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先进铅冷快堆和加速器驱动次临界系统商业化的关键材料问题是结构材料与铅基冷却剂之间的相容性问题, 结构钢材料需要在高温液态铅铋共晶中具有优异的抗腐蚀能力. 含铝强化奥氏体钢(alumina-forming austenite steel, AFA钢)因其表面可以形成Al2O3膜而在极端环境中具有良好的耐蚀性能. 本文研究了降低Ni元素成分和高温预氧化对AFA钢耐铅铋腐蚀性能的影响, 利用扫描电子显微镜、能量色散X射线光谱仪、X射线衍射技术, 对AFA钢在550 ℃液态铅铋饱和溶氧条件下腐蚀600 h的氧化层形貌及结构进行表征. 结果表明: 降低合金中Ni含量和高温预氧化处理都会促进样品表面形成保护性Al2O3氧化膜, 进而降低腐蚀层厚度, 提升材料耐铅铋腐蚀性能.The key material issue for the commercialization of advanced lead cooled fast reactors and accelerator driven subcritical systems is the compatibility between structural materials and lead based coolants. Structural steel materials require excellent corrosion resistance in high-temperature liquid lead bismuth eutectic (LBE) alloy. Aluminum forming austenitic steel (AFA steel) has excellent corrosion resistance in extreme environments due to its ability to form an Al2O3 film on its surface. However, excessively high Ni elements are more easily dissolved or oxidized in LBE than Fe and Cr elements. Therefore, this work investigates the effect of reducing Ni element composition (25-Ni steel and 18-Ni steel) on the corrosion resistance of steel in LBE. Surface treatment can protect the substrate from corrosion to some extent, so herein we explore whether it has a protective effect on AFA steel in LBE by generating Al2O3 through high-temperature pre oxidation. The morphology and structure of the oxide layer of AFA steel corroded for 600 h in LBE with saturated dissolved oxygen at 550 ℃ are characterized by scanning electron microscope (SEM), energy dispersive spectrometer (EDS), X-ray diffraction (XRD), and other technologies. The results indicate that the oxide film formed after corrosion of 18-Ni steel is thinner than that after corrosion of 25-Ni steel. Performing high-temperature pre oxidation is beneficial to forming a protective Al2O3 oxide film on the surface of the sample, thereby reducing the thickness of the oxide layer and improving the material’s LBE corrosion resistance. The reduction in thickness of the oxide layer generated after pre oxidation of 18-Ni steel is greater than that of 25-Ni steel, so the anti-corrosion effect of 18-Ni steel after pre oxidation is better than that of 25-Ni steel.
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Keywords:
- aluminum forming austenitic steel /
- oxide layer /
- lead bismuth eutectic /
- high temperature pre oxidation
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图 1 锻造态钢的EBSD图和SEM图 (a) 18-Ni钢EBSD图; (b) 基于图(a)的18-Ni钢相分布图; (c) 18-Ni钢SEM图, 右上角图像放大了α相区域; (d) 25-Ni钢EBSD图; (e) 基于图(d)的25-Ni钢相分布图; (f) 25-Ni钢SEM图
Fig. 1. EBSD and SEM images of steels: (a) EBSD images of 18-Ni steel; (b) phase distribution of 18-Ni steel; (c) SEM image of 18-Ni steel, the upper right corner picture magnifies the of α phase area; (d) 25-Ni steel EBSD image; (e) phase distribution of 25-Ni steel; (f) 25-Ni steel SEM image.
图 2 不同成分钢相体积占比随温度变化相图 (a) 18-Ni钢; (b) 25-Ni钢
Fig. 2. Phase volume-temperature phase diagrams of different steels: (a) 18-Ni steel; (b) 25-Ni steel.
图 3 锻造态样品在550 ℃ LBE腐蚀600 h后宏观形貌图 (a) 18-Ni钢; (b) 25-Ni钢
Fig. 3. Macro morphology of the forged steels after 600 h LBE corrosion at 550 ℃: (a) 18 Ni steel; (b) 25-Ni steel.
图 4 锻造态18-Ni钢和25-Ni钢在550 ℃ LBE中腐蚀600 h后表面XRD图
Fig. 4. XRD patterns of forged 18-Ni steel and 25-Ni steel after 600 h LBE corrosion at 550 ℃.
图 5 样品在550 ℃ LBE腐蚀600 h后表面SEM图 (a), (b) 18-Ni钢; (c), (d) 25-Ni钢
Fig. 5. The surface SEM image of the sample after LBE corrosion at 550 °C for 600 h: (a), (b) 18-Ni steel; (c), (d) 25-Ni steel.
图 6 锻造态样品在550 ℃ LBE中腐蚀600 h的截面SEM图 (a) 18-Ni钢; (b) 25-Ni钢
Fig. 6. SEM images show the cross-sectional oxide layer morphology of the forged steels after LBE corrosion at 550 °C: (a) 18-Ni steel; (b) 25-Ni steel.
图 7 锻造态样品在550 ℃ LBE中腐蚀600 h的截面EDS图 (a) 18-Ni钢; (b) 25-Ni钢
Fig. 7. Cross-section EDS diagram of forged steels after LBE corrosion at 550 °C: (a) 18-Ni steel; (b) 25-Ni steel.
图 8 锻造态钢和850 ℃高温预氧化后钢的XRD图
Fig. 8. XRD patterns of the forged steels and pre-oxidized steels at 850 ℃.
图 9 850 ℃预氧化20 h后18-Ni钢和25-Ni钢的拉曼光谱图
Fig. 9. Raman spectra of different samples obtained with 532 nm excitation wavelength: (a) 18-Ni steel; (b) 25-Ni steel.
图 10 850 ℃预氧化20 h后18-Ni钢的表面SEM图
Fig. 10. SEM images of the surface of 18-Ni steel after pr-oxidation at 850 ℃ for 20 h.
图 11 850 ℃预氧化20 h后25-Ni钢的表面SEM图
Fig. 11. SEM image of the surface of 25-Ni steel after pre-oxidation at 850 ℃ for 20 h.
图 12 850 ℃预氧化20 h后18-Ni钢和25-Ni钢的截面EDS图 (a) 18-Ni钢; (b) 25-Ni钢
Fig. 12. Cross-section EDS diagrams of 18-Ni steel and 25-Ni steel after pre-oxidation at 850 ℃ for 20 h: (a) 18-Ni steel; (b) 25-Ni steel.
图 13 预氧化后的18-Ni钢和25-Ni钢在550 ℃ LBE腐蚀600 h后的XRD图
Fig. 13. The XRD diagram of pre-oxidized 18-Ni steel and 25-Ni steel after LBE corrosion at 550 ℃.
图 14 预氧化样品在550 ℃ LBE腐蚀600 h后的表面SEM图 (a), (b) 18-Ni钢; (c), (d) 25-Ni钢
Fig. 14. Surface SEM images of pre oxidized samples after LBE corrosion at 550 ℃ for 600 h: (a) (b) 18-Ni steel; (c), (d) 25-Ni steel.
图 15 预氧化样品在550 ℃ LBE腐蚀600 h后的截面EDS图 (a) 18-Ni钢; (b) 25-Ni钢
Fig. 15. Cross section EDS diagram of pre-oxidized sample after 600 h of LBE corrosion at 550 ℃: (a) 18-Ni steel; (b) 25-Ni steel.
图 16 锻造态样品钢腐蚀过程示意图 (a) 18-Ni钢; (b) 25-Ni钢
Fig. 16. Schematic diagram shows the corrosion process of the forged steels: (a) 18-Ni steel; (b) 25-Ni steel.
图 17 预氧化后样品钢腐蚀过程示意图 (a) 18-Ni钢; (b) 25-Ni钢
Fig. 17. Schematic diagram shows the corrosion process of the pre-oxidized steels: (a) 18-Ni steel; (b) 25-Ni steel.
表 1 18-Ni钢和25-Ni钢的实际化学成分(质量分数, %)
Table 1. The actual chemical composition of 18-Ni steel and 25-Ni steel (mass percentage, %).
Ni Cr Al Mo Nb Fe 18-Ni 19.25 14.21 2.66 3.62 1.8 Bal. 25-Ni 26.67 14.11 2.76 3.55 1.81 Bal. 
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区域 Cr Al Fe Nb O 点1 0.3 0 43.3 2.7 53.6 点2 2.2 13.6 10.6 12.4 47.0 点3 1.9 16.6 7.3 2.0 48.2 点4 1.3 0.5 58.9 0.7 35.5 点5 18.8 1.9 36.4 2.2 37.0 点6 8.6 8.6 34.0 17.5 7.9
下载: 导出CSV
区域 Cr Al Fe O 点7 3.28 1.51 50.12 38.59 点8 9.94 14.24 44.26 9.46 点9 7.56 2.18 51.11 36.15 点10 25.00 5.88 38.62 22.34 点11 15.42 0.69 75.67 5.20
下载: 导出CSV
区域 Cr Al Fe Ni O 点12 9.2 4.4 49.5 4.2 30.9 点13 1.5 39.7 2.6 2.1 53.5 点14 1.1 1.1 85.7 0.0 10.9 点15 2.1 17.8 7.4 20.9 5.20
下载: 导出CSV
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Google Scholar
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Google Scholar
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