synchrotron radiation observation of deformation and annealing processes of aluminum single crystal

Shiro, Ayumi*; Okada, Tatsuya*; Shobu, Takahisa

Mechanical Engineering Journal (Internet), 8(6), p.21-00106_1 - 21-00106_8, 2021/12

https://doi.org/10.1299/mej.21-00106

The objective of the present study was to carry out observations of deformation and annealing processes of aluminum single crystals using a synchrotron radiation X-rays at SPring-8. Al single-crystalline samples having a 111 orientation parallel to the longitudinal direction were grown by a Bridgman method. The samples were deformed in tension to a nominal strain of 0.08 at room temperature using an in-line tensioning apparatus. Post-deformation annealing at 480 C was subsequently carried out in the same apparatus. A two-dimensional detector was used to detect multiple diffracted beams from the sample during the deformation and annealing processes. The volume irradiated by the X-ray beam was found to be composed of three regions having a small orientation difference, which was attributable to sub-grained microstructures of the sample. Detailed analyses of a diffraction spot intensity showed that the sub-grained microstructures were surpassed by dislocated microstructures with the increase in the tensile strain. During the post-deformation annealing, diffraction spots from a recrystallized grain first appeared at 180 s after the temperature reached 480 C. Coexistence of diffraction spots from the deformation matrix and recrystallized grain lasted only for about 22 s in the irradiated volume. The migration rate of the boundary between the deformation matrix and recrystallized grain was estimated to be of the order of several micrometers/s.

Internal strain distribution of laser lap joints in steel under loading studied by high-energy synchrotron radiation X-rays

Shobu, Takahisa; Shiro, Ayumi*; Kono, Fumiaki*; Muramatsu, Toshiharu; Yamada, Tomonori; Naganuma, Masayuki; Ozawa, Takayuki

Quantum Beam Science (Internet), 5(2), p.17_1 - 17_9, 2021/06

https://doi.org/10.3390/qubs5020017

The automotive industries employ laser beam welding because it realizes a high energy density without generating irradiation marks on the opposite side of the irradiated surface. Typical measurement techniques such as strain gauges and tube X-rays cannot assess the localized strain at a joint weld. Herein high-energy synchrotron radiation X-ray diffraction was used to study the internal strain distribution of laser lap joint PNC-FMS steels (2- and 5-mm thick) under loading at a high temperature. As the tensile load increased, the local tensile and compressive strains increased near the interface. These changes agreed well with the finite element analysis results. However, it is essential to complementarily utilize internal defect observations by X-ray transmission imaging because the results depend on the defects generated by laser processing.

Double-exposure method with synchrotron white X-ray for stress evaluation of coarse-grain materials

Suzuki, Kenji*; Shiro, Ayumi*; Toyokawa, Hidenori*; Saji, Choji*; Shobu, Takahisa

Quantum Beam Science (Internet), 4(3), p.25_1 - 25_14, 2020/09

https://doi.org/10.3390/qubs4030025

It is difficult to evaluate stress by the strain scanning method using a conventional diffractometer and a point detector since the two-dimensional diffraction pattern of a material composed of coarse grains does not have a ring but a spotty. To solve this problem, we proposed a double exposure method using a two-dimensional detector and monochromatized X-rays. In this study, we have developed a technique to apply that technique to white X-rays. The diffraction obtained by irradiating white X-rays for a material with of coarse grains becomes a Laue spot. Therefore, we have carried out developing a CdTe pixel two-dimensional detector that can limit the energy to be detected, and we evaluated the stress using that detector. As a result, we succeeded to measure the strain distribution of a bending specimen made to austenitic stainless steel. In the future, we would like to improve this technology and apply it to actual machine materials.

Characterization of microstructures by X-ray diffraction line profile analysis, 2; Line profile analysis using synchrotron radiation

Shobu, Takahisa; Shiro, Ayumi*; Yoshida, Yutaka*

Zairyo, 69(4), p.343 - 347, 2020/04

https://doi.org/10.2472/jsms.69.343

Dislocation density is a very important physical quantity in the evaluation of fatigue of metallic materials. Generally, the dislocation density is evaluated by a scanning electron microscope. Recently, a method generated the dislocation density from the width of the X-ray diffraction profile has been proposed. In this study, we report the application of this technology to synchrotron radiation. Five diffraction profiles were obtained with a two-dimensional detector during tensile loading of the austenitic stainless steel SUS316L, and the dislocation density was calculated from the line profile analysis. As a result, the dislocation density increased sharply after plastic deformation, and the value was in good agreement with the result separately measured with a scanning electron microscope. In the future, it is expected that the line profile analysis will contribute to the elucidation of the mechanism of fatigue fracture by measuring the dislocation density from the local area in materials.

Analysis of atomistic structural deformation characteristics of calcium silicate hydrate in 53-year-old tricalcium silicate paste using atomic pair distribution function

Bae, S.*; Jee, H.*; Suh, H.*; Kanematsu, Manabu*; Shiro, Ayumi*; Machida, Akihiko*; Watanuki, Tetsu*; Shobu, Takahisa; Morooka, Satoshi; Geng, G.*; et al.

Construction and Building Materials, 237, p.117714_1 - 117714_10, 2020/03

https://doi.org/10.1016/j.conbuildmat.2019.117714

Stress measurement of coarse grains using double exposure method

Suzuki, Kenji*; Shobu, Takahisa; Shiro, Ayumi*

Zairyo, 68(4), p.312 - 317, 2019/04

https://doi.org/10.2472/jsms.68.312

Materials after thermal processing such as welding often have coarse grains. To understand the residual stress after processing is very important from the viewpoint of the soundness of the structure. In this study, we proposed a double exposure method that combines a two-dimensional detector and high-energy synchrotron radiation as an X-ray stress measurement method for materials with coarse grains, and confirmed its practicality. As a result of measuring the residual stress of the plastic bending specimen and the indentation specimen of the aluminum alloy (A5052), the effectiveness of this measurement method was clarified because the residual stress distribution was in good agreement with the finite element analysis.

Strain measurement in Ti layers of CFRP/Ti laminates by synchrotron X-ray diffraction

Akita, Koichi; Nakatani, Hayato*; Ogihara, Shinji*; Shobu, Takahisa; Shiro, Ayumi*; Igawa, Naoki; Shimojo, Yutaka

SPring-8/SACLA Riyo Kenkyu Seikashu (Internet), 6(1), p.105 - 108, 2018/01

http://doi.org/10.18957/rr.6.1.105

no abstracts in English

Development of CdTe pixel detectors combined with an aluminum Schottky diode sensor and photon-counting ASICs

Toyokawa, Hidenori*; Saji, Choji*; Kawase, Morihiro*; Wu, S.*; Hurukawa, Yukihito*; Kajiwara, Kentaro*; Sato, Masugu*; Hirono, Toko*; Shiro, Ayumi*; Shobu, Takahisa; et al.

Journal of Instrumentation (Internet), 12(1), p.C01044_1 - C01044_7, 2017/01

https://doi.org/10.1088/1748-0221/12/01/C01044

We have been developing CdTe pixel detectors combined with a Schottky diode sensor and photon-counting ASICs. The hybrid pixel detector was designed with a pixel size of 200 micro-meter by 200 micro-meter and an area of 19 mm by 20 mm or 38.2 mm by 40.2 mm. The photon-counting ASIC, SP8-04F10K, has a preamplifier, a shaper, 3-level window-type discriminators and a 24-bits counter in each pixel. The single-chip detector with 100 by 95 pixels successfully operated with a photon-counting mode selecting X-ray energy with the window comparator and stable operation was realized at 20C. We have performed a feasibility study for a white X-ray microbeam experiment. Laue diffraction patterns were measured during the scan of the irradiated position in a silicon steel sample. The grain boundaries were identified by using the differentials between adjacent images at each position.

In situ X-ray diffraction study of the oxide formed on alloy 600 in borated and lithiated high-temperature water

Watanabe, Masashi*; Yonezawa, Toshio*; Shobu, Takahisa; Shiro, Ayumi; Shoji, Tetsuo*

Corrosion, 72(9), p.1155 - 1169, 2016/09

https://doi.org/10.5006/1994

Hydrostatic compression behavior and high-pressure stabilized -phase in -based titanium aluminide intermetallics

Liss, K.-D.*; Funakoshi, Kenichi*; Dippenaar, R. J.*; Higo, Yuji*; Shiro, Ayumi*; Reid, M.*; Suzuki, Hiroshi; Shobu, Takahisa; Akita, Koichi

Metals, 6(7), p.165_1 - 165_22, 2016/07

https://doi.org/10.3390/met6070165

Titanium aluminides find application in modern light-weight, high-temperature turbines, such as aircraft engines, but suffer from poor plasticity during manufacturing and processing. Huge forging presses enable materials processing in the 10 GPa range and hence, it is necessary to investigate the phase-diagrams of candidate materials under these extreme conditions. Here we report on an in-situ synchrotron X-ray diffraction study in a large-volume-press of a modern ( + ) two-phase material, Ti-45Al-7.5Nb-0.25C, under pressures up to 9.6 GPa and temperatures up to 1686 K. At room temperature, the volume response to pressure is accommodated by the transformation rather than volumetric strain, expressed by apparently high bulk moduli of both constituent phases. Crystallographic aspects, specifically lattice strain and atomic order are discussed in detail. It is interesting to note that this transformation takes place despite an increase in atomic volume, which is due to the high ordering energy of . Upon heating under high pressure, both the eutectoid and -solvus transition temperatures are elevated, and a third, cubic -phase is stabilized above 1350 K. Earlier research has shown that this -phase is very ductile during plastic deformation, essential in near-conventional forging processes. Here, we were able to identify an ideal processing window for near-conventional forging, while the presence of the detrimental -phase is not present under operating conditions. Novel processing routes can be defined from these findings.