挤压铸造Mg-Nd(-Zr)合金工艺及凝固行为研究
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摘要
挤压铸造不仅可以细化晶粒还可以消除铸件中的缩松等缺陷,从而达到提高合金的力学性能的目的。挤压铸造理论与应用的研究近年来受到了越来越多的重视,但是其中关于镁合金的研究较少,而且现有的研究主要集中在常规Mg-Al系合金上,对于具有显著时效强化效果的镁稀土合金则几乎没有研究。即使在对Mg-Al系合金的现有研究中,对于共晶相Mg17Al12体积分数随压力的增加而增加的机制仍未获得令人信服的解释。另一方面,我国是镁和稀土的生产大国,新型镁稀土合金的研究对我国具有重要的战略意义。因此,研究压力下镁合金中固溶度变化规律,指导选择适合挤压铸造的镁稀土合金,进而对镁稀土合金在挤压铸造条件下的凝固行为和组织结构演化进行系统深入研究,从而优化挤压铸造工艺参数和完善挤压铸造理论,具有显著的研究意义和紧迫性。
本文首先以Mg-9Al合金、Mg-5Zn合金和纯镁为研究对象,采用扫描电子显微镜(SEM)、光学显微镜(OM)、X射线衍射仪(XRD)和正电子湮没实验(PAT)等分析手段探讨了压力对共晶相体积分数以及镁晶格常数的影响,进而分析其对合金固溶度的影响,为挤压铸造用镁稀土合金成分的选择提供理论依据。通过对压力下凝固时偏摩尔体积变化的讨论发现,压力下合金元素原子半径的改变可能是压力下合金固溶度变化的主要原因,并在此基础上得到了固溶度随压力变化趋势的经验公式,并预测和验证了Mg-Nd合金中Nd的固溶度具有随着压力的增加而增大的趋势。
在此基础上,本文选择Mg-2.5wt%Nd二元合金为重点研究对象,通过金相、SEM、TEM、EELS、拉伸试验等方法,系统研究了挤压铸造工艺参数和形核剂(Zr)对Mg-Nd合金组织及力学性能的影响,重点分析了压力对Mg-Nd合金中形核和长大的影响,并取得如下主要研究结果:
合金液浇注温度对挤压铸造的Mg-2.5Nd合金的宏观组织具有决定性的影响。当浇注温度高于某一临界浇注温度(例如浇注温度725°C和750°C)时,Mg-2.5Nd合金的宏观组织由粗大的柱状晶以及中心的等轴晶组成,并且随着压力的增加合金的晶粒尺寸越来越大。相反,当浇注温度低于该临界浇注温度(例如浇注温度为700°C)时,随着压力的增加合金的晶粒尺寸逐渐降低,当压力从60MPa升高到120MPa时合金的晶粒尺寸降低最为明显,继续增加压力则晶粒细化趋势明显趋缓。相对而言,模具温度对宏观组织的影响较小,只能降低晶粒尺寸,不能改变合金的晶粒结构(也就是组织由粗大的柱状晶和等轴晶转变为细小的等轴晶)。从挤压铸造中压力随时间的变化曲线可以看出,浇注温度、模具温度以及加压前等待时间共同决定加压时熔体的实际温度。通过理论分析发现加压时熔体的实际温度才是决定晶粒尺寸随压力的变化趋势的关键因素,当加压时熔体的温度高于压力下合金液相线温度时,随着压力的升高合金的晶粒尺寸逐渐增大;相反,当加压时熔体的温度低于高压下合金液相线温度时,增加压力可以降低合金的晶粒尺寸。进一步分析发现,当宏观组织由细小晶粒组成时,显微组织呈大小晶粒交错的双峰组织结构。双峰组织中的大晶粒由浇注温度、模具温度和加压前等待时间决定,浇注温度和模具温度越低,加压前等待时间越短,双峰组织中的大晶粒的晶粒尺寸越小。双峰组织中的小晶粒由压力决定,压力越大,双峰组织中的小晶粒的晶粒尺寸越小。挤压铸造Mg-2.5Nd合金的屈服强度与延伸率随着浇注温度和模具温度的降低以及凝固压力的升高而明显升高,并且合金的密度也随着压力的升高而升高。
当Mg-2.5Nd中存在异质形核剂Zr时,挤压铸造过程中合金的凝固仍以异质形核为主。在相同工艺条件下,Zr含量越高,合金的晶粒尺寸越小;当Zr含量为0.46%时,增大压力对合金的晶粒尺寸影响不明显,此时异质形核已占主导地位。挤压铸造Mg-2.5Nd-0.4Zr合金的延伸率与密度随着凝固压力的升高而升高,但屈服强度变化不大。
Mg-2.5Nd合金固溶处理过程中在晶界附近出现了NdH_2相,该相尺寸较大,会促进裂纹的萌生与扩展。加入Zr以后,固溶态Mg-2.5Nd合金的晶界上没有发现NdH_2相,而在晶粒中间发现可能为ZrH_2的细小析出物。
合金的凝固过程由形核和长大组成,而形核率的大小是决定合金晶粒度的关键因素。凝固曲线显示,当浇注温度为725oC时,挤压铸造Mg-2.5Nd合金的凝固温度为645~646oC,比重力铸造试样的凝固温度约高5oC;当浇注温度为700oC时,挤压铸造Mg-2.5Nd合金的凝固温度和重力铸造试样的凝固温度相同。形核机理研究结果表明,当加压时熔体的温度高于压力下合金的液相线温度时,增加压力可以提高合金的临界形核自由能,降低临界形核密度从而使形核率降低;与之相反,当加压时熔体的温度低于压力下合金的液相线温度时,增加压力可以降低合金的临界形核自由能,提高临界形核密度从而提高形核率。晶粒长大机制研究结果表明增大压力可以增加原子向固-液界面上的附着速度,降低凝固前沿的不稳定波长,从而提高合金的凝固速度。
本研究为选择适合挤压铸造的合金成分提供了一种思路,并且为选择挤压铸造镁稀土工艺参数提供了可靠的实验数据和理论分析。通过调整浇注温度、模具温度和压力可以改变合金的组织结构,从而获得致密度高、细小而均匀的合金组织,达到提高合金力学性能的目的。
The squeeze-cast process, combining the advantages of the casting and forging processes, has been widely used to produce quality castings. Because of the high pressure applied during solidification, porosities caused by both gas and shrinkage can be prevented or eliminated. The cooling rate of the casting can be increased by applied high pressure during solidification, since heat transfer between the casting and the die is improved by pressurization, which results in the formation of fine-grained structures. Although squeeze cast has gained more and more attention and application., limit researches have been done about squeeze-cast magnesium alloy, and these researches mainly focus on Mg-Al system and rarely on Mg-RE system (RE: rare earth elements). According to the existing research results of squeeze-cast Mg-Al series, it is still not clear why the volume fraction of Mg17Al12 increases with the increment of applied pressure, which goes against the squeeze-cast alloy design. Moreover, it has been demonstrated that rare earth is the most effective element to improve the properties of magnesium alloys especially at elevated temperatures, and the resources of magnesium and rare earth are abundant in our country. Therefore, it is necessary to discuss the change of solid solubility with applied pressure in order to provide the theory to the squeeze-cast alloy design and do systematic research on the squeeze cast Mg-RE alloy.
By scanning electron microscopy (SEM), optical microscopy (OM), X-ray diffractometer (XRD) and positron annihilation technique (PAT), the effect of applied pressure on the solid solubility is investigated by changing the volume fraction of eutectic phase and lattice constant of magnesium element on base of Mg-9Al alloy, Mg-5Zn alloy and pure magnesium. According to the discussion of the change in partial molar volume on solidification of solute in dilute solutions, it is found that the change of atomic radius may be the basic reason for the variation of solid solubility under applied pressure. And the empirical formula for the change trend of solid solubility with applied pressure is obtained. And the solid solubility of Nd in Mg is predicted and verified.
Based on the study of solid solubility, Mg-2.5wt%Nd is selected as material for investigation here. By OM, SEM, transmission electron microscopy (TEM), electron energy loss spectroscopy (EELS) and tensile test, the effects of process parameters and nucleating agents on the macrostructure, microstructure and mechanical properties of Mg-Nd alloy are studied and the effects of applied pressure on the nucleation and growth of Mg-Nd alloy are especially focused on. The main results can be summarized as follows:
Pouring temperature has a decisive effect on the macrostructure of squeeze-cast Mg-2.5Nd alloy. When the pouring temperatures are 725°C and 750°C, there are no obviously differences among the grain structure and the grain structures mainly consist of a band of thick columnar grains surrounding some large equiaxed grains in the center, but the grains tend to be coarse with the increment of applied pressure. However, when the pouring temperature is 700°C, the average grain sizes of the samples are decreased with the increment of applied pressure. When the applied pressure is 120MPa, the grains structure changes from coarse columnar and equiaxed grains into fine grains. On the other side, die temperature has small effect on the squeeze-cast Mg-Nd alloy, and can not change the grain structure, but low die temperature decreases the grain size. It is the practical melt temperature at the time of a pressure application that decides the relationship between grain size and applied pressure. When the practical melt temperature is above the melting point under applied pressure, the applied pressure leads to grain coarsening; while it is below the melting point under applied pressure, grains are refined by applied pressure. Further analysis of the fine grains, it is found that the microstructure of squeeze-cast Mg-2.5Nd alloy exhibits distinct regions of fine and coarse structure (Bi-modal structure). As a result, decreasing die temperature as well as pouring temperature and increasing applied pressure can improve the mechanical properties, especially elongation and tensile strength.
The microstructure of solution-treated Mg-Nd alloy is composed ofα-Mg and NdH2. The NdH2 particles are located at or near the grain boundaries, which worsens the alloy’s mechanical property, especially the cracking and fracture behaviors. Also, the NdH2 particles become another defects of hydrogen in magnesium alloy except of hydrogen embrittlement and pores. However, in the case of solution-treated Mg-Nd-Zr alloy, there are no NdH2 particles at or near the grain boundaries. While, some small particles, which might be ZrH2 phase, are distributed in grains.
In squeeze casting process, the nucleation of Mg-Nd alloy is still dominated by heterogeneous nucleation when Zr element exists. When process parameters of squeeze cast are same, the grain size decreases with the increment of Zr content; however, applied pressure has no obvious effect on the grain size when the Zr content is 0.46%.
The freezing curves show that the solidification temperature is about 645~646 oC, 5 oC higher than that of the sample by gravity cast under the condition of pouring temperature at 725 oC and applied pressure at 120MPa, while the solidification temperature is the same as that of the sample by gravity case when the pouring temperature is 700 oC and applied pressure is 120MPa. Study on nucleation in squeeze cast shows that if the practical melt temperature at the time of pressure application is above the melting point under applied pressure, the increment of applied pressure enhances the critical nucleation free energy and reduces the nucleation rate. On the contrary, if the practical melt temperature at the time of pressure application is below the melting point under applied pressure, the increment of applied pressure can decrease the critical nucleation free energy and enhance the nucleation rate. The study on growth of a formed nucleus shows that the increment of applied pressure can increase the speed of atoms attaching to solid-liquid interface, and decrease the unstable wavelength of a growing global grain, resulting in the increment of solidification rate.
The study of this thesis provides a new approach for the squeeze-cast alloy design, reliable data and theoretical analysis for the process parameters of squeeze-cast Mg-RE alloy. Microstructure can be controlled through adjusting applied pressure, die and pouring temperatures, which then results in the high density, fine and uniform microstructure to improve the mechanical properties.
本文首先以Mg-9Al合金、Mg-5Zn合金和纯镁为研究对象,采用扫描电子显微镜(SEM)、光学显微镜(OM)、X射线衍射仪(XRD)和正电子湮没实验(PAT)等分析手段探讨了压力对共晶相体积分数以及镁晶格常数的影响,进而分析其对合金固溶度的影响,为挤压铸造用镁稀土合金成分的选择提供理论依据。通过对压力下凝固时偏摩尔体积变化的讨论发现,压力下合金元素原子半径的改变可能是压力下合金固溶度变化的主要原因,并在此基础上得到了固溶度随压力变化趋势的经验公式,并预测和验证了Mg-Nd合金中Nd的固溶度具有随着压力的增加而增大的趋势。
在此基础上,本文选择Mg-2.5wt%Nd二元合金为重点研究对象,通过金相、SEM、TEM、EELS、拉伸试验等方法,系统研究了挤压铸造工艺参数和形核剂(Zr)对Mg-Nd合金组织及力学性能的影响,重点分析了压力对Mg-Nd合金中形核和长大的影响,并取得如下主要研究结果:
合金液浇注温度对挤压铸造的Mg-2.5Nd合金的宏观组织具有决定性的影响。当浇注温度高于某一临界浇注温度(例如浇注温度725°C和750°C)时,Mg-2.5Nd合金的宏观组织由粗大的柱状晶以及中心的等轴晶组成,并且随着压力的增加合金的晶粒尺寸越来越大。相反,当浇注温度低于该临界浇注温度(例如浇注温度为700°C)时,随着压力的增加合金的晶粒尺寸逐渐降低,当压力从60MPa升高到120MPa时合金的晶粒尺寸降低最为明显,继续增加压力则晶粒细化趋势明显趋缓。相对而言,模具温度对宏观组织的影响较小,只能降低晶粒尺寸,不能改变合金的晶粒结构(也就是组织由粗大的柱状晶和等轴晶转变为细小的等轴晶)。从挤压铸造中压力随时间的变化曲线可以看出,浇注温度、模具温度以及加压前等待时间共同决定加压时熔体的实际温度。通过理论分析发现加压时熔体的实际温度才是决定晶粒尺寸随压力的变化趋势的关键因素,当加压时熔体的温度高于压力下合金液相线温度时,随着压力的升高合金的晶粒尺寸逐渐增大;相反,当加压时熔体的温度低于高压下合金液相线温度时,增加压力可以降低合金的晶粒尺寸。进一步分析发现,当宏观组织由细小晶粒组成时,显微组织呈大小晶粒交错的双峰组织结构。双峰组织中的大晶粒由浇注温度、模具温度和加压前等待时间决定,浇注温度和模具温度越低,加压前等待时间越短,双峰组织中的大晶粒的晶粒尺寸越小。双峰组织中的小晶粒由压力决定,压力越大,双峰组织中的小晶粒的晶粒尺寸越小。挤压铸造Mg-2.5Nd合金的屈服强度与延伸率随着浇注温度和模具温度的降低以及凝固压力的升高而明显升高,并且合金的密度也随着压力的升高而升高。
当Mg-2.5Nd中存在异质形核剂Zr时,挤压铸造过程中合金的凝固仍以异质形核为主。在相同工艺条件下,Zr含量越高,合金的晶粒尺寸越小;当Zr含量为0.46%时,增大压力对合金的晶粒尺寸影响不明显,此时异质形核已占主导地位。挤压铸造Mg-2.5Nd-0.4Zr合金的延伸率与密度随着凝固压力的升高而升高,但屈服强度变化不大。
Mg-2.5Nd合金固溶处理过程中在晶界附近出现了NdH_2相,该相尺寸较大,会促进裂纹的萌生与扩展。加入Zr以后,固溶态Mg-2.5Nd合金的晶界上没有发现NdH_2相,而在晶粒中间发现可能为ZrH_2的细小析出物。
合金的凝固过程由形核和长大组成,而形核率的大小是决定合金晶粒度的关键因素。凝固曲线显示,当浇注温度为725oC时,挤压铸造Mg-2.5Nd合金的凝固温度为645~646oC,比重力铸造试样的凝固温度约高5oC;当浇注温度为700oC时,挤压铸造Mg-2.5Nd合金的凝固温度和重力铸造试样的凝固温度相同。形核机理研究结果表明,当加压时熔体的温度高于压力下合金的液相线温度时,增加压力可以提高合金的临界形核自由能,降低临界形核密度从而使形核率降低;与之相反,当加压时熔体的温度低于压力下合金的液相线温度时,增加压力可以降低合金的临界形核自由能,提高临界形核密度从而提高形核率。晶粒长大机制研究结果表明增大压力可以增加原子向固-液界面上的附着速度,降低凝固前沿的不稳定波长,从而提高合金的凝固速度。
本研究为选择适合挤压铸造的合金成分提供了一种思路,并且为选择挤压铸造镁稀土工艺参数提供了可靠的实验数据和理论分析。通过调整浇注温度、模具温度和压力可以改变合金的组织结构,从而获得致密度高、细小而均匀的合金组织,达到提高合金力学性能的目的。
The squeeze-cast process, combining the advantages of the casting and forging processes, has been widely used to produce quality castings. Because of the high pressure applied during solidification, porosities caused by both gas and shrinkage can be prevented or eliminated. The cooling rate of the casting can be increased by applied high pressure during solidification, since heat transfer between the casting and the die is improved by pressurization, which results in the formation of fine-grained structures. Although squeeze cast has gained more and more attention and application., limit researches have been done about squeeze-cast magnesium alloy, and these researches mainly focus on Mg-Al system and rarely on Mg-RE system (RE: rare earth elements). According to the existing research results of squeeze-cast Mg-Al series, it is still not clear why the volume fraction of Mg17Al12 increases with the increment of applied pressure, which goes against the squeeze-cast alloy design. Moreover, it has been demonstrated that rare earth is the most effective element to improve the properties of magnesium alloys especially at elevated temperatures, and the resources of magnesium and rare earth are abundant in our country. Therefore, it is necessary to discuss the change of solid solubility with applied pressure in order to provide the theory to the squeeze-cast alloy design and do systematic research on the squeeze cast Mg-RE alloy.
By scanning electron microscopy (SEM), optical microscopy (OM), X-ray diffractometer (XRD) and positron annihilation technique (PAT), the effect of applied pressure on the solid solubility is investigated by changing the volume fraction of eutectic phase and lattice constant of magnesium element on base of Mg-9Al alloy, Mg-5Zn alloy and pure magnesium. According to the discussion of the change in partial molar volume on solidification of solute in dilute solutions, it is found that the change of atomic radius may be the basic reason for the variation of solid solubility under applied pressure. And the empirical formula for the change trend of solid solubility with applied pressure is obtained. And the solid solubility of Nd in Mg is predicted and verified.
Based on the study of solid solubility, Mg-2.5wt%Nd is selected as material for investigation here. By OM, SEM, transmission electron microscopy (TEM), electron energy loss spectroscopy (EELS) and tensile test, the effects of process parameters and nucleating agents on the macrostructure, microstructure and mechanical properties of Mg-Nd alloy are studied and the effects of applied pressure on the nucleation and growth of Mg-Nd alloy are especially focused on. The main results can be summarized as follows:
Pouring temperature has a decisive effect on the macrostructure of squeeze-cast Mg-2.5Nd alloy. When the pouring temperatures are 725°C and 750°C, there are no obviously differences among the grain structure and the grain structures mainly consist of a band of thick columnar grains surrounding some large equiaxed grains in the center, but the grains tend to be coarse with the increment of applied pressure. However, when the pouring temperature is 700°C, the average grain sizes of the samples are decreased with the increment of applied pressure. When the applied pressure is 120MPa, the grains structure changes from coarse columnar and equiaxed grains into fine grains. On the other side, die temperature has small effect on the squeeze-cast Mg-Nd alloy, and can not change the grain structure, but low die temperature decreases the grain size. It is the practical melt temperature at the time of a pressure application that decides the relationship between grain size and applied pressure. When the practical melt temperature is above the melting point under applied pressure, the applied pressure leads to grain coarsening; while it is below the melting point under applied pressure, grains are refined by applied pressure. Further analysis of the fine grains, it is found that the microstructure of squeeze-cast Mg-2.5Nd alloy exhibits distinct regions of fine and coarse structure (Bi-modal structure). As a result, decreasing die temperature as well as pouring temperature and increasing applied pressure can improve the mechanical properties, especially elongation and tensile strength.
The microstructure of solution-treated Mg-Nd alloy is composed ofα-Mg and NdH2. The NdH2 particles are located at or near the grain boundaries, which worsens the alloy’s mechanical property, especially the cracking and fracture behaviors. Also, the NdH2 particles become another defects of hydrogen in magnesium alloy except of hydrogen embrittlement and pores. However, in the case of solution-treated Mg-Nd-Zr alloy, there are no NdH2 particles at or near the grain boundaries. While, some small particles, which might be ZrH2 phase, are distributed in grains.
In squeeze casting process, the nucleation of Mg-Nd alloy is still dominated by heterogeneous nucleation when Zr element exists. When process parameters of squeeze cast are same, the grain size decreases with the increment of Zr content; however, applied pressure has no obvious effect on the grain size when the Zr content is 0.46%.
The freezing curves show that the solidification temperature is about 645~646 oC, 5 oC higher than that of the sample by gravity cast under the condition of pouring temperature at 725 oC and applied pressure at 120MPa, while the solidification temperature is the same as that of the sample by gravity case when the pouring temperature is 700 oC and applied pressure is 120MPa. Study on nucleation in squeeze cast shows that if the practical melt temperature at the time of pressure application is above the melting point under applied pressure, the increment of applied pressure enhances the critical nucleation free energy and reduces the nucleation rate. On the contrary, if the practical melt temperature at the time of pressure application is below the melting point under applied pressure, the increment of applied pressure can decrease the critical nucleation free energy and enhance the nucleation rate. The study on growth of a formed nucleus shows that the increment of applied pressure can increase the speed of atoms attaching to solid-liquid interface, and decrease the unstable wavelength of a growing global grain, resulting in the increment of solidification rate.
The study of this thesis provides a new approach for the squeeze-cast alloy design, reliable data and theoretical analysis for the process parameters of squeeze-cast Mg-RE alloy. Microstructure can be controlled through adjusting applied pressure, die and pouring temperatures, which then results in the high density, fine and uniform microstructure to improve the mechanical properties.
引文
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