往复挤压ZK60与GW102K镁合金的组织演变及强韧化机制研究
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摘要
本文以商业牌号高强度变形镁合金ZK60和新型高强度稀土镁合金GW102K为研究对象,利用往复挤压大塑性变形工艺制备块体超细晶镁合金,旨在提高镁合金的室温力学性能和塑性成形能力。重点研究往复挤压镁合金的组织演变规律及细化机制、室温变形行为和断裂机制,揭示往复挤压镁合金的强韧化机制。以期提出改善镁合金力学性能和成形性能的有效方法及理论。获得如下结果:
本文首先利用有限元数值模拟方法分析了往复挤压模具结构和工艺参数对材料流动的影响,优化了往复挤压模具及工艺,并利用物理实验验证了数值模拟结果的可靠性。往复挤压工艺数值模拟发现,模具结构和往复挤压工艺参数对材料应变的分布具有很大影响。模具过渡角越大、模具入口角越小、摩擦越小试样应变分布越均匀,但小量摩擦有利于应变的均匀分布。较小的挤压比可防止材料在变形过程中失稳;模具入口角为45°时应变分布最均匀,载荷最低;挤压速度对应变分布基本没有影响;根据变形温度的不同,塑变生热和摩擦生热能在4至8道次内弥补模具向环境散热引起的温降。对流场的模拟和实验研究发现,随着往复挤压道次的增加流线逐渐变得紊乱。材料的流动规律是:试样表层的材料背向流动,心部相向流动,进而在试样的上下两部分各形成一个流动漩涡。
利用金相显微镜(OM)、扫描电镜(SEM)、电子背散射技术(EBSD)和透射电镜(TEM)从不同尺度分析了往复挤压变形温度和变形道次对ZK60和GW102K两种镁合金微观组织的影响规律。结果表明,往复挤压对ZK60和GW102K镁合金都具有强烈的细化能力,细化效率随道次增加而逐渐下降。往复挤压温度越低或挤压道次越多则组织越细、分布越均匀。随着往复挤压道次的增加或挤压温度的下降,大角度晶界数量增加,晶粒平均位向差增加。
采用X射线衍射(XRD)和EBSD分析了往复挤压过程中镁合金织构的演变规律。发现晶粒在往复挤压过程中取向不断发生变化,挤压变形时{0002}基面向平行于挤压轴方向转动,镦粗变形时向垂直于挤压轴转动。往复挤压后挤压态镁合金的< 10 10>丝织构消失,进而转变为一种{0002}基面与挤压轴夹角20～30o的< 2201>丝织构。增加往复挤压道次或降低变形温度,织构强度趋于下降,但织构类型不变。往复挤压过程中镁合金组织的细化机制研究发现,其基本细化机制为动态再结晶细化,但在不同变形条件下具有不同的再结晶产生机制。在低温低变形量的粗晶镁合金中,通常以形核于孪晶界的非连续动态再结晶(DDRX)为主,以连续动态再结晶(CDRX)和旋转动态再结晶(RDRX)为辅;在中高温条件下以CDRX和RDRX为主,以DDRX为辅。第二相的细化机制主要是机械破碎。
通过室温拉伸考查了往复挤压对镁合金室温力学性能的影响规律。结果显示,随着往复挤压道次的增加,ZK60合金的屈服强度和抗拉强度都逐渐下降,下降速率由快变慢;伸长率大幅上升,最高达到41%,比往复挤压前提高了2.6倍。另一方面,随着往复挤压道次的增加,GW102K合金的屈服强度和抗拉强度都显著增加,伸长率更是提高了3.2倍,达到22%。变形温度对两种合金力学性能的影响规律基本相同,即变形温度升高,屈服强度和抗拉强度降低,往复挤压还能显著降低挤压态镁合金的力学性能各向异性,消除挤压态镁合金的拉压不对称性。
基于室温拉伸过程中的组织观察,分析了往复挤压ZK60和GW102K镁合金的室温变形机制和断裂机制。结果显示两种挤压态镁合金室温变形都很不均匀,裂纹主要形核于孪晶界和聚集的粗大第二相上。断裂形式在粗晶区为解理或准解理脆性断裂,在细晶区则为韧性断裂。往复挤压后ZK60合金室温变形均匀性显著提高,孪生数量逐渐下降,变形以滑移为主,断裂形式表现为微孔缩聚的穿晶韧性断裂。GW102K合金往复挤压后孪生仍为重要变形机制,裂纹仍主要萌生于第二相聚集区和孪晶界上,但断口上撕裂棱数量显著增多,均匀性也显著提高。
以纯镁为参照,分析讨论了两种合金中不同性质和数量的第二相粒子对往复挤压过程中镁合金组织演变和力学性能的影响规律。研究发现,第二相的种类、数量和分布对往复挤压镁合金的组织和力学性能具有重要影响。ZK60合金中主要第二相MgZn2含量为2～4%(体积分数),尺寸小,分布均匀。而GW102K合金中主要第二相Mg24(Gd, Y)5含量5～9%,尺寸大,主要分布在晶界上,阻碍了变形过程中晶粒的转动。使得GW102K合金织构集中度低,强度高,塑性差,且未出现随往复挤压道次增加强度下降的现象。
往复挤压镁合金强韧化机制的研究表明,往复挤压镁合金综合力学性的提高是细晶强化、织构强化、第二相强化、位错强化、晶界强化等多种机制协同作用的结果。晶粒细化后孪生减少,非基面滑移和晶界滑移激活,变形均匀性提高,是往复挤压镁合金主要的强韧化机制。织构主要通过改变基面取向因子来影响镁合金力学性能,是镁合金综合力学性能和各向同性提高的主要影响因素。第二相的数量、尺寸及分布可改变镁合金的变形机制从而影响其力学性能。因此,往复挤压镁合金的强韧化机制是以细晶强化、织构强化和第二相强化为主的复合强化机制。
Cyclic extrusion and compression (CEC) was used to produce ultra-fine grain size ZK60 and GW102K Mg alloys, in order to improve their mechanical properties and plastic deformation ability at room temperature (RT). The emphases were placed on the microstructure evolution, grain refinement mechanism, plastic deformation behavior, and the strengthening mechanism of CEC processed magnesium alloys.
In order to optimize and provide an insight into the mechanics of the CEC processing, the flow field, stress field, temperature field and strain field of ZK60 alloy during CEC was simulated using finite element method (FEM). The effects of process parameters on the distribution of strain were investigated. Physical modeling (PM) experiment with same material was carried out to verify the results of the numerical simulations. Results show that the die geometry and process parameters have a significant effect on the strain distribution. A bigger corner radius and a lower extrusion angle are useful to improve the strain homogeneity. A little friction between die and billet is beneficial to strain homogeneity, but the high friction is detrimental. Result of FEM and PM shows that two vortex flow regions with opposite flow direction are formed inside the cylindrical billet during CEC deformation. Although the deformation is inhomogeneous in both end regions of billet, a uniform region of equivalent strain exists, and the extent of uniform deformation increased with the increase of billet length.
The effects of CEC pass and CEC temperature on the grain size, grain boundaries structure and texture of ZK60 and GW102K Mg alloys were investigated by optical microscopy (OM), transmission electron microscopy (TEM), scanning electron microscopy (SEM) and electron backscattered diffraction (EBSD). The results show that magnesium alloys can be refined effectively by CEC, and the grain refining efficiency decreases with the increase of CEC pass number. Low CEC temperature and high CEC pass should be used to produce ultra-fine grain size Mg alloys. With the increase of the pass number or decrease of the deformation temperature, the number fraction of low angle grain boundaries (LAGBs) tends to decrease while the average misorientation tends to increase for both of ZK60 and GW102K alloys.
Texture evolution of ZK60 and GW102K alloy during CEC processing was studied using X-ray diffraction (XRD) and EBSD. Results shows that the texture of Mg alloys are affected by CEC pass number, CEC temperature and the second phase. The initial ED // < 10 10> fiber texture of extruded Mg alloys was disintegrated after CEC processing and developed a new < 2 201> fiber texture, in which the basal plane inclined 20～30o to extrusion direction. The texture intensity tends to decrease with the increase of accumulated strains or with the decrease of deformation temperature or with the increase of second phase. Thus, compared to pure Mg and ZK60 alloy, the intensity of texture of GW102K alloy is lowest.
The grain refining mechanism of Mg alloys during CEC was studied. Results show that the primary refining mechanism is dynamic recrystallization (DRX). In the condition of low deformation temperature and low accumulated strains, the refining mechanism is dominated by discontinuous dynamic recrystallization (DDRX) and assisted by continuous dynamic recrystallization (CDRX) and rotation dynamic recrystallization (RDRX). In the case of high temperature and high CEC pass, the refining mechanism is combined both the CDRX and RDRX, while assisted by the DDRX. For the second phase, it is mechanical cracking refining mechanism.
The effect of CEC processing on the mechanical properties of ZK60 and GW102K alloys were investigated by tensile testing at RT. Results show that the yield strength (YS) and ultimate tensile strength (UTS) of ZK60 alloy decreased with the increase of CEC pass, although the grain size were refined dramatically. On the other hand, the elongation of ZK60 alloy increased obviously after CEC processing. Different from ZK60 alloy, the YS and UTS of GW102K alloy increased with the increase of CEC pass. The grain size and YS of GW102K alloy is consistent with Hall-Petch relationship. Similar to ZK60, the elongation of GW102K alloy was dramatically increased after CEC. The temperature has similar effect to both of ZK60 and GW102K alloys, i.e., the YS and UTS decreased and elongation increased with the increased of the CEC temperature. Moreover, the intensity of strength-differential effect (SDE) of as-extruded ZK60 alloy was decreased noticeably.
The plastic deformation behavior and fracture mode of CEC processed ZK60 and GW102K alloys at RT were investigated by OM, SEM and TEM. Results show that the plastic deformation of as-extruded Mg alloys tends to be rather heterogeneous. In the coarse grains the twinning is predominant deformation mechanism and in the fine grains it is dislocation. Twin boundaries are main crack nucleation sites. After CEC the non-basal dislocation activated and the fraction of twinning decreased, and the deformation became more homogeneous. Furthermore, the main fracture mode changed from quasi cleavage to ductile dimple.
The effect of second phase on the microstructure and mechanical properties of ZK60 and GW102K alloys were studied. Results show that the volume of Mg24(Gd, Y)5, i.e. the main second phase in GW102K alloy, is about 5～9%. It is much more than that of MgZn2 in ZK60 (2～4%). The MgZn2 is fine and homogeneously distributed in matrix. Whereas, the Mg24(Gd, Y)5 mainly distributed near the grain boundaries. During CEC processing, the grain boundary sliding (GBS) in GW102K alloy was retarded. As a result, GW102K alloy has a higher strength and a lower elongation and a lower texture intensity than that of ZK60 alloy. Study
The mechanical properties of CEC processed Mg alloy depends on its grain size, texture type, texture intensity, second phase volume and distribution, dislocation density, grain boundary structure, and so on. The strengthening mechanism can be described as a compound strengthening mechanism, which predominated by grain refinement strengthening, texture strengthening and second phase strengthening.
本文首先利用有限元数值模拟方法分析了往复挤压模具结构和工艺参数对材料流动的影响,优化了往复挤压模具及工艺,并利用物理实验验证了数值模拟结果的可靠性。往复挤压工艺数值模拟发现,模具结构和往复挤压工艺参数对材料应变的分布具有很大影响。模具过渡角越大、模具入口角越小、摩擦越小试样应变分布越均匀,但小量摩擦有利于应变的均匀分布。较小的挤压比可防止材料在变形过程中失稳;模具入口角为45°时应变分布最均匀,载荷最低;挤压速度对应变分布基本没有影响;根据变形温度的不同,塑变生热和摩擦生热能在4至8道次内弥补模具向环境散热引起的温降。对流场的模拟和实验研究发现,随着往复挤压道次的增加流线逐渐变得紊乱。材料的流动规律是:试样表层的材料背向流动,心部相向流动,进而在试样的上下两部分各形成一个流动漩涡。
利用金相显微镜(OM)、扫描电镜(SEM)、电子背散射技术(EBSD)和透射电镜(TEM)从不同尺度分析了往复挤压变形温度和变形道次对ZK60和GW102K两种镁合金微观组织的影响规律。结果表明,往复挤压对ZK60和GW102K镁合金都具有强烈的细化能力,细化效率随道次增加而逐渐下降。往复挤压温度越低或挤压道次越多则组织越细、分布越均匀。随着往复挤压道次的增加或挤压温度的下降,大角度晶界数量增加,晶粒平均位向差增加。
采用X射线衍射(XRD)和EBSD分析了往复挤压过程中镁合金织构的演变规律。发现晶粒在往复挤压过程中取向不断发生变化,挤压变形时{0002}基面向平行于挤压轴方向转动,镦粗变形时向垂直于挤压轴转动。往复挤压后挤压态镁合金的< 10 10>丝织构消失,进而转变为一种{0002}基面与挤压轴夹角20～30o的< 2201>丝织构。增加往复挤压道次或降低变形温度,织构强度趋于下降,但织构类型不变。往复挤压过程中镁合金组织的细化机制研究发现,其基本细化机制为动态再结晶细化,但在不同变形条件下具有不同的再结晶产生机制。在低温低变形量的粗晶镁合金中,通常以形核于孪晶界的非连续动态再结晶(DDRX)为主,以连续动态再结晶(CDRX)和旋转动态再结晶(RDRX)为辅;在中高温条件下以CDRX和RDRX为主,以DDRX为辅。第二相的细化机制主要是机械破碎。
通过室温拉伸考查了往复挤压对镁合金室温力学性能的影响规律。结果显示,随着往复挤压道次的增加,ZK60合金的屈服强度和抗拉强度都逐渐下降,下降速率由快变慢;伸长率大幅上升,最高达到41%,比往复挤压前提高了2.6倍。另一方面,随着往复挤压道次的增加,GW102K合金的屈服强度和抗拉强度都显著增加,伸长率更是提高了3.2倍,达到22%。变形温度对两种合金力学性能的影响规律基本相同,即变形温度升高,屈服强度和抗拉强度降低,往复挤压还能显著降低挤压态镁合金的力学性能各向异性,消除挤压态镁合金的拉压不对称性。
基于室温拉伸过程中的组织观察,分析了往复挤压ZK60和GW102K镁合金的室温变形机制和断裂机制。结果显示两种挤压态镁合金室温变形都很不均匀,裂纹主要形核于孪晶界和聚集的粗大第二相上。断裂形式在粗晶区为解理或准解理脆性断裂,在细晶区则为韧性断裂。往复挤压后ZK60合金室温变形均匀性显著提高,孪生数量逐渐下降,变形以滑移为主,断裂形式表现为微孔缩聚的穿晶韧性断裂。GW102K合金往复挤压后孪生仍为重要变形机制,裂纹仍主要萌生于第二相聚集区和孪晶界上,但断口上撕裂棱数量显著增多,均匀性也显著提高。
以纯镁为参照,分析讨论了两种合金中不同性质和数量的第二相粒子对往复挤压过程中镁合金组织演变和力学性能的影响规律。研究发现,第二相的种类、数量和分布对往复挤压镁合金的组织和力学性能具有重要影响。ZK60合金中主要第二相MgZn2含量为2～4%(体积分数),尺寸小,分布均匀。而GW102K合金中主要第二相Mg24(Gd, Y)5含量5～9%,尺寸大,主要分布在晶界上,阻碍了变形过程中晶粒的转动。使得GW102K合金织构集中度低,强度高,塑性差,且未出现随往复挤压道次增加强度下降的现象。
往复挤压镁合金强韧化机制的研究表明,往复挤压镁合金综合力学性的提高是细晶强化、织构强化、第二相强化、位错强化、晶界强化等多种机制协同作用的结果。晶粒细化后孪生减少,非基面滑移和晶界滑移激活,变形均匀性提高,是往复挤压镁合金主要的强韧化机制。织构主要通过改变基面取向因子来影响镁合金力学性能,是镁合金综合力学性能和各向同性提高的主要影响因素。第二相的数量、尺寸及分布可改变镁合金的变形机制从而影响其力学性能。因此,往复挤压镁合金的强韧化机制是以细晶强化、织构强化和第二相强化为主的复合强化机制。
Cyclic extrusion and compression (CEC) was used to produce ultra-fine grain size ZK60 and GW102K Mg alloys, in order to improve their mechanical properties and plastic deformation ability at room temperature (RT). The emphases were placed on the microstructure evolution, grain refinement mechanism, plastic deformation behavior, and the strengthening mechanism of CEC processed magnesium alloys.
In order to optimize and provide an insight into the mechanics of the CEC processing, the flow field, stress field, temperature field and strain field of ZK60 alloy during CEC was simulated using finite element method (FEM). The effects of process parameters on the distribution of strain were investigated. Physical modeling (PM) experiment with same material was carried out to verify the results of the numerical simulations. Results show that the die geometry and process parameters have a significant effect on the strain distribution. A bigger corner radius and a lower extrusion angle are useful to improve the strain homogeneity. A little friction between die and billet is beneficial to strain homogeneity, but the high friction is detrimental. Result of FEM and PM shows that two vortex flow regions with opposite flow direction are formed inside the cylindrical billet during CEC deformation. Although the deformation is inhomogeneous in both end regions of billet, a uniform region of equivalent strain exists, and the extent of uniform deformation increased with the increase of billet length.
The effects of CEC pass and CEC temperature on the grain size, grain boundaries structure and texture of ZK60 and GW102K Mg alloys were investigated by optical microscopy (OM), transmission electron microscopy (TEM), scanning electron microscopy (SEM) and electron backscattered diffraction (EBSD). The results show that magnesium alloys can be refined effectively by CEC, and the grain refining efficiency decreases with the increase of CEC pass number. Low CEC temperature and high CEC pass should be used to produce ultra-fine grain size Mg alloys. With the increase of the pass number or decrease of the deformation temperature, the number fraction of low angle grain boundaries (LAGBs) tends to decrease while the average misorientation tends to increase for both of ZK60 and GW102K alloys.
Texture evolution of ZK60 and GW102K alloy during CEC processing was studied using X-ray diffraction (XRD) and EBSD. Results shows that the texture of Mg alloys are affected by CEC pass number, CEC temperature and the second phase. The initial ED // < 10 10> fiber texture of extruded Mg alloys was disintegrated after CEC processing and developed a new < 2 201> fiber texture, in which the basal plane inclined 20～30o to extrusion direction. The texture intensity tends to decrease with the increase of accumulated strains or with the decrease of deformation temperature or with the increase of second phase. Thus, compared to pure Mg and ZK60 alloy, the intensity of texture of GW102K alloy is lowest.
The grain refining mechanism of Mg alloys during CEC was studied. Results show that the primary refining mechanism is dynamic recrystallization (DRX). In the condition of low deformation temperature and low accumulated strains, the refining mechanism is dominated by discontinuous dynamic recrystallization (DDRX) and assisted by continuous dynamic recrystallization (CDRX) and rotation dynamic recrystallization (RDRX). In the case of high temperature and high CEC pass, the refining mechanism is combined both the CDRX and RDRX, while assisted by the DDRX. For the second phase, it is mechanical cracking refining mechanism.
The effect of CEC processing on the mechanical properties of ZK60 and GW102K alloys were investigated by tensile testing at RT. Results show that the yield strength (YS) and ultimate tensile strength (UTS) of ZK60 alloy decreased with the increase of CEC pass, although the grain size were refined dramatically. On the other hand, the elongation of ZK60 alloy increased obviously after CEC processing. Different from ZK60 alloy, the YS and UTS of GW102K alloy increased with the increase of CEC pass. The grain size and YS of GW102K alloy is consistent with Hall-Petch relationship. Similar to ZK60, the elongation of GW102K alloy was dramatically increased after CEC. The temperature has similar effect to both of ZK60 and GW102K alloys, i.e., the YS and UTS decreased and elongation increased with the increased of the CEC temperature. Moreover, the intensity of strength-differential effect (SDE) of as-extruded ZK60 alloy was decreased noticeably.
The plastic deformation behavior and fracture mode of CEC processed ZK60 and GW102K alloys at RT were investigated by OM, SEM and TEM. Results show that the plastic deformation of as-extruded Mg alloys tends to be rather heterogeneous. In the coarse grains the twinning is predominant deformation mechanism and in the fine grains it is dislocation. Twin boundaries are main crack nucleation sites. After CEC the non-basal dislocation activated and the fraction of twinning decreased, and the deformation became more homogeneous. Furthermore, the main fracture mode changed from quasi cleavage to ductile dimple.
The effect of second phase on the microstructure and mechanical properties of ZK60 and GW102K alloys were studied. Results show that the volume of Mg24(Gd, Y)5, i.e. the main second phase in GW102K alloy, is about 5～9%. It is much more than that of MgZn2 in ZK60 (2～4%). The MgZn2 is fine and homogeneously distributed in matrix. Whereas, the Mg24(Gd, Y)5 mainly distributed near the grain boundaries. During CEC processing, the grain boundary sliding (GBS) in GW102K alloy was retarded. As a result, GW102K alloy has a higher strength and a lower elongation and a lower texture intensity than that of ZK60 alloy. Study
The mechanical properties of CEC processed Mg alloy depends on its grain size, texture type, texture intensity, second phase volume and distribution, dislocation density, grain boundary structure, and so on. The strengthening mechanism can be described as a compound strengthening mechanism, which predominated by grain refinement strengthening, texture strengthening and second phase strengthening.
引文
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