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本文基于注氢纯铁和铁基二元合金(Fe-3%Cr、Fe-1.4%Ni和Fe-1.4%Mn, 质量分数)开展常规透射电镜(200 kV)的原位表征观察, 揭示了材料中辐照位错环的形态、尺寸演化行为及退火温度影响, 并依据辐照损伤演化理论、退火过程中位错环平均尺寸变化推断得到空位型位错环形成温度的范围. 注氢纯铁中空位型位错环的形成温度( T c)约为500 ℃; 添加Ni可使 T c降低至 ~450 ℃, 添加Cr可使 T c升高至600 ℃以上, 而Mn的作用与Cr相似, 亦可使 T c升高. 注氘实验和热脱附谱分析进一步表明, 纯铁和铁基二元合金中空位型位错环的形成温度受氢同位素与空位结合、释放过程影响. 合金元素Ni对氢同位素与空位的结合、释放有促进作用, 故导致 T c降低; 而Cr和Mn均对氢同位素与空位的结合、释放产生抑制作用, 故导致 T c升高. 本文展示的有关合金元素对空位型位错环形成温度影响的研究将有助于更深刻理解铁基合金体系中损伤结构演化和辐照肿胀产生机理.Reduced activation ferritic/martensitic (RAFM) steels have been considered as a family of prime candidate structural materials for fusion reactors due to low radioactivity and good resistance to irradiation swelling. Various types of defects such as dislocation loops can form in these materials during irradiation. Effects of alloying elements in iron on the formation and migration of dislocation loops have been widely investigated. However, most studies dealt with interstitial-type dislocation loops in iron alloys, while very few focused on vacancy-type dislocation loops. Previous high voltage electron microscope (HVEM) studies from the authors' group have shown that interstitial loops are fully eliminated in hydrogen-ion-implanted α-Fe at 500 ℃, only vacancy loops remain and can achieve up to 100 nm in size. The addition of Ni in α-Fe can reduce the formation temperature of vacancy-type dislocation loops ( T c) to ~450 ℃, while the addition of Cr can increase the temperature to above 600 ℃. However, these experiments are usually difficult to perform due to the scarce resource of HVEM facilities. In this work, in-situ observations by conventional transmission electron microscope (CTEM, 200 kV) are systematically carried out on the hydrogen-ion-implanted α-Fe and Fe-based binary alloys (Fe-3wt.%Cr, Fe-1.4wt.%Ni and Fe-1.4wt.%Mn). The evolutions of morphology and average size of dislocation loops under different annealing temperatures are investigated. The formation temperatures of vacancy-type dislocation loops are determined from the change of average loop size with annealing temperature. The results are consistent with previous studies by HVEM. The effect of Mn atoms in α-Fe is similar to that of Cr atoms, which leads to T cincrease, and the addition of Ni in α-Fe can reduce T c. Furthermore, the results of D thermal desorption spectrum analysis show that T cis affected by the binding and release process of hydrogen isotopes to vacancies in α-Fe. Alloying element Ni promotes the binding and release of hydrogen isotopes to vacancies, which leads to T cdecrease. Cr and Mn inhibit the binding and release of hydrogen isotopes to vacancies, causing T cto increase.
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材料 用途 温度/℃ 注入离子 注入能量/keV 注入剂量/(ions·m–2) 纯铁/铁基二元合金* TEM 25 H+ 30 1×1021 TDS 25 D+ 30 1×1021 注: *铁基二元合金指Fe-3Cr, Fe-1.4Ni和Fe-1.4Mn合金. 
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