The BCC FCC hierarchical martensite transformation under dynamic impact in FeMnAlNiTi alloy

Li, C.*; Fang, W.*; Yu, H. Y.*; Peng, T.*; Yao, Z. T.*; Liu, W. G.*; Zhang, X.*; 徐 平光; Yin, F.*

Materials Science & Engineering A, 892, p.146096_1 - 146096_11, 2024/02

https://doi.org/10.1016/j.msea.2024.146096

The quasi-static superelastic responses and hierarchical martensite transformation from body-centered cubic (BCC) to face-centered cubic (FCC) under dynamic impact in FeMnAlNiTi alloys were investigated. Polycrystalline and oligocrystalline alloys were produced through solution heat treatment and cyclic heat treatment processes, respectively. The results show the volume fraction of residual martensite for oligocrystalline alloys is lower, which exhibits better superelastic responses compared with polycrystalline alloys. Dynamic impact tests indicate that, despite the weakening of the grain boundary strengthening effect, the ultimate strength of the oligocrystalline alloys closely matches that of the polycrystalline alloys under dynamic impact. The martensite transformation of the FeMnAlNiTi alloy is characterized as hierarchical under dynamic impact, and increasing strain rates and grain sizes can enhance the BCC FCC martensite transformation, resulting in higher martensite phase fractions for oligocrystalline alloys. The increase in ultimate strength is attributed to the dynamic Hall-Petch effect introduced by more martensite phase interfaces under dynamic impact.

Recrystallization of bulk nanostructured magnesium alloy AZ31 after severe plastic deformation; An in situ diffraction study

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, 23 Pages, 2024/00

https://doi.org/10.1007/s10853-023-09250-4

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.

Cryogenic impact fracture behavior of a high-Mn austenitic steel using electron backscatter diffraction and neutron Bragg-edge transmission imaging

Wang, Y. W.*; Wang, H. H.*; Su, Y. H.; 徐 平光; 篠原 武尚

Materials Science & Engineering A, 887, p.145768_1 - 145768_13, 2023/11

https://doi.org/10.1016/j.msea.2023.145768

A unique impact fracture behavior is found in a high-Mn austenitic steel (24Mn-4Cr-0.4C-0.3Cu) in this work. The steel exhibits concurrent twinning-induced plasticity (TWIP) effect and the transformation-induced plasticity (TRIP) effect. By analyzing the load-deflection curves recorded during Charpy impact testing, the resistance to crack initiation and propagation is quantified from the absorbed energy. The high-Mn steel demonstrates good resistance to crack initiation at 273 K and 77 K. However, as the temperature decreases from 273 K to 77 K, there is an accelerated transition from stable crack growth to unstable crack growth during impact, resulting in the deterioration of resistance to crack propagation. The plastic deformation of the impact-tested samples, especially in the region close to the crack-path profile was quantitatively analyzed using neutron Bragg-edge transmission (BET) imaging. The deformation zones, divided by using the width of the 200 Bragg edge, exhibit good agreement with the impact absorbed energy characteristics obtained from dynamic load-deflection curves. Moreover, the unstable growth transition point was roughly determined on the impact-tested sample. Then, the electron backscatter diffraction (EBSD) technique is employed to examine the deformation microstructure along the crack-path in the impact-tested samples. The results revealed the dual roles of TRIP effect in impact toughness of the high-Mn steel. On one hand, the TRIP effect plays a positive role in improving resistance to crack initiation and propagation. On the other hand, the excessive accumulation of brittle /'-martensite caused by the enhanced TRIP effect at 77 K leads to quasi-cleavage fracture, thereby playing a negative role. Finally, we discussed the prominent toughening mechanisms associated with the TWIP and TRIP effects, which greatly impact the impact fracture behavior.

Fatigue crack non-propagation behavior of a gradient steel structure from induction hardened railway axles

Zhang, H.*; Wu, S. C.*; Ao, N.*; Zhang, J. W.*; Li, H.*; Zhou, L.*; 徐 平光; Su, Y. H.

International Journal of Fatigue, 166, p.107296_1 - 107296_11, 2023/01

https://doi.org/10.1016/j.ijfatigue.2022.107296

Abnormal damages in railway axles can lead to a significant hazard to running safety and reliability. To this end, a surface treatment was selected to effectively inhibit fatigue crack initiation and growth. In this study, a single edge notch bending fatigue test campaign with artificial notches was conducted to elucidate the fatigue crack non-propagation behavior in railway S38C axles subjected to an induction hardening process. The fatigue cracking behavior in the gradient structure was revealed by optical microscopy, electron backscatter diffraction, and fractography. The microhardness distribution was measured using a Vickers tester. The obtained results show that the microhardness of the strengthening layer is nearly triple that of the matrix. Owing to the gradient microstructures and hardness, as well as compressive residual stress, the fatigue long crack propagates faster once it passes through the hardened zone (approximately 2.0 mm in the radial depth). Thereafter, local retarding (including deflection, branching, and blunting) of the long crack occurs because of the relatively coarse ferrite and pearlite in the transition region and matrix. Totally, this fatigue cracking resistance is reasonably believed to be due to the gradient microstructure and residual stress. These findings help to tailor a suitable detection strategy for maximum defects or cracks in railway axles.

Heat-induced structural changes in magnesium alloys AZ91 and AZ31 investigated by in situ synchrotron high-energy X-ray diffraction

Liu, X. J.*; 徐 平光; 城 鮎美*; Zhang, S. Y.*; 菖蒲 敬久; 行武 栄太郎*; 秋田 貢一*; Zolotoyabko, E.*; Liss, K.-D.*

Journal of Materials Science, 57(46), p.21446 - 21459, 2022/12

https://doi.org/10.1007/s10853-022-07917-y

In situ time/temperature-resolved synchrotron high-energy X-ray diffraction is applied to study heat-mediated structural changes and phase transformations in rolled sheets of AZ91 and AZ31 magnesium alloys. Azimuthal diffraction intensities along the Debye-Scherrer rings (AT-plots) are used to obtain information on grain recovery and recrystallization temperatures as well as temperature-assisted grain rotations. The azimuthally integrated diffraction intensities, plotted as functions of the scattering vector (QT-plots), provide vital data on the temperature-dependent lattice parameters of the Mg/Al matrix and intermetallic precipitates, as well as on the evolution of the precipitates' volume fraction. It was found that in AZ31, the main precipitates are of the AlMn type, which is rather stable in the investigated temperature range (up to 773 K). In contrast, in AZ91, the major intermetallic precipitates, AlMg, undergo complete dissolution above 600 K. It is caused by the enhanced diffusion of Al into the Mg/Al matrix, which according to the Al-Mg phase diagram, can adopt more Al at elevated temperatures. This diffusion is revealed by the proportional diminishing of the matrix lattice parameter (chemical strain), allowing us to quantify the Al content in the matrix. Fast temperature-dependent manipulation with intermetallic content in the Mg/Al alloy can, in principle, be used for controlling its mechanical properties.

Improvement of neutron diffraction at compact accelerator-driven neutron source RANS using peak profile deconvolution and delayed neutron reduction for stress measurements

岩本 ちひろ*; 高村 正人*; 上野 孝太*; 片岡 美波*; 栗原 諒*; 徐 平光; 大竹 淑恵*

ISIJ International, 62(5), p.1013 - 1022, 2022/05

https://doi.org/10.2355/isijinternational.ISIJINT-2021-420

Neutron diffraction is a powerful non-destructive method for evaluating the microscopic structure and internal stress of metal plates as a bulk average. Precise neutron diffraction measurements with a high intensity neutron beam have already been carried out at large-scale neutron facilities. However, it is not easy to provide users with enough experimental opportunities. We are working on upgrading the neutron diffractometer with techniques of time-of-flight to enable stress measurements at RIKEN accelerator-driven compact neutron source (RANS). To improve neutron diffraction resolution, delayed neutrons, which expand neutron beam pulse width, should be suppressed. However, it is difficult to separate the delayed neutrons experimentally. In this study, a new analysis method has been proposed to deconvolute the diffraction peak from the delayed neutron component. Moreover, a new collimator system, called decoupled collimator system, has been developed to reduce the number of delayed neutrons. The diffraction patterns from a powder sample of pure body-centered cubic iron were measured with the decoupled collimator and the diffraction peak of {211} reflection was analyzed by the new analysis method using a model function of a single exponential decay function convoluted with a Gaussian function. By this method, the decoupled collimator system has been confirmed to achieve a smaller measurement limit of lattice strain than a small-aperture polyethylene collimator system and a non-collimator system. The currently available was 6.710, this means that the internal stress up to 130 MPa can be well evaluated for steel materials with a Young's modulus of 200 GPa at RANS.

Multiple wavelengths texture measurement using angle dispersive neutron diffraction at WOMBAT

徐 平光; Liss, K.-D.*

Quantum Beam Science (Internet), 5(2), p.11_1 - 11_14, 2021/06

AA2020-0801.pdf:11.28MB

https://doi.org/10.3390/qubs5020011

In contrast to conventional angle dispersive neutron diffractometers with a single-tube detector or a small-size linear position-sensitive detector, the WOMBAT diffractometer at Australian Nuclear Science and Technology Organisation (ANSTO) is equipped with a large-area curved position-sensitive detector, spanning 120 for the scattering angle 2 and 15 for the azimuth , respectively. Here, WOMBAT was employed to establish a texture measurement environment for complex textured samples, through measuring neutron diffractograms at two selected wavelengths on a typical reference sample of martensite-austenite multilayered steel sheet. All neutron patterns were simultaneously Rietveld analyzed using the software, Materials Analysis Using Diffraction (MAUD). The shorter wavelength enabled to collect the martensite diffraction peaks 110, 200, 211, 220, 310, 222 as well as the austenite diffraction peaks 111, 200, 220, 311, 222, 331 diffraction peaks simultaneously by pre-setting the detector range to 2 = 30150. The longer wavelength enabled to separate the overlapping strong martensite peak 110 and austenite peak 111 more reliably. Moreover, the detector panel division along the vertical direction covers a good stereographic coverage in the azimuthal angle. Such combination of multiple wavelength neutron diffraction combined with simultaneous Rietveld texture analysis was confirmed much valuable to realize high precision measurements for complex textured samples at an orientation distribution function (ODF) graticule of 5, and in a much shorter beam time than the conventional angle dispersive method.

In-house texture measurement using a compact neutron source

徐 平光; 池田 義雅*; 箱山 智之*; 高村 正人*; 大竹 淑恵*; 鈴木 裕士

Journal of Applied Crystallography, 53(2), p.444 - 454, 2020/04

AA2019-0242.pdf:2.9MB

https://doi.org/10.1107/S1600576720002551

In order to improve the instrumental accessibility of neutron diffraction technique, the emerging compact neutron sources and in-house neutron diffractometers as a good complementary way have caused wide attention while their analysis precision seems problematic for the practical application. As a challenging project, the RIKEN accelerator-driven compact neutron source (RANS) was employed to establish the technical environment for texture measurement, and the recalculated pole figures and the orientation distribution function (ODF) of an interstitial-free (IF) steel sheet obtained from RANS were compared with the results from another two neutron diffractometers well-established for texture measurement. Moreover, the parameter "square integration of ODF difference" originally for evaluating the numerical error between the measured and simulated textures was generalized here to examine the reliability of RANS texture measurement. These quantitative comparisons revealed that the precise neutron diffraction texture measurement at RANS has been realized successfully and the following technical optimizations are much valuable, including the thickness selection of polyethylene moderator, the sample-to-detector distance, the BC shielding sheets for the reduced background noise, and the fine region division of the neutron detector panel. Moreover, the Rietveld texture analysis improves the texture reliability through avoiding the unfavorable influence of the uncertain diffraction intensity involved in the low counting, long wavelength incident neutrons at large scattering angles. Above technical results may accelerate the development of other easily accessible engineering materials evaluation techniques using compact neutron source, and also help to improve the data-collecting efficiency for various time-sliced scattering experiments at large neutron facilities.

Evaluation of residual stress relaxation in a rolled joint by neutron diffraction

林 眞琴*; Root, J. H.*; Rogge, R. B.*; 徐 平光

Quantum Beam Science (Internet), 2(4), p.21_1 - 21_16, 2018/12

AA2018-0259.pdf:2.23MB

https://doi.org/10.3390/qubs2040021

The rolled joint of pressure tube, consisting of three axial symmetric parts, modified SUS403 stainless steel, Zr-2.5Nb pressure tube and Inconel-718, has been examined by neutron diffraction for residual stresses. It was heat treated at 350C for 30, 130 and 635 hours to simulate the thermal aging of the rolled joint over the lifetime of the advanced thermal reactor at 288C for 1, 5 and 30 years. The crystal lattice strains at various locations in the rolled joint before and after the aging treatments were measured by neutron diffraction and the residual stress distribution in the rolled joint was evaluated by using the Kroner elastic model and the generalized Hooke's law. In the crimp region of the rolled joint, it was found that the aging treatment had weak effect on the residual stresses in the Inconel and the SUS403. In the non-aged Zr-2.5Nb, the highest residual stresses were found near its interface with the SUS430. In the Zr-2.5Nb in the crimp region near its interface with the SUS430, the average compressive axial stress was -440 MPa, having no evident change during the long-time aging. In the Zr-2.5Nb outside closest to the crimp region, the tensile axial and hoop stresses were relieved during the 30 hours aging. The hoop stresses in the crimp region evolved from an average tensile stress of 80 MPa to an average compressive stress of 230 MPa after the 635 hours aging, suggesting that the rolled joint had a good long-term sealing ability against the leakage of high temperature water.

種々な方法によるMn-Si-C鋼の残留オーステナイト体積率測定の比較

友田 陽*; 関戸 信彰*; 徐 平光; 川崎 卓郎; Harjo, S.; 田中 雅彦*; 篠原 武尚; Su, Y. H.; 谷山 明*

鉄と鋼, 103(10), p.570 - 578, 2017/10

https://doi.org/10.2355/tetsutohagane.TETSU-2017-045

Various methods were employed to measure the austenite volume fraction in a 1.5Mn-1.5Si-0.2C steel. It has been confirmed that the volume fractions determined by transmission electron microscopy, scanning electron microscopy/electron back scatter diffraction, X-ray diffraction and neutron diffraction exhibit a general trend to become larger in this order, although the values obtained by X-ray and neutron diffraction are similar in the present steel because austenite is relatively stable. The austenite volume fractions determined by diffraction methods have been found to be affected by the measuring specimen direction, i.e., texture, even by applying the conventional correcting procedure. To avoid this influence, it is recommended to measure both of volume fraction and texture simultaneously using neutron diffraction. Although synchrotron X-ray shows higher angle resolution, its small incident beam size brings poor statistic reliability. The influence of texture cannot be avoided for transmission Bragg edge measurement, either, which must be overcome to realize 2D or 3D volume fraction mapping.