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Ying, H.*; Yang, X.*; He, H.*; Yan, A.*; An, K.*; Ke, Y.*; Wu, Z.*; Tang, S.*; Zhang, Z.*; Dong, H.*; et al.
Scripta Materialia, 250, p.116181_1 - 116181_7, 2024/09
Nanoscale chemical fluctuations and their effect on the deformation behavior of CrFeCoNi-based high-entropy alloys (HEAs) were investigated using small-angle scattering and in situ neutron diffraction measurements. Small-angle scattering results demonstrated the presence of nano (10 nm) chemical fluctuations in the as-prepared CrFeCoNiPd HEAs, which was attributed to the negative mixing of enthalpy and the significant atomic radius difference between Pd and the constituent elements in the CrFeCoNi-based alloys. Subsequent tensile tests demonstrated that the yield and tensile strengths of the as-prepared CrFeCoNiPd HEA surpass those of the as-prepared CrMnFeCoNi HEA. Neutron diffraction data analysis revealed an anomalous response of dislocation evolution with the strain.
中本 美緒*; 菅野 未知央*; 荻津 透*; 杉本 昌弘*; 谷口 諒*; 廣瀬 清慈*; 川崎 卓郎; Gong, W.; Harjo, S.; 淡路 智*; et al.
IEEE Transactions on Applied Superconductivity, 34(5), p.8400806_1 - 8400806_6, 2024/08
For an accelerator magnet, a certain mechanical strength is required to sustain against a transverse compression stress due to Lorentz force. A bronze-route NbSn wire with Cu-Nb reinforcement was developed by Tohoku University and Furukawa Electric to enhance the strength against axial tension. The Cu-Nb reinforcement wire also exhibited some indication of strength improvement against transverse compression; however, the details of a reinforcement mechanism for the transverse compression stress have not been clarified. In this study, the internal strains of NbSn bronze-route wires with and without the Cu-Nb reinforcement under transverse compression stress were evaluated by neutron diffraction at BL19 (TAKUMI) in J-PARC. The samples were attached to jig with solder only at the ends and compression was applied at the center of the samples with 30-mm anvil with 5-mm wide and 8- to 15-mm high beam. Since a critical current, Ic of a superconducting wire depends on the three-dimensional strain, internal strain of NbSn along the axial and two orthogonal radial directions were evaluated at room temperature (RT). In the different setup, Ic measurements of the wires under transverse compression stresses were also performed at 4.2 K and 14.5 T. Using 3-mm wide anvil, the transverse compression was applied at 4.2 K or RT. The neutron diffraction results indicated no significant differences in the internal strains of NbSn under transverse compression between the samples with and without Cu-Nb reinforcement, while the Ic measurements showed potential increase in the irreversible stress () for Cu-Nb reinforced wires. The reason for this discrepancy was discussed based on the difference in the experimental setups for each measurement.
Nguyen, T.-D.*; Singh, C.*; Kim, Y. S.*; Han, J. H. *; Lee, D.-H.*; Lee, K.*; Harjo, S.; Lee, S. Y.*
Journal of Materials Research and Technology, 31, p.1547 - 1556, 2024/07
This study investigates the mechanical properties of a friction-stir-welded (FSW) AA6061-T6 aluminum alloy at ultra-low temperature (ULT) of 20 K. In-situ neutron diffraction and orientation imaging microscopy were employed to compare the tensile deformation behavior of the base metal (BM) and heat-affected zone (HAZ) in the FSW aluminum plate. The results demonstrate that compared to room-temperature (RT), ULT induces a significant improvement in tensile strength and ductility in both the BM and HAZ. The enhanced mechanical properties in BM at ULT result from a more homogeneous deformation than occurs at RT. On the other hand, HAZ at ULT exhibits an even lower yield strength than at RT, but the strain hardening rate (SHR) is the most significant among the alloys, leading to a tensile strength of 346 MPa and the highest ductility of 46.8%. The lowest yield strength corresponds to the lowest-hardness zones in HAZ, caused by dissolved/coarsened precipitates during the FSW process.
Harjo, S.; Gong, W.; 川崎 卓郎
日本材料学会第58回X線材料強度に関するシンポジウム講演論文集, p.51 - 54, 2024/07
In-situ neutron diffraction was used to study tensile deformation in an extruded AZ31 alloy. The aim was to validate existing methods and develop new ones for stress evaluation in magnesium alloys. Results showed varied increases in lattice strains among grains, posing challenges for conventional procedures. A new method, considering grain volume fraction and multiple orientations, proved highly accurate. When simultaneous hk.l peaks weren't available, the 12.1 peak was recommended for stress evaluation, showing a linear relationship with applied stress throughout deformation.
Harjo, S.; Gong, W.; 相澤 一也; 山崎 倫昭*; 川崎 卓郎
日本材料学会第58回X線材料強度に関するシンポジウム講演論文集, p.58 - 60, 2024/07
The experiment and analysis procedures for a sample exhibiting multimodal structures were outlined. The sample, a MgZnY alloy, initially comprised two phases: the HCP matrix (Mg) and the long-period stacking ordered phase (LPSO), constituting approximately 25% of the volume. Through hot extrusion at 623 K with an extrusion ratio (R) of 5.0, the alloy was rendered multimodal. Specifically, at an R value of 5.0, dynamic recrystallization occurred partially within the Mg phase, resulting in a bimodal microstructure. This microstructure consisted of a deformed Mg component and a recrystallized Mg component. An analysis employing Electron Backscatter Diffraction (EBSD) data facilitated multimodal characterization, enabling successful determination of stresses within the individual Mg components, as well as the LPSO phase stress.
Harjo, S.
Isotope News, (793), p.13 - 16, 2024/06
高強度マグネシウム(Mg)合金の高温押出加工による大幅な強度増加の機構を引張変形その場中性子回折実験によってどのように解明したかについて紹介する。高温押出加工の条件により組織が複雑化し、構成相それぞれの組織からの強度への寄与について解説する。
Ma, Y.*; Naeem, M.*; Zhu, L.*; He, H.*; Sun, X.*; Yang, Z.*; He, F.*; Harjo, S.; 川崎 卓郎; Wang, X.-L.*
Acta Materialia, 270, p.119822_1 - 119822_13, 2024/05
We report an in situ neutron diffraction study of 316 L that reveals an extraordinary work-hardening rate (WHR) of 7 GPa at 15 K. Detailed analyses show that the major contribution to the excellent strength and ductility comes from the transformation-induced plasticity (TRIP) effect, introduced by the austenite-to-martensite (-to-') phase transition. A dramatic increase in the WHR is observed along with the transformation; the WHR declined when the austenite phase is exhausted. During plastic deformation, the volume-fraction weighted phase stress and stress contribution from the '-martensite increase significantly. The neutron diffraction data further suggest that the -to-' phase transformation was mediated by the -martensite, as evidenced by the concurrent decline of the phase with the phase.
Kim, Y. S.*; Chae, H.*; Lee, D.-Y.*; Han, J. H. *; Hong, S.-K.*; Na, Y. S.*; Harjo, S.; 川崎 卓郎; Woo, W.*; Lee, S.-Y.*
Materials Science & Engineering A, 899, p.146453_1 - 146453_7, 2024/05
This work focused on the mechanical properties and serration-involved deformation behavior of advanced alloys at 15 K. Evolution of stacking faults and -martensite improved the mechanical performance of CoCrNi alloys, and significant strain-induced martensite transformation of DED-SS316L led to superior strength and strain hardening. A magnitude in stress drop was governed by dislocation density, phase type, and lattice defects, irrespective of processing method. FCC {200} notably was influenced recovery behavior after stress drop, and the contribution of strain energy density by serration on tensile toughness was the greatest for HR-CoCrNi.
Chae, H.*; Huang, E.-W.*; Jain, J.*; Lee, D.-H.*; Harjo, S.; 川崎 卓郎; Lee, S. Y.*
Metals and Materials International, 30(5), p.1321 - 1330, 2024/05
In situ neutron diffraction during tensile deformation was performed for the stainless steels prepared by the additive manufacturing (AM) processes with two strategies: vertically built and horizontally built. The AM steels were further aged without solid solution treatment. As the results, the retained austenite was found to be more stable because the chemical composition became homogeneous by aging, and the onset of deformation induced martensitic transformation was delayed.
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, 59(14), p.5831 - 5853, 2024/04
被引用回数:0 パーセンタイル:0.00(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.
Mao, W.; Gong, W.; Harjo, S.; 諸岡 聡; Gao, S.*; 川崎 卓郎; 辻 伸泰*
Journal of Materials Science & Technology, 176, p.69 - 82, 2024/03
被引用回数:0 パーセンタイル:0.00(Materials Science, Multidisciplinary)Fe-24Ni-0.3C(wt.%)準安定オーステナイト鋼の降伏応力は、平均結晶粒径が35m(粗粒[CG])から0.5m(超微細粒[UFG])に減少すると3.5倍(158551MPa)に増加したが、引張伸びは大きく維持された(0.870.82)。結晶粒径が力学特性と変形機構に及ぼす影響を定量的に明らかにするため、室温での引張変形中にCGとUFG Fe-24Ni-0.3C鋼のその場中性子回折測定を行った。CGとUFG試料における塑性変形の初期段階は転位すべりによって支配され、変形後期には変形誘起マルテンサイト変態(DIMT)も生じた。結晶粒の微細化により、DIMTの開始応力が大きく増加し、ひずみに関するDIMTの速度が抑制されることがわかった。結果として、(i)結晶粒微細化によりオー ステナイトが安定化し、DIMTに対して最も安定な結晶粒である111//LD(LD:負荷方向)オーステナイト粒でのDIMTの開始が大幅に遅れた。その結果、UFG試験片の111//LDオーステナイト粒のほとんどはマルテンサイトに変態しなかった。(ii)結晶粒の微細化は、マルテンサイト変態の自己促進効果も抑制した。それにもかかわらず、UFG試験片の変態速度が低いDIMTは、CG試験片のより応力を増加させるのに効率がよく、変形中に均一な変形を維持するのに適していた。以上の現象は、UFG準安定オーステナイト鋼の優れた強度と延性の両立に相互に寄与している。
Gong, W.; Gholizadeh, R.*; 川崎 卓郎; 相澤 一也; Harjo, S.
Magnesium Technology 2024, p.89 - 90, 2024/03
Mg and its alloys generally exist as a single hcp crystal structure at room temperature. It is widely recognized that the application of Mg alloys is hindered by their limited formability at room temperature, primarily attributable to the scarcity of readily activated deformation modes within the hcp phase. The addition of Li in Mg alloy can stable the bcc phase at room temperature, and these dual-phase (hcp+bcc) Mg-Li alloys exhibit excellent formability. The Li-enriched bcc phase has been frequently considered as the origin for improving formability. However, these Mg-Li alloys show poor work-hardening ability and the resultant low strength at room temperature. Considering that the dislocation recovery can be suppressed by decreasing the deformation temperature and the activity of deformation mode may be changed with temperature, we investigated the deformation behavior of a commercial LZ91 magnesium alloy at cryogenic temperatures using in-situ neutron diffraction.
萩原 幸司*; 眞山 剛*; 山崎 倫昭*; Harjo, S.; 徳永 透子*; 山本 和輝*; 杉田 三佳*; 青山 海琳*; Gong, W.; 西本 宗矢*
International Journal of Plasticity, 173, p.103865_1 - 103865_21, 2024/02
The unique control mechanisms of the plastic deformation of two-phase extruded alloy composed of Mg and long-period stacking ordered (LPSO) phase were clarified by comparison with those of other Mg solid-solution alloys, focusing on the question of why do the Mg/LPSO two-phase alloys exhibit both large elongation and high strength? The stress-strain curves for each grain in the alloys could be imaginary estimated using neutron diffraction analysis during the tensile test. The results demonstrate that the deformation behaviors of the worked and recrystallized grains are significantly different in all the Mg-extruded alloys owing to the strong plastic anisotropy in Mg with hexagonal close-packed (hcp) structure. Therefore, the deformation behavior is controlled by a composite-like deformation mechanism, even in single-phase Mg solid-solution alloys.
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.
鉄と鋼, 110(3), p.197 - 204, 2024/02
被引用回数:0 パーセンタイル:0.02The 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.
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.
鉄と鋼, 110(3), p.205 - 216, 2024/02
被引用回数:0 パーセンタイル:0.02deformation 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.
山下 享介*; Harjo, S.; 川崎 卓郎; 諸岡 聡; Gong, W.; 藤井 英俊*; 友田 陽*
ISIJ International, 64(2), p.192 - 201, 2024/01
被引用回数:0 パーセンタイル:0.02neutron diffraction measurements were performed on Fe-33Ni-0.004C alloy (33Ni alloy) and Fe-27Ni-0.5C alloy (27Ni-0.5C alloy) during cooling from room temperature to the cryogenic temperature (4 K) to evaluate changes in the lattice constants of austenite and martensite, and changes in the tetragonality of martensite due to thermally induced martensitic transformation. As the martensitic transformation progressed, the lattice constants of austenite in both alloys deviated to smaller values than those predicted considering the thermal shrinkage, accompanied by an increase in the full width at half maximum of austenite. The fresh martensite formed in both alloys had a body-centered tetragonal (BCT) structure, regardless of the carbon content. The tetragonality of martensite decreased with progressive martensitic transformation during cooling in the 33Ni alloy, but was almost constant in the 27Ni-0.5C alloy. This suggests that carbon is necessary to maintain the tetragonality of martensite during cooling. The tetragonality of martensite in the 27Ni-0.5C alloy decreased during room temperature aging because of carbon mobility.
Zhang, Y.*; 丸澤 賢人*; 工藤 航平*; 諸岡 聡; Harjo, S.; 宮本 吾郎*; 古原 忠*
ISIJ International, 64(2), p.245 - 256, 2024/01
被引用回数:0 パーセンタイル:0.02As-quenched martensite in carbon steels needs to be tempered to restore its ductility and toughness for practical applications. During tempering of martensite, microstructural evolutions induced by a series of reactions relevant to carbon diffusion is known to occur. In this study, multi-aspect characterization using advanced techniques such as in-situ neutron diffraction, transmission electron microscopy and three-dimensional atom probe tomography, was performed to investigate the changes in tetragonality, physical properties, microstructure and solute carbon content in high-carbon martensite, with an aim to clarify its low-temperature tempering behaviors. A binary alloy with a chemical composition of Fe-0.78 mass%C was austenitized and quenched to prepare the as-quenched martensite, followed by tempering in continuous heating at different heating rates. It was found that various reactions occurred sequentially during tempering, starting from the structure modulation generated by carbon clustering in the 0th stage, then followed by the precipitation of metastable -carbide particles on linear features in the 1st stage, towards the later decomposition of retained austenite and precipitation of cementite in the 2nd and 3rd stages, respectively. After analyzing the experimental results, the solute carbon content in martensite tempered under various conditions was found to be in good agreement with that estimated from the lattice volume expansion, whereas the evaluation based on the tetragonality might lead to some underestimation of the solute carbon content in martensite tempered at high temperatures.
上路 林太郎*; Gong, W.; Harjo, S.; 川崎 卓郎; 柴田 曉伸*; 木村 勇次*; 井上 忠信*; 土田 紀之*
ISIJ International, 64(2), p.459 - 465, 2024/01
Deformation-induced martensitic transformation (DIMT) during tensile or compressive deformations of the bainitic steels with various carbon content (0.15%C, 0.25%C, 0.62%C) was studied. In all of the bainitic steels, the tensile deformation exhibited larger work hardening than the compression. This difference indicates the suppression of the DIMT at the compression, and actually the measurements of electron back scattering diffraction (EBSD) confirmed the less reduction of retained austenite at the compression of all the bainitic steels. Additionally, the steel with the highest carbon content was examined by in situ neutron diffraction and clarified the difference similar to that obtained by the EBSD measurement. The regression of the relation between the fraction of austenite and applied strain with the conventional empirical equation revealed that the kinetic of DIMT is strongly dependent with the stress polarity, but not significantly changed by the carbon content.
Zhou, 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:0.00(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.
徐 平光; Zhang, S.-Y.*; Harjo, S.; Vogel, S. C.*; 友田 陽*
Quantum Beam Science (Internet), 8(1), p.7_1 - 7_13, 2024/01
Comprehensive information about the microstructure and crystal structure evolution during the preparation/production processes of various materials is in great demand in order to precisely control the microstructure morphology and the preferred orientation characteristics for the excellent strength-ductility-toughness balance of advanced engineering materials. isothermal annealing experiments of cold rolled 17Ni-0.2C (mass %) martensitic steel sheets were carried out by using the TAKUMI and ENGIN-X time-of-flight neutron diffractometers, respectively. The inverse pole figures based on full-profile refinement were extracted to roughly evaluate the preferred orientation features along three principal sample directions of investigated steel sheets using the General Structure Analysis System (GSAS) software with built-in generalized spherical harmonic functions. The consistent rolling direction (RD) inverse pole figures from TAKUMI and ENGIN-X have confirmed that the time-of-flight neutron diffraction has high repeatability and statistical reliability, revealing that the principal preferred orientation evaluation of steel materials is available through 90 TD ND (transverse direction normal direction) rotation of the investigated specimen on the sample stage during two neutron diffraction experiments. Moreover, these RD, TD and ND inverse pole figures before and after in situ experiments were compared with the corresponding inverse pole figures recalculated respectively from the MUSASI-L complete pole figure measurement and the HIPPO in situ microstructure evaluation. The similar orientation distribution characteristics suggested that the principal preferred orientation evaluation method can be applied to in situ microstructure evolution of bulk orthorhombic materials and spatially resolved principal preferred orientation mappings of large engineering structure parts.