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neutron diffractionZhou, Y.*; Song, W.*; Zhang, F.*; Wu, Y.*; Lei, Z.*; Jiao, M.*; Zhang, X.*; Dong, J.*; Zhang, Y.*; Yang, M.*; et al.
Journal of Alloys and Compounds, 971, p.172635_1 - 172635_7, 2024/01
被引用回数：0 パーセンタイル：0(Chemistry, Physical)The grain orientation-dependent lattice strain evolution of a (TiZrHfNb)
refractory high-entropy alloy (HEA) during tensile loading has been investigated using neutron diffraction. The equivalent strain-hardening rate of each of the primary 
-oriented grain families was found to be relatively low, manifesting the macroscopically weak work-hardening ability of such a body-centered cubic (BCC)-structured HEA. This finding is indicative of a dislocation planar slip mode that is confined in a few single-slip planes and leads to in-plane softening by high pile-up stresses.
Liss, K.-D.*; Han, J.-K.*; Blankenburg, M.*; Lienert, U.*; Harjo, S.; 川崎 卓郎; 徐 平光; 行武 栄太郎*; Kawasaki, M.*
Journal of Materials Science, 23 Pages, 2024/00
被引用回数：0 パーセンタイル：0(Materials Science, Multidisciplinary)The magnesium alloy AZ31, which has undergone high-pressure torsion processing, was subjected to in situ annealing micro-beam synchrotron high-energy X-ray diffraction and compared to the as-received rolled sheet material that was investigated through in situ neutron diffraction. While the latter only exhibits thermal expansion and minor recovery, the nanostructured specimen displays a complex evolution, including recovery, strong recrystallization, phase transformations, and various regimes of grain growth. Nanometer-scale grain sizes, determined using Williamson-Hall analysis, exhibit seamless growth, aligning with the transition to larger grains, as assessed through the occupancy of single grain reflections on the diffraction rings. The study uncovers strain anomalies resulting from thermal expansion, segregation of Al atoms, and the kinetics of vacancy creation and annihilation. Notably, a substantial number of excess vacancies were generated through high-pressure torsion, and maintained for driving the recrystallization and forming highly activated volumes for diffusion and phase precipitation during heating. The unsystematic scatter observed in the Williamson-Hall plot indicates high dislocation densities following severe plastic deformation, which significantly decreases during recrystallization. Subsequently, dislocations reappear during grain growth, likely in response to torque gradients in larger grains. It is worth noting that the characteristics of unsystematic scatter differ for dislocations created at high and low temperatures, underscoring the strong temperature dependence of slip system activation.
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：13 パーセンタイル：98.47(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).
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：18 パーセンタイル：94.44(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.
Lee, M.-S.*; 川崎 卓郎; 山下 享介*; Harjo, S.; Hyun, Y.-T.*; Jeong, Y.*; Jun, T.-S.*
Scientific Reports (Internet), 12(1), p.3719_1 - 3719_10, 2022/03
被引用回数：6 パーセンタイル：63.54(Multidisciplinary Sciences)Titanium has a significant potential for the cryogenic industrial fields such as aerospace and liquefied gas storage and transportation due to its excellent low temperature properties. To develop and advance the technologies in cryogenic industries, it is required to fully understand the underlying deformation mechanisms of Ti under the extreme cryogenic environment. Here, we report a study of the lattice behaviour in grain families of Grade 2 CP-Ti during in-situ neutron diffraction test in tension at temperatures of 15-298 K. Combined with the neutron diffraction intensity analysis, EBSD measurements revealed that the twinning activity was more active at lower temperature, and the behaviour was complicated with decreasing temperature.
Luo, M.-Y.*; Lam, T.-N.*; Wang, P.-T.*; Tsou, N.-T.*; Chang, Y.-J.*; Feng, R.*; 川崎 卓郎; Harjo, S.; Liaw, P. K.*; Yeh, A.-C.*; et al.
Scripta Materialia, 210, p.114459_1 - 114459_7, 2022/03
被引用回数：14 パーセンタイル：91.47(Nanoscience & Nanotechnology)The effect of grain size on strain-controlled low-cycle fatigue (LCF) properties in the CoCrFeMnNi high-entropy alloys (HEAs) was investigated towards the distinct microstructural developments during cyclic loading at a strain amplitude of 
1.0%. A much more prominent secondary cyclic hardening (SCH) behavior at the final deformation stage was observed in the fine-grained (FG) than in the coarse-grained (CG) CoCrFeMnNi. In-situ neutron-diffraction and microscopic examination, strongly corroborated by molecular dynamic (MD) simulations, indicated that dislocation activities from planar slip to wavy slip-driven subgrain structures within the grains acted as the primary cyclic-deformation behaviors in the FG CoCrFeMnNi. Differently observed in the cyclic behavior of the CG CoCrFeMnNi was due to a transition from the planar dislocation slip to twinning.
Lam, T.-N.*; Luo, M.-Y.*; 川崎 卓郎; Harjo, S.; Jain, J.*; Lee, S.-Y.*; Yeh, A.-C.*; Huang, E.-W.*
Crystals (Internet), 12(2), p.157_1 - 157_9, 2022/02
被引用回数：6 パーセンタイル：86.22(Crystallography)In this research, we systematically investigated equiatomic CoCrFeNi and CoCrFeMnNi high-entropy alloys (HEAs). Both of these HEA systems are single-phase, face-centered-cubic (FCC) structures. Specifically, we examined the tensile response in as-cast quaternary CoCrFeNi and quinary CoCrFeMnNi HEAs at room temperature. Compared to CoCrFeNi HEA, the elongation of CoCrFeMnNi HEA was 14% lower, but the yield strength and ultimate tensile strength were increased by 17% and 6%, respectively. The direct real-time evolution of structural defects during uniaxial straining was acquired via in situ neutron-diffraction measurements. The dominant microstructures underlying plastic deformation mechanisms at each deformation stage in as-cast CoCrFeNi and CoCrFeMnNi HEAs were revealed using the Convolutional Multiple Whole Profile (CMWP) software for peak-profile fitting. The possible mechanisms are reported.
Naeem, M.*; He, H.*; Harjo, S.; 川崎 卓郎; Lin, W.*; Kai, J.-J.*; Wu, Z.*; Lan, S.*; Wang, X.-L.*
Acta Materialia, 221, p.117371_1 - 117371_18, 2021/12
被引用回数：31 パーセンタイル：94.71(Materials Science, Multidisciplinary)We studied the deformation behavior of CrFeCoNi high-entropy alloy by in situ neutron diffraction at room temperature, intermediate low temperature of 140 K, low temperatures of 40 K (no serrated deformation) and 25 K (with massive serrations). The contributions from different deformation mechanisms to the yield strength and strain hardening have been estimated. The athermal contributions to the yield strength were 
183 MPa at all temperatures, while the Peierls stress increased significantly at low temperatures (from 148 MPa at room temperature to 493 MPa at 25 K). Dislocations contributed to 94% strain hardening at room temperature. Although the dislocation strengthening remained the major hardening mechanism at very low temperatures, the planar faults contribution increased steadily from 6% at room temperature to 28% at 25 K.
Naeem, M.*; Zhou, H.*; He, H.*; Harjo, S.; 川崎 卓郎; Lan, S.*; Wu, Z.*; Zhu, Y.*; Wang, X.-L.*
Applied Physics Letters, 119(13), p.131901_1 - 131901_7, 2021/09
被引用回数：9 パーセンタイル：64.95(Physics, Applied)We investigated the in situ deformation behavior of the CrCoNi medium-entropy alloy at a cryogenic temperature of 140 K and compared it with deformation at room temperature. The sample exhibited higher strength and larger ductility at the cryogenic temperature. The CrCoNi alloy remained single-phase face-centered cubic at room temperature, while deformation at 140 K resulted in a martensitic transformation to the hexagonal close-packed structure. The phase transformation, an additional deformation mechanism to stacking faults, twinning, and dis- location slip, resulted in a higher work hardening at cryogenic temperature. The study addresses the structure metastability in the CrCoNi alloy, which led to the formation of epsilon-martensite from the intrinsic stacking faults.
Zhang, X. X.*; Knoop, D.*; Andr
, H.*; Harjo, S.; 川崎 卓郎; Lutz, A.*; Lahres, M.*
International Journal of Plasticity, 140, p.102972_1 - 102972_20, 2021/05
被引用回数：28 パーセンタイル：94.42(Engineering, Mechanical)To better understand and predict the mechanical properties of additive manufacturing (AM) Al-Si-Mg alloys, developing a physically-based constitutive model is crucial. Among different models, the dislocation-density-based Kocks-Mecking (K-M) constitutive model has been widely used. In-situ neutron diffraction, a powerful method to measure the phase stress and dislocation density in bulk polycrystalline materials under loading, is employed to investigate the AM AlSi3.5Mg1.5 and AlSi3.5Mg2.5 (wt.%) alloys. Based on the present measured and previous experimental data, a multiscale constitutive model is developed for different AM Al-Si-Mg alloys.
He, H.*; Naeem, M.*; Zhang, F.*; Zhao, Y.*; Harjo, S.; 川崎 卓郎; Wang, B.*; Wu, X.*; Lan, S.*; Wu, Z.*; et al.
Nano Letters, 21(3), p.1419 - 1426, 2021/02
被引用回数：41 パーセンタイル：95.42(Chemistry, Multidisciplinary)In CrCoNi, a so-called medium-entropy alloy, an fcc-to-hcp phase transformation has long been anticipated. Here, we report an in situ loading study with neutron diffraction, which revealed a bulk fcc-to-hcp phase transformation in CrCoNi at 15 K under tensile loading. By correlating deformation characteristics of the fcc phase with the development of the hcp phase, it is shown that the nucleation of the hcp phase was triggered by intrinsic stacking faults. The confirmation of a bulk phase transformation adds to the myriads of deformation mechanisms available in CrCoNi, which together underpin the unusually large ductility at low temperatures.
Zhang, X. X.*; Andr, H.*; Harjo, S.; Gong, W.*; 川崎 卓郎; Lutz, A.*; Lahres, M.*
Materials & Design, 198, p.109339_1 - 109339_9, 2021/01
被引用回数：43 パーセンタイル：94.78(Materials Science, Multidisciplinary)Here, in-situ neutron diffraction is employed to explore the residual strains, stresses, and dislocation density in the LPBF AlSi10Mg during loading-unloading-reloading deformation. It is found that the maximum residual stresses of the Al and Si phases in the loading direction reach up to about -115 (compressive) and 832 (tensile) MPa, respectively. A notable dislocation annihilation phenomenon is observed in the Al matrix: the dislocation density decreases significantly during unloading stages, and the amplitude of this reduction increases after experiencing a larger plastic deformation. At the macroscale, this dislocation annihilation phenomenon is associated with the reverse strain after unloading. At the microscale, the annihilation phenomenon is driven by the compressive residual stress in the Al matrix. Meanwhile, the annihilation of screw dislocations during unloading stages contributes to the reduction in total dislocation density.
Lam, T.-N.*; Lee, S. Y.*; Tsou, N.-T.*; Chou, H.-S.*; Lai, B.-H.*; Chang, Y.-J.*; Feng, R.*; 川崎 卓郎; Harjo, S.; Liaw, P. K.*; et al.
Acta Materialia, 201, p.412 - 424, 2020/12
被引用回数：34 パーセンタイル：91.08(Materials Science, Multidisciplinary)We examined fatigue-crack-growth behaviors of CoCrFeMnNi high-entropy alloys (HEAs) under as-fatigued and tensile-overloaded conditions using neutron-diffraction measurements coupled with diffraction peak-profile analyses. We applied both high-resolution transmission electron microscopy (HRTEM) and neutron-diffraction strain mapping for the complementary microstructure examinations. Immediately after a single tensile overload, the crack-growth-retardation period was obtained by enhancing the fatigue resistance, as compared to the as-fatigued condition. The combined mechanisms of the overload-induced larger plastic deformation, the enlarged compressive residual stresses and plastic-zone size, the crack-tip blunting ahead of the crack tip, and deformation twinning governed the pronounced macroscopic crack-growth-retardation behavior following the tensile overload.
Naeem, M.*; He, H.*; Harjo, S.; 川崎 卓郎; Zhang, F.*; Wang, B.*; Lan, S.*; Wu, Z.*; Wu, Y.*; Lu, Z.*; et al.
Scripta Materialia, 188, p.21 - 25, 2020/11
被引用回数：56 パーセンタイル：97.36(Nanoscience & Nanotechnology)The deformation behavior of CrMnFeCoNi high entropy alloy was investigated by in situ neutron diffraction at an ultralow temperature of 15 K. Analysis of the diffraction peak widths showed an extremely high dislocation density at 15 K, reaching 10
m. In addition, the dislocation density was found to closely follow the development of texture caused by deformation. In contrast to deformation by dislocation slip at room temperature, the ultralow-temperature deformation also involved stacking faults, twinning and serrations. The deformation pathway at ultralow temperature is outlined which is responsible for the extraordinary strength-ductility combination.
Woo, W.*; Naeem, M.*; Jeong, J.-S.*; Lee, C.-M.*; Harjo, S.; 川崎 卓郎; He, H.*; Wang, X.-L.*
Materials Science & Engineering A, 781, p.139224_1 - 139224_7, 2020/04
被引用回数：39 パーセンタイル：93.25(Nanoscience & Nanotechnology)To elucidate deformation behavior behind the exceptional mechanical properties of CrCoNi based medium entropy alloys, the deformation related microstructural parameters were determined by using in situ neutron diffraction and peaks profile analysis methods. Superior tensile strength and elongation of the CrCoNi alloy is relevant to higher twin fault probability (
, up to 3.8%) and dislocation density (
, up to 9.7 10 m) compared to those (1.3% and 3.4 10 m, respectively) of the CrCoNiFe at 293K. Meanwhile, at 140K, the of the CrCoNiFe significantly increased up to 4.4% with the stable of 5.0 10 m and its mechanical properties overwhelm those of the CrCoNi at 273K. Such twinning dominant deformation mechanism at low temperature is also assured by lower stacking fault energy (SFE) of the CrCoNiFe at 140K compared to those of the CrCoNi and CrCoNiFe alloys at 293K.
Bae, J. W.*; Jung, J.*; Kim, J. G.*; Park, J. M.*; Harjo, S.; 川崎 卓郎; Woo, W.*; Kim, H. S.*
Materialia, 9, p.100619_1 - 100619_15, 2020/03
In the present study, an integrated experimental-numerical analysis on ferrous medium-entropy alloy (FMEA) was conducted to understand the micromechanical response of the constituent phases in the FMEA at -137
C. The initial face-centered cubic (FCC) single phase microstructure of the FMEA was transformed to body-centered cubic (BCC) martensite during tensile deformation at -137C, resulting in improved low-temperature mechanical properties. The microstructure evolution due to deformation-induced phase transformation mechanism and strain partitioning behavior was analyzed using 
electron backscatter diffraction. The mechanical responses related to the stress partitioning between constituent phases and deformation-induced transformation rate were measured using neutron diffraction in combination with the nanoindentation analysis.
Naeem, M.*; He, H.*; Zhang, F.*; Huang, H.*; Harjo, S.; 川崎 卓郎; Wang, B.*; Lan, S.*; Wu, Z.*; Wang, F.*; et al.
Science Advances (Internet), 6(13), p.eaax4002_1 - eaax4002_8, 2020/03
被引用回数：147 パーセンタイル：99.05(Multidisciplinary Sciences)High-entropy alloys exhibit exceptional mechanical properties at cryogenic temperatures, due to the activation of twinning in addition to dislocation slip. The coexistence of multiple deformation pathways raises an important question regarding how individual deformation mechanisms compete or synergize during plastic deformation. Using in situ neutron diffraction, we demonstrate the interaction of a rich variety of deformation mechanisms in high-entropy alloys at 15 K, which began with dislocation slip, followed by stacking faults and twinning, before transitioning to inhomogeneous deformation by serrations. Quantitative analysis showed that the cooperation of these different deformation mechanisms led to extreme work hardening. The low stacking fault energy plus the stable face-centered cubic structure at ultralow temperatures, enabled by the high-entropy alloying, played a pivotal role bridging dislocation slip and serration.
池田 修悟*; 金子 耕士; 田中 佑季*; 川崎 卓郎; 花島 隆泰*; 宗像 孝司*; 中尾 朗子*; 鬼柳 亮嗣; 大原 高志; 望月 健生*; et al.
Journal of the Physical Society of Japan, 89(1), p.014707_1 - 014707_7, 2020/01
被引用回数：1 パーセンタイル：11.81(Physics, Multidisciplinary)Magnetism in EuNiIn has been studied by specific heat, magnetic susceptibility, magnetization, 
Eu M
ssbauer spectroscopy, and neutron diffraction experiments. The specific heat shows two magnetic transitions at 
and 
at zero magnetic field. An antiferromagnetic ground state of EuNiIn has a uniaxial magnetic anisotropy along the b-axis, revealed by the magnetic susceptibility and the Mssbauer spectroscopy. Single crystal neutron diffraction experiments clarify that this antiferromagnetic structure in the ground state is characterized by the commensurate propagation vector 
= (1/2, 1/2, 1/2) which reveals no distinct anomaly at . The magnetization curve along the b-axis at 2 K shows four successive magnetic field-induced transitions up to 50 kOe and, reaches 7 
/f.u. above 190 kOe, The magnetic phase diagram in EuNiIn has unique characteristics with five magnetic states in low magnetic field.
Woo, W.*; Jeong, J.-S.*; Kim, D.-K.*; Lee, C. M.*; Choi, S.-H.*; Suh, J.-Y.*; Lee, S. Y.*; Harjo, S.; 川崎 卓郎
Scientific Reports (Internet), 10(1), p.1350_1 - 1350_15, 2020/01
被引用回数：64 パーセンタイル：94.51(Multidisciplinary Sciences)Stacking fault energies (SFE) were determined in additively manufactured (AM) stainless steel (SS 316 L) and equiatomic CrCoNi medium-entropy alloys. In situ neutron diffraction was performed to obtain a number of faulting-embedded diffraction peaks simultaneously from a set of (hkl) grains during deformation. The peak profiles diffracted from imperfect crystal structures were analyzed to correlate stacking fault probabilities and mean-square lattice strains to the SFE. The result shows that averaged SFEs are 32.8 mJ/m
for the AM SS 316 L and 15.1 mJ/m for the AM CrCoNi alloys. Meanwhile, during deformation, the SFE varies from 46 to 21 mJ/m (AM SS 316 L) and 24 to 11 mJ/m (AM CrCoNi) from initial to stabilized stages, respectively. The transient SFEs are attributed to the deformation activity changes from dislocation slip to twinning as straining.
Wang, B.*; He, H.*; Naeem, M.*; Lan, S.*; Harjo, S.; 川崎 卓郎; Nie, Y.*; Wang, X.-L.*; 他7名*
Scripta Materialia, 155, p.54 - 57, 2018/10
被引用回数：58 パーセンタイル：94.98(Nanoscience & Nanotechnology)The deformation behavior of an equi-atomic face-centered-cubic CoCrFeNi high entropy alloy was investigated by in-situ neutron diffraction under tensile loading up to 40% applied strain. A three-stage deformation behavior was fully captured by lattice strain and texture evolution. In spite of the chemical complexity, the deformation in CoCrFeNi is dominated by dislocation activities. Analysis of diffraction and microscopy data shows that the deformation progresses from dislocation slip to severe entanglement, where a sharp increase in dislocation density was observed. The neutron diffraction data, corroborated by transmission electron microscopy analysis, provided microscopic insights of the previously reported three-stage hardening behavior.
