正电子湮没谱学在金属材料氢/氦行为研究中的应用

朱特; 曹兴忠

doi:10.7498/aps.69.20200724

摘要

用于核反应堆的金属结构材料中氢/氦泡的前躯体——(氢/氦)-空位复合体的形成受到温度、辐照剂量等多方面因素的影响, 研究其在材料中的形成和演化行为对气泡形核的理解及先进核反应堆材料的发展起着至关重要的作用. 然而, 受到分辨率的局限, 这种原子尺度的微结构很难用电镜等常规方法进行表征, 以致于该问题的研究上可利用的数据相对较少. 正电子湮没谱学是一种研究材料中微观缺陷的特色表征方法, 近些年来慢正电子束流和新型核探测谱仪技术的不断发展以及基于慢束发展起来的多种实验测试方法的改进, 使正电子湮没技术应用已拓展到金属材料中氢/氦行为的研究领域, 在金属材料表面氢/氦辐照损伤的研究中发挥了重要作用. 本文结合国内外相关进展以及本课题组的一些研究成果评述了正电子湮没谱学在金属材料氢氦行为研究中的应用, 着重讨论了正电子湮没寿命谱、多普勒展宽谱、符合多普勒展宽三种测量方法在如下金属材料氢/氦行为研究中的优势: 1)氢/氦气泡尺寸和浓度的估算; 2)高能氢/氦离子辐照损伤缺陷及缺陷的退火、时效的演化行为; 3)不同形变程度样品中氢/氦与形变缺陷的相互作用; 4)不同能量或剂量氢/氦离子辐照对材料造成的损伤以及氢氦协同作用.

关键词:

Abstract

An important feature of the irradiation process in nuclear system is the formation of large displacement cascades, in which primary knock-on atoms and secondary particles formed by nuclear reactions generate a considerable number of defects such as dislocations, vacancies and transmutation gases. Predicting and mitigating the adverse effects of damage defect and transmutation hydrogen/helium produced by high-dose neutron irradiation on the mechanical properties of structural materials is the most significant challenge facing the current development of nuclear energy. To solve this problem, understanding the interaction mechanism between hydrogen/helium atoms and micro-defects is a very important breakthrough. Precursors of helium/ hydrogen bubble, small helium/hydrogen-filled vacancy complexes, may play an important role in realizing bubble nucleation, and the formation of these complexes is affected by many factors. However, only a little information about helium/hydrogen-vacancy clusters’ behavior has been obtained in metal/alloy materials. This is mainly limited by the characterization methods, such as the limited resolution of transmission electron microscope (TEM). Helium/hydrogen-vacancy clusters cannot be observed by TEM before the formation of helium bubbles. Applications of positron annihilation to the study of crystal lattice defects started around 1970s, when it was realized that positron annihilation is particularly sensitive to vacancy-type defects and that annihilation properties manifest the nature of each specific type of defect. In recent years, with the continuous development of slow positron beam and the improvement of various experimental testing methods based on slow positron beam, the application of positron annihilation technology has been extended to the research field of hydrogen/helium behavior in metal materials, which plays an important role in studying the hydrogen/helium radiation damage to metal materials. In this review, the basic principles of positron annihilation spectroscopy are briefly discussed and the three most important measurement methods used for hydrogen/helium effect studies are described (i.e. positron annihilation lifetime spectroscopy (PALS), Doppler broadening spectroscopy (DBS), coincidence Doppler broadening spectroscopy (CDBS)). In this paper, the application of positron annihilation spectroscopy to the study of hydrogen/helium behavior in metal materials is reviewed in combination with the reported relevant developments (including our research group’s achieve-ments). The advantages of three commonly used measurement methods in the following specific studies are highlighted: 1) The estimation of bubble size and concentration; 2) irradiation damage induced by hydrogen/helium; 3) the evolution behavior of irradiation-induced defects in the heat treatment process; 4) sy-nergistic effect of hydrogen and helium.

Keywords:

作者及机构信息

朱特,
曹兴忠

中国科学院高能物理研究所, 多学科研究中心, 北京　100049

通信作者: 曹兴忠, caoxzh@ihep.ac.cn

Authors and contacts

Multi-discipline Research Center, Institute of High Energy Physics, Chiese Academy of Sciences, Beijing 100049, China

Corresponding author: Cao Xing-Zhong, caoxzh@ihep.ac.cn

文章全文 : translate this paragraph

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施引文献

图 1 DBS中参数的定义

Fig. 1. The parameter definition in the Doppler broadening spectrum.

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图 2 纯铁的CDB与一维多普勒展宽能谱比较

Fig. 2. Peak-to-valley ratio of CDB system in the pure iron.

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图 3 金属钨中单个空位包含单个氢原子时的正电子波函数^[26]　(a) 三维立体图; (b)等高线图

Fig. 3. Calculated localized wave function of a positron trapped in a mono-vacancy bound with one hydrogen atom in tungsten^[26]: (a) Isometric plot; (b) contour plot.

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图 4 不同尺寸的氢氦-空位复合体中正电子寿命^[26]

Fig. 4. Calculated positron lifetime in nano-void containing 1 V, 2 V, 6 V, and various H/He atoms^[26].

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图 5 SRIM模拟氢氦离子辐照低活化钢导致的辐照损伤及氢/氦浓度深度分布

Fig. 5. Profiles of damage and atom concentration in RAFM steel irradiated with 250 keV He²⁺ and 130 keV H⁺ calculated with SRIM.

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图 6 VEPFIT拟合氢氦辐照样品的S参数随注入深度的变化

Fig. 6. Fitted S parameters versus VEPFIT for irradiated samples.

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图 7 氦辐照Fe17Cr14.5Ni等时退火过程S-E曲线随温度变化过程^[34]

Fig. 7. Variation of S parameters versus incident positron energy for He⁺ irradiated Fe17Cr14.5Ni alloy during isochronal annealing^[34].

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图 8 氢辐照FeCu等时退火过程ΔS-E曲线随温度变化过程^[35]

Fig. 8. Evolution of the S parameters in H-ions irradiated FeCu alloys during isochronal annealing^[35].

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图 9 氢离子辐照FeCu等时退火过程S-W参数的变化^[35]

Fig. 9. S-W plots for the H-ions irradiated samples during isochronal annealing^[35].

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图 10 Fe9Cr合金氦离子辐照前后S (∆S)参数随正电子注入能量的变化^[36]

Fig. 10. S-parameter and ∆S as a function of positron incident energy (mean implantation depth) in irradiated Fe9Cr alloys and for unirradiated specimen^[36].

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图 11 Fe9Cr合金氦离子辐照前后S-W的变化^[36]

Fig. 11. W-parameter as a function of the S-parameter for irradiated Fe9Cr alloys and for unirradiated one^[36].

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图 12 氦离子注入充分退火和形变的纯铁样品 S-E曲线变化^[39]

Fig. 12. Evolution of the S parameters in well-annealed Fe and deformed Fe with He-ions irradiation^[39].

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图 13 氦离子辐照不同形变量的304不锈钢辐照前后S-E曲线变化^[40]

Fig. 13. S-E curves for deformed 304 steel irradiated with He-ions^[40].

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图 14 氢氦离子辐照RAFM钢正电子慢束结果^[47]

Fig. 14. S-parameter (a) and ∆S/S (b) as a function of incident positron energy. ∆S_He + ∆S_H and ∆S_{He + H} parameter were also shown in (c)^[47].

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图 15 高能Ar辐照W合金注氘前后的正电子慢束结果^[48]

Fig. 15. The S parameter versus depth in the argon-damaged tungsten samples (0/1/6 dpa) with and without deuterium plasma exposure^[48].

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图 16 高能Au辐照多晶W样品注氦前后(a) S-D (深度)曲线, (b) S-W 曲线^[49]

Fig. 16. (a) The S parameter versus depth in the tungsten samples, and the (S, W) plots are shown in (b)^[49].

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图 17 形变316 L钢样品低能高剂量氦等离子体辐照前后的S-E曲线^[52]

Fig. 17. Evolution of S-E curves in deformed 316 L steel exposed to high flux and low energy helium plasma^[52].

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图 18 氦辐照前后Fe9Cr合金中W参数随正电子能量的变化

Fig. 18. Evolution of the W parameters in Fe9Cr alloy with He-ions irradiation.

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图 19 注量为1 × 10¹⁵和1 × 10¹⁶ He⁺/cm²的氦辐照Fe9Cr样品CDB测试曲线^[63]

Fig. 19. CDB ratio curves for the Fe9Cr alloy irradiated with a dose of 1 × 10¹⁵ and 1 × 10¹⁶ He⁺/cm²^[63].

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图 20 氦或中子辐照的纯Ni(a)和Cu(b)样品的CDB测试曲线^[66]

Fig. 20. CDB ratio curves for the Ni irradiated with He-ions (a) and for the Cu irradiated with neutron^[66](b).

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图 21 氦辐照的316L样品退火前后的CDB测试曲线

Fig. 21. CDB ratio curves for the He-ions irradiated 316L samples during isochronal annealing.

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正电子湮没谱学在金属材料氢/氦行为研究中的应用