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段野下 宙志*; 長谷川 寛*; 樋口 翔*; 松田 広志*; Gong, W.; 川崎 卓郎; Harjo, S.; 梅澤 修*
Scripta Materialia, 236, p.115648_1 - 115648_5, 2023/11
被引用回数：0Work-hardening behavior of a lath martensitic Fe-18Ni alloy during tensile deformation is discussed based on the Taylor's equation. The dislocation characteristics are monitored using in situ neutron diffraction. In the specimens of as-quenched (AQ) and tempered at 573 K (T573), the dislocations are extremely dense and randomly arranged. The dislocations in AQ and T573 form dislocation cells as deformation progresses. Consequently, a composite condition comprising cell walls and cell interiors is formed, and the coefficient 
in the Taylor's equation increases. Cells are already present in the specimen tempered at 773 K (T773), which has a low dislocation density and a large fraction of edge-type dislocations. As deformation continues, the dislocation density of T773 increases, its cell size decreases, and its composite condition become stronger. Simultaneously, the edge-type dislocation fraction decreases, keeping unchanged. Thus, both the dislocation arrangement and character affected , thereby affecting the work-hardening behavior.
Mao, W.; Gao, S.*; Gong, W.; Bai, Y.*; Harjo, S.; Park, M.-H.*; 柴田 曉伸*; 辻 伸泰*
Acta Materialia, 256, p.119139_1 - 119139_16, 2023/09
被引用回数：0変形誘起塑性(TRIP)鋼は、変形誘起マルテンサイト変態(DIMT)に伴う加工硬化率の向上により、強度と延性の優れた組み合わせを示す。TRIP鋼や合金の加工硬化挙動におけるDIMTの役割を定量的に評価することは、強度と延性の両立を可能にする先進材料を設計するための指針を与えるが、変形中に相組成が変化し続け、応力と塑性ひずみの両方が構成相間で動的に分配されるため、その評価は困難である。本研究では、Fe-24Ni-0.3C(wt.%)TRIPオーステナイト鋼の引張変形とその場中性子回折測定を行った。中性子回折測定による応力分割と相分割に基づく解析手法を提案し、試験片の引張流動応力と加工硬化率を、オーステナイト母相,変形誘起マルテンサイト、DIMT変態速度に関連する因子に分解し、試料の加工硬化挙動における各因子の役割を考察した。さらに、回折プロファイル解析により測定した転位密度を用いてオーステナイトとマルテンサイト間の塑性ひずみ分配を間接的に推定し、材料中のオーステナイトとマルテンサイト間の応力・ひずみ分配の全体像を構築した。その結果、変形誘起マルテンサイト変態速度とマルテンサイトが負担する相応力の両方が、材料の全体的な引張特性に重要な役割を果たしていることが示唆された。提案した分解解析法は、TRIP現象を示す多相合金の機械的挙動を調べるために広く適用できる可能性がある。
Mg and long-period stacking ordered phases in a Mg-Zn-Y alloy by hot-extrusion with low extrusion ratioHarjo, S.; Gong, W.; 相澤 一也; 川崎 卓郎; 山崎 倫昭*
Acta Materialia, 255, p.119029_1 - 119029_12, 2023/08
被引用回数：1 パーセンタイル：0.01(Materials Science, Multidisciplinary)An as-cast sample and two hot-extruded samples with different extrusion ratios (R) of Mg
Zn
Y
alloy containing the HCP matrix (Mg) and the long-period stacking ordered phase (LPSO) of about 25-vol%, were used in tensile deformation in situ neutron diffraction experiments, to elucidate the effects of uniquely different microstructural evolutions in Mg and LPSO with varying the R value to the mechanical properties. Mg behaved as the soft phase and LPSO as the hard phase, and hot-extrusion improved the strength of both. At the R value of 5.0, a bimodal microstructure was created in Mg, increasing largely the yield strength of Mg. With increasing the R value to 12.5, the bimodal microstructure of Mg collapsed and the yield strength of Mg decreased. However, the strength of LPSO increased monotonously with increasing the R value due to the developments of kink bands and texture.
neutron diffraction study on the deformation behavior of the plastic inorganic semiconductor AgSWang, Y.*; Gong, W.; 川崎 卓郎; Harjo, S.; Zhang, K.*; Zhang, Z. D.*; Li, B.*
Applied Physics Letters, 123(1), p.011903_1 - 011903_6, 2023/07
被引用回数：0Bulk AgS is a plastic inorganic semiconductor at room temperature. It exhibits a compressive strain greater than 50%, which is highly different from brittle conventional counterparts, such as silicon. Here, we present the experimental investigation of the deformation behavior in a plastic inorganic semiconductor AgS using 
neutron diffraction during compressive deformation at room and elevated temperatures. At room temperature, the lattice strain partitioning among 
-orientated grain families could be responsible for the significant work-hardening behavior in the bulk AgS with a monoclinic structure. The rapid accumulation of lattice defects and remarkable development of the deformation texture suggest that dislocation slip promotes plasticity. At 453 K, a monoclinic phase transforms into a body-centered cubic phase. A stress plateau appears at 
-4.8 MPa, followed by a rehardening state. The deformation mode of bulk AgS at the initial stage is likely attributable to the migration of silver ions, and as strain increases, it is closer to that of room temperature, leading to rehardening.
neutron diffractionGong, W.; Harjo, S.; 友田 陽*; 諸岡 聡; 川崎 卓郎; 柴田 曉伸*; 辻 伸泰*
Acta Materialia, 250, p.118860_1 - 118860_16, 2023/05
被引用回数：0 パーセンタイル：0.01(Materials Science, Multidisciplinary)Martensitic transformation is accompanied by the generation of microscale and macroscale internal stresses during cooling below the martensitic transformation start temperature. These internal stresses have been determined through X-ray or neutron diffraction, but the reported results are not consistent, probably because the measured lattice parameter is influenced not only by the internal stress but also by several factors, including solute elements and crystal defects. Therefore, neutron diffraction combined with dilatometry measurements during martensitic transformation and subsequent cyclic tempering were performed for an Fe-18Ni alloy. The phase strains calculated by lattice parameter variations show that a hydrostatic compressive strain in austenite and a tensile strain in martensite arose as the martensitic transformation progressed during continuous cooling or isothermal holding. However, the phase stresses of austenite and martensite estimated from these strains failed to hold stress balance law when dense crystal defects involved in the processes. After these crystal defects were removed by appropriate tempering, the stress balance law held well. Meanwhile, the phase stresses of austenite and martensite were changed to opposite, revealing their true identity. Various crystal defects in austenite and martensite, introduced by plastic accommodation, were suggested to affect their lattice parameters and then their phase stresses.
Kwon, H.*; Sathiyamoorthi, P.*; Gangaraju, M. K.*; Zargaran, A.*; Wang, J.*; Heo, Y.-U.*; Harjo, S.; Gong, W.; Lee, B.-J.*; Kim, H. S.*
Acta Materialia, 248, p.118810_1 - 118810_12, 2023/04
被引用回数：0 パーセンタイル：0.01(Materials Science, Multidisciplinary)Maraging steels, known for ultrahigh strength and good fracture toughness, derive their superior properties from lath martensite structure with high-density nanoprecipitates. In this work, we designed a novel Fe-based medium-entropy alloy with a chemical composition of Fe
Co
Ni
Mo
in atomic% by utilizing the characteristics of the maraging steels. By a single-step aging of only 10 min at 650 
C, the alloy showed microstructures consisting of a very high number density of (Fe, Co, Ni)
Mo
-type nanoprecipitates in lath martensite structure and reverted FCC phase, which led to ultrahigh yield strength higher than 2 GPa. This work demonstrates a novel direction to produce strong and ductile materials by expanding the horizons of material design with the aid of high-entropy concept and overcoming the limits of conventional materials.
Woo, W.*; Kim, Y. S.*; Chae, H. B.*; Lee, S. Y.*; Jeong, J. S.*; Lee, C. M.*; Won, J. W.*; Na, Y. S.*; 川崎 卓郎; Harjo, S.; et al.
Acta Materialia, 246, p.118699_1 - 118699_13, 2023/03
被引用回数：4 パーセンタイル：98.77(Materials Science, Multidisciplinary)In situ neutron diffraction experiments have been performed under loading in cast-wrought (CW) and additively manufactured (AM) equiatomic CoCrNi medium-entropy alloys. The diffraction line profile analysis correlated the faulting-embedded crystal structure to the dislocation density, stacking/twin fault probability, and stacking fault energy as a function of strain. The results showed the initial dislocation density of 1.8
10
m
in CW and 1.310
m in AM. It significantly increased up to 1.310
m- in CW and 1.710 m in AM near fracture. The dislocation density contributed to the flow stress of 470 MPa in CW and 600 MPa in AM, respectively. Meanwhile, the twin fault probability of CW (2.7%) was about two times higher than AM (1.3%) and the stacking fault probability showed the similar tendency. The twinning provided strengthening of 360 MPa in CW and 180 MPa in AM. Such a favorable strengthening via deformation twinning in CW and dislocation slip in AM was attributed to the stacking fault energy. It was estimated as 18.6 mJ/m
in CW and 37.5 mJ/m in AM by the strain field of dislocations incorporated model. Dense dislocations, deformation twinning, and atomic-scale stacking structure were examined by using electron backscatter diffraction (EBSD) and transmission electron microscopy (TEM).
西田 真之*; Harjo, S.; 川崎 卓郎; 山下 享介*; Gong, W.
Quantum Beam Science (Internet), 7(1), p.8_1 - 8_15, 2023/03
In this study, the thermal stress alterations generated in a tungsten fiber reinforced titanium composite (W/Ti composite) were evaluated by the neutron stress measurement method at cryogenic temperatures. The W/Ti composite thermal loads were repeated from room temperature to the cryogenic temperature (10 K), and alterations in thermal residual stress were evaluated using the neutron in situ stress measurement method. In this measurement, the stress alterations in the titanium matrix and the tungsten fibers were measured. This measurement was carried out by TAKUMI (MLF-BL19) of J-PARC, a neutron research facility in the Japan Atomic Agency. The measurement method of TAKUMI is the time-of-flight (TOF) method. Owing to this measurement method, the measurement time was significantly shortened compared to the angle-dispersion type measurement by a diffractometer. As a result of the measurement, large compressive stresses of about 1 GPa were generated in the tungsten fibers, and tensile stresses of about 100 MPa existed in the titanium matrix. The thermal stresses due to the temperature change between room temperature and cryogenic temperature is caused by the difference of thermal expansions between the tungsten fibers and the titanium matrix, and these stress values can be approximated by a simple elastic theory equation.
neutron diffraction studyGong, W.; 川崎 卓郎; Zheng, R.*; 眞山 剛*; Sun, B.*; 相澤 一也; Harjo, S.; 辻 伸泰*
Scripta Materialia, 225, p.115161_1 - 115161_5, 2023/03
被引用回数：2 パーセンタイル：53.96(Nanoscience & Nanotechnology)Deformation behavior during uniaxial compression at 21 K and 298 K in a commercial AZ31 magnesium alloy was studied by neutron diffraction. Decreasing the deformation temperature resulted in a slight increase in yield stress (115 MPa 
139 MPa), but a remarkable enhancement in both the fracture stress (365 MPa 551 MPa) and fracture strain (12.8% 16.5%). The low temperature sensitivity of the {10
2} extension twinning which governed the macroscopic yielding led to the slight increase in yield stress. At 21K, basal slip was suppressed, while the extension twinning was promoted resulted in higher twin volume fraction. In the late stage of deformation, the {101}-{102} double twinning was suppressed, which is considered to be the reason to delay the fracture at 21 K.
Lam, T.-N.*; Chin, H.-H.*; Zhang, X.*; Feng, R.*; Wang, H.*; Chiang, C.-Y.*; Lee, S. Y.*; 川崎 卓郎; Harjo, S.; Liaw, P. K.*; et al.
Acta Materialia, 245, p.118585_1 - 118585_9, 2023/02
被引用回数：2 パーセンタイル：32.61(Materials Science, Multidisciplinary)The present study investigates the crystallographic-texture effects on the improved fatigue resistance in the CoCrFeMnNi high-entropy alloys (HEAs) with the full-size geometry of the ASTM Standards E647-99. We exploited X-ray nano-diffraction mapping to characterize the crystal-deformation levels ahead of the crack tip after stress unloading under both constant- and tensile overloaded-fatigue conditions. The crack-tip blunting-induced much higher deformation level was concentrated surrounding the crack-tip which delays the fatigue-crack growth immediately after a tensile overload. The predominant deformation texture orientation in the Paris regime was investigated, using electron backscatter diffraction and orientation distribution function analyses. The twinning formation-driven shear deformation gave rise to the development of the Goss-type texture within the plastic deformation regime under a tensile-overloaded-fatigue condition, which was attributed to enhance the crack deflection and thus the tensile induced crack-growth-retardation period in the CoCrFeMnNi HEA.
Mg/LPSO dual-phase magnesium alloy monitored by neutron diffractionHarjo, S.; Gong, W.; 相澤 一也; 川崎 卓郎; 山崎 倫昭*; 眞山 剛*; 河村 能人*
Materials Transactions, 64(4), p.766 - 773, 2023/02
被引用回数：1 パーセンタイル：79.89(Materials Science, Multidisciplinary)To elucidate the effect of extrusion ratio in hot-extrusion on the deformation behavior during compression of MgZnY alloy containing about 25-vol% long-period stacking ordered phase (LPSO) in the HCP structured matrix (Mg), neutron diffraction measurements were performed under compressive loading using four types of samples: as-cast and after hot extrusion at 623 K with extrusion ratios of 5.0, 7.5 and 12.5. The macroscopic yielding was observed to appear by the occurrence of basal slip of Mg in the as-cast sample and at the onset of twinning in the hot extruded samples. The applied stress to initiate slip, twinning, and kinking increased by hot extrusion and then decreased with increasing extrusion ratio. LPSO shared higher stress than Mg and the ratio to the strength increased as the extrusion ratio increased.
neutron diffraction澤口 孝宏*; 友田 陽*; 吉中 奎貴*; Harjo, S.
Acta Materialia, 242, p.118494_1 - 118494_14, 2023/01
被引用回数：0 パーセンタイル：0(Materials Science, Multidisciplinary)Fe-Mn-Si-based alloys, show superior resistance to plastic fatigue compared to the conventional steels, which is ascribed to the reversible back-and-forth movement of Shockley partial dislocations associated with a reversible martensitic transformation between the face-centered cubic 
-austenite and hexagonal close-packed 
-martensite. The purpose of this study was to gather evidence of the reversible martensitic transformation using in situ neutron diffraction under cyclic loading. Three Fe-30Mn-Si-Al alloys with different Gibbs free energy differences at 298 K were studied to unravel the effect of phase stability on the degree of reversibility.
phase to 
phase in zirconium alloy revealed by in-situ neutron diffraction during high temperature deformationGuo, B.*; Mao, W.; Chong, Y.*; 柴田 曉伸*; Harjo, S.; Gong, W.; Chen, H.*; Jonas, J. J.*; 辻 伸泰*
Acta Materialia, 242, p.118427_1 - 118427_11, 2023/01
被引用回数：2 パーセンタイル：32.61(Materials Science, Multidisciplinary)Dynamic transformation from alpha (HCP) to beta (BCC) phase in a zirconium alloy was revealed by the use of in-situ neutron diffraction during hot compression. The dynamic transformation was unexpectedly detected during isothermal compression at temperatures of 900C and 950C (alpha + beta two-phase region) and strain rates of 0.01 s
and 0.001 s, even though equilibrium two-phase states were achieved prior to the hot compression. Dynamic transformation was accompanied by diffusion of Sn from beta to alpha phase, which resulted in changes of lattice parameters and a characteristic microstructure of alpha grains. The details of dynamic transformation are discussed using the evolution of lattice constants.
土田 紀之*; 上路 林太郎*; Gong, W.; 川崎 卓郎; Harjo, S.
Scripta Materialia, 222, p.115002_1 - 115002_6, 2023/01
被引用回数：4 パーセンタイル：68.37(Nanoscience & Nanotechnology)The present study investigated the tensile deformation behavior of quenched and tempered martensite steels at various austenitization and tempering temperatures using in situ neutron diffraction experiments. Phase lattice strains in the bcc and cementite (
) phases and dislocation structures in the bcc phase were analyzed. The phase lattice strain in bcc became almost stagnant after yielding as the tempering temperature increased. The phase lattice strain in increased linearly with an increase in the flow stress, independent of the austenitization and tempering temperatures. The stress partitioning between bcc and was confirmed after the yielding of bcc, which contributed to the work hardening. The phase stresses of bcc and and their stress partitioning improve the mechanical properties of martensite steels, which can be summarized by the systematic changes in phase lattice strain and dislocation properties due to the austenitization and tempering temperatures.
Wei, D.*; Gong, W.; 都留 智仁; Lobzenko, I.; Li, X.*; Harjo, S.; 川崎 卓郎; Do, H.-S.*; Bae, J. W.*; Wagner, C.*; et al.
International Journal of Plasticity, 159, p.103443_1 - 103443_18, 2022/12
被引用回数：12 パーセンタイル：96.77(Engineering, Mechanical)Face-centered cubic single-phase high-entropy alloys (HEAs) containing multi-principal transition metals have attracted significant attention, exhibiting an unprecedented combination of strength and ductility owing to their low stacking fault energy (SFE) and large misfit parameter that creates severe local lattice distortion. Increasing both strength and ductility further is challenging. In the present study, we demonstrate via meticulous experiments that the CoCrFeNi HEA with the addition of the substitutional metalloid Si can retain a single-phase FCC structure while its yield strength (up to 65%), ultimate strength (up to 34%), and ductility (up to 15%) are simultaneously increased, owing to a synthetical effect of the enhanced solid solution strengthening and a reduced SFE. The dislocation behaviors and plastic deformation mechanisms were tuned by the addition of Si, which improves the strain hardening and tensile ductility. The present study provides new strategies for enhancing HEA performance by targeted metalloid additions.
observation of twinning and detwinning in AZ31 alloyGong, W.; Zheng, R.*; Harjo, S.; 川崎 卓郎; 相澤 一也; 辻 伸泰*
Journal of Magnesium and Alloys (Internet), 10(12), p.3418 - 3432, 2022/12
被引用回数：12 パーセンタイル：94.02(Metallurgy & Metallurgical Engineering)Twinning and detwinning behavior of a commercial AZ31 magnesium alloy during cyclic compression-tension deformation with a total strain amplitude of 4% (
2%) was evaluated using the complementary techniques of neutron diffraction, identical area electron backscatter diffraction, and transmission electron microscopy. In-situ neutron diffraction demonstrates that the compressive deformation was dominated by twin nucleation, twin growth, and basal slip, while detwinning dominated the unloading of compressive stresses and subsequent tension stage. A large number of 
-component dislocations observed in twins and the detwinned regions were attributed to the dislocation transmutation during the twinning and detwinning. The accumulation of barriers including twin boundaries and various types of dislocations enhanced the interactions of migrating twin boundary with these barriers during twinning and detwinning, which is considered to be the origin for increasing the work hardening rate in cyclic deformation of the AZ31 alloy.
Wei, D.*; Gong, W.; Wang, L.*; Tang, B.*; 川崎 卓郎; Harjo, S.; 加藤 秀実*
Journal of Materials Science & Technology, 129, p.251 - 260, 2022/12
被引用回数：14 パーセンタイル：97.75(Materials Science, Multidisciplinary)Owing to their attractive structure and mechanical properties, high-entropy alloys (HEAs) and medium-entropy alloys (MEAs) have attracted considerable research interest. The strength of HEAs/MEAs with a single face-centered cubic (FCC) phase, on the other hand, requires improvement. Therefore, in this study, we demonstrate a strategy for increasing the room-temperature strength of FCC-phase HEAs/MEAs by tuning cryo-pre-straining-induced crystal defects via the temperature-dependent stacking fault energy-regulated plasticity mechanism. Through neutron diffraction line profile analysis and electron microscope observation, the effect of the tuned defects on the tensile strength was clarified. This study discussed the possibility of developing single-phase high-performance HEAs by tuning pre-straining-induced crystal defects.
neutron diffractionWei, D.*; Gong, W.; 都留 智仁; 川崎 卓郎; Harjo, S.; Cai, B.*; Liaw, P. K.*; 加藤 秀実*
International Journal of Plasticity, 158, p.103417_1 - 103417_17, 2022/11
被引用回数：13 パーセンタイル：97.75(Engineering, Mechanical)In this study, we investigated the yielding and hardening behaviors of the Cantor alloy and FCC-phase Co-rich HEAs with different SFEs by in situ neutron diffraction combined with the first-principles method and electron-microscopy characterizations. The Co-rich HEAs exhibited a higher intrinsic yield strength than the Cantor alloy, mainly because of the larger shear modulus or modulus misfit, and grain refinement being more effective in improving the yield strength of low-SFE HEAs. Furthermore, higher flow stresses and better ductility of the Co-rich HEAs are attributed to the greater dislocation density and a larger number of stacking faults, which enhanced the strain-hardening rate during tensile deformation. The low SFE promoted mechanical twinning, and martensitic transformation contributed to higher strain-hardening rates.
neutron diffraction and electron microscopy studyZheng, R.*; Gong, W.; Du, J.-P.*; Gao, S.*; Liu, M.*; Li, G.*; 川崎 卓郎; Harjo, S.; Ma, C.*; 尾方 成信*; et al.
Acta Materialia, 238, p.118243_1 - 118243_15, 2022/10
被引用回数：9 パーセンタイル：90.29(Materials Science, Multidisciplinary)Grain refinement can lead to the strengthening of metallic materials according to the Hall-Petch relationship. However, our recent results suggested that grain boundary sliding is the dominant deformation mode in bulk ultrafine grained (UFG) pure Mg at room temperature, leading to softening. Here, for the first time, we report that the Hall-Petch strengthening can be regained in bulk UFG pure Mg at cryogenic temperature. At 77K, the UFG pure Mg with a mean grain size of 0.6 
m exhibited ultrahigh tensile yield strength and ultimate tensile strength of 309 MPa and 380 MPa, respectively. Combined neutron diffraction and electron microscopy investigation indicated that residual dislocation structures and deformation twins hardly formed in the UFG specimen during tensile test at 298K. In contrast, fast accumulation of lattice defects and remarkable reorientation were evident at 77K, suggesting that the grain-boundary-mediated process was suppressed and the plastic deformation was dominated by dislocation slip and deformation twinning. In addition, all the pure Mg specimens exhibited pronounced strain hardening at 77 K, which was mainly attributed to the suppressed grain boundary sliding and dynamic recovery. The mean dislocation density and relative fractions of dislocations with various Burgers vectors of the UFG specimen deformed at 77K were determined quantitatively from neutron diffraction data.
Xu, X.*; 大平 拓実*; Xu, S.*; 平田 研二*; 大森 俊洋*; 植木 洸輔*; 上田 恭介*; 成島 尚之*; 長迫 実*; 貝沼 亮介*; et al.
Advanced Materials & Processes, 180(7), p.35 - 37, 2022/10
Metallic biomaterials are widely used to replace or support failing hard tissues due to excellent mechanical properties and high wear resistance, with demand increasing as the global population continues to age. It is widely accepted that successful metallic biomaterials should have good biocompatibility, high corrosion resistance, and strong wear resistance. In addition, a low Young's modulus similar to human bone is now recognized as another important factor, in order to avoid bone atrophy due to the stress shielding effect. While the Young's modulus of stainless steels and conventional fcc CoCr alloys is as high as 190-240 GPa, for -type Ti-base alloys it is generally in the range of 50-80 GPa. Young's modulus values are as low as 35 GPa for Ti-Nb-Ta-Zr, close to that of human bone at approximately 10-30 GPa. However, Ti-base alloys come with the compromise of low wear resistance. In fact, alloys that feature a low Young's modulus along with high wear resistance have been difficult to realize. This article explores the recently developed bcc CoCr-base alloy Co-Cr-Al-Si as a potential solution to these issues, i.e., the difficulty in combining a low Young's modulus with high wear resistance, and the challenge of realizing large superelastic strains.
