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論文

中性子回折により検討したTRIP鋼におけるオーステナイトの粒応力とマルテンサイト変態の関係

Harjo, S.; 川崎 卓郎; 土田 紀之*; 諸岡 聡; Gong, W.

鉄と鋼, 107(10), p.887 - 896, 2021/10

In situ neutron diffraction measurements of two low-alloy TRIP steels and a 304-type stainless steel during tensile and creep tests were performed at room temperature. Changes in the diffraction pattern, the peak integrated intensities of austenite ($$gamma$$) and the peak positions of $$gamma$$ were analyzed and discussed to understand a relationship between intergranular stress in $$gamma$$ and the occurrence of martensitic transformation during deformation. From tensile loading, it was found that the susceptibility of martensitic transformation depended on $$gamma$$-($$textit{hkl}$$) grains, in which $$gamma$$-(111) grains underwent martensitic transformation at the latest. The $$gamma$$-($$textit{hkl}$$) dependence in the susceptibility of martensitic transformation was found to be controlled by the shear stress levels in $$gamma$$-($$textit{hkl}$$) grains, which were affected by the intergranular stress partitioning during deformation.

論文

Temperature effects on local structure, phase transformation, and mechanical properties of calcium silicate hydrates

Im, S.*; Jee, H.*; Suh, H.*; 兼松 学*; 諸岡 聡; 小山 拓*; 西尾 悠平*; 町田 晃彦*; Kim, J.*; Bae, S.*

Journal of the American Ceramic Society, 104(9), p.4803 - 4818, 2021/09

 被引用回数:0 パーセンタイル:0.02(Materials Science, Ceramics)

This study aims to elucidate the effect of heating on the local atomic arrangements, structure, phase transformation, and mechanical properties of synthesized calcium-silicate-hydrate (C-S-H). The alteration in the atomic arrangement of the synthesized C-S-H (Ca/Si = 0.8) and the formation of crystalline phases that occurred in three distinct transformation stages of dehydration (105-200 $$^{circ}$$C), decomposition (300-600 $$^{circ}$$C), and recrystallization (700-1000 $$^{circ}$$C) were investigated via powder X-ray diffraction, $$^{29}$$Si nuclear magnetic resonance spectroscopy, and thermogravimetric analysis. Further, the deformation of the local atomic bonding environment and variations in mechanical properties during the three stages were assessed via pair distribution function analysis based on in-situ total X-ray scattering. The results revealed that the C-S-H paste before heating exhibited a lower elastic modulus in real space than that in the reciprocal space in the initial loading stage because water molecules acted as a lubricant in the interlayer. At the dehydration stage, the strain as a function of external loading exhibited irregular deformation owing to the formation of additional pores induced by the evaporation of free moisture. At the decomposition stage, the structural deformation of the main d-spacing (d $$approx$$ 3.0 ${AA}$) was similar to that of the real space before the propagation of microcracks. At the recrystallization stage, the elastic modulus increased to 48 GPa owing to the thermal phase transformation of C-S-H to crystalline $$beta$$-wollastonite. The results provide direct experimental evidence of the micro- and nanostructural deformation behavior of C-S-H pastes after exposure to high temperature under external loading.

論文

Hydrogen permeation property of bulk cementite

足立 望*; 上野 春喜*; 尾上 勝彦*; 諸岡 聡; 戸高 義一*

ISIJ International, 61(8), p.2320 - 2322, 2021/08

 被引用回数:0 パーセンタイル:0(Metallurgy & Metallurgical Engineering)

This study investigated the hydrogen permeation property of cementite by fabricating bulk cementite sample using the process combining the mechanical ball milling and subsequent pulse current sintering. The bulk cementite sample having a 96 vol% of cementite was successfully fabricated. The prepared bulk cementite showed no signal of hydrogen permeation during the 3.5 day of electrochemical hydrogen permeation test. The morphology of blister formed in the sample indicated that diffusion coefficient of hydrogen in cementite is very small.

論文

Work hardening behavior of dual phase copper-iron alloy at low temperature

山下 享介*; 古賀 紀光*; 川崎 卓郎; 諸岡 聡; 友野 翔平*; 梅澤 修*; Harjo, S.

Materials Science & Engineering A, 819, p.141509_1 - 141509_10, 2021/07

 被引用回数:0 パーセンタイル:0(Nanoscience & Nanotechnology)

In-situ neutron diffraction measurements were performed on a cold-rolled copper-iron (Cu-Fe) alloy during tensile tests at 293 K and 150 K. The roles of Cu and Fe on the deformation behavior of alloys were discussed and clarified. The strength and work-hardening rate of the alloy increased with decreasing test temperature. Furthermore, the phase stress of Fe increased considerably with decreasing test temperature; however, the response of this stress to the applied true stress exhibited no dependence on the temperature. The phase stresses of Cu changed only slightly with decreasing test temperature. However, the Cu phase stress response to the applied true stress increased with decreasing test temperature, indicating an increase in the work-hardening rate. The strengthening of Fe and the increase in the work-hardening of Cu contributed to an increase in the strength and work-hardening rate of the Cu-Fe alloy at low temperatures.

論文

Analysis and mapping of detailed inner information of crystalline grain by wavelength-resolved neutron transmission imaging with individual Bragg-dip profile-fitting analysis

櫻井 洋亮*; 佐藤 博隆*; 足立 望*; 諸岡 聡; 戸高 義一*; 加美山 隆*

Applied Sciences (Internet), 11(11), p.5219_1 - 5219_17, 2021/06

 被引用回数:1 パーセンタイル:76.99(Chemistry, Multidisciplinary)

As a new method for evaluating single crystal and oligocrystal, pulsed neutron Bragg-dip transmission analysis/imaging method is being developed. In this study, a single Bragg-dip profile fitting analysis method was newly developed, and applied for analyzing detailed inner information in a crystalline grain position-dependently. In the method, the spectrum profile of a single Bragg-dip is analyzed at each position over a grain. As a result, it is expected that changes of crystal orientation, mosaic spread angle and thickness of a perfect crystal can be evaluated from the wavelength, the width and the integrated intensity of the Bragg-dip, respectively. For confirming this effectiveness, the method was applied to experimental data of position-dependent Bragg-dip transmission spectra of a Si-steel plate consisting of oligocrystals. As a result, inner information of multiple crystalline grains could be visualized and evaluated. The small change of crystal orientation in a grain, about 0.4$$^{circ}$$, could be observed by imaging the Bragg-dip wavelengths. By imaging the Bragg-dip widths, both another grain and mosaic block in a grain were detected. Furthermore, imaging results of the integrated intensities of Bragg-dips were consistent with the results of Bragg-dip width imaging. These small crystallographic changes have not been observed and visualized by previous Bragg-dip analysis methods.

論文

Carbonated nanohydroxyapatite from bone waste and its potential as a super adsorbent for removal of toxic ions

関根 由莉奈; 南川 卓也; 山田 鉄兵*; 松村 大樹; 根本 善弘*; 竹口 雅樹*; 杉田 剛; 下山 巖; 香西 直文; 諸岡 聡

Journal of Environmental Chemical Engineering, 9(2), p.105114_1 - 105114_12, 2021/04

 被引用回数:0 パーセンタイル:0(Engineering, Environmental)

有害金属除去は安心安全社会構築のために必要な技術である。本研究では、骨の有するイオン交換能を最大限に活用して廃材を用いた有害金属除去材料の開発を行った。炭酸塩水溶液に骨を浸漬することで高炭酸含有ナノアパタイトが形成することを見出した。この材料は、通常の骨、また合成アパタイトに比べて約250、4500倍高いストロンチウム吸着性能を示した。本材料は廃材を利用していることから、低コストかつ高性能な吸着剤として活用が期待できる。

論文

Relation between intergranular stress of austenite and martensitic transformation in TRIP steels revealed by neutron diffraction

Harjo, S.; 川崎 卓郎; 土田 紀之*; 諸岡 聡; Gong, W.*

ISIJ International, 61(2), p.648 - 656, 2021/02

 被引用回数:0 パーセンタイル:0(Metallurgy & Metallurgical Engineering)

${it In situ}$ neutron diffraction measurements of two low-alloy steels and a 304-type stainless steel during tensile and creep tests were performed at room temperature. Changes in the diffraction pattern, the integrated peak intensities of austenite ($$gamma$$), and the peak positions of $$gamma$$ were analyzed and discussed to elucidate the relationship between intergranular stress in $$gamma$$ and the occurrence of martensitic transformation during deformation. Tensile loading experiments revealed that the susceptibility to martensitic transformation depended on the $$gamma$$-(hkl) grains, where $$gamma$$-(111) grains underwent martensitic transformation at the latest. The $$gamma$$-hkl dependence of the susceptibility to martensitic transformation was found to be controlled by the shear stress levels in $$gamma$$-(hkl) grains, which were affected by the intergranular stress partitioning during deformation.

論文

Determination of atomistic deformation of tricalcium silicate paste with high-volume fly ash

Jee, H.*; Im, S.*; 兼松 学*; 鈴木 裕士; 諸岡 聡; 小山 拓*; 町田 晃彦*; Bae, S.*

Journal of the American Ceramic Society, 103(12), p.7188 - 7201, 2020/12

 被引用回数:2 パーセンタイル:40.39(Materials Science, Ceramics)

We examined the influence of incorporating high-volume fly ash (FA) on the atomic structure and deformation behavior of calcium silicate hydrates (C-S-H) in tricalcium silicate (C$$_{3}$$H) paste upon exposure to external forces. Atomic structural changes and strains under compressive load were assessed using synchrotron in situ high-energy X-ray scattering-based atomic pair distribution function (PDF) analysis. Three different strain types, namely macroscopic strains, measured by a gauge attached to the specimen, strain in reciprocal space, (Bragg peak shifts), and strain in real space (PDF peak shift), were compared. All monitored and calculated strains for C$$_{3}$$H-FA (50 wt.% FA) paste were compared with those of pure C$$_{3}$$H paste. In the range of $$r$$ $$<$$ 10 ${AA}$, PDF analysis showed that C$$_{3}$$H-FA had a similar atomic structure to synthetic C-S-H followed by pure C$$_{3}$$H paste. The atomic strain of C$$_{3}$$H-FA in real space ($$r$$ $$<$$ 20 ${AA}$) was smaller than that of C$$_{3}$$H under compression, which suggests that the incompressibility of C-S-H on an atomistic scale is enhanced by fly ash incorporation. This may be caused by increased silicate polymerization of C-S-H due to the additional silicate provided by the fly ash.

論文

中性子の利用,2; 大強度陽子加速器(J-PARC)を利用した材料評価

諸岡 聡

保全学, 19(1), p.29 - 34, 2020/04

中性子回折法は中性子の優れた透過能を生かすことで、数十mmメーターオーダーの材料深部の応力・ひずみを非破壊で測定できる唯一の測定技術として知られている。特に、ミクロ応力に起因する弾性ひずみ等の情報を得るうえで、中性子回折法は有効な手段であり、ミクロ組織因子のバルク平均と力学特性との関係を求めて、材料開発や既存材料の信頼性を検討するのに適している。このように、中性子回折法は、従来の残留応力に基づく機械部品等の健全性評価だけでなく、材料の力学特性や機能性向上を目指した材料工学研究などへの応用が期待されている。本稿では、中性子回折法によるひずみ測定原理などの基礎を説明するとともに、代表的な鉄鋼材料について中性子回折法によるその場測定により行われた材料評価研究の一端を紹介し、本手法の将来を展望する。

論文

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.*; 兼松 学*; 城 鮎美*; 町田 晃彦*; 綿貫 徹*; 菖蒲 敬久; 諸岡 聡; Geng, G.*; et al.

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

 被引用回数:4 パーセンタイル:69.91(Construction & Building Technology)

Although the atomistic structure and the deformation characteristics of calcium silicate hydrates (C-S-H) are of primary interest in cement chemistry, they have not been fully investigated. In this study, pair distribution function (PDF) analysis was conducted on a 53-year-old fully hydrated tricalcium silicate (C$$_{3}$$S) paste using in situ synchrotron high-energy X-ray scattering to probe the atomic structural deformation of C-S-H under external loading. The results were compared with those from our previous PDF study of a 131-day-old C$$_{3}$$S paste in order to elucidate the effect of aging on the mechanical characteristics of C-S-H. Three different strains measured by the strain gauge, by the lattice shifts (d-spacing) in the reciprocal space, and by the shift of the interatomic distance (r) in the real space were compared. In the range of r $$<$$ 20 ${AA}$, where most of the information was derived from C-S-H, the 53-year-old C$$_{3}$$S paste had a higher overall elastic modulus (18.3 GPa) and better resistance to compressive stress than the 131-day-old C$$_{3}$$S paste (elastic modulus: 8.3 GPa). Moreover, it was found that the macroscopic strains of the 53-year-old C$$_{3}$$S paste were presumably induced by mechanical deformation such as microcracks at the macroscale. The results provide experimental evidence for the atomistic and mesoscale mechanical behavior of C-S-H in the early and late ages.

論文

Role of retained austenite in low alloy steel at low temperature monitored by neutron diffraction

山下 享介; 諸岡 聡; Harjo, S.; 川崎 卓郎; 古賀 紀光*; 梅澤 修*

Scripta Materialia, 177, p.6 - 10, 2020/03

 被引用回数:13 パーセンタイル:94.74(Nanoscience & Nanotechnology)

${it In situ}$ neutron diffraction measurements during tensile tests at low temperatures of a low alloy steel containing retained austenite have been performed. Evolutions of phase fractions and phase stresses were analyzed and discussed with the progress of deformation. The role of austenite in the steel during deformation at low temperatures was observed not to directly in the contribution to the strengths but in the improvement of the elongation by transformation of austenite to martensite -and in the increasing of the work-hardening rate by an increase in the phase fraction of martensite and the work hardening of martensite.

論文

Real time observation of martensite transformation for a 0.4C low alloyed steel by neutron diffraction

Wang, Y.*; 友田 陽*; 大村 孝仁*; 諸岡 聡; Gong, W.*; Harjo, S.

Acta Materialia, 184, p.30 - 40, 2020/02

 被引用回数:10 パーセンタイル:90.5(Materials Science, Multidisciplinary)

A high-intensity and high-resolution neutron diffractometer with a thermomechanically controlled processing simulator was employed in-situ to investigate martensite transformation behavior with and without ausforming for a medium-carbon low-alloy steel. Serial neutron diffraction profiles have revealed that the transformation behavior could be successfully monitored during quenching with and without the ausforming process. The lattice parameter and the full width at half maximum of austenite peaks significantly decreases and increases upon martensite transformation, respectively. After ausforming, the data reveal that lattice parameters are larger in austenite whereas smaller in martensite compared with those in the non-ausformed case, which is ascribed to the introduced dislocations. The cutting-edge operant quantitative measurements with neutron diffraction for steel production is demonstrated.

論文

Anomalous small-angle X-ray scattering (ASAXS) study of irradiation-induced nanostructure change in Fe-ion beam irradiated oxide dispersion-strengthened (ODS) steel

熊田 高之; 大場 洋次郎; 元川 竜平; 諸岡 聡; 冨永 亜希; 谷田 肇; 菖蒲 敬久; 金野 杏彩; 大和田 謙二*; 大野 直子*; et al.

Journal of Nuclear Materials, 528, p.151890_1 - 151890_7, 2020/01

 被引用回数:0 パーセンタイル:0.01(Materials Science, Multidisciplinary)

ステンレス鋼の放射線照射によるナノ構造変化観測用異常分散X線小角散乱(ASAXS)装置を開発した。イオンビーム照射前後のMA956試料の散乱パターンを比較したところ、Cr析出物の形状は全く変化していないことが判明した。

論文

コンター法を用いた実構造物の残留応力計測

生島 一樹*; 柴原 正和*; 河尻 義貴*; 沖見 優衣*; 内田 友樹*; 秋田 貢一*; 鈴木 裕士; 諸岡 聡

日本船舶海洋工学会論文集, (30), p.123 - 130, 2019/12

本研究では、コンター法を用いてビードオンプレート試験片の残留応力分布を測定した。測定した残留応力分布を中性子回折法で測定した残留応力分布と熱弾性塑性有限要素法で計算した残留応力分布を比較した。その結果、これら3つの方法で得られた残留応力分布は良好に一致していることがわかった。また、実構造物の測定で想定される非対称切削における残留応力を測定するためのコンター法では、切削面上の反力の平衡を考慮した。提案手法をマルチパス溶接継手の残留応力測定に適用した。測定結果から、提案手法は非対称試験片におけるマルチパス溶接継手の残留応力分布を測定できることが示した。

論文

パーライトにおける内部応力の動的緩和と結晶方位関係の選択

雨宮 雄太郎*; 中田 伸生*; 諸岡 聡; 小坂 誠*; 加藤 雅治*

鉄と鋼, 105(2), p.314 - 323, 2019/02

 被引用回数:3 パーセンタイル:37.05(Metallurgy & Metallurgical Engineering)

パーライト変態中の応力緩和機構をより深く理解するために、電子線後方散乱回折法(EBSD)を用いて、セメンタイトの格子定数比を局所分析した。その結果、ラメラ状態のセメンタイトの格子定数比は球状態のセメンタイト粒子と大きく異なることを発見した。これは、パーライト組織がラメラ構造を維持する限り、ある程度の内部応力を保持することを実証した結果である。さらに、パーライト組織中の内部応力は、923Kの等温保持により、鉄原子の界面原子拡散が生じ、徐々に減少することを発見した。しかしながら、マイクロメカニクスを用いたPitsch-Petchの方位関係を満足させたフェライトとセメンタイトを仮定した内部応力の理論計算では、ミスフィット転位や構造レッジの導入により、パーライト変態中に多くの内部応力が緩和するという結果が得られている。つまり、パーライト組織の持つ内部応力は2つの異なるプロセスによって、動的緩和が進行すると考えられる。すなわち、それは、ナノ組織の形成による緩和と、時間に依存した焼鈍による緩和である。また、EBSD分析と中性子回折により測定したセメンタイトの格子定数は、異なる値を示した。これは、パーライトの階層組織に起因した局所情報とバルク平均情報の差異であると考えられる。

論文

原子力材料評価のための最新ナノミクロ分析技術の新展開,2; 中性子回折法による材料強度研究

諸岡 聡; 鈴木 裕士

日本原子力学会誌ATOMO$$Sigma$$, 60(5), p.289 - 293, 2018/05

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、数センチメートルオーダーの材料深部の応力・ひずみを非破壊で測定できる唯一の測定技術であり、種々の機械構造物の製品開発や機械設計、材料開発や既存材料の信頼性評価に大きく貢献できる。本講座では、中性子回折法による応力・ひずみ測定技術の原理および工学回折装置の特徴について述べるとともに、その応用例として、溶接部の残留応力測定、およびステンレス鋼の変形挙動その場観察について紹介する。

論文

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:11 パーセンタイル:78.1(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.

論文

Prediction method of improved residual stress distribution by shot peening using large scale analysis method

生島 一樹*; 柴原 正和*; 西川 聡*; 古川 敬*; 秋田 貢一; 鈴木 裕士; 諸岡 聡

E-Journal of Advanced Maintenance (Internet), 9(3), p.NT87_1 - NT87_5, 2017/11

In this work, an analysis system that can analyze the modification of the residual stress distribution by peening is proposed based on IEFEM. In the proposed analysis system, IEFEM is extended to consider the dynamic effect to analyze the dynamic phenomenon with an impulsive load. The impulsive load due to the collision of shots is modeled as an equivalent load model. The equivalent load model is integrated with IEFEM considering the dynamic effect to calculate spatially and temporally random load in dynamic analyses. Using the proposed analysis system, the residual stress distribution modification by shot peening in a multi-pass welded pipe joint is predicted. The residual stress distributions obtained by the analysis are compared with those measured by X-ray diffraction (XRD), and the effect of the number of shot collisions on the change in residual stress distribution is discussed.

論文

Changes of dislocation density and dislocation arrangement during tensile deformation in lath martensitic steels

Harjo, S.; 川崎 卓郎; 諸岡 聡

Advanced Experimental Mechanics, 2, p.112 - 117, 2017/10

To understand strengthening mechanism in lath martensitic steels, in situ neutron diffractions during tensile deformation for 22SiMn2TiB steel and Fe-18Ni alloy were performed using TAKUMI of J-PARC. Profile analyses were performed using Convolutional Multiple Whole Profile (CMWP) fitting and Williamson-Hall (W-H) methods. As results, the dislocation densities as high as 10$$^{15}$$ m$$^{-2}$$ in the as-quenched states of both steels were determined hardly to change or slightly increase by the CMWP method. The reliability of the dislocation density obtained from the W-H method was low, because the whole profile was not considered for the analysis. In the former method, the values of parameter M related to dislocations arrangement was found to decrease rapidly for both steels at the beginning of plastic deformation. Hence, high work hardening in the lath martensitic steels was considered due to the dislocations rearrangements with plastic deformation.

論文

Study on shot peened residual stress distribution under cyclic loading by numerical analysis

生島 一樹*; 木谷 悠二*; 柴原 正和*; 西川 聡*; 古川 敬*; 秋田 貢一; 鈴木 裕士; 諸岡 聡

溶接学会論文集(インターネット), 35(2), p.75s - 79s, 2017/06

In this research, to investigate the effect of shot peening on operation, an analysis method to predict the behavior of stress distribution on shot peening was proposed. In the proposed system, the load distribution on the collision of shots was modeled, and it was integrated with the dynamic analysis method based on the Idealized explicit FEM (IEFEM). The thermal elastic plastic analysis method using IEFEM was applied to the analysis of residual stress distribution of multi-pass welded pipe joint. The computed residual stress distribution was compared with the measured residual stress distribution using X-ray diffraction (XRD). As a result, it was shown that the both welding residual stress distribution agree well with each other. Considering the computed welding residual stress distribution, the modification of stress distribution due to shot peening was predicted by the proposed analysis system.

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