Temperature-dependent deformation behavior of dual-phase medium-entropy alloy; In-situ neutron diffraction study

Gu, G. H.*; Jeong, S. G.*; Heo, Y.-U.*; Harjo, S.; Gong, W.; Cho, J.*; Kim, H. S.*; 他4名*

Journal of Materials Science & Technology, 223, p.308 - 324, 2025/07

https://doi.org/10.1016/j.jmst.2024.11.057

Face-centered cubic (FCC) equi-atomic multi-principal element alloys (MPEAs) exhibit excellent mechanical properties from cryogenic to room temperatures. At room temperature, deformation is dominated by dislocation slip, while at cryogenic temperatures (CTs), reduced stacking fault energy enhances strain hardening with twinning. This study uses in-situ neutron diffraction to analyze the temperature-dependent deformation behavior of Al(CoNiV), a dual-phase (FCC/BCC) medium-entropy alloy (MEA). At liquid nitrogen temperature (LNT), deformation twinning in the FCC matrix leads to additional strain hardening through the dynamic Hall-Petch effect, giving the appearance of improved strengthening at LNT. In contrast, BCC precipitates show dislocation slip at both 77 K and 298 K, with temperature-dependent lattice friction stress playing a significant role in strengthening. The study enhances understanding of deformation behaviors and provides insights for future alloy design.

Grain refinement of dual phase steel maximizes deformation ability of martensite, leading to simultaneous enhancement of strength and ductility

Park, M.-H.*; 柴田 曉伸*; Harjo, S.; 辻 伸泰*

Acta Materialia, 292, p.121061_1 - 121061_13, 2025/06

https://doi.org/10.1016/j.actamat.2025.121061

Dual-phase (DP) steel, composed of soft ferrite and hard martensite, offers excellent strength-ductility balance and low cost. This study found that refining the DP microstructure enhanced both yield strength and strain hardening, improving strength and ductility. Digital image correlation (DIC) revealed strain localization in ferrite, but refinement reduced strain differences between ferrite and martensite, suppressing crack initiation. More ferrite/martensite interfaces promoted plasticity in martensite via enhanced deformation constraint. neutron diffraction showed martensite bore higher phase stress, which increased with refinement. By combining -DIC and neutron data, individual stress-strain curves for ferrite and martensite were constructed for the first time, explaining the strength-ductility synergy through interphase constraint. These findings offer guidance for designing heterostructured materials to overcome the strength-ductility trade-off.

Experimental investigation of phase transformations in steel using X-ray and neutron diffraction

友田 陽*; Harjo, S.; 徐 平光; 諸岡 聡; Gong, W.; Wang, Y.*

Metals, 15(6), p.610_1 - 610_19, 2025/05

https://doi.org/10.3390/met15060610

Lattice parameters of product and matrix phases in steels have been measured using in situ X-ray and neutron diffraction during forward and reverse transformations. These parameters are influenced by temperature, transformation-induced internal stresses, alloying element partitioning, crystal defects, and magnetic strains. Disentangling these contributions is essential for understanding lattice behavior. This review explores internal strain (stress) associated with ferrite, pearlite, bainite, martensite, and reverse austenite transformations, emphasizing the distinction between diffusional and displacive mechanisms. It also examines how plastic deformation of austenite affects subsequent bainite or martensite formation. The roles of dislocations and vacancies are identified as critical areas for further research.

Role of solute hydrogen on mechanical property enhancement in Fe-24Cr-19Ni austenitic steel; An neutron diffraction study

伊東 達矢; 小川 祐平*; Gong, W.; Mao, W.*; 川崎 卓郎; 岡田 和歩*; 柴田 曉伸*; Harjo, S.

Acta Materialia, 287, p.120767_1 - 120767_16, 2025/04

https://doi.org/10.1016/j.actamat.2025.120767

Incorporating solute hydrogen into Fe-Cr-Ni-based austenitic stainless steels enhances both strength and ductility, providing a promising solution to hydrogen embrittlement by causing solid-solution strengthening and assisting deformation twinning. However, its impacts on the relevant lattice defects evolution (, dislocations, stacking faults, and twins) during deformation remains unclear. This study compared the tensile deformation behavior in an Fe-24Cr-19Ni (mass%) austenitic steel with 7600 atom ppm hydrogen-charged (H-charged) and without hydrogen-charged (non-charged) using neutron diffraction. Hydrogen effects on the lattice expansion, solid-solution strengthening, stacking fault probability, stacking fault energy, dislocation density, and strain/stress for twin evolution were quantitatively evaluated to link them with the macroscale mechanical properties. The H-charged sample showed improvements in yield stress, flow stress, and uniform elongation, consistent with earlier findings. However, solute hydrogen exhibited minimal influences on the evolution of dislocation and stacking fault. This fact contradicts the previous reports on hydrogen-enhanced dislocation and stacking fault evolutions, the latter of which can be responsible for the enhancement of twinning. The strain for twin evolution was smaller in the H-charged sample compared to the non-charged one. Nevertheless, when evaluated as the onset stress for twin evolution, there was minimal change between the two samples. These findings suggest that the increase in flow stress due to the solid-solution strengthening by hydrogen is a root cause of accelerated deformation twinning at a smaller strain, leading to an enhanced work-hardening rate and improved uniform elongation.

In situ neutron diffraction study of strain evolution and load partitioning during elevated temperature tensile test in HIP-Treated electron beam powder bed fusion manufactured Ti-6Al-4V

Pandian, K.*; Neikter, M.*; Ekh, M.*; Harjo, S.; 川崎 卓郎; Woracek, R.*; Hansson, T.*; Pederson, R.*

JOM, 77(4), p.1803 - 1815, 2025/04

https://doi.org/10.1007/s11837-025-07128-1

To produce dense Ti-6Al-4V components, electron beam powder bed fusion is typically followed by post-heat treatment like hot isostatic pressing (HIP). Standard HIP at 920C/100 MPa for 2 h coarsens the microstructure and reduces yield strength, while low-temp HIP at 800C/200 MPa for 2 h limits coarsening and retains strength comparable to as-built material. A coarser microstructure negatively affects tensile properties. Tensile tests at various temperatures suggest that thermally activated slip systems may influence elongation, requiring further study. In situ neutron time-of-flight diffraction during tensile loading enables analysis of strain evolution and slip plane activity. A two-phase elastic-plastic self-consistent model was used to compare with experiments. Results show basal slip {0002} activated at 20C, pyramidal slip {10-11} at 350C, and phase carrying higher stress than in the plastic regime.

Robustness of ferromagnetism in van der Waals magnet FeGeTe to hydrostatic pressure

Wang, Y.*; Zeng, X.-T.*; Li, B.*; Su, C.*; 服部 高典; Sheng, X.-L.*; Jin, W.*

Chinese Physics B, 34(4), p.046203_1 - 046203_6, 2025/03

https://doi.org/10.1088/1674-1056/adb26f

二次元ファンデルワールス強磁性体FeGeTe(FGT)は、その高いキュリー温度、容易な調整性、空気中での優れた構造安定性から、スピントロニクスデバイスへの応用に大きな可能性を秘めている。理論的研究により、外部パラメータとしての圧力が強磁性特性に大きく影響することが示されている。本研究では、5GPaまでの高圧中性子粉末回折(NPD)実験を行い、FGTの静水圧による構造及び磁気特性の変化を調べた。NPDデータは、静水圧による見かけ上の抑制にもかかわらず、FGTにおける強磁性の頑健性を明らかにした。圧力が0から5GPaまで増加すると、キュリー温度は225(5)Kから175(5)Kまで単調減少し、Feの秩序モーメントが劇的に抑制されることがわかった。圧力による構造相転移は5GPaまで観測されなかったが、結合長と結合角の変化を定量的に解析した結果、交換相互作用が大きく変化していることがわかった。

Solid-state Alder-ene reaction of 1-hexene under high pressure

Xu, J.*; Lang, P.*; Liang, S.*; Zhang, J.*; Fei, Y.*; Wang, Y.*; Gao, D.*; 服部 高典; 阿部 淳*; Dong, X.*; et al.

Journal of Physical Chemistry Letters (Internet), p.2445 - 2451, 2025/00

https://doi.org/10.1021/acs.jpclett.4c03696

アルダー-エン反応は、アルケンとアリル水素との化学反応であり、C-C結合を構築する効率的な方法である。従来、この反応には触媒、高温、あるいは光触媒が必要であった。本研究では、触媒を用いずに室温下で加圧することで成功した1-ヘキセンのアルダー-エン反応を報告する。1-ヘキセンは4.3GPaで結晶化し、18GPaで重合してオレフィンを形成する。ガスクロマトグラフィー-質量分析法により、1-ヘキセンが高圧下でのアルダー-エン反応により二量体を生成することを発見した。その場中性子回折から、この反応過程はトポケミカル則に従わないことがわかった。理論計算により、1つのC-H 結合と2つのアルケン結合を含む6員環遷移状態が示され、そのエネルギーは20GPaまで圧縮すると明らかに減少した。本研究は、触媒を用いずに室温でアルダー-エン反応を実現する新規かつ有望な方法を提供し、この重要な反応の応用を拡大するものである。

令和3・4年度JRR-3中性子ビーム利用における独自利用研究・技術開発報告

物質科学研究センター

JAEA-Review 2024-037, 141 Pages, 2024/11

JAEA-Review-2024-037.pdf:13.08MB

JRR-3(Japan Research Reactor No.3)には、日本原子力研究開発機構(原子力機構)が所管する15台の中性子ビーム利用実験装置が設置されており、装置高度化を含めた原子力機構の独自利用を行うとともに施設供用装置として外部利用者に供し、様々な研究成果を創出している。本報告書は、運転再開後の令和3年度、令和4年度の独自利用研究および中性子ビーム利用実験装置の高度化などの技術開発の進捗状況を取りまとめたものである。

Deformation behavior of ultrafine-grained TRIP steel observed by neutron diffraction

Harjo, S.; Mao, W.*; Gong, W.; 川崎 卓郎

Proceedings of the 7th International Symposium on Steel Science (ISSS 2024), p.205 - 208, 2024/11

https://doi.org/10.2355/isijisss.2024.0_205

This study aimed to elucidate the effect of grain size on the deformation behavior of TRIP steel. We prepared metastable austenitic Fe-24Ni-0.3C steel samples with average grain sizes of 35 m (coarse grain: CG) and 0.5 m (ultrafine-grain: UFG) for in situ neutron diffraction studies during tensile deformation at room temperature. Our observations revealed increases in dislocation density in both samples prior to DIMT, indicating that plastic deformation precedes DIMT regardless of grain size. In the UFG sample, a significant rise in dislocation density occurred just around the yielding point with minimal increases in macroscopic plastic strain. Additionally, the dislocations exhibited strong dipole arrangements.

Pearlite growth kinetics in Fe-C-Mn eutectoid steels; Quantitative evaluation of energy dissipation at pearlite growth front via experimental approaches

Zhang, Y.-J.*; 梅田 岳昌*; 諸岡 聡; Harjo, S.; 宮本 吾郎*; 古原 忠*

Metallurgical and Materials Transactions A, 55(10), p.3921 - 3936, 2024/10

https://doi.org/10.1007/s11661-024-07518-1

In this study, a series of eutectoid steels with Mn addition up to 2 mass% were isothermally transformed at various temperatures from 873 K to 973 K to clarify the pearlite growth kinetics and the underlying thermodynamics at its growth front. The microscopic observation indicates the acceleration in pearlite growth rate and refinement in lamellar spacing by decreasing the transformation temperature or the amount of Mn addition. After analyzing the solute distribution at pearlite growth front via three-dimensional atom probe, no macroscopic Mn partitioning across pearlite/austenite interface is detected, whereas Mn segregation is only observed at ferrite/austenite interface. Furthermore, in-situ neutron diffraction measurements performed at elevated temperatures reveals that the magnitude of elastic strain generated during pearlite transformation is very small.