Mg-Al-Si合金半固态组织演变及其影响因素
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摘要
镁合金在汽车制造、电子通讯和航空航天等领域得到了广泛的应用，但是在Mg-Al-Si合金中易于形成粗大的汉字状共晶Mg_2Si相，对镁合金的性能造成了严重的影响。半固态加工技术作为镁合金的先进成形工艺，近年来已经得到了迅速的发展，但是国内外对Mg-Al-Si合金半固态组织的研究较少，对其非枝晶组织演变机制的研究还不够深入。本论文以Mg-9Al-1Si合金为主要研究对象，采用应变诱发法（SIMA）和等温热处理法成功制备出了Mg-Al-Si合金半固态坯料，研究了半固态工艺参数（预变形量、等温温度和等温时间）及合金成分（Al含量和Si含量）对Mg-Al-Si合金半固态非枝晶组织的影响规律，并对Mg-Al-Si合金的半固态非枝晶组织演变及其影响因素进行了探讨。通过研究不但可以明确半固态工艺参数（预变形量、等温温度和等温时间）及合金成分（Al含量和Si含量）对合金半固态组织的影响，而且对于揭示Mg-Al-Si合金半固态非枝晶组织的演变机制，丰富半固态理论基础，具有明显的理论意义和工程实用价值。
采用应变诱发法（SIMA）和等温热处理法分别制备出了具有非枝晶组织的Mg-9Al-1Si合金半固态坯料，并且通过金相组织观察发现，采用SIMA法制备的合金半固态组织中的α-Mg晶粒和汉字状共晶Mg_2Si实现了双重球化，而与SIMA法不同的是，由于采用等温热处理法在半固态处理前没有对合金进行预变形处理，所以在此半固态工艺下制备得到的非枝晶组织中的α-Mg晶粒虽然实现了球化，但是组织中的Mg_2Si颗粒却大部分以多角形块状的形式存在。
通过对SIMA法工艺参数的研究发现：随着预变形量的增加，半固态组织中的α-Mg晶粒尺寸明显减小，圆整度增大，液相量增多；Mg_2Si颗粒的尺寸虽然没有显著变化，但是其形状因子不断增加。随着等温温度和等温时间的增加，半固态组织中的α-Mg晶粒尺寸增大，圆整度提高，液相量不断增多；Mg_2Si颗粒的尺寸增大，形状因子增加。在本实验条件下，采用SIMA法获得的优化工艺参数为：预变形量为30%，等温温度为570℃，等温时间为20min。
通过对等温热处理法工艺参数的研究发现：随着等温温度和等温时间的增加，半固态组织中的α-Mg晶粒尺寸增大，圆整度提高，液相量不断增多；Mg_2Si颗粒的尺寸增大，数量减少，并且其出现多角形块状的几率增加，形状因子不断降低。在本实验条件下，采用等温热处理法获得的优化工艺参数为：等温温度为570℃，等温时间为20min。
通过研究合金成分（Al含量和Si含量）对Mg-Al-Si合金半固态非枝晶组织的影响可以发现：随着Al含量的增加，半固态组织中的α-Mg晶粒尺寸不断减小，圆整度提高，液相量明显增多；由于Al含量增加使Mg-Al-Si合金从亚共晶成分转变成为过共晶成分，从而导致汉字状共晶Mg_2Si转变为多角形块状的初生Mg_2Si。随着Si含量的增加，在合金半固态组织中α-Mg晶粒的晶界处分布着较多粗大的Mg_2Si颗粒，这些Mg_2Si颗粒阻碍了α-Mg晶粒的合并长大，使得α-Mg晶粒尺寸减小；在经过不同半固态处理工艺后，Mg-Al-Si合金中粗大树枝状的初生Mg_2Si都转变为近球形颗粒。
通过以上研究可以得到Mg-Al-Si合金半固态非枝晶组织的演变机制，主要包括α-Mg晶粒的球化机制、汉字状共晶Mg_2Si相的球化机制和树枝状初生Mg_2Si的球化机制这三个方面。采用SIMA法获得的Mg-Al-Si合金半固态组织中的α-Mg晶粒的球化机理除了枝晶熔断机制外，主要是液相沿亚晶界的熔渗机制，而采用等温热处理法获得的Mg-Al-Si合金半固态组织中α-Mg晶粒的球化机理主要是枝晶熔断机制；汉字状共晶Mg_2Si的球化机理为溶解-析出机制；树枝状初生Mg_2Si的球化机理为枝晶根部熔断机制及“雷利（Rayleigh）形状失稳”机制。
Magnesium alloys are the lightest structural materials widely commercially available andhave great potential for applications in automotive, aerospace industries and others in recentyears. However, the challenge of Mg-Al-Si alloy is that the Mg_2Si phase is prone to formingundesirable, coarse Chinese script shape under low solidification rate resulting from theeutectic reaction, which would greatly deteriorate the mechanical properties of the magnesiumalloys and become a principal obstacle for the application of Si-containing magnesium alloys.SSM processing is regarded as an advanced forming technology for magnesium alloy, but theresearch of semisolid process for Mg-Al-Si alloy is less. In this thesis, the Mg-9Al-1Si alloysemisolid billets were fabricated by strain-induced melt activation (SIMA) process andsemisolid isothermal heat-treatment process, and the effects of different heat-treatmentprocessing parameters (compressive ratio, holding temperature and holding time) and thealloy content (Al and Si content) on the semisolid microstructures of Mg-Al-Si alloy werestudied. Moreover, the semisolid microstructural evolution and influence factors for theMg-Al-Si alloy were also investigated. Through the research not only can determine theisothermal processing parameters, but also can enrich semisolid theoretical basis, theinfluence of theoretical significance is obviously.
Experimental results indicated that a non-dendritic microstructure of Mg-9Al-1Si alloycould be obtained by the strain-induced melt activation (SIMA) process and semisolidisothermal heat treatment process, respectively. The morphology of α-Mg grains transformedfrom dendritic shape to spherical shape and the eutectic Mg_2Si phase transformed fromChinese script shape to globular shape during the SIMA process. Compared with the SIMAprocess, without the compressive processing, although the morphology of α-Mg grainstransformed from dendritic shape to spherical shape but the eutectic Mg_2Si phase transformedfrom Chinese script shape to polygon shape during the semisolid isothermal heat treatment.
With the compressive ratio varying from0%to30%, the volume fraction of liquidgradually increased, average size of α-Mg grains increased and the globular tendency becamemore obviously. With the compressive ratio increased, the average size Mg_2Si particle wasnot significant change but its shape factor increased. With the holding temperature varyingfrom560℃to575℃, the average size of α-Mg grain and its globular tendency increased andthe volume fraction of liquid increased. The average size and shape factor of Mg_2Si particleincreased. With the holding time varying from5min to30min, the volume fraction of liquid gradually increased, average size of α-Mg grains increased and the globular tendency becamemore obviously, the average size and shape factor of Mg_2Si particle increased. The resultsshowed that the optimized SIMA processing parameters were suggested at570℃for20minand compressive ratio was chosen30%for the Mg-9Al-1Si alloys.
With the holding temperature varying from560℃to575℃, the volume fraction ofliquid gradually increased, average size of α-Mg grains increased and the globular tendencybecame more obviously, the average size of Mg_2Si particle increased but its shape factordecreased. With the holding time varying from5min to30min, the average size of α-Mg grainand its globular tendency increased, the volume fraction of liquid increased, the average sizeof Mg_2Si particle increased but its shape factor decreased obviously. The results showed thatthe optimized semisolid isothermal heat treatment parameters were suggested at570℃for20min for the Mg-9Al-1Si alloys.
The effects of the alloy content (Al and Si content) on the as-cast and semisolidmicrostructures of Mg-Al-Si alloy were investigated. With the Al content increased, thehypoeutectic composition transformed into hypereutectic composition in the as-castmicrostructure of Mg-Al-Si alloy; the liquid phase increased, the morphology of α-Mg grainbecame more globular and its size decreased in the semisolid microstructure of Mg-Al-Sialloy. With the Si content increased, abundant polygonal primary Mg_2Si phase existed in thesemisolid microstructure of Mg-Al-Si alloy, the primary Mg_2Si particle distributed in theα-Mg grain boundary and hampered its growth resulted in α-Mg grain size decreased. Afterdifferent semisolid process, all the dentritic Mg_2Si changed into nearly spherical particles.
The semisolid microstructural evolution mechanisms for Mg-Al-Si alloys were studied,including the spheroidization mechanism of α-Mg grain, the spheroidization mechanism ofeutectic Mg_2Si phase and primary Mg_2Si phase at grain boundary. The results indicated thatthe spheroidization mechanism of α-Mg grain produced by isothermal heat-treatment processwas the dendrites melting mechanism. However, the penetration of liquid phase along thesub-grain boundary was the main spheroidization mechanism of α-Mg grain produced bySIMA process. The spheroidization mechanism of eutectic Mg_2Si should be attributed to theresolution precipitation. The spheroidization mechanism of primary Mg_2Si was associatedwith the dendrites melting and “Rayleigh shape instability”.
采用应变诱发法（SIMA）和等温热处理法分别制备出了具有非枝晶组织的Mg-9Al-1Si合金半固态坯料，并且通过金相组织观察发现，采用SIMA法制备的合金半固态组织中的α-Mg晶粒和汉字状共晶Mg_2Si实现了双重球化，而与SIMA法不同的是，由于采用等温热处理法在半固态处理前没有对合金进行预变形处理，所以在此半固态工艺下制备得到的非枝晶组织中的α-Mg晶粒虽然实现了球化，但是组织中的Mg_2Si颗粒却大部分以多角形块状的形式存在。
通过对SIMA法工艺参数的研究发现：随着预变形量的增加，半固态组织中的α-Mg晶粒尺寸明显减小，圆整度增大，液相量增多；Mg_2Si颗粒的尺寸虽然没有显著变化，但是其形状因子不断增加。随着等温温度和等温时间的增加，半固态组织中的α-Mg晶粒尺寸增大，圆整度提高，液相量不断增多；Mg_2Si颗粒的尺寸增大，形状因子增加。在本实验条件下，采用SIMA法获得的优化工艺参数为：预变形量为30%，等温温度为570℃，等温时间为20min。
通过对等温热处理法工艺参数的研究发现：随着等温温度和等温时间的增加，半固态组织中的α-Mg晶粒尺寸增大，圆整度提高，液相量不断增多；Mg_2Si颗粒的尺寸增大，数量减少，并且其出现多角形块状的几率增加，形状因子不断降低。在本实验条件下，采用等温热处理法获得的优化工艺参数为：等温温度为570℃，等温时间为20min。
通过研究合金成分（Al含量和Si含量）对Mg-Al-Si合金半固态非枝晶组织的影响可以发现：随着Al含量的增加，半固态组织中的α-Mg晶粒尺寸不断减小，圆整度提高，液相量明显增多；由于Al含量增加使Mg-Al-Si合金从亚共晶成分转变成为过共晶成分，从而导致汉字状共晶Mg_2Si转变为多角形块状的初生Mg_2Si。随着Si含量的增加，在合金半固态组织中α-Mg晶粒的晶界处分布着较多粗大的Mg_2Si颗粒，这些Mg_2Si颗粒阻碍了α-Mg晶粒的合并长大，使得α-Mg晶粒尺寸减小；在经过不同半固态处理工艺后，Mg-Al-Si合金中粗大树枝状的初生Mg_2Si都转变为近球形颗粒。
通过以上研究可以得到Mg-Al-Si合金半固态非枝晶组织的演变机制，主要包括α-Mg晶粒的球化机制、汉字状共晶Mg_2Si相的球化机制和树枝状初生Mg_2Si的球化机制这三个方面。采用SIMA法获得的Mg-Al-Si合金半固态组织中的α-Mg晶粒的球化机理除了枝晶熔断机制外，主要是液相沿亚晶界的熔渗机制，而采用等温热处理法获得的Mg-Al-Si合金半固态组织中α-Mg晶粒的球化机理主要是枝晶熔断机制；汉字状共晶Mg_2Si的球化机理为溶解-析出机制；树枝状初生Mg_2Si的球化机理为枝晶根部熔断机制及“雷利（Rayleigh）形状失稳”机制。
Magnesium alloys are the lightest structural materials widely commercially available andhave great potential for applications in automotive, aerospace industries and others in recentyears. However, the challenge of Mg-Al-Si alloy is that the Mg_2Si phase is prone to formingundesirable, coarse Chinese script shape under low solidification rate resulting from theeutectic reaction, which would greatly deteriorate the mechanical properties of the magnesiumalloys and become a principal obstacle for the application of Si-containing magnesium alloys.SSM processing is regarded as an advanced forming technology for magnesium alloy, but theresearch of semisolid process for Mg-Al-Si alloy is less. In this thesis, the Mg-9Al-1Si alloysemisolid billets were fabricated by strain-induced melt activation (SIMA) process andsemisolid isothermal heat-treatment process, and the effects of different heat-treatmentprocessing parameters (compressive ratio, holding temperature and holding time) and thealloy content (Al and Si content) on the semisolid microstructures of Mg-Al-Si alloy werestudied. Moreover, the semisolid microstructural evolution and influence factors for theMg-Al-Si alloy were also investigated. Through the research not only can determine theisothermal processing parameters, but also can enrich semisolid theoretical basis, theinfluence of theoretical significance is obviously.
Experimental results indicated that a non-dendritic microstructure of Mg-9Al-1Si alloycould be obtained by the strain-induced melt activation (SIMA) process and semisolidisothermal heat treatment process, respectively. The morphology of α-Mg grains transformedfrom dendritic shape to spherical shape and the eutectic Mg_2Si phase transformed fromChinese script shape to globular shape during the SIMA process. Compared with the SIMAprocess, without the compressive processing, although the morphology of α-Mg grainstransformed from dendritic shape to spherical shape but the eutectic Mg_2Si phase transformedfrom Chinese script shape to polygon shape during the semisolid isothermal heat treatment.
With the compressive ratio varying from0%to30%, the volume fraction of liquidgradually increased, average size of α-Mg grains increased and the globular tendency becamemore obviously. With the compressive ratio increased, the average size Mg_2Si particle wasnot significant change but its shape factor increased. With the holding temperature varyingfrom560℃to575℃, the average size of α-Mg grain and its globular tendency increased andthe volume fraction of liquid increased. The average size and shape factor of Mg_2Si particleincreased. With the holding time varying from5min to30min, the volume fraction of liquid gradually increased, average size of α-Mg grains increased and the globular tendency becamemore obviously, the average size and shape factor of Mg_2Si particle increased. The resultsshowed that the optimized SIMA processing parameters were suggested at570℃for20minand compressive ratio was chosen30%for the Mg-9Al-1Si alloys.
With the holding temperature varying from560℃to575℃, the volume fraction ofliquid gradually increased, average size of α-Mg grains increased and the globular tendencybecame more obviously, the average size of Mg_2Si particle increased but its shape factordecreased. With the holding time varying from5min to30min, the average size of α-Mg grainand its globular tendency increased, the volume fraction of liquid increased, the average sizeof Mg_2Si particle increased but its shape factor decreased obviously. The results showed thatthe optimized semisolid isothermal heat treatment parameters were suggested at570℃for20min for the Mg-9Al-1Si alloys.
The effects of the alloy content (Al and Si content) on the as-cast and semisolidmicrostructures of Mg-Al-Si alloy were investigated. With the Al content increased, thehypoeutectic composition transformed into hypereutectic composition in the as-castmicrostructure of Mg-Al-Si alloy; the liquid phase increased, the morphology of α-Mg grainbecame more globular and its size decreased in the semisolid microstructure of Mg-Al-Sialloy. With the Si content increased, abundant polygonal primary Mg_2Si phase existed in thesemisolid microstructure of Mg-Al-Si alloy, the primary Mg_2Si particle distributed in theα-Mg grain boundary and hampered its growth resulted in α-Mg grain size decreased. Afterdifferent semisolid process, all the dentritic Mg_2Si changed into nearly spherical particles.
The semisolid microstructural evolution mechanisms for Mg-Al-Si alloys were studied,including the spheroidization mechanism of α-Mg grain, the spheroidization mechanism ofeutectic Mg_2Si phase and primary Mg_2Si phase at grain boundary. The results indicated thatthe spheroidization mechanism of α-Mg grain produced by isothermal heat-treatment processwas the dendrites melting mechanism. However, the penetration of liquid phase along thesub-grain boundary was the main spheroidization mechanism of α-Mg grain produced bySIMA process. The spheroidization mechanism of eutectic Mg_2Si should be attributed to theresolution precipitation. The spheroidization mechanism of primary Mg_2Si was associatedwith the dendrites melting and “Rayleigh shape instability”.
引文
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