Pub Date : 2025-01-03DOI: 10.1007/s11085-024-10325-z
B. A. Pint, D. Sulejmanovic, C. G. Parker, Y.-F. Su, M. J. Lance, R. Pillai
To address the considerable interest in LiF-BeF2 (FLiBe) compatibility for fission and fusion reactor applications, static and flowing compatibility experiments were conducted to assess the compatibility with type 316H stainless steel. In static testing at 550° and 650 °C, small mass changes were measured and posttest characterization of the FLiBe showed increased levels of Fe, Cr, Ni and Mn in the salt. Adding Be in the static salt test reduced the dissolution of Fe and Ni. An initial assessment of mass transfer in flowing FLiBe without a Be addition was conducted using a monometallic 316H thermal convection loop (TCL) operated for 1000 h with a peak temperature of 650 °C. Similar to prior results in flowing FLiNaK salt, the 316H specimens exhibited small mass losses in the hot leg. Posttest characterization of the 316H specimens suggested Cr surface depletion in the hot and cold legs and possibly Fe deposition in the cold leg. To further understand this behavior, Cr and Fe dissolution was measured in static FLiBe at 550–650 °C.
{"title":"Assessing Stainless Steel Compatibility in Flowing FLiBe Salt","authors":"B. A. Pint, D. Sulejmanovic, C. G. Parker, Y.-F. Su, M. J. Lance, R. Pillai","doi":"10.1007/s11085-024-10325-z","DOIUrl":"10.1007/s11085-024-10325-z","url":null,"abstract":"<div><p>To address the considerable interest in LiF-BeF<sub>2</sub> (FLiBe) compatibility for fission and fusion reactor applications, static and flowing compatibility experiments were conducted to assess the compatibility with type 316H stainless steel. In static testing at 550° and 650 °C, small mass changes were measured and posttest characterization of the FLiBe showed increased levels of Fe, Cr, Ni and Mn in the salt. Adding Be in the static salt test reduced the dissolution of Fe and Ni. An initial assessment of mass transfer in flowing FLiBe without a Be addition was conducted using a monometallic 316H thermal convection loop (TCL) operated for 1000 h with a peak temperature of 650 °C. Similar to prior results in flowing FLiNaK salt, the 316H specimens exhibited small mass losses in the hot leg. Posttest characterization of the 316H specimens suggested Cr surface depletion in the hot and cold legs and possibly Fe deposition in the cold leg. To further understand this behavior, Cr and Fe dissolution was measured in static FLiBe at 550–650 °C.</p></div>","PeriodicalId":724,"journal":{"name":"Oxidation of Metals","volume":"102 1","pages":""},"PeriodicalIF":2.1,"publicationDate":"2025-01-03","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142912842","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"材料科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2024-12-06DOI: 10.1007/s11085-024-10322-2
A. Chyrkin, J. Froitzheim, W. J. Quadakkers
The transition from external to internal oxidation of a binary Fe-10Cr alloy has been investigated in Fe/FeO Rhines pack (RP) and H2/H2O between 850 and 900 °C. Internal oxidation is facilitated by increasing temperature and presence of water vapor. A classical Wagnerian diffusion analysis predicts external oxidation for ferritic (BCC) Fe-10Cr and internal oxidation for austenitic (FCC) Fe-10Cr. The α-to-γ transformation is demonstrated to be the primary factor promoting internal oxidation in Fe–Cr around 900 °C. Water vapor is believed to promote internal oxidation due to a higher reactivity of H2O compared to O2 and higher preferential adsorption of the H2O molecule.
{"title":"Transition from Internal to External Oxidation in Binary Fe–Cr Alloys Around 900 °C","authors":"A. Chyrkin, J. Froitzheim, W. J. Quadakkers","doi":"10.1007/s11085-024-10322-2","DOIUrl":"10.1007/s11085-024-10322-2","url":null,"abstract":"<div><p>The transition from external to internal oxidation of a binary Fe-10Cr alloy has been investigated in Fe/FeO Rhines pack (RP) and H<sub>2</sub>/H<sub>2</sub>O between 850 and 900 °C. Internal oxidation is facilitated by increasing temperature and presence of water vapor. A classical Wagnerian diffusion analysis predicts external oxidation for ferritic (BCC) Fe-10Cr and internal oxidation for austenitic (FCC) Fe-10Cr. The α-to-γ transformation is demonstrated to be the primary factor promoting internal oxidation in Fe–Cr around 900 °C. Water vapor is believed to promote internal oxidation due to a higher reactivity of H<sub>2</sub>O compared to O<sub>2</sub> and higher preferential adsorption of the H<sub>2</sub>O molecule.</p></div>","PeriodicalId":724,"journal":{"name":"Oxidation of Metals","volume":"102 1","pages":"1 - 22"},"PeriodicalIF":2.1,"publicationDate":"2024-12-06","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://link.springer.com/content/pdf/10.1007/s11085-024-10322-2.pdf","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142778586","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"材料科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2024-11-28DOI: 10.1007/s11085-024-10323-1
Juho Lehmusto, Anton Ievlev, James Kurley III, Bruce A. Pint
The goal of this study was to use 18O-enriched water to better understand the role of H2O in high-temperature oxidation. Seven model and three commercial M-Cr and M-Cr-Al alloys were studied in air with 10% of H2O at 800 °C for 5 h. Oxygen from water vapor was more reactive than oxygen from the air and 18O enriched at the outermost layers of the formed Cr- and Al-rich oxides. Alloys with Al and/or Ti additions showed signs of internal oxidation but 18O was not enriched inside the alloy in locations with internal oxidation. Depending on the alloy Al content, the oxide went from Al oxidation beneath a chromia scale to external alumina scale formation.
本研究的目的是利用富含 18O 的水更好地了解 H2O 在高温氧化中的作用。水蒸气中的氧比空气中的氧更具活性,18O 富集在所形成的富铬和富铝氧化物的最外层。添加了 Al 和/或 Ti 的合金显示出内部氧化的迹象,但在合金内部氧化的位置,18O 并未富集。根据合金铝含量的不同,氧化物从铬鳞下面的铝氧化到外部氧化铝鳞的形成。
{"title":"High-Temperature Oxidation Study in a Multi-Oxidant Environment Using 18O Tracer","authors":"Juho Lehmusto, Anton Ievlev, James Kurley III, Bruce A. Pint","doi":"10.1007/s11085-024-10323-1","DOIUrl":"10.1007/s11085-024-10323-1","url":null,"abstract":"<div><p>The goal of this study was to use <sup>18</sup>O-enriched water to better understand the role of H<sub>2</sub>O in high-temperature oxidation. Seven model and three commercial M-Cr and M-Cr-Al alloys were studied in air with 10% of H<sub>2</sub>O at 800 °C for 5 h. Oxygen from water vapor was more reactive than oxygen from the air and <sup>18</sup>O enriched at the outermost layers of the formed Cr- and Al-rich oxides. Alloys with Al and/or Ti additions showed signs of internal oxidation but <sup>18</sup>O was not enriched inside the alloy in locations with internal oxidation. Depending on the alloy Al content, the oxide went from Al oxidation beneath a chromia scale to external alumina scale formation.</p></div>","PeriodicalId":724,"journal":{"name":"Oxidation of Metals","volume":"102 1","pages":"1 - 18"},"PeriodicalIF":2.1,"publicationDate":"2024-11-28","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://link.springer.com/content/pdf/10.1007/s11085-024-10323-1.pdf","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142737339","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"材料科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2024-11-28DOI: 10.1007/s11085-024-10324-0
Tilen Balaško, Barbara Šetina Batič, Jaka Burja
The transformation of wüstite (FeO) in the oxide layer formed during high temperature oxidation (600 °C and 700 °C) on hot-worked tool steel was investigated. Wüstite plays an important role in the oxide layer of these steels used for hot working. However, understanding its transformation behavior during cooling is crucial for controlling the final oxide layer structure. Slow cooling rates have a significant influence on the final wüstite content, resulting in inaccurate representations of the composition of the oxide layer at temperatures above 570 °C. The aim of this study was to determine the influence of cooling rate on the wüstite content in the oxide layer after high temperature oxidation. It was found that for hot-worked steel samples oxidized at 700 °C or higher, a cooling rate of more than 1000 °C min−1 is required to suppress the eutectoid transformation and maintain the realistic wüstite content. At lower temperatures (570 °C–600 °C), a cooling rate of more than 100 °C min−1 is required to achieve the wüstite content observed at oxidation temperatures in the oxide layer. Overall, the hematite and magnetite contents also vart with the cooling rate, which is associated with changes in the wüstite content.
{"title":"Influence of the Cooling Rate on the Wüstite Content in Oxide Layers Formed During High-Temperature Oxidation of Hot-Worked Tool Steel with High Thermal Conductivity","authors":"Tilen Balaško, Barbara Šetina Batič, Jaka Burja","doi":"10.1007/s11085-024-10324-0","DOIUrl":"10.1007/s11085-024-10324-0","url":null,"abstract":"<div><p>The transformation of wüstite (FeO) in the oxide layer formed during high temperature oxidation (600 °C and 700 °C) on hot-worked tool steel was investigated. Wüstite plays an important role in the oxide layer of these steels used for hot working. However, understanding its transformation behavior during cooling is crucial for controlling the final oxide layer structure. Slow cooling rates have a significant influence on the final wüstite content, resulting in inaccurate representations of the composition of the oxide layer at temperatures above 570 °C. The aim of this study was to determine the influence of cooling rate on the wüstite content in the oxide layer after high temperature oxidation. It was found that for hot-worked steel samples oxidized at 700 °C or higher, a cooling rate of more than 1000 °C min<sup>−1</sup> is required to suppress the eutectoid transformation and maintain the realistic wüstite content. At lower temperatures (570 °C–600 °C), a cooling rate of more than 100 °C min<sup>−1</sup> is required to achieve the wüstite content observed at oxidation temperatures in the oxide layer. Overall, the hematite and magnetite contents also vart with the cooling rate, which is associated with changes in the wüstite content.</p></div>","PeriodicalId":724,"journal":{"name":"Oxidation of Metals","volume":"102 1","pages":"1 - 14"},"PeriodicalIF":2.1,"publicationDate":"2024-11-28","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://link.springer.com/content/pdf/10.1007/s11085-024-10324-0.pdf","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142737342","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"材料科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2024-10-26DOI: 10.1007/s11085-024-10321-3
Maria del Mar Juez Lorenzo, Vladislav Kolarik, Khyati Sethia, Petr Strakos
Analysis of scanning electron microscope (SEM) images is crucial for characterising aluminide diffusion coatings deposited via the slurry route on steels, yet challenging due to various factors like imaging artefacts, noise, and overlapping features such as resin, precipitates, cracks, and pores. This study focuses on determining the thicknesses of the coating layers Fe2Al5 and, if present, FeAl, pore characteristics, and chromium precipitate fractions after the heat treatment that forms the diffusion coating. A deep learning SEM image segmentation model utilising U-Net architecture is proposed. Ground truth data were generated using the trainable Weka segmentation plugin in ImageJ, manually refined for accuracy, and supplemented with synthetic data from Blender 3D software for data augmentation of a limited number of SEM label images. The deep learning model trained on a combination of synthetic and real SEM data achieved mean dice scores of 98.7% ± 0.2 for the Fe2Al5 layer, 82.6% ± 8.1 for pores, and 81.48% ± 3.6 for precipitates when evaluated on manually labelled SEM data. The deep learning procedure was applied to evaluate a series of SEM images of diffusion coatings obtained with three different slurry compositions. The evaluation revealed that using a slurry without a rheology modifier may lead to a thicker partial Fe2Al5 layer that is formed by inward diffusion. The relation between the outward and inward diffusion Fe2Al5 layers was not affected by the coating thickness. The thinner diffusion coating presents lower pores and chromium precipitate fractions independently of the slurry selected.
扫描电子显微镜 (SEM) 图像分析对于确定通过浆料路线沉积在钢材上的铝化物扩散涂层的特性至关重要,但由于成像伪影、噪声和重叠特征(如树脂、沉淀物、裂纹和孔隙)等各种因素的影响,这种分析具有挑战性。本研究的重点是确定形成扩散涂层的热处理后的涂层厚度 Fe2Al5 和 FeAl(如果存在)、孔隙特征和铬析出物分数。本文提出了一种利用 U-Net 架构的深度学习 SEM 图像分割模型。使用 ImageJ 中可训练的 Weka 分割插件生成地面实况数据,并进行人工改进以确保准确性,同时使用 Blender 3D 软件中的合成数据对数量有限的 SEM 标签图像进行数据增强。在人工标注的 SEM 数据上进行评估时,结合合成和真实 SEM 数据训练的深度学习模型对 Fe2Al5 层的平均骰子分数为 98.7% ± 0.2,对孔隙的平均骰子分数为 82.6% ± 8.1,对沉淀物的平均骰子分数为 81.48% ± 3.6。深度学习程序被用于评估使用三种不同浆料成分获得的一系列扩散涂层的 SEM 图像。评估结果表明,使用不含流变修饰剂的浆料可能会导致通过内向扩散形成较厚的部分 Fe2Al5 层。外向扩散和内向扩散 Fe2Al5 层之间的关系不受涂层厚度的影响。较薄的扩散涂层呈现较低的孔隙和铬沉淀分数,与所选浆料无关。
{"title":"Segmentation and Metallographic Evaluation of Aluminium Slurry Coatings Using Machine Learning Techniques","authors":"Maria del Mar Juez Lorenzo, Vladislav Kolarik, Khyati Sethia, Petr Strakos","doi":"10.1007/s11085-024-10321-3","DOIUrl":"10.1007/s11085-024-10321-3","url":null,"abstract":"<div><p>Analysis of scanning electron microscope (SEM) images is crucial for characterising aluminide diffusion coatings deposited via the slurry route on steels, yet challenging due to various factors like imaging artefacts, noise, and overlapping features such as resin, precipitates, cracks, and pores. This study focuses on determining the thicknesses of the coating layers Fe<sub>2</sub>Al<sub>5</sub> and, if present, FeAl, pore characteristics, and chromium precipitate fractions after the heat treatment that forms the diffusion coating. A deep learning SEM image segmentation model utilising U-Net architecture is proposed. Ground truth data were generated using the trainable Weka segmentation plugin in ImageJ, manually refined for accuracy, and supplemented with synthetic data from Blender 3D software for data augmentation of a limited number of SEM label images. The deep learning model trained on a combination of synthetic and real SEM data achieved mean dice scores of 98.7% ± 0.2 for the Fe<sub>2</sub>Al<sub>5</sub> layer, 82.6% ± 8.1 for pores, and 81.48% ± 3.6 for precipitates when evaluated on manually labelled SEM data. The deep learning procedure was applied to evaluate a series of SEM images of diffusion coatings obtained with three different slurry compositions. The evaluation revealed that using a slurry without a rheology modifier may lead to a thicker partial Fe<sub>2</sub>Al<sub>5</sub> layer that is formed by inward diffusion. The relation between the outward and inward diffusion Fe<sub>2</sub>Al<sub>5</sub> layers was not affected by the coating thickness. The thinner diffusion coating presents lower pores and chromium precipitate fractions independently of the slurry selected.</p></div>","PeriodicalId":724,"journal":{"name":"Oxidation of Metals","volume":"101 6","pages":"1497 - 1512"},"PeriodicalIF":2.1,"publicationDate":"2024-10-26","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://link.springer.com/content/pdf/10.1007/s11085-024-10321-3.pdf","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142573712","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"材料科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2024-09-25DOI: 10.1007/s11085-024-10311-5
Thomas Gheno, Walid Djedaa
The diffusion properties of polycrystalline materials depend on their grain shape and size, which determine the spatial distribution of grain boundaries. These morphological characteristics are of interest when evaluating an alloy ability to form a protective oxide scale by selective oxidation at high temperature. The composition changes induced by selective oxidation in 2D polycrystals were studied by finite element simulations. We examined the effect of the grain boundary orientation in lamellar polycrystals, and the effects of the grain size distribution in random equiaxed polycrystals. Fine-grained polycrystals were found to behave as uniform media. The effective diffusivity of fine lamellar polycrystals depends on the grain boundary orientation and is bounded by the upper and lower composite diffusivities, while the effective diffusivity of fine equiaxed polycrystals can be estimated by a modified Hart equation. The behavior of coarser equiaxed polycrystal was shown to vary according to the local grain size: the concentration at the alloy-scale interface is fully determined by the local grain size in larger grains, while it is affected by the surrounding grains in finer grains. Increasing the grain size dispersion led to a more scattered response and shifted the minimum interface concentrations toward lower values, which is expected to have a detrimental effect on the oxidation resistance.
{"title":"Modeling the Role of the Grain Structure in the Oxidation of Polycrystals","authors":"Thomas Gheno, Walid Djedaa","doi":"10.1007/s11085-024-10311-5","DOIUrl":"10.1007/s11085-024-10311-5","url":null,"abstract":"<div><p>The diffusion properties of polycrystalline materials depend on their grain shape and size, which determine the spatial distribution of grain boundaries. These morphological characteristics are of interest when evaluating an alloy ability to form a protective oxide scale by selective oxidation at high temperature. The composition changes induced by selective oxidation in 2D polycrystals were studied by finite element simulations. We examined the effect of the grain boundary orientation in lamellar polycrystals, and the effects of the grain size distribution in random equiaxed polycrystals. Fine-grained polycrystals were found to behave as uniform media. The effective diffusivity of fine lamellar polycrystals depends on the grain boundary orientation and is bounded by the upper and lower composite diffusivities, while the effective diffusivity of fine equiaxed polycrystals can be estimated by a modified Hart equation. The behavior of coarser equiaxed polycrystal was shown to vary according to the local grain size: the concentration at the alloy-scale interface is fully determined by the local grain size in larger grains, while it is affected by the surrounding grains in finer grains. Increasing the grain size dispersion led to a more scattered response and shifted the minimum interface concentrations toward lower values, which is expected to have a detrimental effect on the oxidation resistance.</p></div>","PeriodicalId":724,"journal":{"name":"Oxidation of Metals","volume":"101 6","pages":"1481 - 1495"},"PeriodicalIF":2.1,"publicationDate":"2024-09-25","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142573711","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"材料科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}