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論文

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

 被引用回数:0 パーセンタイル:0(Materials Science, Multidisciplinary)

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.

論文

Abnormal grain growth; A Spontaneous activation of competing grain rotation

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

Advanced Engineering Materials, 9 Pages, 2023/00

In polycrystals, grains with certain orientations grow at high temperatures at the expense of grains with other unfavorable orientations. Grain growth involves a variety of situations and mechanisms that make experimental study, modeling, and understanding extremely complex. Normal grain growth occurs in a self-similar manner, with curved grain boundaries serving as the driving force and a parabolic growth law that scales up the grain size by the square root of time. More complex growth forms include boundary pinning of precipitates and other boundaries, topological transitions that alter driving forces, grain coalescence and anomalous grain growth, but these are considered "erratic" and their initiation is an open question in modern research, without a simple experimental approach on how they should be studied. Here, we show that grain rotation upon coalescence is spontaneously activated between one grain and a favorable neighbor, through the necessary diffusive mass transport at further boundaries of the same grain leading to their activation and a competitive "erratic" reorientation in a zigzag way, while other grains in the matrix remain stable. After two grains have eventually coalesced, their surrounding boundaries are still activated leading to further rotation and growth, filling the missing puzzle stone in thermodynamic theory between normal and abnormal growth, the latter stating that abnormal growth only takes place when the size of the growing grain is already large. Prerequisites and postulates of abnormal grain growth are based on advantageous texture, grain boundary mobility, enhanced diffusion kinetics and coalescence, which can be well explained by our observations. Moreover, our observations have been enabled through a novel experimental approach using the white-beam X-ray Laue diffraction method in bulk transmission mode on a polycrystalline.

論文

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

 被引用回数:3 パーセンタイル:38.91(Materials Science, Multidisciplinary)

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, Al$$_{12}$$Mg$$_{17}$$, 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.

論文

角度分散法中性子回折によるバルク材料の集合組織解析

徐 平光; 秋田 貢一; 鈴木 裕士; 盛合 敦; 鈴木 徹也*; 行武 栄太郎*

日本材料学会第46回X線材料強度に関するシンポジウム講演論文集, p.24 - 27, 2012/07

Conventional X-ray diffraction and recent electron backscattering diffraction are widely employed to investigate the surface texture information for a specific sample, but the neutron diffraction is well known to directly measure the bulk average texture information with high statistics. In order to increase the accessibility to neutron diffraction bulk texture measurement instruments, JAEA has upgraded two angle dispersive neutron diffractometer RESA-2 and MUSASI-L. In this paper, the bulk texture measurement environments based on the angle dispersive neutron diffraction were introduced, and the application research cases to the bulk texture changes during the isothermal annealing of ARBed IF steels and during the warm press deformation of a magnesium alloy were reported here to show the good texture evaluation reliability.

口頭

Various applications of bulk texture measurement technique by neutron diffraction

徐 平光; 鈴木 徹也*; 行武 栄太郎*; 諸岡 聡*

no journal, , 

For sheet/pipeline metallic materials, texture control is one of important technical fields in order to realize good formability. Though the X-ray diffraction and the electron backscattering diffraction are usually used in the texture researches, the neutron diffraction can directly measure the bulk textures of various materials and provide high statistical texture information for the material property simulation. In this paper, several research cases of bulk texture measurements based on MUSASI-L/RESA-2 neutron diffractometer were introduced, including IF steel, multilayered steel composite, magnesium alloy and titanium alloy, suggesting that the broad application of bulk texture evaluation technique has become available in Japan.

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