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.

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.

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.

Colossal negative thermal expansion induced by magnetic phase competition on frustrated lattices in Laves phase compound (Hf,Ta)Fe

Li, B.; Luo, X. H.*; Wang, H.*; Ren, W. J.*; Yano, S.*; Wang, C.-W.*; Gardner, J. S.*; Liss, K.-D.*; Miao, P.*; Lee, S.-H.*; et al.

Physical Review B, 93(22), p.224405_1 - 224405_6, 2016/06

https://doi.org/10.1103/PhysRevB.93.224405

Competition between ferromagnetic and antiferromagnetic phases on frustrated lattices in hexagonal Laves phase compound HfTaFe is investigated by using neutron diffraction as a function of temperature and magnetic fields and density-functional-theory calculations. At 325 K, the compound orders into the 120 frustrated antiferromagnetic state with well-reduced magnetic moment and an in-plane lattice contraction simultaneously sets in. With further cooling down, however, the accumulated distortion in turn destabilizes this susceptible frustrated structure. The frustration is completely relieved at 255 K when the first-order transition to the ferromagnetic state takes place, where a colossal negative volumetric thermal expansion, /K, is obtained. Meanwhile, the antiferromagnetic state can be suppressed by few Tesla magnetic fields, which results in a colossal positive magnetostriction. Such delicate competition is attributed to the giant magnetic fluctuation inherent in the frustrated antiferromagnetic state. Therefore, the magnetoelastic instability is approached even under a small perturbation.

Phase composition and microstructural analysis of titanium aluminides by , real-time neutron and synchrotron X-ray techniques

Liss, K. D.

no journal, , 

Modern diffraction methods not only reveal quantitative phase analysis on an - heating and cooling cycle, furthermore there is ample of additional information obtained from multi-dimensional diffraction patterns. The author has pioneered novel methods, applied in many cases to -based titanium aluminides. Thus, phase transition parameters can be followed accurately in alloy development. While synchrotron radiation reveals the overall structure, complementary neutron radiation is particular sensitive to atomic order or disorder. Two-dimensional detection allows to obtain grain statistical information in real time, such as growth, refinement, recrystallization, recovery, grain rotation. Orientation correlations between grains and phases are sought by correlations of reflections in reciprocal space. The paper reviews the findings and methods on -based titanium aluminides, as elaborated during the past decade.

High resolution texture measurement by using neutron diffraction

徐 平光; Harjo, S.; 小貫 祐介*; 佐藤 成男*; Lutterotti, L.*; Vogel, S. C.*; Liss, K.-D.*; 富田 俊郎*

no journal, , 

For polycrystalline materials, textures as their crystallographic orientation feature have been paid broad attention because of their important effects on mechanical and physical characteristics. Besides metals and ceramics, the widespread applications of textures involving sheet forming simulation, additive manufacturing, minerals, and rocks have also demonstrated this status. Different with the electron backscattering diffraction (EBSD) and the X-ray diffraction (XRD) for surface texture analysis, the neutron diffraction thanks to the excellent penetrability and the coarse beam spot of thermal neutrons can collect high statistical diffraction pattens, valuable for deeply investigating the microstructure change and the characteristic response of polycrystalline materials. Through the Rietveld texture analysis process combined with other profile-analysis-related material parameters (e.g. stress tensor, phase fraction, dislocation density and/or coherent size), the large-scale neutron diffractometers TAKUMI and iMATERIA with good instrumental resolution (d/d) and high beam flux have higher measurement efficiency, promoting that the precise evaluation of microstructures and related materials parameters of advanced materials. Recently, weak diffraction patterns step-by-step collected in very short time from the RESA angle dispersive neutron diffractometer at JRR-3 have been utilized to realize the precise texture evaluation of various polycrystalline materials. Our international round robin activity for texture analysis confirms that, Rietveld texture analysis using MAUD software may be recommended as a standard bulk texture analysis method, regardless of the neutron source types of steady reactor source or time-pulsed source.