Language：English   Publishing type：Research paper (scientific journal)   Publisher：The Japan Institute of Metals and Materials  

<p>In Al-Zn-Mg alloy, hydrogen (H) leads remarkably to the degradation of mechanical properties. It is indispensable to suppress this phenomenon called hydrogen embrittlement (HE) for developing the high-strength Al-Zn-Mg alloy. Because intergranular fracture (IGF) is mainly observed when HE occurs in the alloy, we need to understand the initiation behavior of IGF in order to suppress HE. Heterogeneous distribution of stress, strain and H concentration usually influence the IGF initiation in polycrystalline material. In the present study, we investigated distribution of stress, strain, and H concentration in actual fractured regions by simulation employing a crystal plasticity finite element method and H diffusion analysis in a 3D image-based model, which was created based on 3D polycrystalline microstructure data obtained from X-ray imaging technique. Combining the simulation and <i>in-situ</i> observation of the tensile test sample by X-ray CT, we examined the distribution of stress, strain, and H concentration in actual crack initiation behavior. Based on this, the condition for intergranular crack initiation were discussed. As a result, it is revealed that stress normal to grain boundary induced by crystal plasticity dominates intergranular crack initiation. In contrast, accumulation of internal H due to the stress has little impact on crack initiation.</p><p> </p><p>This Paper was Originally Published in Japanese in J. JILM <b>73</b> (2023) 530–536. Abstract was slightly modified.</p>

DOI： 10.2320/matertrans.mt-l2024007

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<p>Recent research has shown that some intermetallic compound particles with high interfacial hydrogen trap energies (e.g., Mg₂Si) are prone to damage at high hydrogen concentrations. In this study, the acceleration of particle damage in an A6061 alloy was observed <i>in-situ</i> via X-ray CT. The damage behavior of the particles that are located in the crack tip stress field, where high stress triaxiality causes a local increase in the hydrogen concentration, was analyzed. The influence of hydrogen on the damage behavior of the dispersed Mg₂Si particles was investigated by preparing a material charged with hydrogen to achieve extremely high hydrogen concentration, and further hydrogen enrichment in a crack tip region was also utilized. Interfacial debonding of Mg₂Si particles was frequently observed in the vicinity of a crack tip immediately prior to tensile fracture. Even though the fracture is typical of ductile fracture, hydrogen accelerates particle damage and reduces the macroscopic ductility of the aluminum alloy. This can be considered as a form of hydrogen embrittlement of aluminum alloys. Even in materials with relatively low hydrogen concentrations (0.85 mass ppm), interfacial debonding occurred in the hydrogen-enriched crack tip regions. A higher hydrogen concentration promoted interfacial debonding over a wider range of particle sizes and particle shapes. It can be inferred that localized hydrogen enrichment, which is expected to occur due to external hydrogen exposure, stress corrosion cracking, corrosion or crack tips, can directly contribute to debonding at the Mg₂Si particle/aluminum matrix interface. According to the analysis, reduction of the diameter and simplification of the shape of Mg₂Si particles are effective method for suppressing such hydrogen-induced debonding.</p>

DOI： 10.2320/matertrans.mt-m2024026

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Language：English   Publishing type：Research paper (scientific journal)   Publisher：Elsevier BV  

DOI： 10.1016/j.commatsci.2024.113115

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DOI： 10.1016/j.msea.2024.146607

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DOI： 10.1016/j.ijhydene.2024.05.146

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Language：Japanese   Publishing type：Research paper (scientific journal)   Publisher：The Japan Institute of Metals and Materials  

<p>The surrogate-based microstructural optimization was applied to describe the relationship between local crystallographic microstructure and intergranular hydrogen embrittlement in an Al-Zn-Mg alloy. The support vector machine with an infill sampling criterion was used to realise high-accuracy optimisation with a limited size of data set. The methodology integrates thoroughgoing microstructural quantification, a couple of coarsening processes and the surrogate modelling. An objective function was defined together with 66 design parameters, which quantitatively express the size, shape, orientation and damage during specimen machining for surface grain boundaries and grains. The number of design parameters was then reduced from 66 to 3 during the two-step coarsening process. It has been clarified that intergranular crack initiation is described using the simple size of grains and grain boundaries together with grain boundary orientation with respect to the loading direction. It can be inferred that those design parameters are of crucial importance for crack initiation through the elevation in stress normal to grain boundaries. Correlation between the selected design parameters and crack initiation was rather weak compared to the past application of a similar technique to particle damage. The reason for this was discussed. The present approach offers a cost-efficient solution for the prevention of hydrogen embrittlement through 3D design of crystallographic microstructure, which cannot be obtained with the conventional approaches for developing materials.</p><p> </p><p>Mater. Trans. <b>64</b> (2023) 2729-2738に掲載</p>

DOI： 10.2320/jinstmet.j2023028

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Stress corrosion cracking (SCC) behaviors induced by the combination of external and internal hydrogen (H) in an Al-Zn-Mg-Cu alloy were systematically investigated via in-situ 3D characterization techniques. SCC of the Al-Zn-Mg-Cu alloy could initiate and propagate in the potential crack region where the H concentration exceeded a critical value, in which the nanoscopic H-induced decohesion of η-MgZn2 precipitates resulted in macroscopic cracking. External H that penetrated the alloy from the environment played a crucial role during the SCC of the Al-Zn-Mg-Cu alloy by generating gradient-distributed H-affected zones near the crack tips, which made Al alloys in water environment more sensitive to SCC. Additionally, the pre-existing internal H was driven toward the crack tips during plastic deformation. It was involved in the SCC and made contributions to both the cracks initiation and propagation.

DOI： 10.1016/j.scriptamat.2023.115804

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Language：Others   Publishing type：Research paper (scientific journal)   Publisher：Japan Institute of Metals  

DOI： 10.2320/matertrans.mt-l2023017

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Language：English   Publishing type：Research paper (scientific journal)   Publisher：The Japan Institute of Metals and Materials  

Dominant Factors Controlling the Initiation of Hydrogen Embrittlement in Al-Zn-Mg Alloy

DOI： 10.2320/matertrans.MT-M2023116

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Language：Japanese   Publisher：The Japan Institute of Light Metals  

<p>In Al-Zn-Mg alloy, hydrogen leads to degradation of mechanical properties. It is indispensable to suppress this phenomenon called hydrogen embrittlement (HE) for increasing the strength of Al-Zn-Mg alloy. Intergranular fracture (IGF) mainly occurs when HE affects this alloy. In order to suppress HE, we need to understand the initiation behavior of IGF. Heterogeneous distribution of stress, strain and hydrogen concentration in polycrystalline material have an influence on the IGF initiation. In the present study, distribution of stress, strain and hydrogen concentration in actual fractured regions were investigated by employing a crystal plasticity finite element method and hydrogen diffusion analysis using a 3D-image-based model. This model was created based on 3D polycrystalline microstructure data obtained from X-ray imaging technique. By combining in-situ observation of tensile test of the same sample by X-ray CT with the simulation, we compared distribution of stress, strain and hydrogen concentration with actual crack initiation behavior. Based on this, the condition for intergranular crack initiation were discussed. As a result, it is revealed that stress load perpendicular to grain boundary induced by crystal plasticity dominate intergranular crack initiation. In addition, accumulation of internal hydrogen induced by crystal plasticity had little impact on crack initiation.</p>

DOI： 10.2464/jilm.73.530

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DOI： 10.1016/j.actamat.2023.119188

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Language：Japanese   Publishing type：Research paper (scientific journal)   Publisher：The Japan Institute of Light Metals  

Growth behavior of pores and hydrogen desorption behavior in pure aluminum and A6061 aluminum alloys

DOI： 10.2464/jilm.73.212

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Language：English   Publishing type：Research paper (scientific journal)   Publisher：Association for Materials Protection and Performance ({AMPP})  

<jats:p>7xxx aluminum alloys are representative high-strength aluminum alloys; however, mechanical property degradation due to hydrogen hinders further strengthening. We have previously reported that hydrogen embrittlement in 7xxx alloys originates from trapped hydrogen at the MgZn2 precipitate interface, providing high hydrogen trapping energy. We propose the dispersion of Mn-based second-phase particles as a novel technique for preventing 7xxx aluminum alloy hydrogen embrittlement. In this study, the deformation and fracture behaviors of high hydrogen 7xxx alloys containing 0.0% Mn and 0.6% Mn are observed in situ using synchrotron radiation X-ray tomography. Although no significant differences appear between the two alloys regarding the initiation of quasicleavage cracks, the area fractions of final quasicleavage fractures are 16.5% and 1.0% for 0.0%Mn and 0.6%Mn alloys, respectively; this finding indicates that the Mn addition reduces hydrogen-induced fractures. The obtained macroscopic hydrogen embrittlement is quantitatively analyzed based on hydrogen partitioning in alloys. Adding 0.6% Mn, generating second-phase particles with high hydrogen trapping abilities, significantly suppresses hydrogen-induced quasicleavage fracture. The results of an original hydrogen partitioning analysis show that the dispersion of Mn-based particles (Al12Mn3Si) with high hydrogen trapping abilities reduces the hydrogen concentration at the semicoherent MgZn2 interface and suppresses hydrogen embrittlement.</jats:p>

DOI： 10.5006/4300

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DOI： 10.1016/j.ijfatigue.2022.107428

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Hydrogen drastically embrittles high-strength aluminum alloys, which impedes efforts to develop ultrastrong components in the aerospace and transportation industries. Understanding and utilizing the interaction of hydrogen with core strengthening elements in aluminum alloys, particularly nanoprecipitates, are critical to break this bottleneck. Herein, we show that hydrogen embrittlement of aluminum alloys can be largely suppressed by switching nanoprecipitates from the η phase to the T phase without changing the overall chemical composition. The T phase strongly traps hydrogen and resists hydrogen-assisted crack growth, with a more than 60% reduction in the areal fractions of cracks. The T phase-induced reduction in the concentration of hydrogen at defects and interfaces, which facilitates crack growth, primarily contributes to the suppressed hydrogen embrittlement. Transforming precipitates into strong hydrogen traps is proven to be a potential mitigation strategy for hydrogen embrittlement in aluminum alloys.

DOI： 10.1038/s41467-022-34628-4

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Language：English   Publishing type：Research paper (scientific journal)   Publisher：The Japan Institute of Metals and Materials  

<p>Recent studies have revealed that hydrogen embrittlement in Al–Zn–Mg alloys appears to be dominated by hydrogen partitioning to MgZn₂ precipitates. A method has recently been proposed for reducing the hydrogen concentration at MgZn₂ precipitates by adding specific intermetallic compound particles that have high hydrogen trap energy. In the present study, the effectiveness of Al₇Cu₂Fe particles on suppression of hydrogen embrittlement in Al–Zn–Mg–Cu alloys was evaluated using X-ray microtomography. Quasi-cleavage cracks were found to be initiated in regions where local volume fractions of the Al₇Cu₂Fe particles were relatively low. Hydrogen partitioning to the MgZn₂ precipitate interface was suppressed, even in high hydrogen concentration material, by adding Al₇Cu₂Fe particles. However, the fractional area of the quasi-cleavage fracture in the material with high hydrogen concentration was higher due to insufficient hydrogen diffusion inside the Al₇Cu₂Fe particles and at the interface between the aluminum matrix and the particles. It appears that finely distributed small Al₇Cu₂Fe particles might effectively suppress hydrogen embrittlement.</p>

DOI： 10.2320/matertrans.mt-l2022007

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Language：English   Publishing type：Research paper (scientific journal)   Publisher：Japan Institute of Metals  

In recent years, it has been reported that intermetallic compound particles can suppress hydrogen embrittlement by hydrogen trapping. Some intermetallic particles in aluminum alloys, such as Al7Cu2Fe, have internal hydrogen trap sites; it is proposed that hydrogen embrittlement can be suppressed by preferential hydrogen partitioning in these sites. However, intermetallic compound particles act as fracture origin sites, and excessive addition degrades the mechanical properties of the material. In this study, we quantitatively evaluated the damage and decohesion behavior of intermetallic compound particles in high-hydrogen content 7XXX aluminum alloys by using in situ synchrotron radiation X-ray tomography. The results revealed that the hydrogen particles induced early high-strain localization, and the Al7Cu2Fe particles were damaged in that region due to its brittleness, resulting in early fracture. Hydrogen had no effects on the fracture and debonding behaviors of intermetallic compound particles, suggesting that the observed particle brittle fracture is dependent on their mechanical properties.

DOI： 10.2320/matertrans.mt-l2022020

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Language：English   Publishing type：Research paper (scientific journal)   Publisher：Elsevier BV  

The pursuit of strong and ductile Al alloys with superior resistance to hydrogen embrittlement (HE) is practically significant across the aerospace and transportation industries among others. Unfortunately, effective ways to progress on the strength-HE trade-off for Al-alloys remain elusive. A strategy of suppressing HE by introducing intermetallic compound (IMC) particles to achieve hydrogen redistribution in various trapping sites was proposed. Here, we systematically induce the precipitation of a constant volume fraction of intermetallic compound (IMC) particles by adding one of 14 elements in a ternary Al-Zn-Mg high-strength alloy. We show a strong correlation between hydrogen trapping energies of the IMC obtained from ab initio calculations with the resistance to HE. Mn-rich Al11Mn3Zn2 particles exhibit the highest hydrogen trapping energy (0.859 eV/atom), leading to a decrease by approximately 5 orders of magnitude in the hydrogen occupancy in eta(2) (MgZn2) phase interfaces and grain boundaries, where HE cracks initiate. The Mn-addition did not deteriorate the ductility and most Al11Mn3Zn2 particles remained intact during plastic deformation which was revealed by in-situ 3D X-ray tomography. Hydrogen-induced strain localization at eta(2) phase interfaces and grain boundaries were inhibited due to strong hydrogen trapping capacity of Al11Mn3Zn2, hence preventing HE cracks initiation. Our approach effectively suppresses hydrogen-induced cracks without sacrificing the ductility, and our strategy can help the design roadmap of HE-tolerant high-strength metallic alloys. (C) 2022 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.

DOI： 10.1016/j.actamat.2022.118110

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A combination of X-ray nano-tomography and pencil-beam diffraction tomography was utilized for multimodal assessment of the mechanically induced transformation of individual retained austenite grains during tensile deformation in a 0.1C-5Mn-1Si multi-phase steel. In the present study, a newly developed high energy (20 - 30 keV) and high resolution (spatial resolution of 0.16 µm in this study) X-ray nano-tomography technique was applied for the first time to the in-situ observation of a steel under external loading. The gradual transformation, plastic deformation, and rotation behaviour of the individual austenite grains were clearly observed in 3D. It was revealed that the early stage of the transformation was dominated by the stress-assisted transformation that can be associated with measured mechanical driving force, whilst the overall transformation was dominated by the strain-induced transformation that is interrelated with measured dislocation multiplication. The transformation behaviour of individual grains was classified according to their initial crystallographic orientation and size. Noteworthy was the high stability of coarse austenite grains (i.e., 2.5 μm or larger in diameter), contrary to past reports in the literature. Characteristic rotation behaviour and wide data dispersion were also observed in the case of the individual austenite grains. It was conclusively demonstrated that such characteristic behaviour partly originated from interactions with surrounding soft and hard phases. The origins of these characteristics are discussed by combining the image-based and diffraction-based information.

DOI： 10.1016/j.actamat.2022.117956

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Language：Japanese   Publishing type：Research paper (scientific journal)   Publisher：The Japan Institute of Light Metals  

Influence of hydrogen on the damage behavior of IMC particles in Al-Zn-Mg-Cu alloys

DOI： 10.2464/jilm.72.411

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Language：English   Publishing type：Research paper (scientific journal)   Publisher：Elsevier BV  

We directly captured, classified, and evaluated 3D particle debonding and fracture behavior in a H-charged 7075 Al alloy throughout the entire tensile deformation using synchrotron X-ray tomography and microstructural feature tracking techniques. The effects of particle size, shape, spatial clustering and stress state on strain-dependent particle damage were identified and isolated from each other. Moreover, state-of-the-art imaging and tracking techniques enabled the establishment of spatially and time-resolved hydrogen distributions during deformation. Based on realistic hydrogen partitioning among various nanoscopic trap sites, the contributions of particles to hydrogen trapping and the hydrogen effect at individual damaged particles were assessed quantitatively. Fracturing of coarse and irregular Al7Cu2Fe particles was found to be the predominant particle damage mode due to the spatial clustering and brittleness of these particles, but a hydrogen effect was not observed. The debonding of Mg2Si particles seemed to be the result of competition between hydrogen and clustering-induced stress localization, but detrimental effects of hydrogen on ductile fracture induced by accelerating interfacial debonding were found to be limited. The quantitative evaluation of particle damage in the present model material clarified a viable strategy for mitigating hydrogen embrittlement, which involves introducing and modifying intermetallic particles with strong hydrogen trapping capacities.

DOI： 10.1016/j.actamat.2022.117658

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DOI： 10.2320/matertrans.L-M2020873

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Hydrogen in materials degrades mechanical properties, which is widely recognized as hydrogen embrittlement. To understand hydrogen embrittlement, it is necessary to clarify the accumulation behavior of hydrogen under stress. The neutron radiography and neutron tomography techniques are applied to examine whether hydrogen accumulation behavior can be visualized directly. Palladium specimens with and without hydrogen were prepared for the neutron imaging experiment under stress. Solute hydrogen has caused distinct contrast change in both the neutron radiography and neutron tomography. Hydrogen distribution at a notch-tip in a loaded specimen has not been visualized in the tomographic cross-sectional images. It can be inferred that this is fundamentally attributable to low spatial resolution of the present imaging set-up, and possibility to visualize hydrogen distribution due to loading is discussed.

DOI： 10.2320/jinstmet.J2020017

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DOI： 10.1016/j.mtla.2020.100667

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DOI： 10.1016/j.engfracmech.2019.106503

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DOI： 10.2464/jilm.69.186

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Assessment of hydrogen embrittlement behavior in Al-Zn-Mg alloys by multimodal 3D image-based simulation

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Role of T phase in the hydrogen embrittlement suppression for Al-Zn-MgCu alloys

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Event date： 2016.6

Language：Japanese   Presentation type：Oral presentation (general)  

Venue：九州大学 筑紫キャンパス   Country：Japan  

Event date： 2016.5

Language：Japanese   Presentation type：Oral presentation (general)  

Venue：大阪大学 吹田キャンパス   Country：Japan  

Event date： 2016.3

Language：Japanese   Presentation type：Oral presentation (general)  

Venue：東京理科大学 葛飾キャンパス   Country：Japan  

Event date： 2015.11

Language：Japanese   Presentation type：Oral presentation (general)  

Venue：應義塾大学 矢上キャンパス   Country：Japan