3D-characterization of deuterium distributions in zirconium oxide scale using high-resolution SIMS
3D-characterization of deuterium distributions in zirconium oxide scale using high-resolution SIMS
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DOI：
10.1016/j.apsusc.2018.09.101
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发表时间：
2019-01-15
影响因子：
6.7
通讯作者：
Grovenor, Chris
中科院分区：
文献类型：
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作者：
Li, Kexue;Aarholt, Thomas;Grovenor, Chris
在压水堆 (PWR) 中，燃料棒采用锆合金管包覆，因其低中子俘获截面和良好的抗氧化性而被选择。了解 280-350 摄氏度下的包壳水腐蚀反应以及这些 Zr 合金中相关的氢吸收对于压水堆的安全运行和增加燃料的燃耗至关重要。在这里，我们描述了一种基于高分辨率 SIMS 3D 映射的方法，用于测量氧化 Zircloy-4 合金样品中氘的分布。使用深度剖析和横截面这两个分析方向来确保我们了解这些样品中复杂微观结构溅射过程中可能出现的成像伪影。溅射卡特的形貌和溅射速率已通过聚焦离子束 (FIB)/扫描电子显微镜 (SEM) 分析进行校准。 360 摄氏度下的氘扩散系数是根据两个样品的深度剖面计算的。结果表明，可以成功测量同位素加标样品中的 3D 氘分布，但必须注意了解 Cs+ 一次离子轰击期间氘脱气和表面扩散的影响，这会导致横向分辨率降低，从而扭曲表观氘分布。本文的检测方法可以为分析在役锆燃料包壳材料中氢物种的分布提供有用的工具，也可为其他工程材料提供参考。
In pressurised water reactors (PWRs), fuel rods are clad with zirconium alloy tubes chosen for their low neutron capture cross section and good oxidation resistance. Understanding cladding-water corrosion reactions at 280-350 degrees C and the correlated hydrogen pickup into these Zr alloys is crucial to the safe operation of PWRs and to increasing the burnup of the fuel. Here we describe a method based on 3D mapping by high resolution SIMS to measure the distribution of deuterium in oxidised Zircaloy-4 alloy samples. Two analysis directions, depth-profiling and cross-sectional, were used to ensure we understand possible imaging artefacts during sputtering of the complex microstructure in these samples. The topography of the sputtering carter and sputtering rate have been calibrated by Focused Ion Beam (FIB)/Scanning Electron Microscopy (SEM) analysis. The deuterium diffusion coefficients at 360 degrees C is calculated suing the depth profile in both samples. The results show that the 3D deuterium distribution can be successfully measured in isotopically spiked samples, but that care has to be taken to understand the effect of deuterium outgassing and surface diffusion during Cs+ primary ion bombardment, which results in a degraded lateral resolution, which distorts the apparent deuterium distribution. The detection method in this paper can be a useful tool in the analysis of the distribution of hydrogenic species in zirconium fuel cladding materials in service, and can also provide other engineering materials.