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論文

Quantitative analysis of microstructure evolution, stress partitioning and thermodynamics in the dynamic transformation of Fe-14Ni alloy

Li, L.*; 宮本 吾郎*; Zhang, Y.*; Li, M.*; 諸岡 聡; 及川 勝成*; 友田 陽*; 古原 忠*

Journal of Materials Science & Technology, 184, p.221 - 234, 2024/06

Dynamic transformation (DT) of austenite ($$gamma$$) to ferrite ($$alpha$$) in the hot deformation of various carbon steels was widely investigated. However, the nature of DT remains unclear due to the lack of quantitative analysis of stress partitioning between two phases and the uncertainty of local distribution of substitutional elements at the interface in multi-component carbon steels used in the previous studies. Therefore, in the present study, a binary Fe-Ni alloy with $$alpha$$+$$gamma$$ duplex microstructure in equilibrium was prepared and isothermally compressed in $$alpha$$+$$gamma$$ two-phase region to achieve quantitative analysis of microstructure evolution, stress partitioning and thermodynamics during DT. $$gamma$$ to $$alpha$$ DT during isothermal compression and $$alpha$$ to $$gamma$$ reverse transformation on isothermal annealing under unloaded condition after deformation were accompanied by Ni partitioning. The lattice strains during thermomechanical processing were obtained via in-situ neutron diffraction measurement, based on which the stress partitioning behavior between $$gamma$$ and $$alpha$$ was discussed by using the generalized Hooke's law. A thermodynamic framework for the isothermal deformation in solids was established based on the basic laws of thermodynamics, and it was shown that the total Helmholtz free energy change in the deformable material during the isothermal process should be smaller than the work done to the deformable material. Under the present thermodynamic framework, the microstructure evolution in the isothermal compression of Fe-14Ni alloy was well explained by considering the changes in chemical free energy, plastic and elastic energies and the work done to the material. In addition, the stabilization of the soft $$alpha$$ phase in Fe-14Ni alloy by deformation was rationalized since the $$gamma$$ to $$alpha$$ transformation decreased the total Helmholtz free energy by decreasing the elastic and dislocation energies.

論文

${it In situ}$ neutron diffraction revealing the achievement of excellent combination of strength and ductility in metastable austenitic steel by grain refinement

Mao, W.; Gong, W.; Harjo, S.; 諸岡 聡; Gao, S.*; 川崎 卓郎; 辻 伸泰*

Journal of Materials Science & Technology, 176, p.69 - 82, 2024/03

Fe-24Ni-0.3C(wt.%)準安定オーステナイト鋼の降伏応力は、平均結晶粒径が35$$mu$$m(粗粒[CG])から0.5$$mu$$m(超微細粒[UFG])に減少すると3.5倍(158$$rightarrow$$551MPa)に増加したが、引張伸びは大きく維持された(0.87$$rightarrow$$0.82)。結晶粒径が力学特性と変形機構に及ぼす影響を定量的に明らかにするため、室温での引張変形中にCGとUFG Fe-24Ni-0.3C鋼のその場中性子回折測定を行った。CGとUFG試料における塑性変形の初期段階は転位すべりによって支配され、変形後期には変形誘起マルテンサイト変態(DIMT)も生じた。結晶粒の微細化により、DIMTの開始応力が大きく増加し、ひずみに関するDIMTの速度が抑制されることがわかった。結果として、(i)結晶粒微細化によりオー ステナイトが安定化し、DIMTに対して最も安定な結晶粒である$$<$$111$$>$$//LD(LD:負荷方向)オーステナイト粒でのDIMTの開始が大幅に遅れた。その結果、UFG試験片の$$<$$111$$>$$//LDオーステナイト粒のほとんどはマルテンサイトに変態しなかった。(ii)結晶粒の微細化は、マルテンサイト変態の自己促進効果も抑制した。それにもかかわらず、UFG試験片の変態速度が低いDIMTは、CG試験片のより応力を増加させるのに効率がよく、変形中に均一な変形を維持するのに適していた。以上の現象は、UFG準安定オーステナイト鋼の優れた強度と延性の両立に相互に寄与している。

論文

Stress measurement of stainless steel piping welds by complementary use of high-energy synchrotron X-rays and neutrons

三浦 靖史*; 鈴木 賢治*; 諸岡 聡; 菖蒲 敬久

Quantum Beam Science (Internet), 8(1), p.1_1 - 1_14, 2024/03

Probabilistic fracture mechanics (PFM) is expected as a reasonable structural integrity assessment method for nuclear components such as piping, whose main degradation phenomenon is stress corrosion cracking (SCC). Some input parameters are necessary for PFM analysis, and welding residual stress is one of the most important parameters because welding residual stress affects SCC initiation and propagation. Recently, a double exposure method (DEM) with synchrotron X-ray has been proposed, and the method is an expected candidate for the measurement of welding residual stress with a high spatial resolution. In this paper, the DEM was applied to measure the residual stress of the plate specimen, which was cut from the welded pipe using electrical discharge machining, and detailed stress maps under a plane stress state were obtained. Furthermore, the residual stress distributions of the welded pipe under a triaxial stress state were also evaluated using neutron diffraction. From these results, the method for obtaining a detailed stress map of the welded pipe by the complementary use of high-energy synchrotron radiation X-rays and neutrons was proposed.

論文

Martensitic transformation behavior of Fe-Ni-C alloys monitored by ${it in-situ}$ neutron diffraction during cryogenic cooling

山下 享介*; Harjo, S.; 川崎 卓郎; 諸岡 聡; Gong, W.; 藤井 英俊*; 友田 陽*

ISIJ International, 64(2), p.192 - 201, 2024/01

${it In situ}$ neutron diffraction measurements were performed on Fe-33Ni-0.004C alloy (33Ni alloy) and Fe-27Ni-0.5C alloy (27Ni-0.5C alloy) during cooling from room temperature to the cryogenic temperature (4 K) to evaluate changes in the lattice constants of austenite and martensite, and changes in the tetragonality of martensite due to thermally induced martensitic transformation. As the martensitic transformation progressed, the lattice constants of austenite in both alloys deviated to smaller values than those predicted considering the thermal shrinkage, accompanied by an increase in the full width at half maximum of austenite. The fresh martensite formed in both alloys had a body-centered tetragonal (BCT) structure, regardless of the carbon content. The tetragonality of martensite decreased with progressive martensitic transformation during cooling in the 33Ni alloy, but was almost constant in the 27Ni-0.5C alloy. This suggests that carbon is necessary to maintain the tetragonality of martensite during cooling. The tetragonality of martensite in the 27Ni-0.5C alloy decreased during room temperature aging because of carbon mobility.

論文

Key role of temperature on delamination in solid-state additive manufacturing via supersonic impact

Wang, Q.*; Ma, N.*; Huang, W.*; Shi, J.*; Luo, X.-T.*; 冨高 宙*; 諸岡 聡; 渡邊 誠*

Materials Research Letters (Internet), 11(9), p.742 - 748, 2023/09

Cold spray (CS) has emerged as a representative of solid-state additive manufacturing (AM) via supersonic impact. It enables a high deposition rate of solid-state microparticles. Delamination, however, tends to occur when depositing too thick; this remains to be conquered. Here, a CS-like process, warm spray (WS), was presented. Interestingly, it was found that the appropriate increase in particle temperature can effectively reduce the residual stress amplitude, relieving the concentrated tensile stress and safeguarding the additively manufactured components from interfacial delamination even when depositing too thick. The key role of temperature on delamination was identified in solid-state AM via supersonic impact.

論文

Lattice parameters of austenite and martensite during transformation for Fe-18Ni alloy investigated through ${it in situ}$ neutron diffraction

Gong, W.; Harjo, S.; 友田 陽*; 諸岡 聡; 川崎 卓郎; 柴田 曉伸*; 辻 伸泰*

Acta Materialia, 250, p.118860_1 - 118860_16, 2023/05

 被引用回数:0 パーセンタイル:77.63(Materials Science, Multidisciplinary)

Martensitic transformation is accompanied by the generation of microscale and macroscale internal stresses during cooling below the martensitic transformation start temperature. These internal stresses have been determined through X-ray or neutron diffraction, but the reported results are not consistent, probably because the measured lattice parameter is influenced not only by the internal stress but also by several factors, including solute elements and crystal defects. Therefore, ${it in situ}$ neutron diffraction combined with dilatometry measurements during martensitic transformation and subsequent cyclic tempering were performed for an Fe-18Ni alloy. The phase strains calculated by lattice parameter variations show that a hydrostatic compressive strain in austenite and a tensile strain in martensite arose as the martensitic transformation progressed during continuous cooling or isothermal holding. However, the phase stresses of austenite and martensite estimated from these strains failed to hold stress balance law when dense crystal defects involved in the processes. After these crystal defects were removed by appropriate tempering, the stress balance law held well. Meanwhile, the phase stresses of austenite and martensite were changed to opposite, revealing their true identity. Various crystal defects in austenite and martensite, introduced by plastic accommodation, were suggested to affect their lattice parameters and then their phase stresses.

論文

Accuracy of measuring rebar strain in concrete using a diffractometer for residual stress analysis

安江 歩夢*; 川上 真由*; 小林 謙祐*; Kim, J.; 宮津 裕次*; 西尾 悠平*; 向井 智久*; 諸岡 聡; 兼松 学*

Quantum Beam Science (Internet), 7(2), p.15_1 - 15_14, 2023/05

Neutron diffraction is a noncontact method that can measure the rebar strain inside concrete. In this method, rebar strain and stress are calculated using the diffraction profile of neutrons irradiated during a specific time period. In general, measurement accuracy improves with the length of the measurement time. However, in previous studies, the measurement time was determined empirically, which makes the accuracy and reliability of the measurement results unclear. In this study, the relationship between the measurement time and the measurement standard deviation was examined for reinforced concrete specimens under different conditions. The aim was to clarify the accuracy of the measurement of rebar stress using the neutron diffraction method. It was found that if the optical setup of the neutron diffractometer and the conditions of the specimen are the same, there is a unique relationship between the diffraction intensity and the rebar stress standard deviation. Furthermore, using this unique relationship, this paper proposes a method for determining the measurement time from the allowable accuracy of the rebar stress, which ensures the accuracy of the neutron diffraction method.

論文

放射光X線と中性子を相補的に用いた小口径突合せ溶接配管の実応力解析

鈴木 賢治*; 三浦 靖史*; 城 鮎美*; 豊川 秀訓*; 佐治 超爾*; 菖蒲 敬久; 諸岡 聡

材料, 72(4), p.316 - 323, 2023/04

Residual stresses in small-bore butt-welded pipe of austenitic stainless steel have never been measured. It is difficult to obtain a detailed residual stress map of the root welded part, because the gauge volume in neutron diffraction is large. The stress evaluation of the welded part by synchrotron X-rays was also difficult due to the dendritic structure. In this study, a double exposure method (DEM) with high-energy synchrotron X-rays was applied to measuring the details of the residual stress of the welded part, and we succeeded in obtaining the detailed axial and radius stress maps of the root welded part of the plate cut from the welded pipe, though the stress map was under the plane stress condition. The hoop stress map of the butt-welded pipe was obtained using the strain scanning method with neutrons under the triaxial stress state. The axial and radius stress maps under triaxial stress state were made up using the complementary use of the synchrotron X-ray and neutron. As a result, the detailed stress maps of the root welded part of the butt-welded pipe were obtained. The obtained map sufficiently explained the initiation and propagation of SCC.

論文

Insight on the mechanical properties of hierarchical porous calcium-silicate-hydrate pastes according to the Ca/Si molar ratio using ${it in situ}$ synchrotron X-ray scattering and nanoindentation test

Im, S.*; Jee, H.*; Suh, H.*; 兼松 学*; 諸岡 聡; Choe, H.*; 西尾 悠平*; 町田 晃彦*; Kim, J.*; Lim, S.*; et al.

Construction and Building Materials, 365, p.130034_1 - 130034_18, 2023/02

 被引用回数:3 パーセンタイル:58.24(Construction & Building Technology)

Nanocrystalline calcium-silicate-hydrate (C-S-H) is a typical heterogeneous material with a multiscale structure spanning a wide length scale from angstrom to micrometer, and whose structure is determined by the Ca/Si ratio. In this study, we directly applied compressive loads on synthetic C-S-H pastes with Ca/Si ratios of 0.6-1.2 and investigated their mechanical properties using the elastic modulus calculated at three length scale levels (i.e., angstrom to nanometer, micrometer, and millimeter) via in-situ synchrotron X-ray scattering, nanoindentation tests, and strain gauges, respectively. Further, $$^{29}$$Si nuclear magnetic resonance spectroscopy was conducted on the C-S-H pastes to elucidate the alterations in the silicate polymerization. The experimental results confirmed the deformation behavior of the C-S-H paste with different Ca/Si ratios under external loading, which was demonstrated to be transferred from the surface of the pastes to particles owing to the presence of multiscale pores.

論文

Microstructure and plasticity evolution during L$"u$ders deformation in an Fe-5Mn-0.1C medium-Mn steel

小山 元道*; 山下 享介*; 諸岡 聡; 澤口 孝宏*; Yang, Z.*; 北條 智彦*; 川崎 卓郎; Harjo, S.

ISIJ International, 62(10), p.2036 - 2042, 2022/10

 被引用回数:4 パーセンタイル:67.13(Metallurgy & Metallurgical Engineering)

The local plasticity and associated microstructure evolution in Fe-5Mn-0.1C medium-Mn steel (wt.%) were investigated in this study. Specifically, the micro-deformation mechanism during L$"u$ders banding was characterized based on multi-scale electron backscatter diffraction measurements and electron channeling contrast imaging. Similar to other medium-Mn steels, the Fe-5Mn-0.1C steel showed discontinuous macroscopic deformation, preferential plastic deformation in austenite, and deformation-induced martensitic transformation during L$"u$ders deformation. Hexagonal close-packed martensite was also observed as an intermediate phase. Furthermore, an in-situ neutron diffraction experiment revealed that the pre-existing body-centered cubic phase, which was mainly ferrite, was a minor deformation path, although ferrite was the major constituent phase.

論文

Hierarchical deformation heterogeneity during L$"u$ders band propagation in an Fe-5Mn-0.1C medium Mn steel clarified through ${it in situ}$ scanning electron microscopy

小山 元道*; 山下 享介*; 諸岡 聡; Yang, Z.*; Varanasi, R. S.*; 北條 智彦*; 川崎 卓郎; Harjo, S.

ISIJ International, 62(10), p.2043 - 2053, 2022/10

 被引用回数:2 パーセンタイル:34.75(Metallurgy & Metallurgical Engineering)

${it In situ}$ deformation experiments with cold-rolled and intercritically annealed Fe-5Mn-0.1C steel were carried out at ambient temperature to characterize the deformation heterogeneity during L$"u$ders band propagation. Deformation band formation, which is a precursor phenomenon of L$"u$ders band propagation, occurred even in the macroscopically elastic deformation stage. The deformation bands in the L$"u$ders front grew from both the side edges to the center of the specimen. After macroscopic yielding, the thin deformation bands grew via band branching, thickening, multiple band initiation, and their coalescence, the behavior of which was heterogeneous. Thick deformation bands formed irregularly in front of the region where the thin deformation bands were densified. The thin deformation bands were not further densified when the spacing of the bands was below $$sim$$10 $$mu$$m. Instead, the regions between the deformation bands showed a homogeneous plasticity evolution. The growth of the thin deformation bands was discontinuous, which may be due to the presence of ferrite groups in the propagation path of the deformation bands. Based on these observations, a model for discontinuous L$"u$ders band propagation has been proposed.

論文

Revisit deformation behavior of lath martensite

Harjo, S.; Gong, W.; 川崎 卓郎; 諸岡 聡; 山下 享介*

ISIJ International, 62(10), p.1990 - 1999, 2022/10

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

Two mechanisms inconsistent each other, a relaxation of type II internal stress and a presence of mobile dislocation, were previously proposed to describe the low elastic limit of as-quenched lath martensite steels. In this study, neutron diffraction experiments were performed to revisit the deformation behavior of lath martensite steel. The highly dense random arrangement dislocations easily moved at the beginning of deformation, then accumulated, annihilated and changed the arrangement differently depending on the orientation of the packet with respect to the deformation direction. The movement of highly dense random arrangement dislocations played an important role as a mechanism at the beginning of deformation, and can be a true feature of mobile dislocations.

論文

Effect of magnesium silicate hydrate (M-S-H) formation on the local atomic arrangements and mechanical properties of calcium silicate hydrate (C-S-H); In situ X-ray scattering study

Kim, G.*; Im, S.*; Jee, H.*; Suh, H.*; Cho, S.*; 兼松 学*; 諸岡 聡; 小山 拓*; 西尾 悠平*; 町田 晃彦*; et al.

Cement and Concrete Research, 159, p.106869_1 - 106869_17, 2022/09

 被引用回数:3 パーセンタイル:85.78(Construction & Building Technology)

This study explored the effect of M-S-H formation on the local atomic arrangements and mechanical properties of C-S-H. The elastic moduli of the samples were calculated using shifted atomic distances (r) and d-spacings (d) acquired by applying an external load on the pastes during X-ray scattering experiments. The experimental results indicated that the crystal structure of C-S-H remained intact with MgCl$$_{2}$$ addition. At the highest Mg/Si ratio (Ca/Si = 0.6, Mg/Si = 0.2), change in the dominant phase occurred from C-S-H to M-S-H because the low pH environment hindered the formation of C-S-H and facilitated the formation of M-S-H. The elastic modulus decreased with increasing Mg/Si ratio up to 0.1 owing to both C-S-H destabilization and low M-S-H content in the samples. Conversely, the elastic modulus increased in the paste synthesized with the highest Mg/Si ratio because considerable M-S-H had formed, which exhibited a higher elastic modulus than C-S-H.

論文

異形鉄筋の表面形状が鉄筋コンクリートの付着性能に及ぼす影響

小林 謙祐*; 安江 歩夢*; 諸岡 聡; 兼松 学*

コンクリート工学年次論文集(DVD-ROM), 44(1), p.208 - 213, 2022/07

異形鉄筋の表面形状がコンクリートとの付着性能に及ぼす影響を明らかにすることを目的とし、引抜試験および中性子回折法による鉄筋応力測定を実施した。実験結果より、引抜試験における付着応力-自由端すべり量曲線では、表面形状の違いによって大きく異なる結果となった。一方、鉄筋応力の測定では、各水準の応力分布に差異は見られなかった。したがって、鉄筋に自由端すべりが生じる条件下においては、鉄筋の表面形状が付着性能に影響を及ぼすことが推察された。

論文

Deformation texture of bulk cementite investigated by neutron diffraction

足立 望*; 上野 春喜*; 諸岡 聡; 徐 平光; 戸高 義一*

Materials, 15(13), p.4485_1 - 4485_7, 2022/07

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

Understanding of deformation mechanism of cementite such as slip plane are quite important to reveal and improve mechanical property of steels. However, deformation behavior of cementite has not been well investigated because of the difficulty of sample preparation having single phase cementite structure. In this study, by fabricating bulk single phase cementite samples using the method developed by the authors, deformation texture formed by uniaxial compression was investigated using both electron back scatter diffraction and the neutron diffraction. The fabricated sample had a random texture before the compression. After applying compressive strain of 0.5 at 833 K, (010) fiber texture was formed along compressive axis. It has been suggested from this trend that the primary slip plane of cementite is (010).

論文

Volatilization of B$$_{4}$$C control rods in Fukushima Daiichi nuclear reactors during meltdown; B-Li isotopic signatures in cesium-rich microparticles

笛田 和希*; 高見 龍*; 蓑毛 健太*; 諸岡 和也*; 堀江 憲路*; 竹原 真美*; 山崎 信哉*; 斉藤 拓巳*; 塩津 弘之; 大貫 敏彦*; et al.

Journal of Hazardous Materials, 428, p.128214_1 - 128214_10, 2022/04

 被引用回数:4 パーセンタイル:64.87(Engineering, Environmental)

Boron carbide control rods remain in the fuel debris of the damaged reactors in the Fukushima Daiichi Nuclear Power Plant, potentially preventing re-criticality; however, the state and stability of the control rods remain unknown. Sensitive high-resolution ion microprobe analyses have revealed B-Li isotopic signatures in radioactive Cs-rich microparticles (CsMPs) that formed by volatilization and condensation of Si-oxides during the meltdowns. The CsMPs contain 1518-6733 mg kg$$^{-1}$$ of $$^{10+11}$$B and 11.99-1213 mg kg$$^{-1}$$ of Li. The $$^{11}$$B/$$^{10}$$B (4.15-4.21) and $$^{7}$$Li/$$^{6}$$Li (213-406) isotopic ratios are greater than natural abundances ($$sim$$4.05 and $$sim$$12.5, respectively), indicating that $$^{10}$$B(n,$$alpha$$)$$^{7}$$Li reactions occurred in B$$_{4}$$C prior to the meltdowns. The total amount of B released with CsMPs was estimated to be 0.024-62 g, suggesting that essentially all B remains in reactor Units 2 and/or 3 and is enough to prevent re-criticality; however, the heterogeneous distribution of B needs to be considered during decommissioning.

論文

Dynamic accommodation of internal stress and selection of crystallographic orientation relationship in pearlite

雨宮 雄太郎*; 中田 伸生*; 諸岡 聡; 小坂 誠*; 加藤 雅治*

ISIJ International, 62(2), p.282 - 290, 2022/02

 被引用回数:2 パーセンタイル:34.75(Metallurgy & Metallurgical Engineering)

To gain a deeper understanding of the dynamic accommodation mechanism of the internal stress in pearlite originating from the lattice misfit between ferrite and cementite phases, the lattice parameter ratios of cementite, b$$theta$$/a$$theta$$ and c$$theta$$/a$$theta$$, were locally analyzed in detail using the electron backscatter diffraction (EBSD) technique. The EBSD analysis revealed that the lattice parameter ratios of the cementite lamellae clearly differed from those of the spheroidized cementite particles, indicating that pearlite has a certain amount of internal stress as long as it maintains a lamellar structure. The internal stress in pearlite gradually decreased during the isothermal holding at 923 K after the pearlitic transformation due to the interfacial atomic diffusion of Fe atoms. However, a comparison with the theoretical values obtained from the Pitsch-Petch orientation relationship revealed that a large amount of internal stress had been already accommodated during the pearlitic transformation by the introduction of misfit dislocations and structural ledges on ferrite/cementite lamellar interfaces, i.e., the internal stress of pearlite is dynamically reduced by two different processes; built-in accommodation upon pearlitic transformation and additional time-dependent relaxation after pearlitic transformation. On the other hand, the analysis of the EBSD and neutron diffraction results yielded intriguingly different lattice parameters of cementite, indicating that various crystallographic orientation relationships between ferrite and cementite coexist in pearlite. Furthermore, the elastic strain energy analysis suggests that the invariant-line criterion on the ferrite/cementite interface plays an important role for the selection of orientation relationships in pearlite.

論文

Characterization of deformation by cold rolling in ferritic steel containing Cu particles using neutron transmission analysis

大場 洋次郎; 諸岡 聡; 大石 一城*; 鈴木 淳市*; 土山 聡宏*

ISIJ International, 62(1), p.173 - 178, 2022/01

 被引用回数:1 パーセンタイル:34.75(Metallurgy & Metallurgical Engineering)

Neutron transmission spectra of Cu steel were measured to characterize the change of microstructures by cold rolling. Bragg edges in neutron attenuation coefficients indicate the rotation of {110} planes of ferrite grains and is useful to characterize the evolution of preferred orientations with the cold rolling. In addition, SANS contribution in the neutron attenuation coefficients provides the nanostructural information about the deformation of the Cu precipitates. These results demonstrate that the neutron transmission analysis is beneficial for microstructural characterization in steels.

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

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

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:8 パーセンタイル:84.8(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.

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