Quantitative analysis of microstructure evolution, stress partitioning and thermodynamics in the dynamic transformation of Fe-14Ni alloy

Li, L.*; 宮本 吾郎*; Zhang, Y.*; Li, M.*; 諸岡 聡; 及川 勝成*; 友田 陽*; 古原 忠*

Journal of Materials Science & Technology, 184, p.221 - 234, 2024/06

https://doi.org/10.1016/j.jmst.2023.10.037

Dynamic transformation (DT) of austenite () to ferrite () in the hot deformation of various carbon steels was widely investigated. However, the nature of DT remains unclear due to the lack of quantitative analysis of stress partitioning between two phases and the uncertainty of local distribution of substitutional elements at the interface in multi-component carbon steels used in the previous studies. Therefore, in the present study, a binary Fe-Ni alloy with + duplex microstructure in equilibrium was prepared and isothermally compressed in + two-phase region to achieve quantitative analysis of microstructure evolution, stress partitioning and thermodynamics during DT. to DT during isothermal compression and to reverse transformation on isothermal annealing under unloaded condition after deformation were accompanied by Ni partitioning. The lattice strains during thermomechanical processing were obtained via in-situ neutron diffraction measurement, based on which the stress partitioning behavior between and was discussed by using the generalized Hooke's law. A thermodynamic framework for the isothermal deformation in solids was established based on the basic laws of thermodynamics, and it was shown that the total Helmholtz free energy change in the deformable material during the isothermal process should be smaller than the work done to the deformable material. Under the present thermodynamic framework, the microstructure evolution in the isothermal compression of Fe-14Ni alloy was well explained by considering the changes in chemical free energy, plastic and elastic energies and the work done to the material. In addition, the stabilization of the soft phase in Fe-14Ni alloy by deformation was rationalized since the to transformation decreased the total Helmholtz free energy by decreasing the elastic and dislocation energies.

Fe-5Mn-0.1C中Mn鋼におけるリューダース変形中の微視組織および塑性の発達

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

https://doi.org/10.2355/tetsutohagane.TETSU-2023-038

The 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.

Stress evaluation method by neutron diffraction for HCP-structured magnesium alloy

Harjo, S.; Gong, W.; 川崎 卓郎

Quantum Beam Science (Internet), 7(4), p.32_1 - 32_13, 2023/12

https://doi.org/10.3390/qubs7040032

Tensile deformation in situ neutron diffraction of an extruded AZ31 alloy was performed to validate conventional procedures and to develop new procedures for stress evaluation from lattice strains by diffraction measurements of HCP-structured magnesium alloys. Increases in the lattice strains with respect to the applied true stress after yielding largely vary among [] grains. The newly proposed procedure of stress evaluation from the lattice strains shows very high accuracy and reliability by weighting the volume fraction of [] grains and evaluating them in many [] orientations in addition to multiplication by the diffraction elastic constant. When multiple peaks cannot be obtained simultaneously, we recommend to use the 12.1 peak for stress evaluation.

中性子回折によるハイエントロピー合金の変形挙動のその場観察

Harjo, S.

日本結晶学会誌, 65(3), p.178 - 182, 2023/08

https://doi.org/10.5940/jcrsj.65.178

Observations of deformation behavior of high entropy alloys using neutron diffraction measurements during deformation at various temperatures are reviewed. Neutrons are used to investigate stresses and crystallographic microstructures inside engineering materials, taking advantage of their large penetrating power and the ability to see the arrangement of atoms by diffraction methods. The important structural details of high entropy alloys such as internal stresses, phase conditions, dislocations, texture etc. are discussed in relation to the deformation conditions. Some highlights are introduced: (a) Cooperative deformation in CrMnFeCoNi alloy at ultralow temperatures, (b) Stacking fault energies in CrFeCoNi and CrCoNi alloys, and (c) Load redistribution in eutectic high entropy alloy AlCoCrFeNi during high temperature deformation.

Accuracy of measuring rebar strain in concrete using a diffractometer for residual stress analysis

安江 歩夢*; 川上 真由*; 小林 謙祐*; Kim, J.; 宮津 裕次*; 西尾 悠平*; 向井 智久*; 諸岡 聡; 兼松 学*

Quantum Beam Science (Internet), 7(2), p.15_1 - 15_14, 2023/05

https://doi.org/10.3390/qubs7020015

Neutron diffraction is a noncontact method that can measure the rebar strain inside concrete. In this method, rebar strain and stress are calculated using the diffraction profile of neutrons irradiated during a specific time period. In general, measurement accuracy improves with the length of the measurement time. However, in previous studies, the measurement time was determined empirically, which makes the accuracy and reliability of the measurement results unclear. In this study, the relationship between the measurement time and the measurement standard deviation was examined for reinforced concrete specimens under different conditions. The aim was to clarify the accuracy of the measurement of rebar stress using the neutron diffraction method. It was found that if the optical setup of the neutron diffractometer and the conditions of the specimen are the same, there is a unique relationship between the diffraction intensity and the rebar stress standard deviation. Furthermore, using this unique relationship, this paper proposes a method for determining the measurement time from the allowable accuracy of the rebar stress, which ensures the accuracy of the neutron diffraction method.

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.

Evidence supporting reversible martensitic transformation under cyclic loading on Fe-Mn-Si-Al alloys using neutron diffraction

澤口 孝宏*; 友田 陽*; 吉中 奎貴*; Harjo, S.

Acta Materialia, 242, p.118494_1 - 118494_14, 2023/01

https://doi.org/10.1016/j.actamat.2022.118494

Fe-Mn-Si-based alloys, show superior resistance to plastic fatigue compared to the conventional steels, which is ascribed to the reversible back-and-forth movement of Shockley partial dislocations associated with a reversible martensitic transformation between the face-centered cubic -austenite and hexagonal close-packed -martensite. The purpose of this study was to gather evidence of the reversible martensitic transformation using in situ neutron diffraction under cyclic loading. Three Fe-30Mn-Si-Al alloys with different Gibbs free energy differences at 298 K were studied to unravel the effect of phase stability on the degree of reversibility.

Rearrangement of hydrogen bonds in dehydrated raffinose tetrahydrate; A Time-of-flight neutron diffraction study

川崎 卓郎; 高橋 美和子*; 鬼柳 亮嗣; 大原 高志

Acta Crystallographica Section C; Structural Chemistry (Internet), 78(12), p.743 - 748, 2022/12

https://doi.org/10.1107/S2053229622010828

Structural changes of the raffinose crystal on dehydration from the pentahydrate to the tetrahydrate were investigated by single-crystal time-of-flight neutron diffraction. It was revealed that during the dehydration, rearrangement occurs in the hydrogen bonds related to the lost water molecule, while the symmetry of the crystal structure is retained. The hydrogen-bonding status of raffinose pentahydrate and tetrahydrate were discussed comprehensively according to Jeffrey's hydrogen-bonding classification. It was shown that water molecules are hydrogen bonded to the surrounding molecules by O-H...O hydrogen bonds and C-H...O hydrogen bonds, and the number of these two types of hydrogen bonds determines the water molecules that are removed by dehydration. The lattice constant c showed a significant decrease on dehydration and further dehydration leads to loss of crystallinity of the raffinose crystals.

In situ neutron diffraction analysis of microstructural evolution-dependent stress response in austenitic stainless steel under cyclic plastic deformation

熊谷 正芳*; 黒田 雅利*; 松野 崇*; Harjo, S.; 秋田 貢一*

Materials & Design, 221, p.110965_1 - 110965_8, 2022/09

https://doi.org/10.1016/j.matdes.2022.110965

Microstructural evolution in austenitic stainless steels during cyclic plastic deformation has been studied via diffraction line profile analysis; however, their microstructure-dependent mechanical response upon stress partitioning in the matrix (austenite) and deformation-induced martensite has remained largely unexplored. In this study, the stress response analysis of austenitic stainless steel was performed using neutron diffraction, to evaluate the phase stresses in the austenite and martensite, and the relation with dislocation data was discussed.

Anisotropic thermal lattice expansion and crystallographic structure of strontium aluminide within Al-10Sr alloy as measured by in-situ neutron diffraction

Liss, K.-D.*; Harjo, S.; 川崎 卓郎; 相澤 一也; 徐 平光

Journal of Alloys and Compounds, 869, p.159232_1 - 159232_9, 2021/07

AA2020-0822.pdf:1.94MB

https://doi.org/10.1016/j.jallcom.2021.159232

The aluminium strontium master alloy Al-10Sr has been investigated by in-situ neutron diffraction upon a heating-cooling cycle, revealing composition, crystallographic structure, lattice evolution and linear thermal expansion coefficients. Expansion of the Al matrix between (23.5 ... 26.7)10 K depends on temperature and fits well to the literature values, extrapolating to higher temperature at 800 K. Thermal expansion is highly anisotropic for tetragonal AlSr by a factor of 1.86 with values of 20.8 and 11.110 K in and -axis. The even large discrepancy to the Al matrix is prone to residual intergranular phase stresses, explaining the brittleness of such composite material. Upon first heating, recovery of the initially plastically deformed materials is observed until 600 K and 700 K, for AlSr and Al. Rietveld analysis refines the 4 Wyckoff positions of the 4/ crystal structure to = 0.39 revealing that local tetrahedrons are regular while local hexagons are stretched, in contrast to the literature. Its lattice parameters report to = 4.44240(48) , = 11.0836(15) at 300 K. Furthermore, the manuscript demonstrates full technical analysis of the neutron data. Findings feed into data bases and an outlook for improving mechanical properties of AlSr composites is given.