小型加速器中性子源RANSを使用した鋼材特性の分析技術開発; ものづくり現場で中性子線を使った材料分析が可能に

徐 平光; 高村 正人*; 岩本 ちひろ*; 箱山 智之*; 大竹 淑恵*; 鈴木 裕士

Isotope News, (774), p.7 - 10, 2021/04

https://www.jrias.or.jp/books/cat3/2021/774.html

近年、地球温暖化対策として、自動車などの軽量化に求められている中、高張力鋼板の成形性向上は重要な開発課題となっている。破断まで優れた伸び特性を持たせた高張力鋼板の開発には、オーステナイト組織の相分率と各構成相の集合組織を正しく制御することは極めて重要である。透過能に優れた中性子回折法は、鋼材内部の結晶情報をバルク平均で得られる特徴を持つことから、相分率と集合組織を測定する上で有力な手段である。しかし、現状では中性子回折測定が可能な中性子源は、研究用原子炉や大型加速器施設などの大型実験施設に限られ、これらは共用施設のため利用者が頻繁に測定する機会を得ることは困難である。そこで、理化学研究所では、大学や企業の研究室、工場などの現場で手軽に使える小型中性子源として「理研小型加速器中性子源RANS」を構築し、日本原子力研究開発機構と協力しながら鋼材特性の分析技術に関する一連の研究開発を進めてきた。本解説論文では、大型実験施設と比べるとビーム強度の低い小型加速器中性子源を用いて実施した、中性子回折法による相分率と集合組織測定に関する共同研究成果と、今後の展望を紹介する。

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.

Determination approach of dislocation density and crystallite size using a convolutional multiple whole profile software

村澤 皓大*; 高村 正人*; 熊谷 正芳*; 池田 義雅*; 鈴木 裕士; 大竹 淑恵*; 浜 孝之*; 鈴木 進補*

Materials Transactions, 59(7), p.1135 - 1141, 2018/07

https://doi.org/10.2320/matertrans.M2017380

Neutron diffraction profile analysis using the whole profile fitting method is useful for obtaining microscopic information on metallic materials. To determine an appropriate fitting approach for obtaining reasonable and non-arbitrary results, we applied diffraction line profile analyses using the Convolutional Multiple Whole Profile (CMWP) method to diffraction patterns obtained using the Engineering Materials Diffractometer (TAKUMI, BL19) at the Materials and Life Science Facility (MLF) of the Japan Proton Accelerator Research Complex (J-PARC). The tensile specimens of 780 MPa grade bainitic steel were uniaxially stretched until the plastic strain reached a value of 0.05. We performed CMWP analyses on the obtained diffraction patterns during tensile test with various initial parameters of dislocation density and crystallite size. These parameters were optimized in the fitting procedures to minimize the weighted sums of squared residuals (WSSRs). Following this approach, we found that unsuitable initial parameter values resulted in unreasonable convergence. Therefore, initial fitting parameters should be chosen to ensure that the initial profiles are as broad as possible. Reasonable results were obtained following this suggestive approach even when the strain anisotropy parameter is set to arbitrary values.

Prospect for application of compact accelerator-based neutron source to neutron engineering diffraction

池田 義雅*; 竹谷 篤*; 高村 正人*; 須長 秀行*; 熊谷 正芳*; 大場 洋次郎*; 大竹 淑恵*; 鈴木 裕士

Nuclear Instruments and Methods in Physics Research A, 833, p.61 - 67, 2016/10

https://doi.org/10.1016/j.nima.2016.06.127

小型中性子源を利用した透過イメージングや小角散乱、反射率測定など、小型中性子源による工学的応用に関する議論が広まるなか、小型中性子源のフラックスの低いゆえに回折実験に関する検討はなされてこなかった。そこで本研究では、理化学研究所の小型加速器中性子源RANSを用いることにより、中性子工学回折実験への応用の可能性について検討した。まず、光学系の最適化によるバックグラウンドノイズの低減により、10分間の測定でも十分に認識可能な回折パターンを得ることができた。110回折のプロファイルから計算した分解能は約2.5%であり、中性子回折によるひずみ測定には不十分である。RANSのモデレータによる減速時間が約30sと分解能の決定に最も支配的なパラメータであることから、モデレータの改良が分解能の向上につながる。一方で、回折パターンの変化から、塑性変形に伴う集合組織の変化をとらえることに成功するとともに、リートベルトコードによる回折パターンのフィッティングにより、オーステナイト相の体積率の評価にも成功した。RANSは、集合組織や残留オーステナイト量の測定を目的とした中性子工学回折の応用に有効と考えられる。

Non-destructive texture measurement of steel sheets with compact neutron source "RANS"

高村 正人*; 池田 義雅*; 須長 秀行*; 竹谷 篤*; 大竹 淑恵*; 鈴木 裕士; 熊谷 正芳*; 浜 孝之*; 大場 洋次郎*

Journal of Physics; Conference Series, 734(Part B), p.032047_1 - 032047_4, 2016/08

https://doi.org/10.1088/1742-6596/734/3/032047

中性子回折法は、中性子線の優れた透過能を活かすことで、金属材料のバルク集合組織を測定できる技術として知られている。しかしながら、この測定技術は、原子炉や加速器施設などの大型実験施設を必要とするため、あまり広く利用されていないのが現状である。一方、理研小型中性子源(RANS)は、実験室レベルで容易に利用できる中性子源として開発されている。本研究では、RANSを用いることにより、塑性変形した鋼板の集合組織の変化を捉えることに成功した。本結果は、金属材料のミクロ組織解析に対する小型中性子源の可能性を示すものであり、塑性変形挙動のより良い理解につながるものと期待される。

Energy resolution evaluation of decoupled neutron moderator for stress measurements via neutron diffraction with compact neutron source

角田 龍之介*; 高村 正人*; 徐 平光; 岩本 ちひろ*; 高梨 宇宙*; 大竹 淑恵*; 栗原 諒*; 高橋 進*; 鈴木 裕士

no journal, , 

During the production of high-strength steel structural parts, the residual stress is necessary to be well controlled for the better dimensional accuracy and the longer service life. The neutron diffraction measurement is a good candidate to monitor the microscopic lattice strain of polycrystalline materials in bulk average. RANS (Riken Accelerator-driven Compact Neutron Source) has been developed and upgraded aiming at in-house, on-site and on-demand measurements to meet with industrial needs. Recently, the phase volume fractions and the bulk textures of steel materials have been measured successfully at RANS. In order to measure the lattice strain at RANS, it is required to improve the energy resolution to observe slight peak shift, and the decoupled moderator is thought as a good solution method for that. In this study, a new decoupled moderator consisting of polyethylene with 20 cmm thickness and BC rubber was designed and fabricated, and its neutron beam characteristic was investigated in order to improve the time energy resolution to realize in-house neutron stress measurement at RANS. Here, the preliminary results of the resolutions comparing between the new decoupled moderator and the traditional coupled moderators with 20 and 40 mm thickness polyethylene will be reported together with the scattering angle dependent instrumental resolution of the linear neutron position-sensitive detector.

Neutron diffraction with RANS for industrial "on-site" applications

高村 正人*; 岩本 ちひろ*; 徐 平光; 角田 龍之介*; 栗原 諒*; 箱山 智之*; 池田 義雅*; 鈴木 裕士; 大竹 淑恵*

no journal, , 

High strength steels are becoming more and more important in automotive body structures for good weight reduction, providing further requirement in the balance between strength and formability. Numerical models in forming simulations taking into account the texture evolution may accurately analyze macroscopic plastic behavior, through referring to local surface texture measurement using Electron backscatter diffraction or X-ray diffraction. In contrast, neutron diffraction may measure the microstructure factors including bulk-averaged texture, enable to more deeply understand the mechanisms of deformation behavior. Such neutron diffraction studies usually require large-scale experimental facilities like a reactor and a large accelerator, so meet certain difficulty in the instrumental accessibility. To solve these problems, Riken Accelerator-driven Compact Neutron Source (RANS) has been developed. On-site evaluation of microstructural factors enables us to analyze metal deformation processes more efficiently. Authors have recently succeeded in accurately measuring the texture evolution of an IF steel and also in determining the retained austenite volume fraction of multi-phase steels, by optimizing the beam condition and layout of collimators, samples, detectors, etc. These results show the possibility of practical use of an in-house compact neutron source in laboratories of universities, research institutes and industrial firms.

ものづくり現場における小型中性子源の利用; 金属加工への活用

高村 正人*; 岩本 ちひろ*; 徐 平光; 上野 孝太*; 栗原 諒*; 鈴木 裕士; 大竹 淑恵*

no journal, , 

Plastic forming processes of metallic sheets, , forging, rolling, bending, pressing, drawing, and extruding, are important manufacturing methods to produce complex mechanical parts. Numerical simulation using the finite element method based on the crystal plasticity theory has been thought valuable to improve the forming accuracy and reduce the forming defects, especially for high strength automotive metallic sheets. For the realization of reliable numerical modelling and the development of strength-formability well-balanced novel metallic sheets, the bulk average microstructure information closely related to the mechanical characteristics is highly expected to be on-site available, or at least may be measured in time through neutron diffraction. Towards these on-site neutron diffraction measurement requirements from forming process designers and materials researchers, RIKEN has developed an accelerator-driven compact neutron source (RANS) and realized the texture and phase fraction measurement at a good precision level. Recently, a novel residual measurement technique using RANS is being carried out.

Collaborative advances in bulk texture measurement techniques based on the JAEA large neutron sources and the RIKEN compact neutron source

徐 平光; 岩本 ちひろ*; 高村 正人*; 大竹 淑恵*; 栗原 諒*; 上野 孝太*; 片岡 美波*; 山本 和喜; Harjo, S.; 菖蒲 敬久

no journal, , 

Neutron diffraction can collect sample-volume averaged diffraction patterns due to the excellent penetrability and the coarse beam spot, valuable for investigating bulk microstructure changes of polycrystalline materials. In recent years, several neutron instruments in Japan have been employed for precise bulk texture evaluation. The engineering materials diffractometer attached with large sample stage and precise radial collimators at J-PARC has realized a reliably combined Rietveld texture evaluation, simultaneously providing crystallographic textures and other profile-analysis-related material parameters such as crystal structures, stress tensors. The RANS compact neutron source has enabled reliable bulk texture evaluation of steel materials through reasonably using a high stereographic angle resolution and a large sample-gauge volume. As a feed-back from the texture measurement technique based on RANS compact neutron source, recently, weak diffraction patterns step-by-step collected in very short time from RESA neutron diffractometer at JRR-3 have been utilized to realize the precise texture evaluation of various polycrystalline materials, , a standard rock material, and different steel materials.

Effect of sample geometry on texture measurement of metallic materials using angle dispersive neutron diffraction

徐 平光; 山本 和喜; 岩本 ちひろ*; 高村 正人*

no journal, , 

While the bulk crystallographic textures are usually evaluated through the relative difference in neutron diffraction intensities of polycrystal materials from various sample orientations, an irregular sample geometric shape (different from a sphere and a cube) has an evident effect on the stereographic orientation distribution of neutron diffraction intensities due to the change in locally diffracted gauge volume and the neutron penetration path, which disturbs the quantitative calculation of real preferred orientation of materials and leads to clear uncertainty in nondestructive bulk texture measurements of finished or semi-finished products. Here, the stereographic diffraction intensity distributions of several high strength low alloy steel samples with same microstructure and texture but in various shapes and sizes were measured using RESA angle dispersive neutron diffraction. By referring to the classic neutron attenuation correction theory, the absorption correction reliability was examined to enable that the relevant intensity ratios among the rolling direction, the normal direction, the transverse direction, etc. are almost consistent with the corresponding data from a referred cubic sample. In the poster session, the recalculated bulk textures using the intensity-corrected diffraction profiles of different shaped samples will be given out to make a further comparison and discussion.