含Sc超高强Al-Zn-Mg-Cu-Zr合金的均匀化和腐蚀行为研究
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摘要
采用活性熔剂保护熔炼,水冷铜模激冷铸造技术制备Al-8.1Zn-2.3Cu-2.05Mg-0.21Sc-0.12Zr合金铸锭。通过金相显微镜(OM)、扫描电镜(SEM),透射电镜(TEM)、差热分析(DSC)和X射线衍射(XRD)等分析手段,研究合金均匀化处理前后合金相组成和化学成分的变化。合金经均匀化、热轧、中间退火、冷轧成2.2 mm厚的板材。研究合金板材在不同时效制度下的晶间腐蚀、剥落腐蚀和应力腐蚀行为,以及不同时效制度下合金板材电化学阻抗谱的变化规律。得出了以下主要结论：
(1)铸态Al-8.1Zn-2.3Cu-2.05Mg-0.21Sc-0.12Zr合金的晶界偏析比较严重,经均匀化处理后,合金晶界变得细小稀疏,合金元素分布趋于均匀,T相(Al2Mg3Zn3)完全回溶到基体中。合金适宜的均匀化处理制度为470℃×24 h,与均匀化动力学分析结果相符。
(2)含Sc超高强Al-Zn-Cu-Mg-Zr合金单级时效后的晶间腐蚀和剥落腐蚀敏感性顺序为：自然时效>欠时效>峰时效>过时效。对合金腐蚀发展过程的电化学阻抗谱进行等效电路拟合,拟合数据与实验结果一致。随着在EXCO溶液中浸泡时间的延长,极化电阻值增大,合金的抗电化学腐蚀性能增强。自然时效态合金的极化电阻(Rpo)值较人工时效态低,表明人工时效处理能提高合金抗应力腐蚀的能力,其中过时效态合金的抗腐蚀性能最好。
(3)与T6峰时效处理相比,双级时效或回归再时效后合金的晶间腐蚀深度都较浅,剥落腐蚀等级较低。电化学阻抗谱分析表明,双级时效和回归再时效处理后,合金的孔隙电容值减小,极化电阻值增大,抗剥落腐蚀性能提高。
(4)在3.5%NaCl溶液中,T6峰时效态合金对应变速率为1×10-6s-1的应力腐蚀最为敏感。T6峰时效态合金应力腐蚀断口呈沿晶腐蚀断裂形貌,应力腐蚀区为准解理形貌,晶界处韧窝小且浅,断口中也存在大量的沿晶裂纹和二次裂纹,而双级时效和回归再时效态合金二次裂纹较少,具有较强的抗应力腐蚀能力。
(5)含Sc超高强Al-Zn-Cu-Mg-Zr合金抗应力腐蚀性能提高的主要原因是晶界析出相聚集粗化并呈断续分布。这种晶界结构一方面阻断了晶界的阳极溶解；另一方面粗大的晶界析出相成为氢原子的不可逆陷阱,降低了晶界的氢脆倾向。
Al-8.1Zn-2.3Cu-2.05Mg-0.21Sc-0.12Zr alloy ingot was prepared by using active flux and water chilling copper mould. The phase constituents and composition distribution of the as-cast and homogenized alloy were studied by optical microscopy (OM), electronic microstructure analysis (SEM, TEM), differential scanning calorimeter (DSC) and X-ray diffraction (XRD). Then, the homogenized alloy was hot rolled, annealed and cold rolled into a sheet with thickness of 2.2 mm. The intergranular corrosion, exfoliation corrosion and stress corrosion behaviour of the alloy were studied, and the experimental results were analysized by means of Electrochemical Impedance Spectroscopy (EIS). The conclusions can be summarized as follows:
(1) The main phases of the as-cast are Serious grain boundary segregation exists in the as-cast Al-8.1Zn-2.3Cu-2.05Mg-0.21Sc-0.12Zr alloy. After homogenization, the grain boundaries become sparse, and the alloying elements distributed uniformly. The T (Al2Mg3Zn3) phase dissolves completely into matrix during homogenization. The proper homogenizing process is 470℃×24 h which is consistent with the result of homogenization kinetics analysis.
(2) The sequence of corrosion susceptibility of the one-stage aged alloys is: over-aged> peak-aged> under-aged> nature-aged. All EIS patterns are simulated, and the good agreement between the experimental results and the simulated results has been obtained. The polarization resistance for the alloys increases with the immersion time, which induces an increase in the electrochemical corrosion resistance of the alloy. On the other hand, the artificial aging heat treatment can provide better electrochemical corrosion behaviour than the naturally aging treatment. And the susceptibility of the over-aged alloy is the lowest.
(3) The RRA or two-stage age treatment can provide the less depth of intergranular corrison and lower exfoliation corrosion grade than T6 peak-aged treatment. The results from the electrochemical impedance show that after the RRA or two-stage age treatment, the C2 to the capacitance of the pore layer decreases and the polarization resistance increases, which means that the RRA and two-stage age treatment can improve the corrosion resistance of the alloy.
(4) The T6 peak-aged alloy is the most susceptible to SCC in 3.5% NaCl solution at 1×10-6s-1. The fractograph of the alloy reveals intergranular fracture, with a small amount dimples along grain boundaries and a large number of secondary cracks. While the number of the secondary cracks is relatively less for the two-step aged or RRA alloy at the same strain rate, indicating that the two-step aging or RRA treatment can improve the resistance to stress corrosion.
(5) The increase of the stress corrison resistance of the alloys is mainly due to the accumulation and discontinuous distribution of grain boundary precipitates. On the one hand, the grain boundary structure block the anodic dissolution of the grain boundary precipitates; on the other hand, the coarse grain boundary precipitates are irreversible hydrogen traps, which reduce the tendency of the grain boundary embrittlement.
(1)铸态Al-8.1Zn-2.3Cu-2.05Mg-0.21Sc-0.12Zr合金的晶界偏析比较严重,经均匀化处理后,合金晶界变得细小稀疏,合金元素分布趋于均匀,T相(Al2Mg3Zn3)完全回溶到基体中。合金适宜的均匀化处理制度为470℃×24 h,与均匀化动力学分析结果相符。
(2)含Sc超高强Al-Zn-Cu-Mg-Zr合金单级时效后的晶间腐蚀和剥落腐蚀敏感性顺序为：自然时效>欠时效>峰时效>过时效。对合金腐蚀发展过程的电化学阻抗谱进行等效电路拟合,拟合数据与实验结果一致。随着在EXCO溶液中浸泡时间的延长,极化电阻值增大,合金的抗电化学腐蚀性能增强。自然时效态合金的极化电阻(Rpo)值较人工时效态低,表明人工时效处理能提高合金抗应力腐蚀的能力,其中过时效态合金的抗腐蚀性能最好。
(3)与T6峰时效处理相比,双级时效或回归再时效后合金的晶间腐蚀深度都较浅,剥落腐蚀等级较低。电化学阻抗谱分析表明,双级时效和回归再时效处理后,合金的孔隙电容值减小,极化电阻值增大,抗剥落腐蚀性能提高。
(4)在3.5%NaCl溶液中,T6峰时效态合金对应变速率为1×10-6s-1的应力腐蚀最为敏感。T6峰时效态合金应力腐蚀断口呈沿晶腐蚀断裂形貌,应力腐蚀区为准解理形貌,晶界处韧窝小且浅,断口中也存在大量的沿晶裂纹和二次裂纹,而双级时效和回归再时效态合金二次裂纹较少,具有较强的抗应力腐蚀能力。
(5)含Sc超高强Al-Zn-Cu-Mg-Zr合金抗应力腐蚀性能提高的主要原因是晶界析出相聚集粗化并呈断续分布。这种晶界结构一方面阻断了晶界的阳极溶解；另一方面粗大的晶界析出相成为氢原子的不可逆陷阱,降低了晶界的氢脆倾向。
Al-8.1Zn-2.3Cu-2.05Mg-0.21Sc-0.12Zr alloy ingot was prepared by using active flux and water chilling copper mould. The phase constituents and composition distribution of the as-cast and homogenized alloy were studied by optical microscopy (OM), electronic microstructure analysis (SEM, TEM), differential scanning calorimeter (DSC) and X-ray diffraction (XRD). Then, the homogenized alloy was hot rolled, annealed and cold rolled into a sheet with thickness of 2.2 mm. The intergranular corrosion, exfoliation corrosion and stress corrosion behaviour of the alloy were studied, and the experimental results were analysized by means of Electrochemical Impedance Spectroscopy (EIS). The conclusions can be summarized as follows:
(1) The main phases of the as-cast are Serious grain boundary segregation exists in the as-cast Al-8.1Zn-2.3Cu-2.05Mg-0.21Sc-0.12Zr alloy. After homogenization, the grain boundaries become sparse, and the alloying elements distributed uniformly. The T (Al2Mg3Zn3) phase dissolves completely into matrix during homogenization. The proper homogenizing process is 470℃×24 h which is consistent with the result of homogenization kinetics analysis.
(2) The sequence of corrosion susceptibility of the one-stage aged alloys is: over-aged> peak-aged> under-aged> nature-aged. All EIS patterns are simulated, and the good agreement between the experimental results and the simulated results has been obtained. The polarization resistance for the alloys increases with the immersion time, which induces an increase in the electrochemical corrosion resistance of the alloy. On the other hand, the artificial aging heat treatment can provide better electrochemical corrosion behaviour than the naturally aging treatment. And the susceptibility of the over-aged alloy is the lowest.
(3) The RRA or two-stage age treatment can provide the less depth of intergranular corrison and lower exfoliation corrosion grade than T6 peak-aged treatment. The results from the electrochemical impedance show that after the RRA or two-stage age treatment, the C2 to the capacitance of the pore layer decreases and the polarization resistance increases, which means that the RRA and two-stage age treatment can improve the corrosion resistance of the alloy.
(4) The T6 peak-aged alloy is the most susceptible to SCC in 3.5% NaCl solution at 1×10-6s-1. The fractograph of the alloy reveals intergranular fracture, with a small amount dimples along grain boundaries and a large number of secondary cracks. While the number of the secondary cracks is relatively less for the two-step aged or RRA alloy at the same strain rate, indicating that the two-step aging or RRA treatment can improve the resistance to stress corrosion.
(5) The increase of the stress corrison resistance of the alloys is mainly due to the accumulation and discontinuous distribution of grain boundary precipitates. On the one hand, the grain boundary structure block the anodic dissolution of the grain boundary precipitates; on the other hand, the coarse grain boundary precipitates are irreversible hydrogen traps, which reduce the tendency of the grain boundary embrittlement.
引文
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