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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

 被引用回数:0 パーセンタイル:100(Chemistry, Multidisciplinary)

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 B$$_{4}$$C 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.


Development of spin-contrast-variation neutron reflectometry for the structural analysis of multilayer films

熊田 高之; 阿久津 和宏*; 大石 一城*; 森川 利明*; 河村 幸彦*; 佐原 雅恵*; 鈴木 淳市*; 鳥飼 直也*

Journal of Applied Crystallography, 52(5), p.1054 - 1060, 2019/10

 被引用回数:0 パーセンタイル:100(Chemistry, Multidisciplinary)



Quasielastic neutron scattering of brucite to analyse hydrogen transport on the atomic scale

奥地 拓生*; 豊岡 尚敬*; Purevjav, N.*; 柴田 薫

Journal of Applied Crystallography, 51, p.1564 - 1570, 2018/12

 被引用回数:0 パーセンタイル:100(Chemistry, Multidisciplinary)

中性子準弾性散乱(QENS)は、鉱物結晶格子内で起こる原子スケール水素拡散プロセスを分析するための新規かつ有効な方法であることが実証されている。この方法は、凝縮体中の拡散性が高い水素原子または水分子の拡散頻度および距離を分析するために敏感であると以前から考えられていた。本論文では、水酸基として結晶格子に結合している非常に遅い運動の水素原子の拡散運動を分析する応用研究の結果が示されている。ブルーサイト鉱物( brucite)、Mg(OH)$$_{2}$$では、水素原子の単一の二次元層面内でのジャンプとそれに最も近い次の層へのジャンプの2種類の水素拡散プロセスが観察された。ブルーサイトの結晶構造内で観察されるこれらの拡散プロセスは、層状構造を有する様々な種類の酸化物およびミネラル内で起こる水素拡散現象にQENS測定が適用可能であることを示している。


Stroboscopic time-of-flight neutron diffraction during cyclic testing using the event data recording system at J-PARC

川崎 卓郎; 稲村 泰弘; 伊藤 崇芳*; 中谷 健; Harjo, S.; Gong, W.*; 相澤 一也

Journal of Applied Crystallography, 51(3), p.630 - 634, 2018/06

 被引用回数:2 パーセンタイル:61.54(Chemistry, Multidisciplinary)

A time-resolved time-of-flight neutron diffraction technique to characterize the structural properties of materials during cyclic tests has been developed. By adopting the developed technique, the behaviors of the crystal lattice and domains of the piezoelectric material in a multilayer-type piezoelectric actuator driven by a cyclic electric field were evaluated. The variation in diffraction intensity during the application of a cyclic electric field was obtained successfully, and the hysteresis-like behaviors of both the lattice strain and the 90$$^{circ}$$ domain switching were revealed.


High stereographic resolution texture and residual stress evaluation using time-of-flight neutron diffraction

徐 平光; Harjo, S.; 小島 真由美*; 鈴木 裕士; 伊藤 崇芳*; Gong, W.; Vogel, S. C.*; 井上 純哉*; 友田 陽*; 相澤 一也; et al.

Journal of Applied Crystallography, 51(3), p.746 - 760, 2018/06

 被引用回数:13 パーセンタイル:11.06(Chemistry, Multidisciplinary)

Neutron diffraction texture measurements provide bulk textures with excellent grain statistics even for large grained materials, together with the crystallographic parameters and microstructure information such as phase fractions, coherent crystallite size, root mean square microstrain, macroscopic/intergranular stress/strain. The procedure for high stereographic resolution texture and residual stress evaluation was established at the TAKUMI engineering materials diffractometer. The pole figure evaluation of a limestone standard sample with a trigonal crystal structure suggested that the obtained precision for texture measurement is comparable with the oversea well-established neutron beam lines utilized for texture measurements. A high strength martensite-austenite multilayered steel was employed for further verification of the reliability of simultaneous Rietveld analysis of multiphase textures and macro stress tensors. By using a geometric mean micro-mechanical model, the macro stress tensor analysis with a plane stress assumption showed a RD-TD in-plane compressive stress (about -330 MPa) in martensite layers and a RD-TD in-plane tensile stress (about 320 MPa) in austenite layers. The phase stress partitioning was ascribed to the additive effect of volume expansion during martensite transformation and the linear contraction misfit during water quenching.


Inverse pole figure mapping of bulk crystalline grains in a polycrystalline steel plate by pulsed neutron Bragg-dip transmission imaging

佐藤 博隆*; 塩田 佳徳*; 諸岡 聡; 戸高 義一*; 足立 望*; 定松 直*; 及川 健一; 原田 正英; Zhang, S.*; Su, Y.; et al.

Journal of Applied Crystallography, 50(6), p.1601 - 1610, 2017/12

 被引用回数:8 パーセンタイル:28.93(Chemistry, Multidisciplinary)

A new mapping procedure for polycrystals using neutron Bragg-dip transmission is presented. This is expected to be useful as a new materials characterization tool which can simultaneously map the crystallographic direction of grains parallel to the incident beam. The method potentially has a higher spatial resolution than neutron diffraction imaging. As a demonstration, a Bragg-dip neutron transmission experiment was conducted at J-PARC on beamline MLF BL10 NOBORU. A large-grained Si-steel plate was used. Since this specimen included multiple grains along the neutron beam transmission path, it was a challenging task for existing methods to analyze the direction of the crystal lattice of each grain. A new data-analysis method for Bragg-dip transmission measurements was developed based on database matching. As a result, the number of grains and their crystallographic direction along the neutron transmission path have been determined.


Energy-resolved small-angle neutron scattering from steel

大場 洋次郎*; 諸岡 聡; 大石 一城*; 鈴木 淳市*; 高田 慎一; 佐藤 信浩*; 井上 倫太郎*; 土山 聡宏*; Gilbert, E. P.*; 杉山 正明*

Journal of Applied Crystallography, 50(2), p.334 - 339, 2017/04

 被引用回数:2 パーセンタイル:67.97(Chemistry, Multidisciplinary)

Recent progress of pulsed neutron sources has enabled energy-resolved analysis of neutron attenuation spectra, which include information on neutron scattering. In this study, a new analysis technique for small-angle neutron scattering (SANS) is demonstrated. A clear difference is observed in the neutron attenuation spectra between steels with different nanostructures; this difference can be understood as arising from attenuation due to SANS. The neutron attenuation spectra, calculated from the corresponding SANS profiles, agree well with the experimentally observed attenuation spectra. This result indicates that measurement of neutron attenuation spectra may enable the development of a novel experimental technique, i.e. energy-resolved SANS (ESANS).


Contrast variation by dynamic nuclear polarization and time-of-flight small-angle neutron scattering, 1; Application to industrial multi-component nanocomposites

能田 洋平*; 小泉 智*; 増井 友美*; 間下 亮*; 岸本 浩通*; 山口 大輔; 熊田 高之; 高田 慎一; 大石 一城*; 鈴木 淳市*

Journal of Applied Crystallography, 49(6), p.2036 - 2045, 2016/12

 被引用回数:10 パーセンタイル:27.22(Chemistry, Multidisciplinary)

We have reported the first attempt with dynamic nuclear polarization (DNP) and contrast variation small-angle neutron scattering (SANS) experiments on model mixtures for industrial tyres conducted at the MLF of J-PARC. We performed time-of-flight SANS (TOF-SANS) experiments, employing neutrons with a wide range, which causes imperfect neutron polarization and variations in the coherent and incoherent scattering lengths. By carefully eliminating the effect of imperfect neutron polarization, separation of the partial scattering functions was successfully demonstrated for the ternary system styrene-butadiene-rubber/silica/carbon.


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


 被引用回数:17 パーセンタイル:15.51(Chemistry, Multidisciplinary)

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 $$sim$$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.


Magnetic scattering in the simultaneous measurement of small-angle neutron scattering and Bragg edge transmission from steel

大場 洋次郎*; 諸岡 聡; 大石 一城*; 佐藤 信浩*; 井上 倫太郎*; 足立 望*; 鈴木 淳市*; 土山 聡宏*; Gilbert, E. P.*; 杉山 正明*

Journal of Applied Crystallography, 49(5), p.1659 - 1664, 2016/10

 被引用回数:7 パーセンタイル:38.97(Chemistry, Multidisciplinary)

Pulsed neutron sources enable the simultaneous measurement of small-angle neutron scattering (SANS) and Bragg edge transmission. This simultaneous measurement is useful for microstructural characterization in steel. Since most steels are ferromagnetic, magnetic scattering contributions should be considered in both SANS and Bragg edge transmission analyses. An expression for the magnetic scattering contribution to Bragg edge transmission analysis has been derived. The analysis using this expression was applied to Cu steel. The ferrite crystallite size estimated from this Bragg edge transmission analysis with the magnetic scattering contribution was larger than that estimated using conventional expressions. This result indicates that magnetic scattering has to be taken into account for quantitative Bragg edge transmission analysis. In the SANS analysis, the ratio of magnetic to nuclear scattering contributions revealed that the precipitates consist of body-centered cubic Cu$$_{0.7}$$Fe$$_{0.3}$$ and pure Cu, which probably has 9R structure including elastic strain and vacancies. These results show that effective use of the magnetic scattering contribution allows detailed analyses of steel microstructure.


Investigation of dissimilar metal welds by energy-resolved neutron imaging

Tremsin, A. S.*; Ganguly, S.*; Meco, S. M.*; Pardal, G.*; 篠原 武尚; Bruce Feller, W.*

Journal of Applied Crystallography, 49(4), p.1130 - 1140, 2016/08

 被引用回数:12 パーセンタイル:24.44(Chemistry, Multidisciplinary)

A nondestructive study of the internal structure and compositional gradient of dissimilar metal-alloy welds through energy-resolved neutron imaging is described in this paper. The presence of Bragg edges in the measured neutron transmission spectra can be used to characterize the internal residual strain within the samples and some microstructural features, while neutron resonance absorption provides the possibility to map the degree of uniformity in mixing of the participating alloys and intermetallic formation within the welds. This paper demonstrates the potential of neutron energy-resolved imaging to measure all these characteristics simultaneously in a single experiment with sub-mm spatial resolution.


SENJU; A New time-of-flight single-crystal neutron diffractometer at J-PARC

大原 高志; 鬼柳 亮嗣; 及川 健一; 金子 耕士; 川崎 卓郎; 田村 格良; 中尾 朗子*; 花島 隆泰*; 宗像 孝司*; 茂吉 武人*; et al.

Journal of Applied Crystallography, 49(1), p.120 - 127, 2016/02

 被引用回数:25 パーセンタイル:5.93(Chemistry, Multidisciplinary)

SENJU, a time-of-flight Laue-type single-crystal neutron diffractometer, was developed at the Materials and Life Science Experimental Facility (MLF) of the Japan Accelerator Research Complex (J-PARC). Molecular structure analysis of a sub-millimeter taurine crystal and magnetic structure analysis of a MnF$$_{2}$$ crystal were performed to evaluate its performance.


High-speed three-dimensional reciprocal-space mapping during molecular beam epitaxy growth of InGaAs

Hu, W.; 鈴木 秀俊*; 佐々木 拓生*; 神津 美和*; 高橋 正光

Journal of Applied Crystallography, 45(5), p.1046 - 1053, 2012/10

 被引用回数:9 パーセンタイル:29.94(Chemistry, Multidisciplinary)

This paper describes the development of a high-speed three-dimensional reciprocal-space mapping method designed for the real-time monitoring of the strain relaxation process during the growth of heterostructure semiconductors. Each three-dimensional map is obtained by combining a set of consecutive images, which are captured during the continuous rotation of the sample, and calculating the reciprocal-space coordinates from the detector coordinate system. Using this method, the strain relaxation process of InGaAs heteroepitaxial films grown on GaAs(001) has been investigated.


Inhomogeneous dynamic nuclear polarization of protons in a lamella-forming diblock copolymer investigated by a small-angle neutron scattering method

能田 洋平; 熊田 高之; 橋本 竹治; 小泉 智

Journal of Applied Crystallography, 44(3), p.503 - 513, 2011/06

 被引用回数:11 パーセンタイル:24.59(Chemistry, Multidisciplinary)



Growth of large protein crystals by a large-scale hanging-drop method

垣之内 啓介*; 中村 努*; 玉田 太郎; 安達 宏昭*; 杉山 成*; 丸山 美帆子*; 高橋 義典*; 高野 和文*; 村上 聡*; 井上 豪*; et al.

Journal of Applied Crystallography, 43(4), p.937 - 939, 2010/08

 被引用回数:4 パーセンタイル:48.86(Chemistry, Multidisciplinary)

本論文は蛋白質の大型結晶成長法について報告である。カットしたピペットチップを用いてハンギング蒸気拡散法による結晶化のための大容量ドロップ(最大で200$$mu$$l)を作製する。結晶は蒸気-液体界面において成長する。成長した結晶は液-液接触により、マクロシーディングを繰り返し実施することや、キャピラリーへのマウントが可能となる。この大容量ハンギングドロップ蒸気拡散法を用いて、古細菌${it Aeropyrum pernix}$ K1由来の抗酸化蛋白質(ApTPx)とニワトリ卵白リゾチームの大型結晶を効率的に産生することが可能となった。この手法により得られたApTPxの大型結晶(6.2mm$$^{3}$$)を用いた中性子回折実験の結果、3.5${AA}$分解能を上回る回折点を確認できた。


Structural development of dynamically asymmetric polymer blends under uniaxial stretching

武野 宏之*; 上原 宏樹*; 村上 昌三*; 竹中 幹人*; Kim, M.*; 長澤 尚胤; 佐々木 園*

Journal of Applied Crystallography, 40(s1), p.s656 - s661, 2007/04

 被引用回数:1 パーセンタイル:84.31(Chemistry, Multidisciplinary)



A Focusing-geometry small-angle neutron scattering instrument with a magnetic neutron lens

奥 隆之; 岩瀬 裕希; 篠原 武尚; 山田 悟; 広田 克也*; 小泉 智; 鈴木 淳市; 橋本 竹治; 清水 裕彦

Journal of Applied Crystallography, 40(s1), p.s408 - s413, 2007/04

 被引用回数:24 パーセンタイル:10.74(Chemistry, Multidisciplinary)

中性子磁気レンズを搭載した集光型中性子小角散乱装置を開発した。中性子磁気レンズ(MNL)は、永久磁石NdFeBと高飽和磁化材料パーメンジュールから成る発展型Halbach永久六極磁石である。磁気レンズの内径は35mm$$Phi$$、長さは1200mmであり、その内部に、六強磁場強度分布$$|$$B$$|$$ =(${it C}$/2)${it r}$ $$^{2}$$, ${it C}$=11,500T/m$$^{2}$$が形成される。ここで、$$r$$は磁石中心軸からの距離である。磁気レンズ内表面での中性子の反射を抑制するため、磁気レンズ内表面は中性子吸収材であるCd薄板で覆われているほか、磁気レンズ内部に30mm$$Phi$$のCdスリットが設置されている。よって、実効的な磁気レンズの口径は30mm$$Phi$$である。磁気レンズは、偏極中性子に対してのみ、集光レンズとして機能するので、中性子偏極素子として、磁気スーパーミラーを装置に搭載した。また、中性子磁気レンズで集光した集光中性子ビームは、大面積の$$^3$$He二次元中性子検出器と高分解能シンチレーション二次元中性子検出器を用いて検出される。講演では、本装置の中性子集光光学系の性能と、集光型小角散乱装置の性能について、議論する。


Hierarchical structure of niobate nanosheets in aqueous solution

山口 大輔; 宮元 展義; 小泉 智; 中戸 晃之*; 橋本 竹治

Journal of Applied Crystallography, 40(s1), p.s101 - s105, 2007/04

 被引用回数:18 パーセンタイル:15.02(Chemistry, Multidisciplinary)



A Combined small-angle scattering study of a chemical reaction at specific sites and reaction-induced self-assembly as a problem in open non-equilibrium phenomena

橋本 竹治; 田中 宏和*; 小泉 智; 中 建介*; 中條 善樹*

Journal of Applied Crystallography, 40(s1), p.s73 - s77, 2007/04

 被引用回数:13 パーセンタイル:20.6(Chemistry, Multidisciplinary)



${it In situ}$ and time-resolved ultra small-angle neutron scattering observation on growing poly(methyl methacrylate)-${it block}$-polystyrene ${it via}$ reversible addition-fragmentation chain transfer living radical polymerization

元川 竜平; 小泉 智; Zhao, Y.*; 橋本 竹治

Journal of Applied Crystallography, 40(s1), p.s645 - s649, 2007/04

 被引用回数:7 パーセンタイル:34.89(Chemistry, Multidisciplinary)


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