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Determining the Role of O2 and H2O Atmosphere Impurities on the Oxidation of IN718 During High Temperature Inert Gas Heat Treatment
IF 2.1 3区 材料科学 Q2 METALLURGY & METALLURGICAL ENGINEERING Pub Date : 2025-02-11 DOI: 10.1007/s11085-025-10328-4
Eric Moreau, Stephen F. Corbin

The influence of trace levels of O2 and H2O, contamination in an inert gas heat treatment atmosphere on the oxidation behvaiour of IN718 was investigated. Heat treatments consisted of holding IN718 at 1050 °C for 2 h in a combined thermogravimetric balance and gas chromatography-mass spectrometer (GCMS). Furnace atmospheres explored included 22–703 ppm O2 and H2O concentrations of 23–387 ppm. The GCMS measurements were able to quantify the O2 and H2O concentrations during heat treatment and revealed that oxidation became measurable at approximately 800 °C. The oxidation rate was parabolic during the 1050 °C isotherm, increasing linearly with an increase in either O2 or H2O concentration up to a value of 480 ppm. Beyond 480 ppm the oxidation remained constant and equivalent to that reported in air. A two layer surface oxide structure consisting of Cr2O3 and TiNbO4 formed when the O2, and H2O content increased beyond 33 and 23 ppm respectively. Dry O2 conditions (i.e. H2O of approximately 25 ppm), caused spalling of the Cr2O3 oxide surface during cooling when the O2 ppm was 124 ppm or above. In higher H2O concentrations the Cr2O3 layer showed good adherence to the base metal and no cracking during cooling. The use of a He–5% H2 carrier gas did not alter the oxidation rate significantly, but did increase the H2O concentration, thus preventing oxide spalling during cooling.

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引用次数: 0
High-Temperature Oxidation Behavior of Pt-10Rh-Zr(Y) Alloys and its Influence on their Mechanical Properties
IF 2.1 3区 材料科学 Q2 METALLURGY & METALLURGICAL ENGINEERING Pub Date : 2025-01-31 DOI: 10.1007/s11085-025-10327-5
Changyi Hu, Yan Wei, Qianqi Wei, Xiangxing Xiao, Xian Wang, Xuehang Wang, Junmei Guo

In most cases, platinum-based alloys are mainly used in high-temperature oxidation environments, and mastering their oxidation behavior and the impact of oxidation on performance is crucial. Two new platinum-based high-temperature alloys, Pt-10Rh-0.5Zr and Pt-10Rh-0.5Zr-0.2Y, were designed and prepared in this study. The research focuses on the high-temperature oxidation behavior of the alloys in air and the influence of oxidation on the room temperature mechanical properties of the alloys. The results show that the relationship between oxidation weight loss and temperature of these two platinum-based alloys conforms to the Arrhenius equation within the temperature range of 1400–1600 ℃, and the oxidation resistance of Pt-10Rh-0.5Zr-0.2Y alloy is better than that of Pt-10Rh.0.5Zr alloy. Examination of the surface and fracture morphology of these oxidized platinum-based alloys revealed that zirconium and yttrium oxide particles, such as ZrO2 and Y2O3, with different morphologies and structures were formed. The study also found that adding a small amount of zirconium and yttrium can significantly improve the room temperature ultimate tensile strength of Pt-10Rh alloy. However, after 20 h of high-temperature oxidation treatment at 1400 and 1500 °C, the tensile strength and plasticity at room temperature of both alloys showed a significant downward trend. Especially, the room temperature plasticity of Pt-10Rh-0.5Zr-0.2Y alloy decreased by more than 80% and exhibited a brittle fracture mode. Our research will contribute to the design and development of new high-temperature platinum-based alloys.

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引用次数: 0
Unraveling the Microstructure Evolution and Element Diffusion Behavior of Gradient Nanostructured Heat-Resistant Stainless Steel during High-Temperature Oxidation 梯度纳米结构耐热不锈钢高温氧化过程中微观组织演变及元素扩散行为的研究
IF 2.1 3区 材料科学 Q2 METALLURGY & METALLURGICAL ENGINEERING Pub Date : 2025-01-16 DOI: 10.1007/s11085-025-10326-6
L. L. Wei, C. H. Xia, Y. G. Wang, J. Kundin, X. J. Jin

Thermal stability of nanocrystalline grains is a crucial factor that determines the unique microstructure and properties of the gradient nanostructured (GNS) materials at elevated temperatures. Nevertheless, oxidation is unavoidable for GNS metal materials utilized at high temperatures, potentially impacting the microstructure stability. In this study, we reveal the correlation between the high-temperature selective oxidation and the thermal stability of GNS layer through experiments and phase-field simulations. The improved oxidation resistance of GNS samples was ascribed to the excellent thermal stability of (Cr, Mn)3O4 oxides and a large proportion of low-energy twin boundaries. After prolonged oxidation, the GNS layer exhibited a bimodal microstructure. To analyze the elemental diffusion mechanism and microstructure evolution in the GNS layer, the phase-field simulation technique was employed. Selective oxidation led to the concentration of chromium reduced in the grain-boundary region, thereby diminishing the thermal stability of the grains and causing abnormal grain growth in the surface layer. Particularly, grain growth had a cumulative effect, the topmost grains coarsening will cause grain growth in the underlying layers, and subsequently, the grains in the interior region will also be gradually affected.

纳米晶粒的热稳定性是决定梯度纳米结构(GNS)材料在高温下独特的微观结构和性能的关键因素。然而,在高温下使用GNS金属材料时,氧化是不可避免的,这可能会影响其微观结构的稳定性。在本研究中,我们通过实验和相场模拟揭示了高温选择性氧化与GNS层热稳定性之间的关系。GNS样品抗氧化性能的提高是由于(Cr, Mn)3O4氧化物具有优异的热稳定性和大量的低能孪晶界。经过长时间氧化后,GNS层呈现双峰结构。为了分析GNS层中元素扩散机理和微观组织演变,采用相场模拟技术。选择性氧化导致晶界区域的铬浓度降低,从而降低了晶粒的热稳定性,导致表层晶粒生长异常。其中,晶粒的生长具有累积效应,最上层晶粒的粗化会引起下垫层晶粒的长大,随后,内部区域的晶粒也会逐渐受到影响。
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引用次数: 0
Assessing Stainless Steel Compatibility in Flowing FLiBe Salt 评估不锈钢在流动FLiBe盐中的相容性
IF 2.1 3区 材料科学 Q2 METALLURGY & METALLURGICAL ENGINEERING Pub Date : 2025-01-03 DOI: 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.

为了解决在裂变和聚变反应堆应用中对LiF-BeF2 (FLiBe)相容性的巨大兴趣,进行了静态和流动相容性实验来评估与316H型不锈钢的相容性。在550°和650°C的静态测试中,测量到微小的质量变化,测试后的表征表明,盐中的Fe, Cr, Ni和Mn含量增加。在静态盐试验中加入Be,降低了Fe和Ni的溶解。在不添加Be的情况下,使用单金属316H热对流环(TCL)在650℃的峰值温度下运行1000 h,对流动的FLiBe的传质进行了初步评估。与先前流动的FLiNaK盐的结果相似,316H样品在热腿中表现出较小的质量损失。316H试样的测试后表征表明,热腿和冷腿中Cr表面损耗,冷腿中可能有铁沉积。为了进一步了解这种行为,在550-650°C的静态FLiBe中测量了Cr和Fe的溶解。
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引用次数: 0
Transition from Internal to External Oxidation in Binary Fe–Cr Alloys Around 900 °C 二元Fe-Cr合金在900℃左右从内部氧化到外部氧化的转变
IF 2.1 3区 材料科学 Q2 METALLURGY & METALLURGICAL ENGINEERING Pub Date : 2024-12-06 DOI: 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.

研究了Fe- 10cr二元合金在850 ~ 900℃的Fe/FeO Rhines pack (RP)和H2/H2O中从外氧化到内氧化的转变。温度的升高和水蒸气的存在促进了内部氧化。经典的瓦格纳扩散分析预测铁素体(BCC) Fe-10Cr的外部氧化和奥氏体(FCC) Fe-10Cr的内部氧化。在900℃左右,α-to-γ转变是促进Fe-Cr内部氧化的主要因素。水蒸气被认为可以促进内部氧化,因为H2O比O2具有更高的反应活性,并且H2O分子具有更高的优先吸附性。
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引用次数: 0
High-Temperature Oxidation Study in a Multi-Oxidant Environment Using 18O Tracer 利用 18O 示踪剂进行多氧化剂环境中的高温氧化研究
IF 2.1 3区 材料科学 Q2 METALLURGY & METALLURGICAL ENGINEERING Pub Date : 2024-11-28 DOI: 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。
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引用次数: 0
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 冷却速率对高导热性热锻工具钢高温氧化过程中形成的氧化层中绿帘石含量的影响
IF 2.1 3区 材料科学 Q2 METALLURGY & METALLURGICAL ENGINEERING Pub Date : 2024-11-28 DOI: 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.

研究了热加工工具钢在高温氧化(600 °C和700 °C)过程中形成的氧化层中绿泥石(FeO)的转变。在这些用于热加工的钢材的氧化层中,武氏体起着重要作用。然而,了解其在冷却过程中的转变行为对于控制最终的氧化层结构至关重要。缓慢的冷却速度对最终的绿柱石含量有很大影响,导致在温度高于 570 °C 时,氧化层成分的表示不准确。本研究的目的是确定冷却速度对高温氧化后氧化层中绿泥石含量的影响。研究发现,对于在 700 ℃ 或更高温度下氧化的热作钢材样品,需要 1000 ℃ min-1 以上的冷却速率才能抑制共晶转变并保持实际的绿泥石含量。在较低温度(570 ℃-600 ℃)下,需要超过 100 ℃ min-1 的冷却速率才能达到氧化温度下氧化层中观察到的绿泥石含量。总体而言,赤铁矿和磁铁矿的含量也会随着冷却速率的变化而变化,这与绿泥石含量的变化有关。
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引用次数: 0
Segmentation and Metallographic Evaluation of Aluminium Slurry Coatings Using Machine Learning Techniques 利用机器学习技术对铝浆涂层进行分段和金相评估
IF 2.1 3区 材料科学 Q2 METALLURGY & METALLURGICAL ENGINEERING Pub Date : 2024-10-26 DOI: 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。
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引用次数: 0
Editorial on Modeling, Prediction and Simulation 关于建模、预测和模拟的社论
IF 2.1 3区 材料科学 Q2 METALLURGY & METALLURGICAL ENGINEERING Pub Date : 2024-10-09 DOI: 10.1007/s11085-024-10319-x
Clara Desgranges, Jérôme Favergeon, Bruce Pint, Daniel Monceau, Laurence Latu‑Romain, Stéphane Mathieu, Fernando Pedraza
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引用次数: 0
Editorial on Oxidation in Complex Atmospheres 复杂大气中的氧化作用》社论
IF 2.1 3区 材料科学 Q2 METALLURGY & METALLURGICAL ENGINEERING Pub Date : 2024-10-05 DOI: 10.1007/s11085-024-10318-y
Stéphane Mathieu, Jérôme Favergeon, Bruce Pint, Daniel Monceau, Clara Desgranges, Laurence Latu‑Romain, Fernando Pedraza
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引用次数: 0
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Oxidation of Metals
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