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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：0 パーセンタイル：0.05(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：0 パーセンタイル：0(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.
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：0 パーセンタイル：0.05(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.
川崎 卓郎; 高橋 美和子*; 鬼柳 亮嗣; 大原 高志
Acta Crystallographica Section C; Structural Chemistry (Internet), 78(12), p.743 - 748, 2022/12
被引用回数：0 パーセンタイル：0.02(Chemistry, Multidisciplinary)Structural changes of the raffinose crystal on dehydration from the pentahydrate to the tetrahydrate were investigated by single-crystal time-of-flight neutron diffraction. It was revealed that during the dehydration, rearrangement occurs in the hydrogen bonds related to the lost water molecule, while the symmetry of the crystal structure is retained. The hydrogen-bonding status of raffinose pentahydrate and tetrahydrate were discussed comprehensively according to Jeffrey's hydrogen-bonding classification. It was shown that water molecules are hydrogen bonded to the surrounding molecules by 
O-H...O hydrogen bonds and 
C-H...O hydrogen bonds, and the number of these two types of hydrogen bonds determines the water molecules that are removed by dehydration. The lattice constant c showed a significant decrease on dehydration and further dehydration leads to loss of crystallinity of the raffinose crystals.
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：3 パーセンタイル：80.2(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：4 パーセンタイル：91.4(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：8 パーセンタイル：95.98(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：5 パーセンタイル：80.2(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：3 パーセンタイル：86.42(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.
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：2 パーセンタイル：77.1(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：0 パーセンタイル：0(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.
CoCrFeNi eutectic high entropy alloyYun, D.*; Chae, H.*; Lee, T.*; Lee, D.-H.*; Ryu, H. J.*; Banerjee, R.*; Harjo, S.; 川崎 卓郎; Lee, S. Y.*
Journal of Alloys and Compounds, 918, p.165673_1 - 165673_7, 2022/10
被引用回数：0 パーセンタイル：0(Chemistry, Physical)In this study, the deformation behavior and strengthening contribution of the FCC phase and B2 phase in AlCoCrFeNi eutectic high entropy alloys (HEAs) were investigated using in-situ neutron diffraction. An FCC matrix phase exhibited a slip-dominant deformation scheme, while twinning hardly contributed to deformation. Applied macroscopic stresses were rarely redistributed to the BCC A2 phase dispersed within the B2 phase, whereas the stress contribution of the B2 phase, which was initially lower than that of the FCC phase, increased significantly with an increase in plastic strain; hence, its contribution to tensile deformation became predominant. This study allows us to postulate a target value of each phase by microstructural tunning to achieve the desired properties of multicomponent phase HEAs.
Lam, T.-N.*; Lee, A.*; Chiu, Y.-R.*; Kuo, H.-F.*; 川崎 卓郎; Harjo, S.; Jain, J.*; Lee, S. Y.*; Huang, E.-W.*
Materials Science & Engineering A, 856, p.143961_1 - 143961_9, 2022/10
被引用回数：1 パーセンタイル：0(Nanoscience & Nanotechnology)Fine melt pool (FMP), coarse melt pool (CMP), and heat affected zone (HAZ) are generally observed in the additive manufactured AlSi10Mg alloys. In this study, we demonstrated that the yield strength can be estimated by the combination of the sizes and volume fractions of FMP, CMP, HAZ together with the second-phase hardening. Two different AlSi10Mg alloys fabricated via powder bed fusion (PBF) process were prepared to examine the lattice strain evolution of constituent phases during uniaxial tensile loading via in-situ neutron diffraction measurements. The horizontally-built (Hz-built) exhibited a much better yield and tensile strength as well as elongation compared to the vertically-built (Vt-built) AlSi10Mg alloy. We reported empirical strength quantification based on the sizes and ratios of fine melt pool (FMP), coarse melt pool (CMP), and heat affected zone (HAZ) together with the possible failure mode to prevent early fracture in the additive manufactured alloys.
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*
Materials Science & Engineering A, 854, p.143795_1 - 143795_12, 2022/09
被引用回数：0 パーセンタイル：0(Nanoscience & Nanotechnology)The role of the dislocation structure on the work-hardening behavior during the tensile deformation of quenched and tempered martensite was studied. The evolution of the dislocation structure during tensile deformation at room temperature in ultralow-carbon 18 mass%Ni martensitic steels under the conditions of as-quenched by subzero-treatment (SZ) and quenched-and-tempered at 573 and 773 K (T573 and T773, respectively) was monitored using in situ time-of-flight neutron diffraction combined with the convolutional multiple whole profile (CMWP) procedure. The changes in the dislocation parameters due to tempering and deformation obtained by the CMWP procedure were explained by the metallurgical phenomena of body-centered cubic iron.
Xu, S.*; 大平 拓実*; 佐藤 駿介*; Xu, X.*; 大森 俊洋*; Harjo, S.; 川崎 卓郎; Seiner, H.*; Zoubkov
, K.*; 村上 恭和*; et al.
Nature Communications (Internet), 13, p.5307_1 - 5307_8, 2022/09
被引用回数：0 パーセンタイル：0(Multidisciplinary Sciences)Crystalline metals can have large theoretical elastic strain limits. However, a macroscopic block of conventional crystalline metals practically suffers a very limited elastic deformation of 
0.5% with a linear stress-strain relationship obeying Hooke's law. Here, we report on the experimental observation of a large tensile elastic deformation with an elastic strain of 
4.3% in a Cu-based single crystalline alloy at its bulk scale at room temperature. The large macroscopic elastic strain that originates from the reversible lattice strain of a single phase is demonstrated by in situ microstructure and neutron diffraction observations. Furthermore, the elastic reversible deformation, which is nonhysteretic and quasilinear, is associated with a pronounced elastic softening phenomenon. The increase in the stress gives rise to a reduced Young's modulus, unlike the traditional Hooke's law behaviour. The experimental discovery of a non-Hookean large elastic deformation offers the potential for the development of bulk crystalline metals as high-performance mechanical springs or for new applications via "elastic strain engineering."
大平 拓実*; Xu, S.*; 平田 研二*; Xu, X.*; 大森 俊洋*; 植木 洸輔*; 上田 恭介*; 成島 尚之*; 長迫 実*; Harjo, S.; et al.
Advanced Materials, 34(27), p.2202305_1 - 2202305_11, 2022/07
被引用回数：1 パーセンタイル：59.23(Chemistry, Multidisciplinary)The demand for biomaterials has been increasing along with the increase in the population of elderly people worldwide. The mechanical properties and high wear resistance of metallic biomaterials makes them well-suited for use as substitutes or as support for damaged hard tissues. However, unless these biomaterials also have a low Young's modulus similar to that of human bones, bone atrophy inevitably occurs. Because a low Young's modulus is typically associated with poor wear resistance, it is difficult to realize a low Young's modulus and high wear resistance simultaneously. Also, the superelastic property of shape memory alloys makes them suitable for biomedical applications, like vascular stents and guide wires. However, due to the low recoverable strain of conventional biocompatible shape memory alloys, the demand for a new alloy system is high. The novel body-center-cubic cobalt-chromium-based alloys in this paper provide a solution to both of these problems. We believe our novel alloys are promising candidates for biomedical applications.
Wei, D.*; Gong, W.; 川崎 卓郎; Harjo, S.; 加藤 秀実*
Scripta Materialia, 216, p.114738_1 - 114738_6, 2022/07
被引用回数：7 パーセンタイル：97.04(Nanoscience & Nanotechnology)Near-equiatomic single-phase twining-induced plasticity (TWIP) high-entropy alloys (HEAs) exhibit a good combination of strength and ductility, but their modest yield strength requires further improvement. Here, we propose a strategy for markedly enhancing their strength while retaining satisfactory ductility, taking advantage of the temperature dependence of the stacking fault energy. The room-temperature strength of a representative TWIP HEA was improved by the cryogenic pre-deformation-induced dislocations, martensite, nanotwins, and stacking faults. The tensile properties were further tuned by subsequent annealing to obtain partially recovered or recrystallized microstructures. The influence of regulated microstructures on the yield strength was clarified by neutron diffraction line profile analysis. This study presents possibilities for fabricating advanced HEAs by tuning the substructures.
-Mg alloys based on peak asymmetry analysis江草 大佑*; 眞鍋 怜*; 川崎 卓郎; Harjo, S.; 佐藤 成男*; 阿部 英司*
Materials Today Communications (Internet), 31, p.103344_1 - 103344_6, 2022/06
被引用回数：0 パーセンタイル：0(Materials Science, Multidisciplinary)Based on X-ray diffraction analysis we attempt to quantify a volume fraction of stacking faults, which are essentially enriched by solute elements (solute-enriched stacking faults; SESFs) in Mg-Zn-Gd alloys with a hexagonal-close-packed () structure. We find that the SESFs with a local face-center-cubic stacking mostly occurs as a limited thickness less than several unit-cell dimensions, causing anisotropic broadening of the diffraction peaks including 
-component. By dealing the SESFs as intergrowth-like precipitates, we have successfully decomposed the asymmetric peak profile into the -matrix and the SESF peaks, by which the relevant volume fractions can be estimated in a highly quantitative manner.
structure observation of pyroelectric ceramics during power generation cycle川崎 卓郎; 福田 竜生; 山中 暁*; 坂本 友和*; 村山 一郎*; 加藤 孝典*; 馬場 将亮*; 橋本 英樹*; Harjo, S.; 相澤 一也; et al.
Journal of Applied Physics, 131(13), p.134103_1 - 134103_7, 2022/04
被引用回数：0 パーセンタイル：0(Physics, Applied)The microscopic origin of the pyroelectric power generation using ferroelectric ceramics for energy harvesting from time-varying waste heat can be understood by conducting 
neutron diffraction measurements. The behavior of the domain orientation and lattice strain in the lead zirconate titanate (PZT)-based ceramics with a tetragonal structure during the novel power generation cycle combining electric field and temperature change were investigated. The [001] domains and the lattice strain of the (111) plane in the direction of parallel to the electric field increase in the process of simultaneous rise in the electric field and temperature, and rapidly decrease in the process of the field drop. The alignment of the domain orientation by the electric field and its randomization by the higher temperature during the cycle are critical features of the current power generation system.
