挤压铸造Al-5.0Cu合金中富铁相形成特点及力学性能研究
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摘要
高强韧的铸造Al-Cu合金广泛应用于航空航天和交通运输等领域。铁是该合金中难以避免但对合金性能危害最大的杂质元素。为了实现Al-Cu合金的高性能，杂质元素铁的含量往往控制非常严格（一般低于0.15%），导致该合金材料的成本大幅上升，同时也限制了回收铝合金的大量使用。因此，采用先进工艺提高Al-Cu合金中杂质Fe的允许含量，成为开发高性能、低成本铝铜合金材料的重要途径之一。
本文采用挤压铸造与Mn中和变质工艺相结合，利用光学显微镜（OM）、定量金相分析、扫描电子显微镜（SEM）、X射线衍射分析（XRD）、差热扫描分析（DSC）、电子探针（EPMA）、透射电子显微镜（TEM）、液淬、深腐蚀等手段研究了挤压铸造铝铜合金中富铁相的形成特点以及Mn含量、Fe含量、挤压压力和热处理对合金室温和高温力学性能的影响，并取得以下结果：
当铁含量从0.1%增加到1.5%，铸态Al-5.0Cu-0.6Mn合金中的富铁相由-Fe(Al15(FeMn)3(CuSi)2)和β-Fe (Al7Cu2(FeMn))逐渐变为Al6(FeMn)和Al3(FeMn)。无论是挤压铸造还是重力铸造，铸态合金的伸长率随着Fe含量增大逐渐降低，但合金的抗拉强度在铁含量为0.5%附近存在峰值。这主要是由于少量的汉字状富铁相有利于强度的提高，而对塑性不利。T5热处理后，直接从液相中形成的β-Fe相很稳定，依然呈针状形貌，而汉字状的-Fe、Al6(FeMn)相和针状Al3(FeMn)转变成了一种新的富铁相(CuFe)-(Al7Cu2(FeMn))。无论是挤压铸造还是重力铸造，当铁含量从0.1%增加到1.5%，T5热处理态合金的力学性能逐渐下降。富铁相导致热处理态挤压铸造Al-5.0Cu-0.6Mn合金力学性能下降的原因是富Cu的(CuFe)相大量形成，消耗了基体中的部分Cu和Mn，导致基体中强化相减少和晶粒尺寸增大。挤压压力从0MPa增加到75MPa时，不同铁含量合金的伸长率增加近2倍。挤压铸造合金力学性能明显优于重力铸造合金，尤其是合金的伸长率，这主要与压力导致孔洞减少，(Al)枝晶和第二相细化，针状富铁相减少有关。
研究了不同Fe含量Al-5.0Cu-0.6Mn合金的高温力学性能。随着拉伸温度的升高，不同Fe含量Al-5.0Cu-0.6Mn合金的抗拉强度、屈服强度都显著地降低，而伸长率都显著地增大。随着Fe含量增大，合金的抗拉强度和屈服强度都显著降低。随着压力的增大，各合金的力学性能都得到了一定程度的提升，尤其是合金的伸长率。然而随着温度的升高，挤压压力对合金强度的提升变得不明显。
研究了不同Mn/Fe比对Al-5.0Cu-0.5Fe合金组织和力学性能的影响。铸态Al-5.0Cu-0.5Fe合金中的富铁相包括汉字状的AlmFe,-Fe, Al6(FeMn),以及针状的-Fe。对于重力铸造合金，当Mn/Fe比为1.6时，铸态合金获得最佳的综合力学性能，这主要是由于所有针状β-Fe都转变成为了汉字状-Fe，铸造缺陷最少。对于挤压铸造合金，Mn/Fe比仅需0.8，所有针状β-Fe都转变成为了汉字状-Fe。合金经过T5热处理后，汉字状的AlmFe,-Fe和Al6(FeMn)相转变成了一种新的汉字状的富铁相(CuFe)。T5热处理态Al-5.0Cu-0.5Fe合金的最合适Mn/Fe比不仅取决于合金中富铁相的形貌以及铸造缺陷，还与热处理后的(Al)枝晶尺寸以及(Al)基体里面的θ’相和T(Al20Cu2Mn3)相数量有关。
研究了铝铜合金凝固过程中富铁相的形成特点。当Fe含量在0.1-1.5%范围内变化时，β-Fe、AlmFe、-Fe、Al6(FeMn)、Al3(FeMn)都有可能成为铝铜合金中的主要富铁相，这取决于合金中不同Mn含量、Fe含量和挤压压力。Mn含量的增加将促进-Fe相的形成，同时抑制AlmFe和β-Fe的形成。液淬试验发现，铝铜合金中首先形成的富铁相为AlmFe、Al6(FeMn)和Al3(FeMn)相。AlmFe和Al3(FeMn)容易在低Fe（低于0.5%）和低Mn（低于0.2%）含量的合金中形成，Al6(FeMn)容易在高Mn（大于0.4%）含量的合金中形成，凝固结束后将部分或全部转变为β-Fe或-Fe。在高铁含量（大于0.5%）的Al-5.0Cu-0.6Mn合金中，Al6(FeMn)和Al3(FeMn)相作为合金中主要稳定富铁相存在。挤压压力可以促进汉字状富铁相AlmFe、-Fe和Al6(FeMn)相的形成，抑制或减少针状β-Fe和Al3(FeMn)相的形成，这主要是由于高的冷却速度以及不同富铁相的晶体结构。挤压压力可以促进富铁相的形核，同时降低合金的扩散系数，从而抑制富铁相的长大。挤压压力提高了-Fe和AlmFe的形成温度，同时降低了β-Fe的形成温度。
研究了铝铜合金固溶处理过程中富铁相特征的演变规律，发现固溶温度、固溶时间和挤压压力都将促进AlmFe、Al6(FeMn)、-Fe和Al3(FeMn)相向β-Fe的转变。新形成的β-Fe易于在-Fe，Al6(FeMn)、AlmFe和Al3(FeMn)与(Al)界面处形核，并沿富铁相长大。
The Al-Cu cast alloys with high strength and toughness are widely used in the aerospaceand transportation industry. The impurity of Fe is inevitable and considered to be the mostdetrimental to mechanical properties. The Fe content is strictly controlled (mostly below0.15%) in order to get high performance properties. This will make the alloys expensive toproduce and limit the use of recycled aluminum alloys. Finding an advanced process toincrease the allowable Fe content of Al-Cu alloys has been became an important way todevelop low cost aluminum alloys with high performance.
In this study, the Al-Cu alloys are prepared by combining squeeze casting and Mnmodification. Various test techniques, including optical microscopy (OM), image analysis,scanning electron microscope (SEM), X-ray diffraction (XRD), differential scanningcalorimeter (DSC),water quenching, deep etched technology, electron probemicro-analyzer (EPMA) and transmission electron microscopy (TEM) are used to examinethe formation of Fe-rich intermetallics in squeeze cast Al-Cu alloys and the effect of Mn andFe content, applied pressure and heat treatment on microstructures and mechanical propertiesat room and elevated temperature of the alloys. The experimental results are as followed:
When the Fe content increases from0.1wt%to1.5wt%, the Fe-rich intermetallics ofas-cast Al-5.0Cu-0.6Mn alloys are-Fe (Al15(FeMn)3(CuSi)2) and β-Fe (Al7Cu2(FeMn)) inlow Fe content, while it will change into Al6(FeMn) and Al3(FeMn) in high Fe content. Theelongations of gravity die cast and squeeze cast alloys decreases gradually with increasing theFe content and there is a peak value of ultimate strength and yield strength for the alloy with0.5wt%Fe. The reason is that the small Chinese-script Fe-rich intermetallics in low Fecontent alloys are useful to improve the alloy strength through second phase hardening,although these brittle second intermetallics will cause a reduction in ductility. The elongationof the alloys with different Fe content increases more than2times when the applied pressureincreases from0MPa to75MPa. The improvement of mechanical properties is due to theporosity reduction,(Al) dendrite refinement and the decreasment of intermetallics. Thechemical composition and the needle-like shape of β-Fe (Al7Cu2Fe) solidified from the Alalloy melt have no change after T5heat treatment. However, the Chinese script-Fe,Al6(FeMn) and needle-like Al3(FeMn) transform partially to a new Chinese script (CuFe)-Al7Cu2(FeMn). When the Fe content increases from0.1wt%to1.5wt%, the mechanicalproperties of both the gravity die cast and squeeze cast alloys decrease gradually with increasing of Fe content. The Fe-rich intermetallics leads to the decrease of mechanicalproperties due to the increase amount of (CuFe), decrease of precipitation particles in (Al)matrix and the increase of (Al) dendrite size. The elongation of the alloys with different Fecontent increases more than2times when the applied pressure increases from0MPa to75MPa. The squeeze cast alloys with different Fe contents have superior mechanical propertiescompared to the gravity die cast alloys, which is mainly attributed to the reduction of porosity,the refinement of Fe-rich intermetallics and (Al) dendrite and the decrease of needle-likeFe-rich intermetallics.
The mechanical properties at elevated temperature of Al-5.0Cu-0.6Mn alloys with differentFe content have been investigated. The ultimate tensile strength and yield strength ofAl-5.0Cu-0.6Mn alloys with different Fe content decrease with incresing the tensiletemperature, while the elongation increases obviously. The ultimate tensile strength and yieldstrength of Al-5.0Cu-0.6Mn alloys with different Fe content decrease with the incresing theFe contetn. The mechanical properties at different temperature increase with increasingapplied pressure, especially the elongation. However, the increasment becomes slightly whenthe temeperature increases.
The effect of Mn/Fe ratio on the microstructure and mechanical properties has been studied.The Fe-rich intermetallics, which may present in Al-5.0Cu-0.5Fe alloys with different Mn/Feraito, including Chinese script AlmFe,-Fe, Al6(FeMn), and needle-like-Fe. The optimalMn/Fe mass ratios is1.6for the best mechanical properties when the applied pressure is0MPa due to the needle-like β-Fe is completely converted to the Chinese script-Fe and theminimum volume percent of prosity. Only Mn/Fe mass ratio of0.8is needed for the completeconvert of β-Fe phase to-Fe phase when the applied pressure is75MPa. After T5heattreatment, the Chinese script AlmFe,-Fe and Al6(FeMn) transform to a new Chinese script(CuFe). The optimal Mn/Fe ratio for the best mechanical properties of heat-treated alloy isdetermined by the morphology of Fe-rich intermetallics, volume fraction of θ’ and T(Al20Cu2Mn3), size of (Al) dendrite and porosity.
The formation of Fe-rich intermetallics during solidification of Al-Cu alloys has beenstudied. When the Fe content varies from0.1%to1.5%, β-Fe, AlmFe,-Fe, Al6(FeMn) andAl3(FeMn) are all possible to be the dominant Fe-rich intermetallic phases in the solidifiedmicrostructure of Al-Cu alloys, depending on different Mn, Fe contents and applied pressures.The Mn addition will promote the formation of-Fe and prevent the formation of AlmFe andβ-Fe. The primary Fe-rich intermetallics which formed from the Al alloy melt are AlmFe,Al6(FeMn) and Al3(FeMn) through observing the microstructures of the water quenched specimens. AlmFe and Al3(FeMn) preferably precipitates in low Mn (below0.2%) and Felevels (below0.5%) alloys. Al6(FeMn) preferably forms at high Mn (above0.4%) contentalloys， they will partly or completely change into β-Fe or-Fe, respectively, aftersolidification. In the Al-5.0Cu-0.6Mn alloys with high Fe content (above1.0%), theAl6(FeMn) and Al3(FeMn) are considered to be the dominate stable Fe-rich intermetallics.The applied pressure is favor to the formation of Chinese script Fe-rich intermetallics AlmFe、
-Fe and Al6(FeMn) and prevents the precipitate of needle-like β-Fe and Al3(FeMn) becausethe high cooling rate and the growth rate of the Fe-rich intermetallics with different crystalstructure. The applied pressure will promote the nucleation rate of Fe-rich intetmetallics anddecrease the diffusion coefficient of elements, which leads to growth inhibition of Fe-richintermetallics. The formation temperature increases for-Fe and AlmFe but decreases forβ-Fe with the increase of applied pressure.
The evolution of Fe-rich intermetallics characteristics during solution heat treatment (SHT)of Al-Cu alloys has been studied. It is found that the SHT temperature and time, the appliedpressure promote the transformation of AlmFe、Al6(FeMn)、-Fe and Al3(FeMn) to new β-Fe.The new β-Fe preferentiallynucleates various points on the interface between the AlmFe,-Fe,Al6(FeMn), Al3(FeMn) and the (Al) matrix, then grows into the Fe-rich intermetallics.
本文采用挤压铸造与Mn中和变质工艺相结合，利用光学显微镜（OM）、定量金相分析、扫描电子显微镜（SEM）、X射线衍射分析（XRD）、差热扫描分析（DSC）、电子探针（EPMA）、透射电子显微镜（TEM）、液淬、深腐蚀等手段研究了挤压铸造铝铜合金中富铁相的形成特点以及Mn含量、Fe含量、挤压压力和热处理对合金室温和高温力学性能的影响，并取得以下结果：
当铁含量从0.1%增加到1.5%，铸态Al-5.0Cu-0.6Mn合金中的富铁相由-Fe(Al15(FeMn)3(CuSi)2)和β-Fe (Al7Cu2(FeMn))逐渐变为Al6(FeMn)和Al3(FeMn)。无论是挤压铸造还是重力铸造，铸态合金的伸长率随着Fe含量增大逐渐降低，但合金的抗拉强度在铁含量为0.5%附近存在峰值。这主要是由于少量的汉字状富铁相有利于强度的提高，而对塑性不利。T5热处理后，直接从液相中形成的β-Fe相很稳定，依然呈针状形貌，而汉字状的-Fe、Al6(FeMn)相和针状Al3(FeMn)转变成了一种新的富铁相(CuFe)-(Al7Cu2(FeMn))。无论是挤压铸造还是重力铸造，当铁含量从0.1%增加到1.5%，T5热处理态合金的力学性能逐渐下降。富铁相导致热处理态挤压铸造Al-5.0Cu-0.6Mn合金力学性能下降的原因是富Cu的(CuFe)相大量形成，消耗了基体中的部分Cu和Mn，导致基体中强化相减少和晶粒尺寸增大。挤压压力从0MPa增加到75MPa时，不同铁含量合金的伸长率增加近2倍。挤压铸造合金力学性能明显优于重力铸造合金，尤其是合金的伸长率，这主要与压力导致孔洞减少，(Al)枝晶和第二相细化，针状富铁相减少有关。
研究了不同Fe含量Al-5.0Cu-0.6Mn合金的高温力学性能。随着拉伸温度的升高，不同Fe含量Al-5.0Cu-0.6Mn合金的抗拉强度、屈服强度都显著地降低，而伸长率都显著地增大。随着Fe含量增大，合金的抗拉强度和屈服强度都显著降低。随着压力的增大，各合金的力学性能都得到了一定程度的提升，尤其是合金的伸长率。然而随着温度的升高，挤压压力对合金强度的提升变得不明显。
研究了不同Mn/Fe比对Al-5.0Cu-0.5Fe合金组织和力学性能的影响。铸态Al-5.0Cu-0.5Fe合金中的富铁相包括汉字状的AlmFe,-Fe, Al6(FeMn),以及针状的-Fe。对于重力铸造合金，当Mn/Fe比为1.6时，铸态合金获得最佳的综合力学性能，这主要是由于所有针状β-Fe都转变成为了汉字状-Fe，铸造缺陷最少。对于挤压铸造合金，Mn/Fe比仅需0.8，所有针状β-Fe都转变成为了汉字状-Fe。合金经过T5热处理后，汉字状的AlmFe,-Fe和Al6(FeMn)相转变成了一种新的汉字状的富铁相(CuFe)。T5热处理态Al-5.0Cu-0.5Fe合金的最合适Mn/Fe比不仅取决于合金中富铁相的形貌以及铸造缺陷，还与热处理后的(Al)枝晶尺寸以及(Al)基体里面的θ’相和T(Al20Cu2Mn3)相数量有关。
研究了铝铜合金凝固过程中富铁相的形成特点。当Fe含量在0.1-1.5%范围内变化时，β-Fe、AlmFe、-Fe、Al6(FeMn)、Al3(FeMn)都有可能成为铝铜合金中的主要富铁相，这取决于合金中不同Mn含量、Fe含量和挤压压力。Mn含量的增加将促进-Fe相的形成，同时抑制AlmFe和β-Fe的形成。液淬试验发现，铝铜合金中首先形成的富铁相为AlmFe、Al6(FeMn)和Al3(FeMn)相。AlmFe和Al3(FeMn)容易在低Fe（低于0.5%）和低Mn（低于0.2%）含量的合金中形成，Al6(FeMn)容易在高Mn（大于0.4%）含量的合金中形成，凝固结束后将部分或全部转变为β-Fe或-Fe。在高铁含量（大于0.5%）的Al-5.0Cu-0.6Mn合金中，Al6(FeMn)和Al3(FeMn)相作为合金中主要稳定富铁相存在。挤压压力可以促进汉字状富铁相AlmFe、-Fe和Al6(FeMn)相的形成，抑制或减少针状β-Fe和Al3(FeMn)相的形成，这主要是由于高的冷却速度以及不同富铁相的晶体结构。挤压压力可以促进富铁相的形核，同时降低合金的扩散系数，从而抑制富铁相的长大。挤压压力提高了-Fe和AlmFe的形成温度，同时降低了β-Fe的形成温度。
研究了铝铜合金固溶处理过程中富铁相特征的演变规律，发现固溶温度、固溶时间和挤压压力都将促进AlmFe、Al6(FeMn)、-Fe和Al3(FeMn)相向β-Fe的转变。新形成的β-Fe易于在-Fe，Al6(FeMn)、AlmFe和Al3(FeMn)与(Al)界面处形核，并沿富铁相长大。
The Al-Cu cast alloys with high strength and toughness are widely used in the aerospaceand transportation industry. The impurity of Fe is inevitable and considered to be the mostdetrimental to mechanical properties. The Fe content is strictly controlled (mostly below0.15%) in order to get high performance properties. This will make the alloys expensive toproduce and limit the use of recycled aluminum alloys. Finding an advanced process toincrease the allowable Fe content of Al-Cu alloys has been became an important way todevelop low cost aluminum alloys with high performance.
In this study, the Al-Cu alloys are prepared by combining squeeze casting and Mnmodification. Various test techniques, including optical microscopy (OM), image analysis,scanning electron microscope (SEM), X-ray diffraction (XRD), differential scanningcalorimeter (DSC),water quenching, deep etched technology, electron probemicro-analyzer (EPMA) and transmission electron microscopy (TEM) are used to examinethe formation of Fe-rich intermetallics in squeeze cast Al-Cu alloys and the effect of Mn andFe content, applied pressure and heat treatment on microstructures and mechanical propertiesat room and elevated temperature of the alloys. The experimental results are as followed:
When the Fe content increases from0.1wt%to1.5wt%, the Fe-rich intermetallics ofas-cast Al-5.0Cu-0.6Mn alloys are-Fe (Al15(FeMn)3(CuSi)2) and β-Fe (Al7Cu2(FeMn)) inlow Fe content, while it will change into Al6(FeMn) and Al3(FeMn) in high Fe content. Theelongations of gravity die cast and squeeze cast alloys decreases gradually with increasing theFe content and there is a peak value of ultimate strength and yield strength for the alloy with0.5wt%Fe. The reason is that the small Chinese-script Fe-rich intermetallics in low Fecontent alloys are useful to improve the alloy strength through second phase hardening,although these brittle second intermetallics will cause a reduction in ductility. The elongationof the alloys with different Fe content increases more than2times when the applied pressureincreases from0MPa to75MPa. The improvement of mechanical properties is due to theporosity reduction,(Al) dendrite refinement and the decreasment of intermetallics. Thechemical composition and the needle-like shape of β-Fe (Al7Cu2Fe) solidified from the Alalloy melt have no change after T5heat treatment. However, the Chinese script-Fe,Al6(FeMn) and needle-like Al3(FeMn) transform partially to a new Chinese script (CuFe)-Al7Cu2(FeMn). When the Fe content increases from0.1wt%to1.5wt%, the mechanicalproperties of both the gravity die cast and squeeze cast alloys decrease gradually with increasing of Fe content. The Fe-rich intermetallics leads to the decrease of mechanicalproperties due to the increase amount of (CuFe), decrease of precipitation particles in (Al)matrix and the increase of (Al) dendrite size. The elongation of the alloys with different Fecontent increases more than2times when the applied pressure increases from0MPa to75MPa. The squeeze cast alloys with different Fe contents have superior mechanical propertiescompared to the gravity die cast alloys, which is mainly attributed to the reduction of porosity,the refinement of Fe-rich intermetallics and (Al) dendrite and the decrease of needle-likeFe-rich intermetallics.
The mechanical properties at elevated temperature of Al-5.0Cu-0.6Mn alloys with differentFe content have been investigated. The ultimate tensile strength and yield strength ofAl-5.0Cu-0.6Mn alloys with different Fe content decrease with incresing the tensiletemperature, while the elongation increases obviously. The ultimate tensile strength and yieldstrength of Al-5.0Cu-0.6Mn alloys with different Fe content decrease with the incresing theFe contetn. The mechanical properties at different temperature increase with increasingapplied pressure, especially the elongation. However, the increasment becomes slightly whenthe temeperature increases.
The effect of Mn/Fe ratio on the microstructure and mechanical properties has been studied.The Fe-rich intermetallics, which may present in Al-5.0Cu-0.5Fe alloys with different Mn/Feraito, including Chinese script AlmFe,-Fe, Al6(FeMn), and needle-like-Fe. The optimalMn/Fe mass ratios is1.6for the best mechanical properties when the applied pressure is0MPa due to the needle-like β-Fe is completely converted to the Chinese script-Fe and theminimum volume percent of prosity. Only Mn/Fe mass ratio of0.8is needed for the completeconvert of β-Fe phase to-Fe phase when the applied pressure is75MPa. After T5heattreatment, the Chinese script AlmFe,-Fe and Al6(FeMn) transform to a new Chinese script(CuFe). The optimal Mn/Fe ratio for the best mechanical properties of heat-treated alloy isdetermined by the morphology of Fe-rich intermetallics, volume fraction of θ’ and T(Al20Cu2Mn3), size of (Al) dendrite and porosity.
The formation of Fe-rich intermetallics during solidification of Al-Cu alloys has beenstudied. When the Fe content varies from0.1%to1.5%, β-Fe, AlmFe,-Fe, Al6(FeMn) andAl3(FeMn) are all possible to be the dominant Fe-rich intermetallic phases in the solidifiedmicrostructure of Al-Cu alloys, depending on different Mn, Fe contents and applied pressures.The Mn addition will promote the formation of-Fe and prevent the formation of AlmFe andβ-Fe. The primary Fe-rich intermetallics which formed from the Al alloy melt are AlmFe,Al6(FeMn) and Al3(FeMn) through observing the microstructures of the water quenched specimens. AlmFe and Al3(FeMn) preferably precipitates in low Mn (below0.2%) and Felevels (below0.5%) alloys. Al6(FeMn) preferably forms at high Mn (above0.4%) contentalloys， they will partly or completely change into β-Fe or-Fe, respectively, aftersolidification. In the Al-5.0Cu-0.6Mn alloys with high Fe content (above1.0%), theAl6(FeMn) and Al3(FeMn) are considered to be the dominate stable Fe-rich intermetallics.The applied pressure is favor to the formation of Chinese script Fe-rich intermetallics AlmFe、
-Fe and Al6(FeMn) and prevents the precipitate of needle-like β-Fe and Al3(FeMn) becausethe high cooling rate and the growth rate of the Fe-rich intermetallics with different crystalstructure. The applied pressure will promote the nucleation rate of Fe-rich intetmetallics anddecrease the diffusion coefficient of elements, which leads to growth inhibition of Fe-richintermetallics. The formation temperature increases for-Fe and AlmFe but decreases forβ-Fe with the increase of applied pressure.
The evolution of Fe-rich intermetallics characteristics during solution heat treatment (SHT)of Al-Cu alloys has been studied. It is found that the SHT temperature and time, the appliedpressure promote the transformation of AlmFe、Al6(FeMn)、-Fe and Al3(FeMn) to new β-Fe.The new β-Fe preferentiallynucleates various points on the interface between the AlmFe,-Fe,Al6(FeMn), Al3(FeMn) and the (Al) matrix, then grows into the Fe-rich intermetallics.
引文
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