Probing deformation behavior of a refractory high-entropy alloy using neutron diffraction

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

https://doi.org/10.1016/j.jallcom.2023.172635

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.

Direct observation of concentration fluctuations in Au-Si eutectic liquid by small-angle neutron scattering

坂口 佳史*; 高田 慎一; 川北 至信; 藤村 由希; 近藤 啓悦

Journal of Physics; Condensed Matter, 35(41), p.415403_1 - 415403_11, 2023/10

https://doi.org/10.1088/1361-648X/ace577

It is well-known that eutectic gold-silicon (Au-Si) alloys exhibit anomalous melting point depression, which is more than 1000 C from the melting point of elemental Si (1414 C). The melting point depression in eutectic alloys is generally explained in terms of a decrease of the free energy by mixing. However, it is difficult to understand the anomalous melting point depression only from the stability of the homogeneous mixing. Some researchers suggest that there are concentration fluctuations in the liquids, where the atoms are inhomogeneously mixed. In this paper, we measure the small-angle neutron scattering (SANS) of AuSi (eutectic composition) and AuSi (off-eutectic composition) at temperatures from room temperature to 900 C in both solid and liquid states to observe such concentration fluctuations directly.

High-density nanoprecipitates and phase reversion via maraging enable ultrastrong yet strain-hardenable medium-entropy alloy

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

https://doi.org/10.1016/j.actamat.2023.118810

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 FeCoNiMo 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.

Evolution of austenite lattice parameter during isothermal transformation in a 0.4 C low alloyed steel

Wang, Y.*; 友田 陽*; 大村 孝仁*; Gong, W.; Harjo, S.

Materialia, 27, p.101685_1 - 101685_9, 2023/03

https://doi.org/10.1016/j.mtla.2023.101685

The evolution of internal stress during displacive transformation is a topic of continuous debate. Neutron diffraction was used to study the isothermal bainite transformation in a 0.4 C low alloyed steel from 773 to 623 K to provide a clearer basis for discussion regarding the change in the austenite lattice parameter. According to diffraction profile analysis, fresh bainite possesses a body-centered tetragonal structure, and its c/a ratio decreases rapidly over time. The austenite lattice parameter increases or decreases depending on whether the transformation temperature is above or below the nose of the Time-Temperature-Transformation (TTT) curve. This isothermal transformation behavior can be divided into two categories: above and below the nose of TTT curve, which correspond to the upper and lower bainites, respectively. The internal stresses caused by the transformation strains are relaxed by dislocation motion and vacancy formation. The yielded dislocations and vacancies not only affect the broadening of both austenite and bainitic ferrite diffraction peaks but also the lattice parameter.

Effect of extrusion ratio in hot-extrusion on kink deformation during compressive deformation in an Mg/LPSO dual-phase magnesium alloy monitored by neutron diffraction

Harjo, S.; Gong, W.; 相澤 一也; 川崎 卓郎; 山崎 倫昭*; 眞山 剛*; 河村 能人*

Materials Transactions, 64(4), p.766 - 773, 2023/02

https://doi.org/10.2320/matertrans.MT-MD2022004

To elucidate the effect of extrusion ratio in hot-extrusion on the deformation behavior during compression of MgZnY alloy containing about 25-vol% long-period stacking ordered phase (LPSO) in the HCP structured matrix (Mg), neutron diffraction measurements were performed under compressive loading using four types of samples: as-cast and after hot extrusion at 623 K with extrusion ratios of 5.0, 7.5 and 12.5. The macroscopic yielding was observed to appear by the occurrence of basal slip of Mg in the as-cast sample and at the onset of twinning in the hot extruded samples. The applied stress to initiate slip, twinning, and kinking increased by hot extrusion and then decreased with increasing extrusion ratio. LPSO shared higher stress than Mg and the ratio to the strength increased as the extrusion ratio increased.

Unexpected dynamic transformation from phase to phase in zirconium alloy revealed by in-situ neutron diffraction during high temperature deformation

Guo, 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

https://doi.org/10.1016/j.actamat.2022.118427

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.

Structure, stability, and actinide leaching of simulated nuclear fuel debris synthesized from UO, Zr, and stainless-steel

桐島 陽*; 秋山 大輔*; 熊谷 友多; 日下 良二; 中田 正美; 渡邉 雅之; 佐々木 隆之*; 佐藤 修彰*

Journal of Nuclear Materials, 567, p.153842_1 - 153842_15, 2022/08

https://doi.org/10.1016/j.jnucmat.2022.153842

福島第一原子力発電所事故では、UOやZr,ステンレス鋼(SUS)の高温反応により燃料デブリが形成されたとみられる。この燃料デブリの化学構造や安定性を理解するため、UO-Zr-SUS系模擬デブリ試料の合成と物性評価を行い、より単純な組成の試料と比較した。模擬デブリ試料の合成では、不活性雰囲気(Ar)もしくは酸化雰囲気(Ar + 2% O)において1600Cで1時間から12時間の加熱処理を行った。NpおよびAmをトレーサーとして添加し、浸漬試験ではUに加えてこれらの核種の溶出を測定した。試料の物性評価は、XRD, SEM-EDX,ラマン分光法およびメスバウアー分光法により行った。その結果、模擬デブリの主なU含有相は、加熱処理時の雰囲気に依らず、Zr(IV)およびFe(II)が固溶したUO相であることが分かった。模擬デブリ試料の純水もしくは海水への浸漬試験では、1年以上の浸漬の後も主な固相の結晶構造には変化が観測されず、化学的に安定であることが示された。さらに、U, Np, Amの溶出率はいずれも0.08%以下と、溶出は極めて限定的であることが明らかとなった。

Irradiation growth behavior and effect of hydrogen absorption of Zr-based cladding alloys for PWR

垣内 一雄; 天谷 政樹; 宇田川 豊

Annals of Nuclear Energy, 171, p.109004_1 - 109004_9, 2022/06

https://doi.org/10.1016/j.anucene.2022.109004

In order to understand the dimensional stability of the fuel rod during long-term use in commercial LWRs, an irradiation growth testing in the Halden reactor of Norway was conducted on various fuel cladding materials including the improved Zr alloy. In this paper, the effect of hydrogen, which was absorbed in the cladding tube due to corrosion, on the irradiation growth behavior was evaluated. Comparison between the specimens with or without pre-charged hydrogen revealed that the effect of hydrogen absorption, accelerating irradiation growth, became significant when the hydrogen content exceeded the hydrogen solubility limit in the corresponding irradiation temperature. Analysis based on this understanding derived growth acceleration effect (0.060.01)%/100 ppm, whose denominator is defined as the amount of absorbed hydrogen involved in hydride precipitation under irradiation as a relevant parameter.

健全性崩壊をもたらす微生物による視認不可腐食の分子生物・電気化学的診断及び抑制技術の開発(委託研究); 令和2年度英知を結集した原子力科学技術・人材育成推進事業

廃炉環境国際共同研究センター; 物質・材料研究機構*

JAEA-Review 2021-059, 71 Pages, 2022/02

JAEA-Review-2021-059.pdf:4.25MB

日本原子力研究開発機構(JAEA)廃炉環境国際共同研究センター(CLADS)では、令和2年度英知を結集した原子力科学技術・人材育成推進事業(以下、「本事業」という)を実施している。本事業は、東京電力ホールディングス株式会社福島第一原子力発電所(以下、「1F」という)の廃炉等をはじめとした原子力分野の課題解決に貢献するため、国内外の英知を結集し、様々な分野の知見や経験を、従前の機関や分野の壁を越えて緊密に融合・連携させた基礎的・基盤的研究及び人材育成を推進することを目的としている。平成30年度の新規採択課題から実施主体を文部科学省からJAEAに移行することで、JAEAとアカデミアとの連携を強化し、廃炉に資する中長期的な研究開発・人材育成をより安定的かつ継続的に実施する体制を構築した。本研究は、研究課題のうち、令和2年度に採択された「健全性崩壊をもたらす微生物による視認不可腐食の分子生物・電気化学的診断及び抑制技術の開発」の令和2年度の研究成果について取りまとめたものである。本研究は、微生物が関与して誘起・加速する金属材料の腐食(微生物鉄腐食)に関して、加速検査試験片、オンサイト遺伝子検査などの革新的な診断技術を開発、1Fで想定される微生物腐食の発生・進行条件の洗い出しを行い、水質や環境コントロールによって微生物腐食を防ぐ方法を提案することを目的とした。さらに、材料・微生物・電気化学を基盤とした研究拠点を発展的に形成し、現場技術者が使用可能な技術の開発、さらには高い学際性を持つリーダー人材の育成を目指す。本年度の実験から特に1Fと関連する環境サンプルから微生物による腐食反応が確認できており、この腐食反応を抑制する条件の特定が今後進むことが期待できる。その他の計画に関しても、次年度以降の重要な実験を始めるための予備的な知見が得られた。

Work hardening behavior of dual phase copper-iron alloy at low temperature

山下 享介*; 古賀 紀光*; 川崎 卓郎; 諸岡 聡; 友野 翔平*; 梅澤 修*; Harjo, S.

Materials Science & Engineering A, 819, p.141509_1 - 141509_10, 2021/07

https://doi.org/10.1016/j.msea.2021.141509

In-situ neutron diffraction measurements were performed on a cold-rolled copper-iron (Cu-Fe) alloy during tensile tests at 293 K and 150 K. The roles of Cu and Fe on the deformation behavior of alloys were discussed and clarified. The strength and work-hardening rate of the alloy increased with decreasing test temperature. Furthermore, the phase stress of Fe increased considerably with decreasing test temperature; however, the response of this stress to the applied true stress exhibited no dependence on the temperature. The phase stresses of Cu changed only slightly with decreasing test temperature. However, the Cu phase stress response to the applied true stress increased with decreasing test temperature, indicating an increase in the work-hardening rate. The strengthening of Fe and the increase in the work-hardening of Cu contributed to an increase in the strength and work-hardening rate of the Cu-Fe alloy at low temperatures.