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

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

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.; 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.

放射光X線回折法を用いた積層型高強度鋼板におけるマルテンサイト層の局所変形挙動評価

小島 真由美*; 城 鮎美*; 鈴木 裕士; 井上 純哉*; 菖蒲 敬久; 徐 平光; 秋田 貢一; 南部 将一*; 小関 敏彦*

材料, 66(6), p.420 - 426, 2017/06

https://doi.org/10.2472/jsms.66.420

The strain distribution in a multilayered steel composite, which consists of martensite and austenite layers, was evaluated by energy dispersive X-ray diffraction to investigate the homogeneity of deformation in the martensite layer under uniaxial loading. A dog-bone shape specimen with a martensite layer with 0.2 mm in a thickness, sandwiching by austenite layers with 0.4 mm in thickness, was utilized in this study. A change in strains as a function of tensile loading was measured at the center of the martensite layer as well as near the interface between the martensite and austenite layers. Furthermore, the residual strain distributions were measured in the martensite layer of the unloaded specimens after different applied strains. As a result, slight inhomogeneous deformation was found at the beginning of the plastic deformation in the martensite layer although no local deformation was recognized even near the interface between austenite and martensite layers. After further deformation, mismatch of plastic deformation between austenite and martensite layers was reduced, and the martensite layer deformed homogeneously. Therefore, an unstable interface phenomenon might not be caused by the intrinsic factors with a mesoscopic scale discussed in this experiment.

Effect of storage environment on hydrogen generation by the reaction of Al with water

Wang, Y.-Q.*; Gai, W.-Z.*; Zhang, X.-Y.*; Pan, H.-Y.*; Cheng, Z.-X.*; 徐 平光; Deng, Z.-Y.*

RSC Advances (Internet), 7(4), p.2103 - 2109, 2017/01

AA2016-0521.pdf:1.55MB

https://doi.org/10.1039/C6RA25563A

Al powder was stored in saturated water vapor, oxygen, nitrogen and drying air separately for a time period up to about six months, the degradation behavior of Al activity was characterized by the reaction of Al with water. It was found that water vapor decreased the induction time for the beginning of Al-water reaction and reduced the total hydrogen generation per unit weight of Al, while oxygen increased the induction time and retarded the Al-water reaction. In contrast, the effect of nitrogen and drying air on Al activity was weak. The mechanism analyses indicated that water vapor promoted the hydration of Al surface passive oxide film and speeded up the reaction of Al with water, while oxygen thickened the passive oxide film of Al surface and prolonged its hydration process. These imply that water vapor rather than oxygen is responsible for the degradation of Al activity during storage under ambient condition.

Rapid measurement scheme for texture in cubic metallic materials using time-of-flight neutron diffraction at iMATERIA

小貫 祐介*; 星川 晃範*; 佐藤 成男*; 徐 平光; 石垣 徹*; 齋藤 洋一*; 轟 秀和*; 林 眞琴*

Journal of Applied Crystallography, 49(5), p.1579 - 1584, 2016/10

AA2016-0186.pdf:1.13MB

https://doi.org/10.1107/S160057671601164X

The authors have developed texture measurement system on a time-of flight neutron diffractometer, iMATERIA (BL20, MLF/J-PARC, Japan). Quantitative Rietveld texture analysis for a duplex stainless steel was possible with one neutron beam exposure for several minutes without sample rotation. The minimum number of diffraction spectra required for the Rietveld texture analysis was experimentally determined as 100. The suggested rapid measurement scheme used 132 spectra and determined volume fractions of texture components in both ferrite and austenite phases, quantitatively. This quantitative and rapid measurement scheme was established by utilizing the features of iMATERIA as a powder diffractometer, i.e. fairly high resolution in d-spacing and numerous detectors equipped in a wide range of scattering angle.

Tensile deformation behavior of hydrogen charged ultrahigh strength steel studied by in situ neutron diffraction

徐 平光; Yin, J*; Zhang, S. Y.*

Acta Metallurgica Sinica, 51(11), p.1297 - 1305, 2015/11

http://www.ams.org.cn/EN/10.11900/0412.1961.2014.00541

The tensile deformation behavior of 1250 MPa ultra-high strength steels with and without hydrogen charging was comparably investigated using neutron diffraction together with the fracture morphology and microstructure observation. Before tensile loading, the (110) lattice spacing of hydrogen charged steel was found larger than that of non-charged sample while the (200) lattice spacing of the former was smaller than that of the latter, suggesting that the hydrogen atoms occupied the tetrahedral center promoted the increment of lattice plane spacing of (110) crystal planes while the balanced internal stress resulted in the proper decrement of (200) lattice plane spacing. In the non-charged sample, the non-linear elastic deformation was observed at 700 MPa in (200) planes, and then at 800 MPa in (110) planes. In the hydrogen charged sample, the non-linear elastic deformation was observed at 300 MPa in (110) planes, and then at 400 MPa in (200) planes. The microstructure observation confirmed the cleavage crack propagation and local crystal rotation in the hydrogen charged sample. Here, a concept about crystallographic orientation dependent micro-yielding was proposed, i.e. the hydrogen charging promoted the (110) preferable micro-yielding rather than (200) preferable micro-yielding, and resulted into a special deformation characteristics.

飛行時間法中性子回折によるバルク材料集合組織測定技術の開発

徐 平光; 星川 晃範*; 林 真琴*; 秋田 貢一; 森井 幸生*; 石垣 徹*

日本材料学会第48回X線材料強度に関するシンポジウム講演論文集, p.7 - 9, 2014/07

Time-of-flight neutron diffraction may evidently accelerate the bulk texture measurement speed through the proper combination of multiple orientations distributed neutron detectors and the simultaneous multiple diffraction peak acquisition, and only few sample rotations are needed to be carried out. In addition to the omega-axis rotatable sample changer, a dedicated omega/chi two-axis rotatable goniometer is under urgent development. It is highly expected to play an important role to evaluate the bulk texture evolution of advanced materials during thermomechanical controlling process. Though the intrinsic difference in neutron diffraction spectra from different orientations (determined by each set of Bragg angle/azimuthal angle) evidently increases the technical difficulty in rapid texture analysis, the development of Materials Analysis Using Diffraction (MAUD, developed by Luca Lutterotti, et al.) and other relevant software/programs are bringing us much convenience. Moreover, in order to increase the accessibility to neutron diffraction bulk texture measurement instruments, the various cooperative researches and the mail-in services are being planned.

Effects of gauge volume on pseudo-strain induced in strain measurement using time-of-flight neutron diffraction

鈴木 裕士; Harjo, S.; 阿部 淳; 徐 平光; 相澤 一也; 秋田 貢一

Nuclear Instruments and Methods in Physics Research A, 715, p.28 - 38, 2013/07

https://doi.org/10.1016/j.nima.2013.03.031

TOF法による中性子ひずみ測定において、中性子線の減衰や表面効果、ひずみ分布などの影響により発生する見かけのひずみ変化に及ぼす測定体積の影響について、焼鈍し材や塑性曲げ材のひずみ測定により検討した。測定体積内の平均ひずみは回折強度重心位置(ncog)に重みが付くため、測定体積の変化によるncog位置の移動に伴い、その重み付き平均ひずみに見かけの変化を生じることがわかった。一方、試料表面近傍のひずみ測定においては、測定体積が試料に完浴状態にない場合に、表面効果による典型的な見かけのひずみ変化が見られた。また、測定体積が試料に完浴状態にあっても、中性子線の減衰によるncog位置の変化に伴う見かけのひずみ変化が見られ、このひずみ変化は測定体積の増加に伴い大きくなることがわかった。これらの見かけのひずみ変化は、従来のモデルにビーム発散の影響を考慮することにより、正確にシミュレーションすることができた。したがって、TOF工学回折計を用いたひずみ測定シミュレーションにおいては、ビーム発散が重要なパラメータとなり得ることを明らかとした。

角度分散法中性子回折集合組織測定技術環境の構築と応用

徐 平光; 秋田 貢一; 鈴木 裕士; 盛合 敦

軽金属学会平成24年度第2回加工と熱処理による優先方位制御研究部会公開講演会資料, p.19 - 20, 2012/10

Though the X-ray diffraction and the electron backscattering diffraction are usually used in the texture evaluation, the neutron diffraction can directly measure the bulk textures of various materials and provide high statistical texture information for predicting the material anisotropic property thanks to the large beam spot and the high matter penetrability, and it can also help to clarify the in situ microstructure evolution under various loading/temperature environments. According to the difference in neutron beam sources, the neutron diffractometers are generally divided into the nuclear reactor-based angle-dispersive instruments and the spallation source-based time-of-flight instruments. At the Japan Research Reactor No.3 and the Japan Proton Accelerator Research Complex, the angle dispersive neutron diffractometers and the time-of-flight neutron diffractometers provide us the possibility to develop and apply the bulk texture evaluation technique to study metallic, ceramic, polymeric, and geologic crystallographic materials. In this presentation, the characteristics of single-tube and 1-demisional position- sensitive-detector angle dispersive neutron diffractometer was simply introduced and its application on the bulk texture evaluation of a magnesium alloy before and after warm press deformation is reported.