变形镁合金的挤压工艺及其组织和力学性能的研究
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摘要
镁合金具有低密度,比强度、比刚度高,阻尼减震性良好,优良的机加工性能和可循环利用,在交通运输,航空航天,计算机通讯和消费电子产品等行业中具有广阔的应用前景,被誉为“21世纪最具发展前途的金属结构材料”,也成为近年来国内外材料界研究的热点之一。变形镁合金比传统铸造镁合金拥有更高的综合性能,应用范围也更加广泛。如何进一步提高变形镁合金的综合性能,满足某些结构件“以镁代铝”,甚至“代钢”的性能要求；减小各向异性,改善镁合金的室温塑性成形能力,简化产品制备工艺,提高生产效率,降低生产成本,扩大镁合金的应用范围是国内外研究的主要方向。
本文针对常用ZK60商用镁合金不能满足高速挤压的需求,通过合金设计和高温热压缩实验,系统的研究了添加不同含量Ce和Cu元素(0.5,1.0,1.5wt.%)ZK60镁合金的高温塑性变形行为,获得了相关的流变应力应变曲线,并分别运用多步回归模型和人工神经网络模型构建了包含应变在内的本构关系方程。结合构建的合金热加工图详细研究了合金在压缩变形中的流变行为和显微组织演变特征。同时还通过挤压实验,系统的研究了两种合金元素和挤压工艺条件对材料组织和性能的影响。在此基础上,成功实现了ZK60-1Ce合金的10m/min高速挤压。
研究发现,ZK60及其添加Ce、Cu元素后的合金在进行高温压缩热变形过程中的流变应力变化规律是先随着真应变的增加到达峰值后又逐渐降低至某一稳态值,表现出较明显的动态再结晶特征。当变形温度一定时,流变应力随应变速率的增大而增大；当应变速率一定时,流变应力随变形温度的升高而降低。在较高的温度和较低的应变速率下变形时,流变应力达到峰值后基本表现为稳态流变特征。基于双曲正弦本构关系模型,建立了固溶态ZK60合金的相关本构方程。同时采用多步回归模型和人工神经网络模型预测了ZK60及其添加Ce、Cu元素后合金的高温流变应力,两种模型的预测结果与实验值吻合的较好。ZK60的高温压缩变形是以位错攀移为控制机制。Ce和Cu元素的加入可提高合金的峰值应力、临界应力和门槛应力,且这些值都随着变形温度的增加而降低。绘制出ZK60及其添加Ce、Cu元素合金的热加工图,发现ZK60及ZK60-0.5Ce合金都在低温高应变速率区出现变形失稳,表现为试样表面出现裂纹,显微组织由孪生与局部流变带构成,同时也得到添加不同合金化元素后ZK60合金的最佳加工条件。添加小于1.0wt.%含量的Ce可提高ZK60合金的加工性能,但1.5wt.%的Ce则使得加工性能下降；Cu元素的加入不能有效改善ZK60合金的加工性能。ZK60合金和ZK60-0.5Ce合金再结晶过程中都是由交滑移所产生的机械回复位错控制着新界面的形成,但ZK60合金再结晶主要受界面形成所控制而ZK60-0.5Ce合金则受界面迁移所控制。合金在挤压过程中均发生了动态再结晶,且形成强烈的基面平行于挤压方向的纤维织构。ZK60合金中的主要第二相为Mg-Zn相；随Ce、Cu元素的加入出现Mg-Zn-Ce和Mg-Zn-Cu第二相,这些硬质相在随后的挤压过程中破碎并沿挤压方向分布,导致第二相粒子激发形核(PSN),促进动态再结晶过程,不同程度地细化晶粒并弱化织构；对比研究发现Ce元素和Cu元素的加入具有相似的效果。ZK60合金屈服强度随着Ce或Cu加入含量的增加大幅提高,而抗拉强度提高幅度并不明显；强度的提高主要归因于弥散强化、析出沉淀强化和晶界强化的综合作用；但合金化元素含量的升高导致大量硬质第二相颗粒生成,其在拉伸试验进行中很容易破裂并成为裂纹源,进而导致材料的延伸率下降。随着挤压温度的上升和挤压速度的提高,再结晶体积分数和平均晶粒尺寸均随之增大；另外,温度升高引起晶粒长大,带状组织的出现和孪生的发生致使合金强度呈现下降趋势；添加Ce元素虽可增强显微组织均匀性但同时发现含Ce合金较ZK60合金对挤压工艺条件更为敏感。本论文可以为改善镁合金的室温塑性成形能力,简化产品制备工艺,提高生产效率,降低生产成本奠定基础。
Magnesium alloys are considered to have the most promising development outlook as metallic structural materials in the21st century due to their high specific strength and specific stiffness, good damping capacity, excellent machinability and easy recycling. Magnesium alloy has become one of the hot topics in the field of materials research around the world. The principle direction to improve the integrated properties of Mg alloy is to satisfy the requirements of some structural materials, such as aluminum, or even steel. Researches which aim to increase the elongation, decrease the anisotropy and improve the plastic deformation capability, simplify fabrication technics, reduce manufacturing cost and expand the application of magnesium alloy are also paid worldwide attention.
The applications of ZK60alloy processed by extrusion have been very limited due to their low extrusion speed. In this study, ZK60alloy was selected as base alloy and we designed the new ZK based Mg alloy by addition of different contents of Ce or Cu elements from0.5wt.%to1.5wt.%. The hot deformation behavior T4-treated ZK60alloy with/without Ce or Cu addition was investigated by compressive test using Gleeble3800thermal-simulator in the temperature range of523-673K and strain rate range of0.001-1s-1. In addition, the strain-dependent constitutive models were established by both regression model and feed-forward back-propagation artificial neural network (ANN) model. The rheological behavior and microstructural evolution during compression test were studied with the processing maps. In addition, this thesis also investigated the effects of alloy elements (Ce or Cu) and extrusion conditions on the microstructure and mechanical properties of ZK60alloy. Based on this, the ZK60-1Ce alloy was successfully extruded at high speed of10m/min.
The results reveal that the flow stress of all alloys is significantly affected by both deformation temperature and strain rate. The flow stress increases with either decreasing deformation temperature or increasing strain rate. The flow stress tends to be constant after a peak value at high deformation temperature and low strain rate. The hot deformation behavior of T4-treated ZK60alloy can be described by the hyperbolic sine constitutive equation. The predicted data sets from both of regression model and ANN model showed good agreement with the experimental ones. The stress exponent n equals five, which implies that the controlled deformation mechanism of ZK60alloy is dislocation climb controlled by grain boundary diffusion. The peak stress, critical stress and threshold stress increases with increasing of content of Ce or Cu element in ZK60alloy, but decreases as the increasing of deformation temperature.
From the processing maps of ZK60and ZK60-0.5Ce, the instability phenomenon can be found located in low temperature and high strain rate region. Samples deformed in this domain will lead to cracks generated at the surface, and the microstructure consisted of twining and local shear band. In addition, the optimum process parameter can also be obtained from the processing maps. The hot workability of ZK60alloy improves up to the addition of1.0wt.%Ce and then deteriorates. There is no obvious improvement of hot workability by addition of Cu. The formation of interface depends on the process of mechanical recovery by cross-slip of screw dislocations in both ZK60and ZK60-0.5Ce alloy. While the DRX of ZK60alloy and ZK60-0.5Ce is controlled by the interface formation and interface migration, respectively. DRX occurs during the extrusion and a strong basal texture is prone to be formed. The main phase in ZK60alloy is α-Mg and Mg-Zn phase, with addition of Ce or Cu. Mg-Zn-Ce and Mg-Zn-Cu phase are generated. Both Ce and Cu had an obvious influence, reducing the average grain size and weakening the basal fiber texture of the as-extruded alloys; these changes were attributed to the promotion of dynamic recrystallization (DRX) by particle stimulated nucleation (PSN). The yield and tensile strengths were improved by the Ce addition attributable to the combination of dispersion strengthening, precipitate strengthening and grain boundary strengthening, while the elongation was decreased due to the increase of large and fragile particles, which are considered as sources of cracks. The grain size and fraction of DRX increases with increasing of extrusion temperature and extrusion speed. The strength of the alloys decreases due to the presence of twinning and unDRX grains. Ce addition makes the microstructure more homogenized. And Ce added alloys significantly depend on the extrusion conditions. In summary, this thesis gives well understanding to the following aspects:improve the workability of Mg alloy at low temperature; simplify the fabrication process, decrease the production cost with enhanced productivity.
本文针对常用ZK60商用镁合金不能满足高速挤压的需求,通过合金设计和高温热压缩实验,系统的研究了添加不同含量Ce和Cu元素(0.5,1.0,1.5wt.%)ZK60镁合金的高温塑性变形行为,获得了相关的流变应力应变曲线,并分别运用多步回归模型和人工神经网络模型构建了包含应变在内的本构关系方程。结合构建的合金热加工图详细研究了合金在压缩变形中的流变行为和显微组织演变特征。同时还通过挤压实验,系统的研究了两种合金元素和挤压工艺条件对材料组织和性能的影响。在此基础上,成功实现了ZK60-1Ce合金的10m/min高速挤压。
研究发现,ZK60及其添加Ce、Cu元素后的合金在进行高温压缩热变形过程中的流变应力变化规律是先随着真应变的增加到达峰值后又逐渐降低至某一稳态值,表现出较明显的动态再结晶特征。当变形温度一定时,流变应力随应变速率的增大而增大；当应变速率一定时,流变应力随变形温度的升高而降低。在较高的温度和较低的应变速率下变形时,流变应力达到峰值后基本表现为稳态流变特征。基于双曲正弦本构关系模型,建立了固溶态ZK60合金的相关本构方程。同时采用多步回归模型和人工神经网络模型预测了ZK60及其添加Ce、Cu元素后合金的高温流变应力,两种模型的预测结果与实验值吻合的较好。ZK60的高温压缩变形是以位错攀移为控制机制。Ce和Cu元素的加入可提高合金的峰值应力、临界应力和门槛应力,且这些值都随着变形温度的增加而降低。绘制出ZK60及其添加Ce、Cu元素合金的热加工图,发现ZK60及ZK60-0.5Ce合金都在低温高应变速率区出现变形失稳,表现为试样表面出现裂纹,显微组织由孪生与局部流变带构成,同时也得到添加不同合金化元素后ZK60合金的最佳加工条件。添加小于1.0wt.%含量的Ce可提高ZK60合金的加工性能,但1.5wt.%的Ce则使得加工性能下降；Cu元素的加入不能有效改善ZK60合金的加工性能。ZK60合金和ZK60-0.5Ce合金再结晶过程中都是由交滑移所产生的机械回复位错控制着新界面的形成,但ZK60合金再结晶主要受界面形成所控制而ZK60-0.5Ce合金则受界面迁移所控制。合金在挤压过程中均发生了动态再结晶,且形成强烈的基面平行于挤压方向的纤维织构。ZK60合金中的主要第二相为Mg-Zn相；随Ce、Cu元素的加入出现Mg-Zn-Ce和Mg-Zn-Cu第二相,这些硬质相在随后的挤压过程中破碎并沿挤压方向分布,导致第二相粒子激发形核(PSN),促进动态再结晶过程,不同程度地细化晶粒并弱化织构；对比研究发现Ce元素和Cu元素的加入具有相似的效果。ZK60合金屈服强度随着Ce或Cu加入含量的增加大幅提高,而抗拉强度提高幅度并不明显；强度的提高主要归因于弥散强化、析出沉淀强化和晶界强化的综合作用；但合金化元素含量的升高导致大量硬质第二相颗粒生成,其在拉伸试验进行中很容易破裂并成为裂纹源,进而导致材料的延伸率下降。随着挤压温度的上升和挤压速度的提高,再结晶体积分数和平均晶粒尺寸均随之增大；另外,温度升高引起晶粒长大,带状组织的出现和孪生的发生致使合金强度呈现下降趋势；添加Ce元素虽可增强显微组织均匀性但同时发现含Ce合金较ZK60合金对挤压工艺条件更为敏感。本论文可以为改善镁合金的室温塑性成形能力,简化产品制备工艺,提高生产效率,降低生产成本奠定基础。
Magnesium alloys are considered to have the most promising development outlook as metallic structural materials in the21st century due to their high specific strength and specific stiffness, good damping capacity, excellent machinability and easy recycling. Magnesium alloy has become one of the hot topics in the field of materials research around the world. The principle direction to improve the integrated properties of Mg alloy is to satisfy the requirements of some structural materials, such as aluminum, or even steel. Researches which aim to increase the elongation, decrease the anisotropy and improve the plastic deformation capability, simplify fabrication technics, reduce manufacturing cost and expand the application of magnesium alloy are also paid worldwide attention.
The applications of ZK60alloy processed by extrusion have been very limited due to their low extrusion speed. In this study, ZK60alloy was selected as base alloy and we designed the new ZK based Mg alloy by addition of different contents of Ce or Cu elements from0.5wt.%to1.5wt.%. The hot deformation behavior T4-treated ZK60alloy with/without Ce or Cu addition was investigated by compressive test using Gleeble3800thermal-simulator in the temperature range of523-673K and strain rate range of0.001-1s-1. In addition, the strain-dependent constitutive models were established by both regression model and feed-forward back-propagation artificial neural network (ANN) model. The rheological behavior and microstructural evolution during compression test were studied with the processing maps. In addition, this thesis also investigated the effects of alloy elements (Ce or Cu) and extrusion conditions on the microstructure and mechanical properties of ZK60alloy. Based on this, the ZK60-1Ce alloy was successfully extruded at high speed of10m/min.
The results reveal that the flow stress of all alloys is significantly affected by both deformation temperature and strain rate. The flow stress increases with either decreasing deformation temperature or increasing strain rate. The flow stress tends to be constant after a peak value at high deformation temperature and low strain rate. The hot deformation behavior of T4-treated ZK60alloy can be described by the hyperbolic sine constitutive equation. The predicted data sets from both of regression model and ANN model showed good agreement with the experimental ones. The stress exponent n equals five, which implies that the controlled deformation mechanism of ZK60alloy is dislocation climb controlled by grain boundary diffusion. The peak stress, critical stress and threshold stress increases with increasing of content of Ce or Cu element in ZK60alloy, but decreases as the increasing of deformation temperature.
From the processing maps of ZK60and ZK60-0.5Ce, the instability phenomenon can be found located in low temperature and high strain rate region. Samples deformed in this domain will lead to cracks generated at the surface, and the microstructure consisted of twining and local shear band. In addition, the optimum process parameter can also be obtained from the processing maps. The hot workability of ZK60alloy improves up to the addition of1.0wt.%Ce and then deteriorates. There is no obvious improvement of hot workability by addition of Cu. The formation of interface depends on the process of mechanical recovery by cross-slip of screw dislocations in both ZK60and ZK60-0.5Ce alloy. While the DRX of ZK60alloy and ZK60-0.5Ce is controlled by the interface formation and interface migration, respectively. DRX occurs during the extrusion and a strong basal texture is prone to be formed. The main phase in ZK60alloy is α-Mg and Mg-Zn phase, with addition of Ce or Cu. Mg-Zn-Ce and Mg-Zn-Cu phase are generated. Both Ce and Cu had an obvious influence, reducing the average grain size and weakening the basal fiber texture of the as-extruded alloys; these changes were attributed to the promotion of dynamic recrystallization (DRX) by particle stimulated nucleation (PSN). The yield and tensile strengths were improved by the Ce addition attributable to the combination of dispersion strengthening, precipitate strengthening and grain boundary strengthening, while the elongation was decreased due to the increase of large and fragile particles, which are considered as sources of cracks. The grain size and fraction of DRX increases with increasing of extrusion temperature and extrusion speed. The strength of the alloys decreases due to the presence of twinning and unDRX grains. Ce addition makes the microstructure more homogenized. And Ce added alloys significantly depend on the extrusion conditions. In summary, this thesis gives well understanding to the following aspects:improve the workability of Mg alloy at low temperature; simplify the fabrication process, decrease the production cost with enhanced productivity.
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