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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：0.01(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.
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：13 パーセンタイル：99.28(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：11 パーセンタイル：98.19(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).
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：5 パーセンタイル：64.46(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.
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：27 パーセンタイル：98.49(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.
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：17 パーセンタイル：93.62(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.
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：3 パーセンタイル：32.54(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：4 パーセンタイル：45.58(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.
Cs activity concentration in the aquatic insect 
(Tricoptera: Stenopsychidae) in the Ota River, Fukushima, Japan石井 弓美子*; 三浦 輝*; Jo, J.*; 辻 英樹*; 斎藤 梨絵; 小荒井 一真; 萩原 大樹; 漆舘 理之*; 錦織 達啓*; 和田 敏裕*; et al.
PLOS ONE (Internet), 17(5), p.e0268629_1 - e0268629_17, 2022/05
被引用回数：3 パーセンタイル：43.07(Multidisciplinary Sciences)本研究では、福島県太田川で採集した解虫性トビケラ(Stenopsyche marmorata)および肉食性ヘビトンボ(Protohermes grandis)幼虫の水生昆虫個体におけるCs放射能濃度のばらつきを調査した。トビケラ幼虫は散発的に高い放射能を示したが、ヘビトンボ幼虫ではばらつきは見られなかった。オートラジオグラフィーと走査型電子顕微鏡による分析から、これらのトビケラ幼虫試料には、不溶性のCs含有ケイ酸塩ガラス粒子である放射性Cs含有微粒子(CsMPs)が含まれていることが確認された。また、CsMPsはトビケラ幼虫の餌となりうるペリフィトンや漂流粒子状有機物にも含まれており、幼虫はCsMPsを同サイズの餌粒子とともに摂取している可能性が示唆された。淡水生態系におけるCsMPsの分布や生物による取り込みは比較的知られていないが、本研究はCsMPsが水生昆虫に取り込まれることを実証している。
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：91.45(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.
Wei, D.*; Wang, L.*; Zhang, Y.*; Gong, W.; 都留 智仁; Lobzenko, I.; Jiang, J.*; Harjo, S.; 川崎 卓郎; Bae, J. W.*; et al.
Acta Materialia, 225, p.117571_1 - 117571_16, 2022/02
被引用回数：59 パーセンタイル：99.75(Materials Science, Multidisciplinary)Recently-developed high-entropy alloys (HEAs) containing multiple principal metallic elements have ex-tended the compositional space of solid solutions and the range of their mechanical properties. Here we show that the realm of possibilities can be further expanded through substituting the constituent metals with metalloids, which are desirable for tailoring strength/ductility because they have chemical interactions and atomic sizes distinctly different from the host metallic elements. Specifically, the metalloid substitution increases local lattice distortion and short-range chemical inhomogeneities to elevate strength, and in the meantime reduces the stacking fault energy to discourage dynamic recovery and encourage defect accumulation via partial-dislocation-mediated activities. These impart potent dislocation storage to improve the strain hardening capability, which is essential for sustaining large tensile elongation. As such, metalloid substitution into HEAs evades the normally expected strength-ductility trade-off, enabling an unusual synergy of high tensile strength and extraordinary ductility for these single-phase solid solutions.
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：87.21(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.
Cr
Fe
C
high-entropy alloyKim, Y. S.*; Chae, H.*; Huang, E.-W.*; Jain, J.*; Harjo, S.; 川崎 卓郎; Hong, S. I.*; Lee, S. Y.*
Materials, 15(4), p.1312_1 - 1312_11, 2022/02
被引用回数：0 パーセンタイル：0(Chemistry, Physical)In this study, we manufactured a non-equiatomic (CoNi)CrFeC high-entropy alloy (HEA) consisting of a single-phase face-centered-cubic structure. The non-equiatomic (CoNi)CrFeC HEA revealed a good combination of strength and ductility in mechanical properties compared to the equiatomic CoNiCrFe HEA, due to both stable solid solution and precipitation-strengthened effects. The non-equiatomic stoichiometry resulted in not only a lower electronegativity mismatch, indicating a more stable state of solid solution, but also a higher stacking fault energy (SFE, 
50 mJ/m) due to the higher amount of Ni and the lower amount of Cr. This higher SFE led to a more active motion of dislocations relative to mechanical twinning, resulting in severe lattice distortion near the grain boundaries and dislocation entanglement near the twin boundaries.
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：94.34(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.
松谷 悠佑; McMahon, S. J.*; Butterworth, K. T.*; 内城 信吾*; 奈良 一志*; 谷内 淑恵*; 嵯峨 涼*; 石川 正純*; 佐藤 達彦; 伊達 広行*; et al.
Physics in Medicine & Biology, 66(7), p.075014_1 - 075014_11, 2021/04
被引用回数：4 パーセンタイル：47.6(Engineering, Biomedical)腫瘍内の低酸素細胞は放射線抵抗性を示し、分割放射線療法の悪性進行を引き起こす。不均質な酸素条件下に存在する腫瘍に線量を付与させる場合、照射野内と照射野外の細胞間で伝達される細胞間シグナリングにより、両者の放射線感受性が変化することが知られている。しかしながら、強度変調照射下において低酸素症が放射線感受性へ与える影響については不明である。本研究では、2種類のがん細胞株(DU145とH1299)を使用して、低酸素症が、照射野内外の細胞に対する放射線感受性(DNA損傷と細胞死)へもたらす影響を研究した。細胞実験の結果から、低酸素症は照射野外の放射線感受性へ明らかに影響を与える一方、その低酸素症の影響の程度(酸素増感効果比)は照射野内細胞よりも小さいことがわかった。DNA損傷ならびに細胞死の両評価対象に対して、照射野外で低減される放射線感受性について一貫した傾向が示された。これらの成果は、強度変調放射線を活用して低酸素下の腫瘍を照射する際の治療計画時において、放射線誘発の細胞間シグナリングを考慮する重要性を示すものである。
Kim, J. G.*; Bae, J. W.*; Park, J. M.*; Woo, W.*; Harjo, S.; Lee, S.*; Kim, H. S.*
Metals and Materials International, 27(2), p.376 - 383, 2021/02
被引用回数：9 パーセンタイル：51.51(Materials Science, Multidisciplinary)Heterogeneous structured materials achieve a combination of high strength and extreme ductility due to synergetic strengthening driven by conditions in the interfacial region. Although the origin of synergetic strengthening has been revealed to be strain incompatibility in the interfacial region, the effect of the strength difference between hard and soft phases on strengthening has not been investigated well. In the work reported in the present paper, the effect of the difference in strength of the hard and soft phases on synergetic strengthening was investigated by conducting in situ neutron diffraction tensile tests. As a result, it was determined that the dislocation density in a layered sheet of high Mn (HMn) steel/interstitial free (IF) steel is higher than that in a layered sheet of HMn/low carbon steel. The big difference in mechanical properties between HMn steel and IF steel induces a high stress gradient and results in additional dislocations.
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：95.34(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.
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：33 パーセンタイル：91.53(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.
Kim, S.*; Lee, B.*; Reeder, J. T.*; Seo, S. H.*; Lee, S.-U.*; Hourlier-Fargette, A.*; Shin, J.*; 関根 由莉奈; Jeong, H.*; Oh, Y. S.*; et al.
Proceedings of the National Academy of Sciences of the United States of America, 117(45), p.27906 - 27915, 2020/11
被引用回数：75 パーセンタイル：93.23(Multidisciplinary Sciences)本研究では、汗のコルチゾール分析のための流動イムノアッセイ、グルコースとアスコルビン酸(ビタミンC)分析のための蛍光測定イメージング、および電極を使用した発汗速度のデジタルトラッキングを組み合わせた、ワイヤレス,バッテリー不要の皮膚インターフェースマイクロ流体システムを実現した。運動している被験者を対象とした体系的なテストにより、本開発デバイスが物理的ストレスと生化学的相関を追跡可能であることが示された。
