Microstructural evolution and mechanical instability of Mar-M509 superalloy fabricated by laser powder bed fusion under short-term thermal exposure

Cao, T.*; Wei, D.*; Gong, W.; 川崎 卓郎; Harjo, S.; 他10名*

Materials Science and Engineering A, 940, p.148534_1 - 148534_16, 2025/09

https://doi.org/10.1016/j.msea.2025.148534

The thermal stability of microstructure and mechanical performance is crucial for the industrial application of laser powder bed fusion (LPBF) superalloy components in gas turbines and jet engines. This work investigated the microstructural evolution and strengthening mechanism of LPBF Mar-M509 cobalt-based superalloy before and after thermal exposure at 1200 C using multi-scale microstructural characterization and in situ neutron diffraction tensile testing. The as-built Mar-M509 superalloy exhibited a heterogeneous microstructural features with coarse columnar and fine equiaxed grains, both containing dendritic and cellular substructures enriched with nanoscale carbides and high-density dislocations. The ultra high strength of the as-built sample was primarily attributed to dislocation-precipitation synergistic strengthening. After thermal exposure at 1200 C for 4 h, the dendritic and cellular substructures disappeared and the dislocation density decreased significantly. This study reveals the microstructural evolution and instability of LPBF Mar-M509 superalloy under high-temperature exposure and the impacts on mechanical properties, which provides critical support for the development of cobalt-based superalloys in high-temperature application fields.

A Lightweight shape-memory alloy with superior temperature-fluctuation resistance

Song, Y.*; Xu, S.*; 佐藤 駿介*; Lee, I.*; Xu, X.*; 大森 俊洋*; 長迫 実*; 川崎 卓郎; 鬼柳 亮嗣; Harjo, S.; et al.

Nature, 638, p.965 - 971, 2025/02

https://doi.org/10.1038/s41586-024-08583-7

In advanced applications like aerospace and space exploration, materials must balance lightness, functionality, and extreme thermal fluctuation resistance. Shape-memory alloys show promise with strength, toughness, and substantial strain recovery due to superelasticity, but maintaining low mass and effective operation at cryogenic temperatures is challenging. We hereby introduce a novel shape-memory alloy that adheres to these stringent criteria. Predominantly composed of Ti and Al with a chemical composition of TiAlCr, this alloy 25 is characterized by a low density (4.3610 kg/m) and a high specific strength (18510 Pam/kg) at room temperature, while exhibiting excellent superelasticity. The superelasticity, owing to a reversible stress-induced phase transformation from an ordered body-centered cubic parent phase to an ordered orthorhombic martensite, allows for a recoverable strain exceeding 7%. Remarkably, this functionality persists across a broad range of temperatures, from deep cryogenic 4.2 K to above room temperature, arising from an unconventional temperature dependence of transformation stresses. Below a certain threshold during cooling, the critical transformation stress inversely correlates with temperature. We interpret this behavior from the perspective of a temperature-dependent anomalous lattice instability of the parent phase. This alloy holds potential in everyday appliances requiring flexible strain accommodations, as well as components designed for extreme environmental conditions such as deep space and liquefied gases.

Stress contribution of B2 phase in AlCoCrFeNi eutectic high entropy alloy

Yun, 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

https://doi.org/10.1016/j.jallcom.2022.165673

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.

In-situ neutron diffraction study of lattice deformation behaviour of commercially pure titanium at cryogenic temperature

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

https://doi.org/10.1038/s41598-022-07640-3

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.

Tensile response of as-cast CoCrFeNi and CoCrFeMnNi high-entropy alloys

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

https://doi.org/10.3390/cryst12020157

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.

Enhancement of fatigue resistance by overload-induced deformation twinning in a CoCrFeMnNi high-entropy alloy

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

https://doi.org/10.1016/j.actamat.2020.10.016

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.

Element effects of Mn and Ge on the tuning of mechanical properties of high-entropy alloys

Lam, T.-N.*; Tsai, C.-W.*; Chen, B.-K.*; Lai, B.-H.*; Liu, H.-C*; 川崎 卓郎; Harjo, S.; Lin, B.-H.*; Huang, E.-W.*

Metallurgical and Materials Transactions A, 51(10), p.5023 - 5028, 2020/10

https://doi.org/10.1007/s11661-020-05932-9

Substitution of Ge for Mn increases the elastic moduli of different orientations of the CoCrFeMnNi-based high-entropy alloy. Our findings indicate that tuning minor element compositions may result in improved strength-ductility combination. The underlying deformation mechanisms of CoCrFeNiGe were examined by neutron diffraction and analysis of the associated diffraction profiles during tensile deformation. The strain-hardening response of CoCrFeNiGe exhibited a dominant mechanism of mechanical twinning at moderate and large strains at room temperature. The evolution of the bulk work hardening rate was consistent with the convolutional multiple whole profile fitting results, which exhibited a continuous increase in twin formation probability.

Work hardening, dislocation structure, and load partitioning in lath-martensite determined by neutron diffraction line profile analysis

Harjo, S.; 川崎 卓郎; 友田 陽*; Gong, W.*; 相澤 一也; Tichy, G.*; Shi, Z.*; Ungr, T.*

Metallurgical and Materials Transactions A, 48(9), p.4080 - 4092, 2017/09

AA2017-0020.pdf:3.33MB

https://doi.org/10.1007/s11661-017-4172-0

neutron diffraction during tensile deformation of lath martensite steel containing 0.22 mass% of carbon, is performed using TAKUMI of J-PARC. The diffraction peaks at plastically deformed states exhibit asymmetries as the reflection of redistributions of the stress and dislocation densities/arrangements in lath-packets where the dislocation glides are favorable (soft packet) and unfavorable (hard packet). The dislocation density is as high as 10 m at the as-quenched state, and then during tensile straining, the load and the dislocation density become different between the two lath-packets. The dislocation character and arrangement vary also in the hard packet, but hardly change in the soft packet. The hard packet plays an important role in the high work hardening in martensite, which could be understood by taking into account not only the increase of the dislocation density but also the change in dislocation arrangement.

Dislocation characteristics of martensitic steel studied by neutron diffraction experiment

川崎 卓郎; Harjo, S.; Gong, W.; 相澤 一也; 岩橋 孝明; Shi, Z.*; Li, J.*; 友田 陽*; Ungr, T.*

JPS Conference Proceedings (Internet), 8, p.031009_1 - 031009_5, 2015/09

https://doi.org/10.7566/JPSCP.8.031009

鉄鋼材料に代表される金属材料の力学的特性を理解するためには、弾性ひずみだけでなく、転位の密度や配列状態など微細構造を評価することが重要である。これらの情報はX線や中性子回折パターンに表れるBraggピークの形状を詳しく解析することで得ることができる。透過能の高い中性子を用いることでバルク状態の材料内部の微細構造に関する情報を得ることができるが、これまで中性子(特にパルス中性子)はあまり適用されてこなかった。我々はJ-PARC物質生命科学実験施設BL19に設置された工学材料回折装置 匠を用いてマルテンサイト鋼の引張り試験その場中性子回折測定を行い、CMWP法と呼ばれる解析法を用いてこの材料の微細構造を調べた。その結果、巨視的なひずみの増加に伴う転位密度の増加は比較的小さく、転位配列の顕著な規則化が観測された。

Trial fabrication of heavy section base metals and welded joints for ITER TF coil

石尾 光太郎*; 中嶋 秀夫; 布谷 嘉彦; 三浦 友史; 川崎 勉*; 辻 博史

Advances in Cryogenic Engineering Materials, 44, p.73 - 80, 1998/00

ITER・TFコイル構造材は、最大約400mmの厚さを持ち、さらに高強度、高靱性が要求される。それゆえ高強度、高靱性を有する極厚母材や溶接継手開発のR&Dが必要になる。我々は、TFコイルの構造材として、1200MPa以上の0.2%耐力と200MPa√m以上の破壊靱性値を持つ、JCS(JJ1、JK2及びJN1鋼)の開発に成功した。JCSの極厚材の製造性及び溶接性を証明するために、200mm厚以上の鍛造材及び、200mm厚板のTIG溶接の試作を行った。4KにおけるJCSの強度、靱性は、たとえ200mm厚溶接でも、NISTのラインより高い値が示された。溶接部は完全オーステナイトであるにもかかわらず、割れや有害なブローホールは観察されなかった。JJ1鋼では、500mm厚鍛造材の試作に成功し、十分に高強度、高靱性が得られ、500mm厚まで供給できることを証明した。