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。

Development of time-of-flight neutron diffraction technique based on compact neutron source for realizing the stress measurement of steel materials

岩本 ちひろ*; 栗原 諒*; 高村 正人*; 高橋 進*; 鈴木 康介*; 徐 平光; 大竹 淑恵*

no journal, , 

Neutron diffraction is a powerful non-destructive method for evaluating the microscopic structure and internal stress of metal as a bulk average. To implement on-site stress measurements via the neutron diffraction at laboratories and factories frequently and even daily, we are working on improving the method of the neutron diffraction measurement and analysis with techniques of time-of-flight to at RIKEN accelerator-driven compact neutron source (RANS). In this study, we have proposed two methods to improve the determination resolution of the diffraction peak position by focusing on delayed neutrons due to scattering from devices such as reflector surrounding the moderator and the polyethylene collimator. First, an analysis method has been proposed to deconvolute original diffraction peak from the delayed neutron component by defining a model function describing the delayed neutron shape. Second, a new collimator system, called decouple collimator, to reduce the number of delayed neutrons has been developed. In this presentation, we will show following two results: First, the performances of these new methods were evaluated to measure diffraction patterns from a powder sample of pure body-centered cubic iron with the decouple collomator, and to analyze the diffraction peak of {211} reflection by the new analysis method using a model function of a single exponential decay function convoluted with a Gaussian function. The diffracted neutron yield increased by a factor of 2 comapred with a traditional small-apperture polyethylene collimator system while the diffraction peak was successfully separated clearly from the delayed neutron component. Second, a trial stress measurement of a carbon steel specimen applied to as-known compressive stress was performed. At present, the applied stress can be measured with an error of up to 200 MPa for the specimen with applied stress of 500 MPa.

鉄鋼材料の集合組織測定研究に関する大型中性子施設とRIKEN小型中性子源の連携

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

no journal, , 

自動車の軽量化のために使用されている高張力薄鋼板は、プレス成形による加工性が低いことから、生産不良が多い。そのため、プレス成形性を向上させる手段の一つとして、鋼材の集合組織制御に期待が寄せられている。実用に供される金属材料の微視組織は不均一な集合組織を有している。圧延板の加工性など金属材料のマクロな特性を議論する際には、金属材料のバルク平均の集合組織を考慮することが適切だと考えられる。中性子線を用いた集合組織測定は、高い透過性と大きなゲージ体積という特徴を生かして、加工性に直結する金属材料のバルク平均情報を容易に測定することができる。しかしながら、日本国内に限らず、世界中には、集合組織が測定できる中性子回折装置が極めて少ない。そこで、我々は研究用原子炉施設(JRR-3)の定常中性子源と大強度陽子加速器施設(J-PARC)のパルス中性子源を用いた集合組織測定技術を確立し、世界トップレベルの測定精度を有する集合組織測定装置を開発した。近年、中性子評価技術をより広く普及するため、理化学研究所が"いつでも、どこでも、手軽に利用できる"をキャッチフレーズとした小型中性子源(RANS)の開発を進めており、我々がこれまでに培ってきたノウハウを最大限に生かして、RANSを用いた粉末回折技術や集合組織測定技術の開発に挑戦してきた。本発表では、JRR-3, J-PARCおよびRANSで開発した鉄鋼材料の集合組織測定技術を簡単に紹介するとともに、中性子回折による集合組織測定研究に関して大型中性子施設と小型中性子源との連携案について議論する。

In-house texture measurement using RIKEN accelerator-driven compact neutron source

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

no journal, , 

Neutron diffraction is known as a powerful probe to determine the bulk averaged microstructural factors of metals and alloys. Compact neutron sources are being paid much attention for providing wide instrumental accessibility towards many potential on-site neutron diffraction applications, because of less technical complexity compared with large-scale neutron facilities. Here, the RIKEN Accelerator-Driven Compact Neutron Source (RANS) has been developed to establish the in-house technical environment of engineering diffraction for texture measurements. The measured texture of an interstitial-free (IF) steel sheet at RANS was found well consistent with the corresponding result obtained from a large-scale high-resolution time-of-flight neutron diffractometer. Such comparison suggests that RANS may be used to evaluate the ex situ texture characteristics of steel materials. Moreover, the increment of the output power and the addition of the neutron detector will be carried out in near future to enable rapid microstructural factor measurement of other high value-added metallic materials.

Texture gradient evaluation of cold bent high-Mn steel plate using RADEN and RESA neutron instruments

徐 平光; Wang, Y. W.*; Su, Y. H.; 岩本 ちひろ*; Wang, H. H.*; 浜 孝之*; 柴山 由樹; 土川 雄介; Parker, J. D.*; 甲斐 哲也; et al.

no journal, , 

For achieving the carbon neutralization through reducing the greenhouse gas emission, the liquefied natural gas (LNG) has been widely employed as the fuel for electric power plants. As economical cryogenic steel for LNG transport and storage, high-Mn steels have been paid much attention for a high possibility to replace expensive high-Ni martensite steels and high Ni-Cr austenite steels. Its superior cryogenic toughness is thought mostly due to the high thermal stability of austenite even at the LNG storage temperature and the evident mechanical twining effect during the cryogenic deformation. Since four-point bending deformation may induce elastoplastic strain and texture gradient distribution valuable to investigate the twinning effect, it is highly expected to carry out the in-situ/ex-situ cryogenic bending deformation experiment for clarifying the shear-induced twinning mechanism. As a preliminary research, cold-bent samples of high-Mn austenite thick steel plates at room temperature were employed to evaluate the twinning-induced shear band microstructure and confirm the 2D mapping of texture gradient distribution using time-of-flight (TOF) Bragg-edge transmission imaging. Comparably, the quantitative change in triaxial strains and crystallographic texture characteristics at five different regions along the bend radius was evaluated for reference using the angle-dispersive neutron diffraction. The conventional electron backscattering diffraction (EBSD) was employed to provide the direct morphologic information of gradient microstructure of cold-bent high-Mn steel plates. The RADEN neutron transmission profiles obtained from the inner surface layer to the 1/2 thickness layer of cold bent sample show an very interesting preferred orientation charactersitics, quite similar with the density distributions of corresponding orienations of complete pole figures obtained from RESA.

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.