55(7), p.1432 - 1438, 2015/07
被引用回数：13 パーセンタイル：53.92(Metallurgy & Metallurgical Engineering)冷間延伸されたパーライト鋼ワイヤにおける転位の分布および異方性を特徴付けるために、X線回折線プロファイル解析をシンクロトロン放射マイクロビームを用いて行った。一般に、塑性せん断ひずみはワイヤの中心よりも表面近くでより激しかったが、中心から表面まで転位密度分布はほぼ一定であった。一方、転位の再配列は、転位の細胞構造を進化させ、表面に近づくほど進んだ。異方性転位密度によって、軸方向および横断方向の硬さの差異が説明できることも明らかになった。高温での回折データに基づく線プロファイル解析を行った。セメンタイトの回収率は一定の速度で進行したが、フェライト相の回収率は温度依存性を示し、フェライト相の回収率はセメンタイト相の回収率とはあまり関係していなかった。
林 健太郎*; 笠原 清司; 栗原 孝平*; 中垣 隆雄*; Yan, X.; 稲垣 嘉之; 小川 益郎
ISIJ International, 55(2), p.348 - 358, 2015/02
被引用回数：8 パーセンタイル：39.68(Metallurgy & Metallurgical Engineering)炭素循環製鉄(iACRES)のフローモデルによるプロセス評価により、iACRESへの高温ガス炉(HTGR)の適用性を評価した。高温電解で高炉ガス中のCO
をCOに還元して高炉にリサイクルするSOECシステムと、ISプロセスで製造したHによる逆シフト反応でCOをCOに還元して高炉にリサイクルするRWGSシステムを検討し、通常の高炉製鉄と比較した。逆シフト反応で消費されない分のHが高炉で鉄源の還元に使われたことが、RWGSシステムの方が原料炭節約とCO排出削減への効果が大きくなった原因であった。どの機器の改良がHTGR熱の効率的利用のために有用化を示すために、HTGR, SOEC, RWGSの熱収支解析を行った。SOECについては、ジュール熱の削減のためにCO電解温度の最適化が求められ、RWGSについては高いISプロセス水素製造効率が要求された。HTGR単位熱量当たりCO排出削減量の比較から、SOECシステムの方がより効率よくHTGR熱を利用できることが示された。
emission reduction of active carbon recycling energy system for ironmaking by modeling with Aspen Plus鈴木 克樹*; 林 健太郎*; 栗原 孝平*; 中垣 隆雄*; 笠原 清司
ISIJ International, 55(2), p.340 - 347, 2015/02
被引用回数：19 パーセンタイル：64.17(Metallurgy & Metallurgical Engineering)製鉄におけるCO排出量削減のために炭素循環製鉄(iACRES)が提案された。iACRESの効果を定量的に評価するために、化学プロセスシミュレータAspen PlusによりiACRESのプロセスフローモデルを作成し、熱物質収支からCO排出量とエクセルギー収支の解析を行った。高温ガス炉(HTGR)のエクセルギーを用いた固体酸化物電解(SOEC)と逆シフト反応をCO再生法として想定し、SOECではCO回収貯蔵の有無も考慮した。iACRESによってCO、Hが高炉に循環されたことによりCO排出量は3-11%削減されたが、CO再生のためにHTGRからのエクセルギーを投入したためエクセルギー有効率は1-7%低下した。
海老原 健一; 岩本 隆*; 松原 幸生*; 山田 紘樹*; 岡村 司*; 漆原 亘*; 大村 朋彦*
ISIJ International, 54(1), p.153 - 159, 2014/01
被引用回数：13 パーセンタイル：53.33(Metallurgy & Metallurgical Engineering)応力腐食割れの原因の1つである水素脆化の機構の理解には、鋼材中における水素の偏析位置(水素存在状態)を同定する必要がある。鋼材試料の一定割合での加熱で脱離する水素の量と試料温度との関係である水素熱脱離曲線は、水素存在状態を同定する有効なデータである。本論文では、実験室でよく用いる方法と実環境での水素侵入を模擬した方法の2通りで予ひずみを与えた高強度鋼に水素を添加した場合、両者の間で見られる水素熱脱離曲線の違いを数値解析で考察した。その結果、両者の違いは添加水素量による初期水素分布の違いに起因することが分かった。また、添加水素量が少ない場合、熱脱離曲線が初期水素分布に影響されやすいことが分かった。尚、本研究は、日本鉄鋼協会における「水素脆化研究の基盤構築」研究会(2009年-2013年)において実施された。
