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Nano-micrometer scale characterization of PWSCC crack tips in the transition zone of 52M overlay and the implication to intergranular cracking 52M 覆盖层过渡区 PWSCC 裂纹尖端的纳米级表征及其对晶间开裂的影响
IF 2.8 2区 工程技术 Q3 MATERIALS SCIENCE, MULTIDISCIPLINARY Pub Date : 2024-09-11 DOI: 10.1016/j.jnucmat.2024.155400

This study examines the microstructural characteristics of the primary water stress corrosion cracking (PWSCC) crack tip in the transition zone (TZ) of the 52 M overlay and its implications for intergranular cracking. In the TZ, the Cr content at grain boundaries near the fusion boundary (FB) is lower than those farther from the FB. Additionally, residual strain at grain boundaries near the FB is higher than that farther away, with the fine-grained zone around the FB showing higher local deformation than the surrounding columnar grains. Stress corrosion cracking (SCC) crack growth rate (CGR) test results indicate that the TZ showed certain SCC sensitivity, and the closer to the FB, the lower the SCC resistance. Analysis of the SCC crack tip found that the distinctive composition distribution of the 52 M overlay TZ, characterized by low Cr and high Fe near the FB, is prone to intergranular oxidation, thereby reducing SCC resistance. Conversely, higher Cr and lower Fe content at grain boundaries in the TZ farther from the FB form dense, Cr-rich oxides ahead of the crack tip that slow SCC crack growth, resulting in the diffusion of oxidation along the dislocation structure into the grains and forming a fibrous oxidation zone.

本研究探讨了 52 M 覆盖层过渡带 (TZ) 中原生水应力腐蚀开裂 (PWSCC) 裂纹尖端的微观结构特征及其对晶间开裂的影响。在 TZ 中,熔融边界 (FB) 附近晶界的铬含量低于远离 FB 的晶界。此外,熔融边界附近晶界的残余应变高于远离熔融边界的晶界,熔融边界周围的细晶粒区显示出比周围柱状晶粒更高的局部变形。应力腐蚀开裂(SCC)裂纹生长率(CGR)测试结果表明,TZ 对 SCC 具有一定的敏感性,越靠近 FB,抗 SCC 能力越低。对 SCC 裂纹尖端的分析发现,52 M 覆盖层 TZ 的独特成分分布(靠近 FB 处为低铬、高铁元素)容易发生晶间氧化,从而降低 SCC 抗性。相反,在远离 FB 的 TZ 晶界上,较高的 Cr 和较低的 Fe 含量在裂纹尖端前方形成致密、富含 Cr 的氧化物,从而减缓 SCC 裂纹的生长,导致氧化物沿着位错结构扩散到晶粒中,形成纤维状氧化区。
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引用次数: 0
Post irradiation examinations of FeCrAl cladding in PWR conditions 在压水堆条件下对铁铬铝包层进行辐照后检查
IF 2.8 2区 工程技术 Q3 MATERIALS SCIENCE, MULTIDISCIPLINARY Pub Date : 2024-09-11 DOI: 10.1016/j.jnucmat.2024.155402
FeCrAl alloys have been one of the prominent Accident Tolerant Fuel (ATF) cladding material candidates, primarily due to their excellent oxidation resistance in high-temperature steam conditions when compared to Zr-based alloys. Prototypic irradiation of fueled FeCrAl rods is a fundamental step in confirming the integral performance behavior during in-pile conditions. Early generation C26M cladding, fabricated through wrought metallurgy techniques, was fueled with UO2 fuel pellets and irradiated in a pressurized water loop in the Advanced Test Reactor (ATR) at the Idaho National Lab (INL) to a burnup (BU) of ∼25 GWd/tHM. After irradiation, the rodlets were nondestructively and destructively examined. Nondestructive examinations included visual exams, profilometry, and gamma scanning. These examinations highlight the unique deposits, BU profile of the rodlets as well as the migration path of fission gases within the rodlet, and typical diametrical morphology of fuel rodlets. During handling, brittle failure of one end cap on one pin occurred. Destructive examinations included microscopy and mechanical testing. Radial cross sections of the cladding were analyzed metallographically through light optical microscopy (LOM), scanning electron microscopy (SEM) highlighting a unique corrosion morphology and micro-cracking (∼20–30 μm past the main oxide layer) at the metal-oxide interface. Ring compression testing (RCT) was used to elucidate the mechanical property change of the FeCrAl cladding after neutron irradiation. In contrast to the non-irradiated material, which remained ductile at all test temperatures between 25 °C and 250 °C, the irradiated cladding fractured in a brittle manner at 50 °C and below. The results of the tests show that some challenges remain in the development of FeCrAl cladding for LWR cladding applications including improvement of in-reactor waterside corrosion performance and the retention of ductility after neutron irradiation.
与 Zr 基合金相比,FeCrAl 合金在高温蒸汽条件下具有优异的抗氧化性,因此一直是主要的事故耐受燃料 (ATF) 覆层材料候选材料之一。燃料铁铬铝棒的原型辐照是确认桩内条件下整体性能行为的基本步骤。通过锻造冶金技术制造的第一代 C26M 堆芯使用二氧化铀燃料颗粒作为燃料,并在爱达荷国家实验室(INL)先进试验反应堆(ATR)的加压水环路中辐照到 25 GWd/tHM 的燃耗(BU)。辐照后,对小棒进行了非破坏性和破坏性检查。非破坏性检查包括目视检查、轮廓测量和伽马扫描。这些检查突出显示了小棒独特的沉积物、BU 剖面以及裂变气体在小棒内的迁移路径和燃料小棒的典型直径形态。在处理过程中,一根燃料棒的端盖发生了脆性破坏。破坏性检查包括显微镜检查和机械测试。通过光学显微镜(LOM)和扫描电子显微镜(SEM)对包层的径向横截面进行了金相分析,突出显示了独特的腐蚀形态和金属-氧化物界面上的微裂纹(超过主氧化层 20-30 μm)。环形压缩试验(RCT)用于阐明中子辐照后铁铬铝包层的机械性能变化。未经辐照的材料在 25 ℃ 至 250 ℃ 之间的所有试验温度下均保持韧性,而经过辐照的包层则在 50 ℃ 及以下温度下发生脆性断裂。试验结果表明,在开发用于低功率堆堆芯的铁铬铝堆芯方面仍存在一些挑战,包括改善反应堆内水侧腐蚀性能以及在中子辐照后保持延展性。
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引用次数: 0
Development of high-temperature-steam resistant UN via the addition of UB2 通过添加 UB2 开发耐高温-耐高温-耐高温-蒸汽联合国
IF 2.8 2区 工程技术 Q3 MATERIALS SCIENCE, MULTIDISCIPLINARY Pub Date : 2024-09-11 DOI: 10.1016/j.jnucmat.2024.155398

A composite UN fuel containing 10wt% UB2 has been manufactured via spark plasma sintering using different milling methods prior to sintering, and the resulting pellets characterised to understand the effects of UB2 location and morphology on UN sintering behaviour and oxidation performance. Differences in microstructure and phases present were observed, with planetary ball milling leading to smaller UB2 inclusions as well as the formation of a UBN phase on sintering. Composite pellets showed an increase in the steam oxidation onset temperature when compared to UN at similar density and manufactured from the same feedstock. Of particular note was the behaviour of one sample with a comparably low density (∼92 %) which had an onset temperature of 823 K and a significantly reduced rate of reaction compared to monolithic UN at similar density. This provides the first confirmatory evidence that UB2 limits the UN-steam reaction by some other mechanism than simply promoting a high-density microstructure. This is supported by examination of post-oxidation composite material, which shows a varied and more complex morphology compared to reference UN samples, including large apparently-bound agglomerates and limited free fine particulate.

通过火花等离子烧结法制造了一种含有 10wt% UB2 的复合 UN 燃料,在烧结前使用了不同的研磨方法,并对得到的颗粒进行了表征,以了解 UB2 的位置和形态对 UN 烧结行为和氧化性能的影响。观察到微观结构和存在的物相存在差异,行星球磨导致 UB2 包裹体变小,并在烧结时形成 UBN 相。与相同原料生产的密度相似的 UN 相比,复合材料颗粒的蒸汽氧化起始温度有所提高。特别值得注意的是密度相当低(∼92 %)的一个样品的表现,其起始温度为 823 K,与密度相似的整体 UN 相比,反应速率明显降低。这首次提供了确凿证据,证明 UB2 通过某种其他机制限制了 UN-蒸汽反应,而不仅仅是促进高密度微结构。对氧化后复合材料的检测也证明了这一点,与参考 UN 样品相比,复合材料的形态多样且更加复杂,包括明显结合的大团聚体和有限的游离细颗粒。
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引用次数: 0
The effect of pre-sintering UO2 granules on the microstructure and the thermal conductivity of UO2–Mo composites fabricated by spark plasma sintering (SPS) 预烧结二氧化铀颗粒对火花等离子体烧结(SPS)制备的二氧化铀-钼复合材料的微观结构和热导率的影响
IF 2.8 2区 工程技术 Q3 MATERIALS SCIENCE, MULTIDISCIPLINARY Pub Date : 2024-09-07 DOI: 10.1016/j.jnucmat.2024.155396

Uranium dioxide (UO2) is the standard fuel used in light water reactors (LWRs). However, it has a low thermal conductivity that ultimately limits its performance both during normal operation and in accident conditions. Adding a material with high thermal conductivity is a potential approach to enhance the thermal conductivity of UO2. Forming an interconnected structure of high-conductivity material can significantly enhance the overall thermal conductivity of the composite. Molybdenum (Mo) has been used as an additive material in UO2 composites previously. A new method for the fabrication of interconnected UO2−Mo composites using pre-sintered UO2 granules to improve the continuity of Mo channels was investigated in this study. UO2–10 wt% Mo composites were produced using UO2 granules and 1073 K and 1473 K pre-sintered UO2 granules, followed by spark plasma sintering (SPS) of the mixtures at 1473 K for 5 min. The composites were characterised using scanning electron microscopy and X-ray diffractometry and their thermal conductivities were measured by the laser flash method and compared with a reference UO2 pellet. At a maximum measurement temperature of 1073 K, a 52 % increase in thermal conductivity was observed in the composites containing UO2 without pre-sintering, and UO2 pre-sintered at 1073 K. The increase was 31 % for composites manufactured from UO2 pre-sintered at 1473 K. These results suggest that higher temperature pre-sintering may be detrimental to forming interconnected Mo structures.

二氧化铀(UO2)是轻水反应堆(LWR)使用的标准燃料。然而,它的导热率较低,最终限制了其在正常运行和事故条件下的性能。添加具有高导热性的材料是提高二氧化铀导热性的潜在方法。形成高导热材料的互连结构可显著提高复合材料的整体导热性。钼(Mo)曾被用作二氧化铀复合材料的添加剂材料。本研究探讨了一种利用预烧结二氧化铀颗粒来改善钼通道连续性的新方法,用于制造相互连接的二氧化铀-钼复合材料。使用二氧化铀颗粒和 1073 K 及 1473 K 预烧结二氧化铀颗粒制备了二氧化铀-10 wt% Mo 复合材料,然后在 1473 K 下对混合物进行火花等离子烧结 (SPS) 5 分钟。使用扫描电子显微镜和 X 射线衍射仪对复合材料进行了表征,并通过激光闪光法测量了其热导率,将其与参考二氧化铀颗粒进行了比较。在 1073 K 的最高测量温度下,未进行预烧结的含有二氧化铀的复合材料和在 1073 K 下预烧结的二氧化铀的热导率增加了 52%,而在 1473 K 下预烧结的二氧化铀制成的复合材料的热导率增加了 31%。
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引用次数: 0
The vacancy-mediated diffusion of transition metal solutes in tungsten: Atomic Kinetic Monte Carlo simulations 钨中过渡金属溶质的空位介导扩散:原子动力学蒙特卡洛模拟
IF 2.8 2区 工程技术 Q3 MATERIALS SCIENCE, MULTIDISCIPLINARY Pub Date : 2024-09-06 DOI: 10.1016/j.jnucmat.2024.155394

The kinetic coupling between vacancy flux and solute flux is crucial for comprehending and forecasting the microstructural evolution of tungsten-based alloys under irradiation. We utilized the Atomic Kinetic Monte Carlo (AKMC) method to systematically explore the vacancy-mediated diffusion of transition metal (TM) solutes in tungsten. The diffusion and transport coefficients of TM solutes were obtained and then used to identify the occurrence of vacancy drag and solute-segregation tendencies. Our findings indicate that TM solutes exhibit faster diffusion rates than tungsten self-diffusion. Ti, V, Nb, Mo, and Ta do not experience vacancy drag, whereas for other TM solutes, vacancy drag is the primary vacancy-mediated diffusion mechanism at low temperatures, transitioning to the inverse Kirkendall mechanism at high temperatures. Moreover, their transition temperatures were determined, showing a parabolic trend in each TM series with peaks observed at Co, Rh, and Pt for the 3d, 4d, and 5d series, respectively. In the temperature range investigated here (600∼3000 K), Ti, Zr, Hf, V, Nb, Ta, and Mo exhibit depletion at vacancy sinks, while other TM solutes enrich at vacancy sinks due to vacancy drag at low temperatures but deplete because of the inverse Kirkendall effect as temperature increases. Additionally, our AKMC results confirmed that, for the solute-vacancy interactions, purely attractive and repulsive interactions lead to the vacancy drag and inverse Kirkendall effect, respectively. While for the complex case, involving both attraction and repulsion, the first-nearest-neighbor (1nn) attraction plays a crucial role in enabling solute diffusion via vacancy drag. Even with a strong 2nn repulsion, the solute can still diffuse through vacancy drag, provided there is a 1nn attraction.

空位通量与溶质通量之间的动力学耦合对于理解和预测辐照下钨基合金的微观结构演变至关重要。我们利用原子动力学蒙特卡洛(AKMC)方法系统地探讨了过渡金属(TM)溶质在钨中由空位介导的扩散。我们获得了 TM 溶质的扩散和传输系数,并利用这些系数确定了空位阻力和溶质分离趋势的发生。我们的研究结果表明,TM 溶质的扩散速度快于钨的自扩散速度。钛、钒、铌、钼和钽不存在空位阻力,而对于其他 TM 溶质,空位阻力在低温下是主要的空位介导扩散机制,在高温下则过渡到逆 Kirkendall 机制。此外,还测定了它们的转变温度,结果显示每个 TM 系列的转变温度呈抛物线趋势,3d、4d 和 5d 系列的峰值分别出现在 Co、Rh 和 Pt 处。在本文研究的温度范围(600∼3000 K)内,Ti、Zr、Hf、V、Nb、Ta 和 Mo 在空位汇处表现出耗竭,而其他 TM 溶质在低温时由于空位阻力而在空位汇处富集,但随着温度的升高则由于反柯肯道尔效应而耗竭。此外,我们的 AKMC 结果证实,在溶质与空位的相互作用中,纯粹的吸引力和排斥力相互作用分别导致了空位阻力和逆柯肯达尔效应。而对于既有吸引力又有排斥力的复杂情况,第一近邻(1nn)吸引力在通过空位阻力实现溶质扩散方面起着至关重要的作用。即使存在很强的 2nn 排斥力,只要存在 1nn 吸引力,溶质仍然可以通过空位拖曳进行扩散。
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引用次数: 0
In-situ measurement of hydrogen isotope behavior in high temperature LBE: Diffusivity, permeability, and solubility 现场测量高温枸杞多糖中的氢同位素行为:扩散性、渗透性和溶解性
IF 2.8 2区 工程技术 Q3 MATERIALS SCIENCE, MULTIDISCIPLINARY Pub Date : 2024-09-06 DOI: 10.1016/j.jnucmat.2024.155392

The Lead-Bismuth Fast Reactor (LBR) emerges as a promising concept due to its superior neutron economy, chemical stability, and thermal properties. From the nuclear safety standpoint, the focus has predominantly been on the behavior of 210Po and other fission products, while the issue of tritium in LBRs has not been sufficiently addressed due to the inconvenience of tritium experiments. Formation of tritium/helium bubbles induces significant local stress and volume expansion, leading to hardening and embrittlement of structural materials, thus expediting their degradation through irradiation effects. Current understanding of tritium transport within liquid Lead-Bismuth Eutectic (LBE) remains incomplete. To bridge this gap, a novel device employing the "permeation pot" method has been developed for the first experimental quantification of diffusivity, permeability, and solubility of hydrogen isotopes in liquid LBE. Notably, hydrogen diffusivity in this medium is found to be three to four orders of magnitude greater than in conventional 316L stainless steel structural material. Furthermore, the temperature-dependence of diffusivity in liquid metals is minimal compared to solids, as indicated by the activation energy. Conversely, solubility in 316L significantly surpasses that in LBE by three to four orders of magnitude. This discrepancy accelerates the tritium release from LBE to structural material, leading to the failure of the structural material.

铅铋快堆(LBR)因其优越的中子经济性、化学稳定性和热特性而成为一个很有前途的概念。从核安全的角度来看,人们主要关注 210Po 和其他裂变产物的行为,而铅铋快堆中的氚问题由于氚实验的不便而未得到充分解决。氚/氦气泡的形成会引起显著的局部应力和体积膨胀,导致结构材料硬化和脆化,从而通过辐照效应加速其降解。目前对氚在液态铅铋共晶(LBE)中传输的了解仍不全面。为了弥补这一缺陷,我们开发了一种采用 "渗透罐 "方法的新型装置,首次对液态铅铋共晶中氢同位素的扩散性、渗透性和溶解性进行了实验量化。值得注意的是,氢在这种介质中的扩散率比在传统 316L 不锈钢结构材料中的扩散率高出三到四个数量级。此外,与固体相比,液态金属中的扩散率与温度的关系很小,这一点可以从活化能看出。相反,在 316L 中的溶解度要比在 LBE 中的溶解度高出三到四个数量级。这种差异加速了氚从 LBE 向结构材料的释放,导致结构材料失效。
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引用次数: 0
Comparative study on high-temperature air and steam oxidation of Cr-coated Zr-4 alloy through experimental and DFT calculation 通过实验和 DFT 计算对铬涂层 Zr-4 合金的高温空气氧化和蒸汽氧化进行比较研究
IF 2.8 2区 工程技术 Q3 MATERIALS SCIENCE, MULTIDISCIPLINARY Pub Date : 2024-09-06 DOI: 10.1016/j.jnucmat.2024.155382

The high-temperature oxidation performance of Cr-coated Zr-4 alloy in air and steam atmosphere is comparatively studied and the mechanism of steam promoted oxidation is revealed by density functional theory (DFT) calculation. The experimental results show that there are significant differences in surface and cross-sectional microstructures after oxidation in the two atmospheres. Dense irregular polyhedral oxides accompanied by randomly occurring micro-cracks are developed after high-temperature air oxidation. While mackerel scale-like or worm-like particles with whisker-like structures accompanied by defects such as pores and micro-cracks are developed after high-temperature steam oxidation. In the high-temperature steam atmosphere, the more vigorous atomic diffusion leads to a thicker Cr-Zr diffusion layer and higher O content, so that after exposure at 1100 °C for 3 and 4 h, the Zr-4 alloy adjacent to the Cr-Zr diffusion layer is oxidized to ZrO2. All the experimental results demonstrate that Cr-coated Zr-4 alloy experiences more severe oxidation in high-temperature steam atmosphere. The DFT calculation results reveal the main reason of steam promoted oxidation is that the interstitial H protons boost the formation of Cr and O vacancies and vacancy pairs in the Cr2O3 oxide scale.

通过密度泛函理论(DFT)计算,比较研究了在空气和蒸汽气氛中镀铬 Zr-4 合金的高温氧化性能,并揭示了蒸汽促进氧化的机理。实验结果表明,在两种气氛中氧化后,表面和横截面的微观结构存在显著差异。高温空气氧化后会形成致密的不规则多面体氧化物,并伴有随机出现的微裂纹。而在高温蒸汽氧化后,则会形成具有须状结构的鲭鱼鳞状或蠕虫状颗粒,并伴有气孔和微裂纹等缺陷。在高温蒸汽气氛中,更剧烈的原子扩散导致更厚的 Cr-Zr 扩散层和更高的 O 含量,因此在 1100 °C 下暴露 3 小时和 4 小时后,邻近 Cr-Zr 扩散层的 Zr-4 合金被氧化成 ZrO2。所有实验结果都表明,在高温蒸汽气氛中,Cr 涂层 Zr-4 合金经历了更严重的氧化。DFT 计算结果表明,蒸汽促进氧化的主要原因是间隙 H 质子促进了 Cr2O3 氧化尺度中 Cr 和 O 空位及空位对的形成。
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引用次数: 0
A modern reappraisal of the U-Zr phase diagram 对 U-Zr 相图的现代重新评估
IF 2.8 2区 工程技术 Q3 MATERIALS SCIENCE, MULTIDISCIPLINARY Pub Date : 2024-09-06 DOI: 10.1016/j.jnucmat.2024.155378
By integrating published experimental data on the uranium-zirconium (U-Zr) system into a machine learning framework, insight into the two differing views on the thermochemical equilibrium, particularly on the U-rich portion of the phase diagram (PD) was developed, ultimately resulting in a new U-Zr PD. Phase diagram sensitivity to model parameters, tolerances, physical preconceptions and experimental biases, are considered to establish the validity of the generated PDs. A systematic assessment of the most reliable and most recent thermochemical data was made, and the traditional modeling bias to search the space of free energy parameters was removed by using recently developed machine learning strategies. The readily validated methodology enables a thermodynamically consistent search of free energy parameters by leveraging modern experimental work from an array of sources including phase transformations, phase transition temperatures, and enthalpy changes between 723-1173 K (450-900°C). These changes include the truncation of β-U stability at 6 at.% Zr, prominent isotherms at 884 K (611°C) and 961 K (688°C), and δ-U-Zr phase boundaries ranging from 66.5 to 80.2 at.% Zr at 823 K (550°C). The newly proposed PD captures fundamental constants measured experimentally and improves the agreement with phase transformation studies such as neutron diffraction with in situ heating. As such, it is proposed that the new U-Zr PD developed in this work be used to resolve the historically opposing views.
通过将已公布的铀-锆(U-Zr)系统实验数据整合到机器学习框架中,深入了解了对热化学平衡的两种不同观点,特别是对相图(PD)富铀部分的不同观点,最终形成了新的铀-锆相图。考虑了相图对模型参数、公差、物理先入为主的观点和实验偏差的敏感性,以确定生成的相图的有效性。对最可靠和最新的热化学数据进行了系统评估,并利用最新开发的机器学习策略消除了搜索自由能参数空间的传统建模偏差。通过利用各种来源的现代实验工作,包括相变、相变温度以及 723-1173 K(450-900°C)之间的焓变,这种经过随时验证的方法能够搜索出热力学上一致的自由能参数。这些变化包括:β-U 稳定性在 6% Zr 时被截断、884 K(611°C)和 961 K(688°C)时的显著等温线以及在 823 K(550°C)时从 66.5% Zr 到 80.2% Zr 的 δ-U-Zr 相界。新提出的 PD 捕获了实验测量的基本常数,并提高了与相变研究(如原位加热的中子衍射)的一致性。因此,建议使用这项工作中开发的新 U-Zr PD 来解决历史上的对立观点。
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引用次数: 0
Interface stability of ultrasonic additively manufactured Zircaloy-4 during hydrothermal corrosion 超声波添加剂制造的 Zircaloy-4 在热液腐蚀过程中的界面稳定性
IF 2.8 2区 工程技术 Q3 MATERIALS SCIENCE, MULTIDISCIPLINARY Pub Date : 2024-09-05 DOI: 10.1016/j.jnucmat.2024.155376

Simulated pressurized water reactor conditions (330 °C, 15.6 MPa, ∼20 ppb oxygen) without irradiation were used to investigate the hydrothermal corrosion behavior of ultrasonic additively manufactured Zircaloy-4 up to 1000 h. X-ray computed tomography allowed for visualization of defects from processing and their progression after corrosion experiments. The specimens were found to have clear variability in the mass change data, compared to typical wrought Zircaloy-4 specimens. The variation in the mass change after exposure was attributed to weld defects connected to the specimen surface which allowed ingress of oxidant into the samples. Defects visualized by computed tomography were found via metallography and characterized. Ultrasonic additively manufactured Zircaloy-4 was found to have comparable corrosion behavior as wrought Zircaloy-4 for specimens which did not have clear surface defects along weld interfaces.

利用模拟加压水反应堆条件(330 °C, 15.6 MPa, ∼20 ppb 氧气)(无辐照)研究了超声波添加剂制造的 Zircaloy-4 长达 1000 小时的热液腐蚀行为。研究发现,与典型的锻造 Zircaloy-4 试样相比,试样的质量变化数据具有明显的差异性。暴露后质量变化的变化归因于与试样表面相连的焊接缺陷,这些缺陷导致氧化剂进入试样。通过金相术发现了计算机断层扫描所能看到的缺陷,并对其进行了表征。对于沿焊接界面没有明显表面缺陷的试样,超声波添加剂制造的 Zircaloy-4 的腐蚀性能与锻造的 Zircaloy-4 相当。
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引用次数: 0
Phase formation of γ-LiAlO2 via transformation of a layered double hydroxide (LDH) by internal gelation 通过层状双氢氧化物(LDH)的内部凝胶化转变形成 γ-LiAlO2 相
IF 2.8 2区 工程技术 Q3 MATERIALS SCIENCE, MULTIDISCIPLINARY Pub Date : 2024-09-05 DOI: 10.1016/j.jnucmat.2024.155379

Interest in controlled deuterium-tritium fusion as a clean-energy technology has grown in recent years. Solid tritium breeder materials, such as γ-LiAlO2, need to release tritium to allow the fusion reaction to occur and control over the microstructure can help tune tritium release. Internal gelation is a synthesis technique that allows control over the sample's microstructure. In this process, droplets of an aqueous precursor are heated to form a gel, which is washed, dried, and calcined to produce oxide spheres. Past attempts applying internal gelation to fabricate γ-LiAlO2 revealed that lithium was lost during wash processes, leading to a lithium deficient final product. To overcome lithium deficiency, the chemistry and reaction pathway must be unraveled. Therefore, this work strove to elucidate the mechanisms of lithium aluminate formation and lithium deficiency. Complementary characterization techniques revealed that lithium aluminate produced via internal gelation formed an aluminum-lithium layered double hydroxide (LDH) structure as an intermediate species. This LDH has a stoichiometry of Li(Al(OH)3)2NO3·xH2O and the 1:2 ratio of Li to Al is thought to limit the overall lithium content of the final lithium aluminate product due to loss of unbound lithium during washing. This work also indicates that infusing amorphous aluminum hydroxide samples with lithium after gelation appears to incorporate lithium beyond this LDH stoichiometric limit and is one potential pathway towards the desired γ-LiAlO2 final product. The results of this work highlight the influence that the LDH intermediate species has upon the formation and stoichiometry of the final, calcined product.

近年来,人们对可控氘氚核聚变这一清洁能源技术的兴趣与日俱增。固体氚增殖材料(如γ-LiAlO2)需要释放氚才能发生聚变反应,而控制微观结构有助于调节氚的释放。内部凝胶化是一种可以控制样品微观结构的合成技术。在这一过程中,水性前体液滴经过加热后形成凝胶,凝胶经过洗涤、干燥和煅烧后生成氧化物球体。过去尝试用内部凝胶法制造γ-LiAlO2时发现,锂在洗涤过程中流失,导致最终产品缺锂。要克服锂缺乏问题,必须解开化学和反应途径。因此,这项研究试图阐明铝酸锂形成和锂缺乏的机理。互补表征技术显示,通过内部凝胶化生成的铝酸锂会形成铝锂层状双氢氧化物(LDH)结构作为中间产物。这种 LDH 的化学计量为 Li(Al(OH)3)2NO3-xH2O,锂与铝的比例为 1:2,这被认为会限制铝酸锂最终产品的总体锂含量,因为未结合的锂会在洗涤过程中流失。这项研究还表明,在凝胶化后向无定形氢氧化铝样品中注入锂,似乎能使锂的含量超过 LDH 的化学计量限制,这也是获得所需的γ-LiAlO2 最终产品的潜在途径之一。这项工作的结果凸显了 LDH 中间物种对最终煅烧产物的形成和化学计量的影响。
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Journal of Nuclear Materials
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