Thermal-shock Properties and Anticorrosion Behavior in Static LBE of Al2O3-TiO2/FeCrAl Coating by Multi-Arc Ion Plating
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摘要: 为探索一种核电用包壳材料FeCrAl合金表面涂层的制备方法，本文利用多弧离子镀技术在FeCrAl合金表面制备了以FeCrAl作为过渡层的Al2O3-TiO2涂层，对试样进行热冲击实验以探究涂层的抗热冲击性能，对试样进行600℃、1000 h静态铅铋合金（LBE）腐蚀实验，研究涂层的耐腐蚀性能，表征和分析了试样经LBE腐蚀前后的相组成和显微形貌。结果表明，通过多弧离子镀制备的Al2O3-TiO2为非晶态，30次热冲击试验后涂层未出现开裂、脱落等现象。腐蚀后，FeCrAl基体试样表面发生明显溶解腐蚀。而X射线衍射分析显示涂层试样在腐蚀后Al2O3发生结晶，表层Al2O3结构收缩出现孔隙，而涂层内部仍保持致密，且截面分析显示LBE未渗入涂层内部。因此，Al2O3-TiO2/FeCrAl涂层能有效地阻止LBE对基体材料的腐蚀。
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关键词:
- FeCrAl合金 /
- 多弧离子镀 /
- Al2O3-TiO2/FeCrAl涂层 /
- 抗热冲击性能 /
- 铅铋合金（LBE）腐蚀
Abstract: This work aims to explore a method for preparing the surface coating of FeCrAl alloy, a cladding material in nuclear power industry. The Al2O3-TiO2 coating with FeCrAl as the intermediate layer was prepared on FeCrAl alloy by multi-arc ion plating. The thermal-shock test was carried out to explore the thermal-shock resistance of the coating. The corrosion resistance of the coating was studied after the static lead-bismuth eutectic (LBE) corrosion test at 600℃ for 1000 h. The phase composition and micromorphologies of substrate and coating samples before and after LBE corrosion were characterized. The results showed that the Al2O3-TiO2 prepared by multi-arc ion plating was amorphous. After 30 thermal shock tests, the coating did not crack or fall off. After the corrosion, the surface of FeCrAl substrate showed obvious dissolution corrosion. GIXRD results showed that Al2O3 crystallization occurred in the coating samples after corrosion. The Al2O3 structure on the surface shrank and pores appeared, while the inner layer of the coating remained dense. The sectional analysis showed that LBE did not penetrate into the coating. Therefore, the Al2O3-TiO2/FeCrAl coating can effectively protect the substrate from LBE corrosion. -
图 2 原始Al2O3-TiO2/FeCrAl涂层试样截面SEM形貌
Figure 2. SEM Morphology of the Original Al2O3-TiO2/FeCrAl Coating Sample Section
图 3 原始Al2O3-TiO2/FeCrAl涂层试样表面SEM形貌及EDS面扫
Figure 3. SEM Morphology and EDS Mapping of the Original Al2O3-TiO2/FeCrAl Coating Sample Surface
图 4 原始Al2O3-TiO2/FeCrAl涂层试样表面GIXRD图谱
Figure 4. GIXRD Pattern of the Original Al2O3-TiO2/FeCrAl Coating Sample Surface
图 5 Al2O3-TiO2/FeCrAl涂层试样热冲击试验0~30次后宏观形貌
Figure 5. Macro-Morphology of the Al2O3-TiO2/FeCrAl Coating Samples after 0~30 Thermal-Shock Tests
图 6 Al2O3-TiO2/FeCrAl涂层试样经30次热冲击试验后 SEM 形貌
Figure 6. SEM Morphology of the Al2O3-TiO2/FeCrAl Coating Samples after Thirty Thermal-shock Tests
图 7 Al2O3-TiO2/FeCrAl涂层试样600℃下LBE腐蚀1000 h后表面SEM形貌及EDS面扫
Figure 7. SEM Morphology and EDS Mapping Analysis of the Al2O3-TiO2/FeCrAl Coating Sample Surface after LBE Corrosion at 600℃ for 1000 h
图 8 Al2O3-TiO2/FeCrAl涂层试样600℃下LBE腐蚀1000 h后表面GIXRD图谱
Figure 8. GIXRD Pattern of the Al2O3-TiO2/FeCrAl Coating Surface after LBE Corrosion at 600℃ for 1000 h
图 9 FeCrAl基体试样600℃下LBE腐蚀1000 h后表面SEM形貌及EDS面扫
Figure 9. SEM Morphology and EDS Mapping of the FeCrAl Substrate Surface after LBE Corrosion at 600℃ for 1000 h
图 10 Al2O3-TiO2/FeCrAl涂层试样600℃下LBE腐蚀1000 h截面SEM形貌及EDS面扫
Figure 10. SEM Morphology and EDS Mapping of the Al2O3-TiO2/FeCrAl Coating Sample Section after LBE Corrosion at 600℃ for 1000 h
图 11 Al2O3-TiO2/FeCrAl涂层LBE腐蚀机理示意图
Figure 11. Schematics of Corrosion Mechanism of the Al2O3-TiO2/FeCrAl Coating after Liquid LBE Corrosion
图 12 FeCrAl基体试样600℃下LBE腐蚀1000 h后试样截面EDS面扫
Figure 12. EDS Mapping of the FeCrAl Substrate Sample Section after LBE Corrosion at 600℃ for 1000 h
表 1 图2 EDS点扫结果
Table 1. EDS Results of Fig.2
点1 点2 点3 元素 原子百分比/% 元素 原子百分比/% 元素 原子百分比/% O 59.69 Al 4.30 O 15.93 Al 24.28 Cr 24.75 Al 10.66 Ti 10.14 Fe 70.95 Cr 12.36 Cr 3.64 Fe 61.05 Fe 2.25 总量 100.00 总量 100.00 总量 100.00 
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表 2 图6 EDS点扫结果
Table 2. EDS Results of Fig.6
点1 点2 元素 原子百分比/% 元素 原子百分比/% O 56.25 Al 4.09 Al 30.46 Ti 0.48 Ti 11.70 Cr 25.83 Cr 0.37 Fe 69.60 Fe 1.22 总量 100.00 总量 100.00
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表 3 图7 EDS点扫结果
Table 3. EDS Results of Fig.7
元素 原子百分比/% O 60.72 Al 30.44 Ti 7.42 Cr 0.54 Fe 0.88 总量 100.00
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