Sn和Ce对Mg-Zn-Mn高强变形镁合金组织和性能的影响
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摘要
本文以开发高性能变形镁合金为研究背景，为了提高Mg-Zn-Mn系高锌变形镁合金的强韧性，扩大其应用范围，在已有研究成果和存在问题的基础上，从组织和性能的控制上着手，作者采用合金化改性的方法在Mg-Zn-Mn合金中单独添加Sn和Ce。首先全面研究了Mg-Zn-Mn-Sn合金的热变形行为、时效行为、显微组织及力学性能，表征了各种时效析出相的形态和晶体学特征，并揭示了时效过程中组织的演变进程；然后系统研究了Ce含量及热处理对Mg-Zn-Mn合金组织和力学性能的影响，确定了稀土相特性和种类；最后探讨了Mg-Zn-Mn-Sn和Mg-Zn-Mn-Ce系合金中Mn元素的作用。
铸态Mg-Zn-Mn合金添加Sn后，其铸态组织由(α-Mg+Mn+Mg7Zn3)组成变为由(α-Mg+Mn+Mg7Zn3+Mg2Sn)组成，Mg2Sn相作为共晶相分布于晶界，此外Sn的添加对铸态组织有一定的细化作用。均匀化处理(330℃/12h+420℃/2h)对Mg-Zn-Mn-Sn合金中的Mg7Zn3共晶相的均匀化溶解很有效，但是对于Mg2Sn共晶化合物的溶解几乎没有作用。Sn添加后，挤压态组织由均匀的再结晶晶粒转变为混晶组织，并且Sn能明显细化挤压态晶粒，因此随着Sn含量增加，挤压态合金的抗拉强度σb和屈服强度σ0.2增加，当Sn添加量达到6%以后，σb和σ0.2才开始略有下降，同时延伸率呈现先增后减的规律，其中当添加1%Sn后，延伸率最优(13.19%)。
合金元素Sn的添加对时效态合金的力学性能有明显影响。随着Sn含量的增加，σb和σ0.2总体呈抛物线式增加，δ逐渐降低，其中当Zn含量为6%时，“固溶+双级时效态”Mg-6Zn-1Mn-4Sn(ZMT614)合金具有最佳的力学性能，即σb、σ0.2和δ分别为390MPa、378MPa和4.16%；当Zn含量为8%，“固溶+双级时效态”Mg-8Zn-1Mn-4Sn(ZMT814)合金具有最佳的力学性能，σb、σ0.2和δ分别为416MPa、393MPa和4.1%。通过组织观察可知Mg-Zn-Mn-Sn合金在时效过程中主要析出三种析出相：β'1(MgZn2)杆状相、β'2(MgZn2)盘状相和不规则形状的Mg2Sn相，因此析出强化是时效态合金的主要强化方式。此外，相比单级时效，双级时效态的析出相更加细小弥散，因此双级时效态合金力学性能更优。
通过采用优化的热处理工艺，150℃双级峰时效态(20h)ZMT614合金的σb和σ0.2高达411MPa和401MPa；240℃双级峰时效态(40min)ZMT614合金的力学性能与180℃双级峰时效(8h)态ZM61合金的力学性能相差不大。
ZMT614合金在180℃等温时效过程中先后析出四类析出相：①在双级预时效阶段析出平行于0001基面的G.P.区，其只作为β'1杆状相的异质形核核心；②垂直于基体0001基面的β'1杆状相；③平行于基体0001基面的β'2盘状相；④不规则的β'(Mg2Sn)相，其直接均匀形核于基体中，大部分β'相析出相惯习面为基体0001基面，小部分β'相与0001基面成一定的角度，可能惯习面为基体锥面。根据时效显微组织的演变过程，可以得出Mg-Zn-Mn-Sn合金在180℃等温时效过程中可能的析出序列，即①在富Mn区(固溶时已析出α-Mn区域): α-Mn→β'1(MgZn2)→β (MgZn)；②在富Zn和Sn区(固溶时未析出α-Mn区域): SSSS→GP zones→β'1(MgZn2)→β'2(MgZn2)→β'(Mg2Sn)→(β (MgZn) and β (Mg2Sn))。
利用Gleeble热模拟试验机对ZMT814镁合金进行了等温压缩试验，研究发现试验合金在等温压缩变形试验过程中存在稳态流变特征，并计算出合金在热变形过程中的材料常数为：变形激活能Q=251.67KJ/mol，应力指数n=13.91，平均应力因子α=0.00665MPa-1，A=3.4289×1024s-1，最后建立了合金的流变应力方程。
此外研究了Ce含量对ZM71合金的显微组织和力学性能的影响。研究结果表明：①在合金中加入Ce之后，生成了Mg-Zn-Ce稀土相τ2相，具体为τ2(Ce(Mg0.5Zn0.5)10.1)和τ2(Ce2Mg53Zn45)；随着Ce含量的增加，τ2相的衍射峰强度不断增加，Mg7Zn3相的衍射峰强度不断减小，当Ce含量增加到2%时，Mg7Zn3相衍射峰几乎没有，说明此时合金主要由α-Mg基体、Mn相和τ2相组成；②Ce的添加对铸态组织有明显的细化作用；热挤压过程中，稀土τ2相能阻碍再结晶晶粒长大，细化晶粒；③Ce元素能够明显细化挤压态合金的组织，所以能提升力学性能，但添加量应控制在1%以内，其中ZM71-0.5Ce具有最佳的综合力学性能，σb、σ0.2和δ分别为318MPa、250MPa和13.6%；④稀土τ相的形成一方面严重降低了合金的MgZn相的时效强化效果，另一方面在拉伸过程中成为裂纹源，所以高锌含量的Mg-Zn-Mn-Ce元素不适合用时效处理来提升挤压态合金的力学性能。
最后还研究了Mn元素对Mg-Zn-Mn-Sn和Mg-Zn-Mn-Ce的影响，发现Mn元素在两种合金中的存在形式和作用机制基本一致。结果表明：①Mn主要以单质相存在，对原有物相组成没有影响；②Mn的添加能细化合金组织；③均匀化、挤压和固溶处理时会析出α-Mn相，形貌主要有球状、棒状和规则多边形三类；④Mn的添加能显著提高挤压态和时效态的力学性能；⑤Mn元素在合金中的作用主要有：改善铸造性能、细化晶粒和异质形核核心等。
In order to improve the strengthening and toughening of the high zinc Mg-Zn-Mnwrought magnesium alloy, Sn and Ce were added separately into the base alloy by usingalloy modification method. Firstly, hot deformation behavior, aging behavior,microstructure and mechanical properties of Mg-Zn-Mn-Sn alloy were investigatedcomprehensively. And the morphology, crystallography, formation mechanism andprecipitation sequence of the precipitates were characterized as well. Secondly, theeffects of Ce content on the microstructure and mechanical properties of Mg-Zn-Mnalloy were studied systematically. At last, the function of Mn element on theMg-Zn-Mn-Sn and Mg-Zn-Mn-Ce alloys was discussed thoroughly.
Sn addition to the Mg-Zn-Mn alloy changed the as-cast microstructure of thealloys from being composed of (α-Mg matrix+Mn+Mg7Zn3) to being composed of(α-Mg matrix+Mn+Mg7Zn3+Mg2Sn), with the FCC structured Mg2Sn distributing at thegrain boundaries as an eutectic phase. In addition, the Sn addition could refine themicrostructure of the as-cast alloys. With the increasing Sn content, the homogenizationeffect was more difficult due to that Mg2Sn eutectic phase could not be effectivelydissolved into the matrix after the homogenization treatment at330℃for12h and420℃for2h. Sn element had an obvious effect on refining the microstructure of as-extrudedalloys by restricting the occurrence of dynamic recrystallization and restraining thegrain growth during extrusion, and improved the mechanical properties. With theincreasing Sn content, the strengths and elongation presented the trend of first increaseand then decrease, and the alloy containing6%Sn had the best strength while the alloycontaining1%Sn had the best elongation.
The Sn addition had a beneficial effect on the mechanical properties of thepeak-aged Mg-Zn-Mn alloy. On one hand, with the increasing of Sn content, theelongation decreased gradually while the ultimate tensile strength (UTS) and yieldstrength (YS) significantly increased, and the maximum was obtained for the alloycontaining4%Sn. Further increasing of Sn content resulted in a slight reduction of thestrengths. On the other hand, the strengths of the double aged samples were higher thanthat of the single aged ones, while the elongations were slightly lower. The mechanicalproperties of the double aged Mg-6Zn-1Mn-4Sn(ZMT614) alloy were the UTS of390MPa, the YS of378MPa and the elongation of4.16%, while those of the double aged Mg-8Zn-1Mn-4Sn(ZMT814) alloy were the UTS of416MPa, the YS of393MPaand the elongation of4.1%. The high-strengths of the aged Mg-Zn-Mn-Sn wroughtalloy were mainly determined by the precipitation strengthening. The high-strengths ofthe peak-aged Mg-Zn-Mn-Sn were mainly determined by the combined precipitationstrengthening of the β1′(MgZn2), β2′(MgZn2) and Mg2Sn precipitates. Moreover, due tothe much finer and far more homogeneously distributed precipitates, the strengths of thedouble aged samples were higher than that of the single aged ones.
The UTS and YS of ZMT614alloy in the double peak-aged at150℃were411MPa and401MPa respectively, which was attained by the optimized heat treatment.In addition, the mechanical properties of ZMT614alloy in the double peak-age at240℃for40min were comparable to that of ZM61alloy in the double peak-aged at180℃for6h.
During the isothermal aging at180℃, the four categories of precipitated phaseswere successively formed. Firstly, the G.P. zones parallel to0001were formedduring the pre-aging stage of double aging, which could only act as the hetergeneousnuclei towards the rod-like β'1phase. Secondly, the0001β'1precipitates wereformed, which were all rod-like with their axis perpendicular to the basal plane0001.Thirdly, the disc-like hexagonal β'2phases with the plate face parallel to the basal plane0001were formed. At last, the Mg2Sn precipitates with common morphology wereformed. Some of the Mg2Sn phase had a orientation relationship of001′1120,110′0001. The crystallographic features of the above four typesof aged precipitates were characterized, and their formation mechanisms were discussedon the basis of the crystallographic features.
Based on the aging precipitation and microstructure evolution, the possibleprecipitation sequence at180℃of Mg-Zn-Mn-Sn alloy could be obtained. Theprecipitation sequence in the Mn-rich region (i.e. the region with α-Mn precipitated inthe solution treated condition) was proposed as follows: α-Mn→β'1(MgZn2)→β(MgZn). And the precipitation sequence in the Zn-rich and Sn-rich region(i.e. the regionfree of α-Mn in the solution treated condition) was proposed as follows: Super saturatedsolid solution(SSSS)→GP zones→β'1(MgZn2)→β'2(MgZn2)→β'(Mg2Sn)→(β (MgZn)and β (Mg2Sn)).
The hot simulation was conducted on ZMT814alloy to investigate its hotdeformation behavior. The results showed that the test alloy had a typical feature ofcontinuous dynamic recrystallization. Then the material constants of the test alloy in the hot deformation were calculated, i.e., Q=251.67KJ/mol, n=13.91, α=0.00665MPa-1,A=3.4289×10~24s~(-1). At last, the flow stress equation was established.
In addition, the effect of Ce content on the microstructure and mechanicalproperties of Mg-7Zn-1Mn alloy were investigated. The results were as follows:①Aternary τ phase was identified in studied alloys, which distributed at grain boundariesand interdendritic, refined the microstructure of as-cast alloys. The τ phase wasidentified as τ2(Ce(Mg0.5Zn0.5)10.1) and τ2(Ce2Mg53Zn45);②Ce element had an obviouseffect on refining the microstructure of as-extruded alloys by restricting the occurrenceof dynamic recrystallization and restraining the grain growth during extrusion andimproved the mechanical properties, but the Ce addition should be no more than1%.Among them, ZM71-0.5Ce alloy had better overall mechanical properties, with the UTSof318MPa, YS of250MPa and elongation of13.6%;③Solution and aging treatmentwas not available for improving mechanical properties of as-extruded Mg-Zn-Mn-Cewith high Zn content.
At last, the effect of Mn on the Mg-Zn-Mn-Sn and Mg-Zn-Mn-Ce alloys wereinvestigated, and found that the existence form and acting mechanism of Mn element inthe both alloys were basically the same. The functions of Mn element in the test alloyswere summarized as follows: improving casting properties, grain refinement andheterogeneous nucleation.
铸态Mg-Zn-Mn合金添加Sn后，其铸态组织由(α-Mg+Mn+Mg7Zn3)组成变为由(α-Mg+Mn+Mg7Zn3+Mg2Sn)组成，Mg2Sn相作为共晶相分布于晶界，此外Sn的添加对铸态组织有一定的细化作用。均匀化处理(330℃/12h+420℃/2h)对Mg-Zn-Mn-Sn合金中的Mg7Zn3共晶相的均匀化溶解很有效，但是对于Mg2Sn共晶化合物的溶解几乎没有作用。Sn添加后，挤压态组织由均匀的再结晶晶粒转变为混晶组织，并且Sn能明显细化挤压态晶粒，因此随着Sn含量增加，挤压态合金的抗拉强度σb和屈服强度σ0.2增加，当Sn添加量达到6%以后，σb和σ0.2才开始略有下降，同时延伸率呈现先增后减的规律，其中当添加1%Sn后，延伸率最优(13.19%)。
合金元素Sn的添加对时效态合金的力学性能有明显影响。随着Sn含量的增加，σb和σ0.2总体呈抛物线式增加，δ逐渐降低，其中当Zn含量为6%时，“固溶+双级时效态”Mg-6Zn-1Mn-4Sn(ZMT614)合金具有最佳的力学性能，即σb、σ0.2和δ分别为390MPa、378MPa和4.16%；当Zn含量为8%，“固溶+双级时效态”Mg-8Zn-1Mn-4Sn(ZMT814)合金具有最佳的力学性能，σb、σ0.2和δ分别为416MPa、393MPa和4.1%。通过组织观察可知Mg-Zn-Mn-Sn合金在时效过程中主要析出三种析出相：β'1(MgZn2)杆状相、β'2(MgZn2)盘状相和不规则形状的Mg2Sn相，因此析出强化是时效态合金的主要强化方式。此外，相比单级时效，双级时效态的析出相更加细小弥散，因此双级时效态合金力学性能更优。
通过采用优化的热处理工艺，150℃双级峰时效态(20h)ZMT614合金的σb和σ0.2高达411MPa和401MPa；240℃双级峰时效态(40min)ZMT614合金的力学性能与180℃双级峰时效(8h)态ZM61合金的力学性能相差不大。
ZMT614合金在180℃等温时效过程中先后析出四类析出相：①在双级预时效阶段析出平行于0001基面的G.P.区，其只作为β'1杆状相的异质形核核心；②垂直于基体0001基面的β'1杆状相；③平行于基体0001基面的β'2盘状相；④不规则的β'(Mg2Sn)相，其直接均匀形核于基体中，大部分β'相析出相惯习面为基体0001基面，小部分β'相与0001基面成一定的角度，可能惯习面为基体锥面。根据时效显微组织的演变过程，可以得出Mg-Zn-Mn-Sn合金在180℃等温时效过程中可能的析出序列，即①在富Mn区(固溶时已析出α-Mn区域): α-Mn→β'1(MgZn2)→β (MgZn)；②在富Zn和Sn区(固溶时未析出α-Mn区域): SSSS→GP zones→β'1(MgZn2)→β'2(MgZn2)→β'(Mg2Sn)→(β (MgZn) and β (Mg2Sn))。
利用Gleeble热模拟试验机对ZMT814镁合金进行了等温压缩试验，研究发现试验合金在等温压缩变形试验过程中存在稳态流变特征，并计算出合金在热变形过程中的材料常数为：变形激活能Q=251.67KJ/mol，应力指数n=13.91，平均应力因子α=0.00665MPa-1，A=3.4289×1024s-1，最后建立了合金的流变应力方程。
此外研究了Ce含量对ZM71合金的显微组织和力学性能的影响。研究结果表明：①在合金中加入Ce之后，生成了Mg-Zn-Ce稀土相τ2相，具体为τ2(Ce(Mg0.5Zn0.5)10.1)和τ2(Ce2Mg53Zn45)；随着Ce含量的增加，τ2相的衍射峰强度不断增加，Mg7Zn3相的衍射峰强度不断减小，当Ce含量增加到2%时，Mg7Zn3相衍射峰几乎没有，说明此时合金主要由α-Mg基体、Mn相和τ2相组成；②Ce的添加对铸态组织有明显的细化作用；热挤压过程中，稀土τ2相能阻碍再结晶晶粒长大，细化晶粒；③Ce元素能够明显细化挤压态合金的组织，所以能提升力学性能，但添加量应控制在1%以内，其中ZM71-0.5Ce具有最佳的综合力学性能，σb、σ0.2和δ分别为318MPa、250MPa和13.6%；④稀土τ相的形成一方面严重降低了合金的MgZn相的时效强化效果，另一方面在拉伸过程中成为裂纹源，所以高锌含量的Mg-Zn-Mn-Ce元素不适合用时效处理来提升挤压态合金的力学性能。
最后还研究了Mn元素对Mg-Zn-Mn-Sn和Mg-Zn-Mn-Ce的影响，发现Mn元素在两种合金中的存在形式和作用机制基本一致。结果表明：①Mn主要以单质相存在，对原有物相组成没有影响；②Mn的添加能细化合金组织；③均匀化、挤压和固溶处理时会析出α-Mn相，形貌主要有球状、棒状和规则多边形三类；④Mn的添加能显著提高挤压态和时效态的力学性能；⑤Mn元素在合金中的作用主要有：改善铸造性能、细化晶粒和异质形核核心等。
In order to improve the strengthening and toughening of the high zinc Mg-Zn-Mnwrought magnesium alloy, Sn and Ce were added separately into the base alloy by usingalloy modification method. Firstly, hot deformation behavior, aging behavior,microstructure and mechanical properties of Mg-Zn-Mn-Sn alloy were investigatedcomprehensively. And the morphology, crystallography, formation mechanism andprecipitation sequence of the precipitates were characterized as well. Secondly, theeffects of Ce content on the microstructure and mechanical properties of Mg-Zn-Mnalloy were studied systematically. At last, the function of Mn element on theMg-Zn-Mn-Sn and Mg-Zn-Mn-Ce alloys was discussed thoroughly.
Sn addition to the Mg-Zn-Mn alloy changed the as-cast microstructure of thealloys from being composed of (α-Mg matrix+Mn+Mg7Zn3) to being composed of(α-Mg matrix+Mn+Mg7Zn3+Mg2Sn), with the FCC structured Mg2Sn distributing at thegrain boundaries as an eutectic phase. In addition, the Sn addition could refine themicrostructure of the as-cast alloys. With the increasing Sn content, the homogenizationeffect was more difficult due to that Mg2Sn eutectic phase could not be effectivelydissolved into the matrix after the homogenization treatment at330℃for12h and420℃for2h. Sn element had an obvious effect on refining the microstructure of as-extrudedalloys by restricting the occurrence of dynamic recrystallization and restraining thegrain growth during extrusion, and improved the mechanical properties. With theincreasing Sn content, the strengths and elongation presented the trend of first increaseand then decrease, and the alloy containing6%Sn had the best strength while the alloycontaining1%Sn had the best elongation.
The Sn addition had a beneficial effect on the mechanical properties of thepeak-aged Mg-Zn-Mn alloy. On one hand, with the increasing of Sn content, theelongation decreased gradually while the ultimate tensile strength (UTS) and yieldstrength (YS) significantly increased, and the maximum was obtained for the alloycontaining4%Sn. Further increasing of Sn content resulted in a slight reduction of thestrengths. On the other hand, the strengths of the double aged samples were higher thanthat of the single aged ones, while the elongations were slightly lower. The mechanicalproperties of the double aged Mg-6Zn-1Mn-4Sn(ZMT614) alloy were the UTS of390MPa, the YS of378MPa and the elongation of4.16%, while those of the double aged Mg-8Zn-1Mn-4Sn(ZMT814) alloy were the UTS of416MPa, the YS of393MPaand the elongation of4.1%. The high-strengths of the aged Mg-Zn-Mn-Sn wroughtalloy were mainly determined by the precipitation strengthening. The high-strengths ofthe peak-aged Mg-Zn-Mn-Sn were mainly determined by the combined precipitationstrengthening of the β1′(MgZn2), β2′(MgZn2) and Mg2Sn precipitates. Moreover, due tothe much finer and far more homogeneously distributed precipitates, the strengths of thedouble aged samples were higher than that of the single aged ones.
The UTS and YS of ZMT614alloy in the double peak-aged at150℃were411MPa and401MPa respectively, which was attained by the optimized heat treatment.In addition, the mechanical properties of ZMT614alloy in the double peak-age at240℃for40min were comparable to that of ZM61alloy in the double peak-aged at180℃for6h.
During the isothermal aging at180℃, the four categories of precipitated phaseswere successively formed. Firstly, the G.P. zones parallel to0001were formedduring the pre-aging stage of double aging, which could only act as the hetergeneousnuclei towards the rod-like β'1phase. Secondly, the0001β'1precipitates wereformed, which were all rod-like with their axis perpendicular to the basal plane0001.Thirdly, the disc-like hexagonal β'2phases with the plate face parallel to the basal plane0001were formed. At last, the Mg2Sn precipitates with common morphology wereformed. Some of the Mg2Sn phase had a orientation relationship of001′1120,110′0001. The crystallographic features of the above four typesof aged precipitates were characterized, and their formation mechanisms were discussedon the basis of the crystallographic features.
Based on the aging precipitation and microstructure evolution, the possibleprecipitation sequence at180℃of Mg-Zn-Mn-Sn alloy could be obtained. Theprecipitation sequence in the Mn-rich region (i.e. the region with α-Mn precipitated inthe solution treated condition) was proposed as follows: α-Mn→β'1(MgZn2)→β(MgZn). And the precipitation sequence in the Zn-rich and Sn-rich region(i.e. the regionfree of α-Mn in the solution treated condition) was proposed as follows: Super saturatedsolid solution(SSSS)→GP zones→β'1(MgZn2)→β'2(MgZn2)→β'(Mg2Sn)→(β (MgZn)and β (Mg2Sn)).
The hot simulation was conducted on ZMT814alloy to investigate its hotdeformation behavior. The results showed that the test alloy had a typical feature ofcontinuous dynamic recrystallization. Then the material constants of the test alloy in the hot deformation were calculated, i.e., Q=251.67KJ/mol, n=13.91, α=0.00665MPa-1,A=3.4289×10~24s~(-1). At last, the flow stress equation was established.
In addition, the effect of Ce content on the microstructure and mechanicalproperties of Mg-7Zn-1Mn alloy were investigated. The results were as follows:①Aternary τ phase was identified in studied alloys, which distributed at grain boundariesand interdendritic, refined the microstructure of as-cast alloys. The τ phase wasidentified as τ2(Ce(Mg0.5Zn0.5)10.1) and τ2(Ce2Mg53Zn45);②Ce element had an obviouseffect on refining the microstructure of as-extruded alloys by restricting the occurrenceof dynamic recrystallization and restraining the grain growth during extrusion andimproved the mechanical properties, but the Ce addition should be no more than1%.Among them, ZM71-0.5Ce alloy had better overall mechanical properties, with the UTSof318MPa, YS of250MPa and elongation of13.6%;③Solution and aging treatmentwas not available for improving mechanical properties of as-extruded Mg-Zn-Mn-Cewith high Zn content.
At last, the effect of Mn on the Mg-Zn-Mn-Sn and Mg-Zn-Mn-Ce alloys wereinvestigated, and found that the existence form and acting mechanism of Mn element inthe both alloys were basically the same. The functions of Mn element in the test alloyswere summarized as follows: improving casting properties, grain refinement andheterogeneous nucleation.
引文
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