铝、镁合金半固态浆料制备技术的研究
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摘要
材料的微观结构是材料科学和工程的核心内容，是材料加工和材料行为之间的关键纽带。因此对材料在成形过程中微观结构的有效控制成为材料工作者孜孜追求的目标。对于金属和合金材料，凝固是最重要的成形途径。建立在现代科学基础上的优质铸件凝固技术正成为材料成形加工的发展方向，优质铸件凝固技术包括压力铸造、精密铸造、连续铸轧、自蔓延高温合成熔铸以及半固态成形等工艺。传统铸造和挤压成形方法是利用工艺过程来获取能够提供零件使用性能的微观结构，相对来说，供给浆料必须是非枝晶结构的半固态金属加工工艺是由材料的微观结构来决定其工艺特征的。半固态金属成形具有许多独特的优点，如近(净)终成形、产品高质量和高性能以及工艺节能等，是21世纪最有前途的金属材料加工技术之一。本文总结了半固态金属加工工艺的发展，触变性结构的流变性能和非枝晶组织的形成机制，介绍了半固态加工的流变成形发展方向。在铸造工程中心的电磁材料加工这一技术研发基础上，试验研究和开发了铝、镁合金半固态浆料的制备技术。同时在国家自然科学基金(50374014)资助下，和北京有色金属研究总院合作开发了阻尼冷却管法制备铝合金半固态浆料的工艺。主要研究内容和结果如下：
1、提出小尺寸供给料在近液相线等温处理后，利用旋转电磁场搅拌制取半固态浆料进行流变成形AZ91镁合金的加工工艺，设计并制作了一套试验装置。利用该装置试验浇注了一系列固相率为3％到40％流变成形件。完成了铸件的金相分析，研究了铸件拉伸性能和微观组织相互关系，并利用连续剖面的二维图像构建初生固相颗粒聚团三维结构和形貌，讨论了在该工艺下触变性结构的形成机制等。实验结果表明：金属熔体缓慢冷却过程中施加旋转电磁场进行搅拌后，在低固相率条件下，由于搅拌作用在熔体中形成了均匀的温度场和溶质浓度分布，因而形成以等轴枝晶为基体的凝固组织，同时在熔体中形成的初生相颗粒数目较少，初生相颗粒在液相基体中存活并长大，在最终凝固组织中形成松散的颗粒聚团。随着浇注温度的降低，固相率上升导致了初生相颗粒数目增多，强烈搅拌引起固相颗粒间的相互作用，造成相邻颗粒间的摩擦和塑性变形，因此形成与低固相率铸件组织中不同的初生颗粒聚团结构，亦即高固相率微观组织中的颗粒聚团结构是许多颗粒焊合在一起形成的紧密结构，在基体中链接成刚性架构。高、低固相率铸件中这种聚团结构特征决定了两者在外力作用下不同的断裂行为和拉伸性能；另外，固相率的增加主要是以形成新晶粒的方式来实现的。
2、研究和分析了在液固两相区内等温处理过程中，高固相体积分数条件下AZ91镁合金的组织演变过程。结果表明：在体系自由能(界面能)降低的驱动下，晶界处的共晶组织首先熔化；随着温度的上升，次枝晶臂熔断，并重新沉淀在主干上；固相颗粒由于体表曲率差效应发生Ostwald熟化过程，枝晶组织演变成球形颗粒。熟化过程中形成晶内小液滴有两种方式：其一是由晶内富Al的质点经过熔化、扩散、合并形成；另一种就是在熟化过程中由于脱落的枝晶臂沉淀生长时搭桥形成。同时建立了枝晶在等温处理过程中演变成球形晶粒的模型，根据Gibbs-Thomson效应推出球化所需时间计算公式：
3、研发了在高速运动的金属液内应用循环冷却手段制取半固态浆料的新工艺。循环冷却水管在和金属流体快速热交换过程中，促进金属液爆发形核并降温至两相区内，形成高密度晶核悬浮分散在液相中的半固态浆料，实现细晶化、净终形的铸件成形。实验过程中组合利用U型冷却水管和旋转电磁场来满足这一工艺要求，应用A356铝合金实验结果表明：向电磁场驱动的高速旋转的金属液中插入循环冷却水管，可以快速带走金属液的热量，促进在金属液中形成高密度晶核并降温至两相区内；旋转电磁场促进了晶核、溶质、温度在液相中的均匀分布；高密度晶核的存在为晶粒以球形方式生长和凝固组织细化提供了必要前提。
4、应用阻尼冷却效应设计了一种半固态浆料的制备工艺，加工了一套实验装置，并进行了A356铝合金的一系列实验。实验结果表明：由于阻尼冷却管的冷却和搅拌作用，低过热度的金属液降温至两相区内，同时金属液中分布大量的游离晶核，从而形成半固态浆料。流变成形铸件的微观结构分析表明：浇注温度越低，铸件晶粒尺寸越小，并且球化程度越高。同时应用冷却斜槽工艺对比实验表明，在同一浇注温度下，阻尼冷却管法制备的铸件晶粒尺寸更加细小圆整。
5、在本文实验的基础上，分析了高密度晶核促进非枝晶组织的形成机制。引入“晶体生长前沿形核”机制和粘性流体的边界层理论，提出“代孕机制”解释强制对流金属液中的形核增殖现象。
Microstructures are at the center of materials science and engineering. They are the strategic link between materials processing and materials behavior. Microstructure control is therefore essential for any processing activity. The most important processing route for metals and alloys is solidification. Solidification technologies of premium castings, including die-casting, investment casting, continuous casting & rolling, self-propagating high temperature synthesis and semisolid processing, etc, have been the dominant research and development. The specific microstructure, which meets the demand of performance, is conventionally obtained by casting and forging process. In comparison with those two methods, SSM(semisolid metal processing) is a new processing route, in which the processing feature depends on the thixotropic structure of the feedstock, which is so called non-dendritic microstructure. SSM is one of the most important processing technologies in 21~(st) century due to its advantages, such as near net-shape forming, high quality and performance of products, and energy-saving, to name a few.
The development of SSM, rheological behavior of the thixotropic structures and the formation mechanism of non-dendritic microstructure are summarized, and rheoforming route, which is the developing front of SSM, is introduced in the present paper. Research and development on semisolid slurry processing technology of Magnesium- and Aluminum-based alloys is fulfilled theoretically and experimentally, based on the abundant experience of EPM(Electromagnetic processing materials) in Foundry Engineering Center. Moreover, Damper cooling method (DCT) is developed to processing semisolid slurry for rheoforming Al-alloys, which is supported by National Natural Science Foundation(50374014) and cooperated with General Research Institute for Nonferrous Metals. The present doctoral dissertation is performed on basis of the above research works. Main research details and results are as follows:
(1) AZ91 magnesium alloy is semisolid processed under experimental conditions designed to yield from 3% to 40% of the primary particles, and the semisolid slurry is produced by electromagnetic stirring after feedstock with small dimension has been isothermally heat treated at near-liquidus temperature. The thixotropic microstructures obtained are characterized in detail and linked to the corresponding tensile properties, and serial sectioning experiments are performed to construct three dimensional morphologies of clusters consisting of conglutinated primary grains. The experimental results indicate that incompact structure agglomerating a few primary solid particles is observed within structures of low solid fraction, while a reduction in the castings' forming temperature and so increasing the fraction of primary solid phase bright out interaction among the primary particles within vigorously stirring melt, and thus causes slide and plastic deformation between or among the neighboring solid particles. In contrast with structure with low solid fraction, this slide and plastic deformation results in differently morphological 3D structures welded together with much more solid particles. The fractographic analysis reveals that fracture mechanism and corresponding morphology of the rapture surface of tensile bars depend on the solid fraction of the primary particles. Moreover, the increase in solid fraction mainly lies on the formation of new particles.
(2) Microstructure evolution of AZ91 magnesium alloy, which is isothermally treated in solid-liquid region at a high volume fraction of solid from as-cast microstructure then transforms to semisolid state, is investigated. The results show that eutectic phase with net-work shape is first to melt, and second dendritic arms disappear or melt off and then re-precipitated on the dendritic trunk. Solid particles go through Ostwald ripening due to Gibbs-Thomson effect resulting from difference of curvatures, and transform into globular particles, and coalesce together with the time. Moreover, the entrapped liquid drops form intra-grain by two mechanisms owing to decreasing interfacial energy: one is that inclusions containing rich solute Al and Zn melt, diffuse and then coalesce together into larger liquid drops during hear treat process; and the other is that second dendrite arms, which melt off and re-precipitate on the trunk, enclose to form liquid drops by bridge-growth. In addition, a model is built and applied to calculate the spheroidizing time of dendritic grain during isothermal heat treatment, and of which calculating formula is proposed as
(3) A novel approach is designed to obtain thixotropic structure of equiaxed or non-dendrtic grains for fine-grain and net-shape forming method, and demonstrated experimentally using A356 aluminum alloy. The circumstance in bulk liquid metal, which would burst into copious nucleation, and at the same time create homogeneous distribution of temperature and solute, is constructed by combined utilization of rotating magnetic fields and a cooling tube. Both microstructures solidified in metal mold and sand mold exhibit non-dendritic characteristic. Analyses of the rheocasting A356 microstructure indicate that high density of nuclei occurs by inserting a cooling tube into rotating slurry at liquidus temperature. In the case of slow cooling rate, mushy slurry obtained with high nuclei density keeps non-dendritic morphology of primary particles with holding time, accompanying with grain particles' coarsening and spheroidizing.
(4) Damper cooling tube method (DCT) processing semisolid slurry is designed, and demonstrated with A356 aluminum alloy in the case of different pouring temperatures. It is shown that there is a direct relationship between the pouring temperature and the grain size and shape factor after comparing and characterizing the castings microstructure: the lower the pouring temperature, the smaller the grain size and shape factor, due to more stray nucleus produced. The reason for this is that the alloy melt is stirred and cooled by DCT. In addition, in comparison with cooling slope process, the grains of castings produced by DCT exhibit finer and more round.
(5) The formation mechanism of non-dendritic structure resulting from high density of nuclei is analyzed in foundation on the aforementioned investigation. The theory of crystal growth front nucleation is introduced with the effect of boundary layer resulting from viscous fluid, and "surrogacy-mechanism" is proposed to explain the copious nucleation of liquid alloy with coerced convection.
1、提出小尺寸供给料在近液相线等温处理后，利用旋转电磁场搅拌制取半固态浆料进行流变成形AZ91镁合金的加工工艺，设计并制作了一套试验装置。利用该装置试验浇注了一系列固相率为3％到40％流变成形件。完成了铸件的金相分析，研究了铸件拉伸性能和微观组织相互关系，并利用连续剖面的二维图像构建初生固相颗粒聚团三维结构和形貌，讨论了在该工艺下触变性结构的形成机制等。实验结果表明：金属熔体缓慢冷却过程中施加旋转电磁场进行搅拌后，在低固相率条件下，由于搅拌作用在熔体中形成了均匀的温度场和溶质浓度分布，因而形成以等轴枝晶为基体的凝固组织，同时在熔体中形成的初生相颗粒数目较少，初生相颗粒在液相基体中存活并长大，在最终凝固组织中形成松散的颗粒聚团。随着浇注温度的降低，固相率上升导致了初生相颗粒数目增多，强烈搅拌引起固相颗粒间的相互作用，造成相邻颗粒间的摩擦和塑性变形，因此形成与低固相率铸件组织中不同的初生颗粒聚团结构，亦即高固相率微观组织中的颗粒聚团结构是许多颗粒焊合在一起形成的紧密结构，在基体中链接成刚性架构。高、低固相率铸件中这种聚团结构特征决定了两者在外力作用下不同的断裂行为和拉伸性能；另外，固相率的增加主要是以形成新晶粒的方式来实现的。
2、研究和分析了在液固两相区内等温处理过程中，高固相体积分数条件下AZ91镁合金的组织演变过程。结果表明：在体系自由能(界面能)降低的驱动下，晶界处的共晶组织首先熔化；随着温度的上升，次枝晶臂熔断，并重新沉淀在主干上；固相颗粒由于体表曲率差效应发生Ostwald熟化过程，枝晶组织演变成球形颗粒。熟化过程中形成晶内小液滴有两种方式：其一是由晶内富Al的质点经过熔化、扩散、合并形成；另一种就是在熟化过程中由于脱落的枝晶臂沉淀生长时搭桥形成。同时建立了枝晶在等温处理过程中演变成球形晶粒的模型，根据Gibbs-Thomson效应推出球化所需时间计算公式：
3、研发了在高速运动的金属液内应用循环冷却手段制取半固态浆料的新工艺。循环冷却水管在和金属流体快速热交换过程中，促进金属液爆发形核并降温至两相区内，形成高密度晶核悬浮分散在液相中的半固态浆料，实现细晶化、净终形的铸件成形。实验过程中组合利用U型冷却水管和旋转电磁场来满足这一工艺要求，应用A356铝合金实验结果表明：向电磁场驱动的高速旋转的金属液中插入循环冷却水管，可以快速带走金属液的热量，促进在金属液中形成高密度晶核并降温至两相区内；旋转电磁场促进了晶核、溶质、温度在液相中的均匀分布；高密度晶核的存在为晶粒以球形方式生长和凝固组织细化提供了必要前提。
4、应用阻尼冷却效应设计了一种半固态浆料的制备工艺，加工了一套实验装置，并进行了A356铝合金的一系列实验。实验结果表明：由于阻尼冷却管的冷却和搅拌作用，低过热度的金属液降温至两相区内，同时金属液中分布大量的游离晶核，从而形成半固态浆料。流变成形铸件的微观结构分析表明：浇注温度越低，铸件晶粒尺寸越小，并且球化程度越高。同时应用冷却斜槽工艺对比实验表明，在同一浇注温度下，阻尼冷却管法制备的铸件晶粒尺寸更加细小圆整。
5、在本文实验的基础上，分析了高密度晶核促进非枝晶组织的形成机制。引入“晶体生长前沿形核”机制和粘性流体的边界层理论，提出“代孕机制”解释强制对流金属液中的形核增殖现象。
Microstructures are at the center of materials science and engineering. They are the strategic link between materials processing and materials behavior. Microstructure control is therefore essential for any processing activity. The most important processing route for metals and alloys is solidification. Solidification technologies of premium castings, including die-casting, investment casting, continuous casting & rolling, self-propagating high temperature synthesis and semisolid processing, etc, have been the dominant research and development. The specific microstructure, which meets the demand of performance, is conventionally obtained by casting and forging process. In comparison with those two methods, SSM(semisolid metal processing) is a new processing route, in which the processing feature depends on the thixotropic structure of the feedstock, which is so called non-dendritic microstructure. SSM is one of the most important processing technologies in 21~(st) century due to its advantages, such as near net-shape forming, high quality and performance of products, and energy-saving, to name a few.
The development of SSM, rheological behavior of the thixotropic structures and the formation mechanism of non-dendritic microstructure are summarized, and rheoforming route, which is the developing front of SSM, is introduced in the present paper. Research and development on semisolid slurry processing technology of Magnesium- and Aluminum-based alloys is fulfilled theoretically and experimentally, based on the abundant experience of EPM(Electromagnetic processing materials) in Foundry Engineering Center. Moreover, Damper cooling method (DCT) is developed to processing semisolid slurry for rheoforming Al-alloys, which is supported by National Natural Science Foundation(50374014) and cooperated with General Research Institute for Nonferrous Metals. The present doctoral dissertation is performed on basis of the above research works. Main research details and results are as follows:
(1) AZ91 magnesium alloy is semisolid processed under experimental conditions designed to yield from 3% to 40% of the primary particles, and the semisolid slurry is produced by electromagnetic stirring after feedstock with small dimension has been isothermally heat treated at near-liquidus temperature. The thixotropic microstructures obtained are characterized in detail and linked to the corresponding tensile properties, and serial sectioning experiments are performed to construct three dimensional morphologies of clusters consisting of conglutinated primary grains. The experimental results indicate that incompact structure agglomerating a few primary solid particles is observed within structures of low solid fraction, while a reduction in the castings' forming temperature and so increasing the fraction of primary solid phase bright out interaction among the primary particles within vigorously stirring melt, and thus causes slide and plastic deformation between or among the neighboring solid particles. In contrast with structure with low solid fraction, this slide and plastic deformation results in differently morphological 3D structures welded together with much more solid particles. The fractographic analysis reveals that fracture mechanism and corresponding morphology of the rapture surface of tensile bars depend on the solid fraction of the primary particles. Moreover, the increase in solid fraction mainly lies on the formation of new particles.
(2) Microstructure evolution of AZ91 magnesium alloy, which is isothermally treated in solid-liquid region at a high volume fraction of solid from as-cast microstructure then transforms to semisolid state, is investigated. The results show that eutectic phase with net-work shape is first to melt, and second dendritic arms disappear or melt off and then re-precipitated on the dendritic trunk. Solid particles go through Ostwald ripening due to Gibbs-Thomson effect resulting from difference of curvatures, and transform into globular particles, and coalesce together with the time. Moreover, the entrapped liquid drops form intra-grain by two mechanisms owing to decreasing interfacial energy: one is that inclusions containing rich solute Al and Zn melt, diffuse and then coalesce together into larger liquid drops during hear treat process; and the other is that second dendrite arms, which melt off and re-precipitate on the trunk, enclose to form liquid drops by bridge-growth. In addition, a model is built and applied to calculate the spheroidizing time of dendritic grain during isothermal heat treatment, and of which calculating formula is proposed as
(3) A novel approach is designed to obtain thixotropic structure of equiaxed or non-dendrtic grains for fine-grain and net-shape forming method, and demonstrated experimentally using A356 aluminum alloy. The circumstance in bulk liquid metal, which would burst into copious nucleation, and at the same time create homogeneous distribution of temperature and solute, is constructed by combined utilization of rotating magnetic fields and a cooling tube. Both microstructures solidified in metal mold and sand mold exhibit non-dendritic characteristic. Analyses of the rheocasting A356 microstructure indicate that high density of nuclei occurs by inserting a cooling tube into rotating slurry at liquidus temperature. In the case of slow cooling rate, mushy slurry obtained with high nuclei density keeps non-dendritic morphology of primary particles with holding time, accompanying with grain particles' coarsening and spheroidizing.
(4) Damper cooling tube method (DCT) processing semisolid slurry is designed, and demonstrated with A356 aluminum alloy in the case of different pouring temperatures. It is shown that there is a direct relationship between the pouring temperature and the grain size and shape factor after comparing and characterizing the castings microstructure: the lower the pouring temperature, the smaller the grain size and shape factor, due to more stray nucleus produced. The reason for this is that the alloy melt is stirred and cooled by DCT. In addition, in comparison with cooling slope process, the grains of castings produced by DCT exhibit finer and more round.
(5) The formation mechanism of non-dendritic structure resulting from high density of nuclei is analyzed in foundation on the aforementioned investigation. The theory of crystal growth front nucleation is introduced with the effect of boundary layer resulting from viscous fluid, and "surrogacy-mechanism" is proposed to explain the copious nucleation of liquid alloy with coerced convection.
引文
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