部分高强耐热稀土镁合金体系的相关系及其凝固组织分析
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摘要
摘要：镁合金是目前实际应用中最轻的金属结构材料,具有比重轻、比强度和比刚度高、良好的电磁屏蔽能力、阻尼减震性好、易切削加工性和可再生利用性等优异性能,在汽车、航空航天及电子产品等领域具有重要的应用价值和广阔的应用前景,被誉为“21世纪绿色工程材料”。然而,镁合金室温强度不高、高温强度低、抗蠕变性能差等缺点,严重阻碍了镁合金的应用。稀土加入镁合金中能够提高其力学性能、抗蠕变性能及耐腐蚀性能等,Mg-Zn合金中添加稀土元素会显著改善合金的力学性能和耐热性。本文结合国家自然科学基金项目(No.50731002)：新型镁合金结构材料相图与合金化研究,通过实验测定和相图计算(CALPHAD)方法,对Mg-Ce-Gd-La-Nd-Pr-Sm-Zn多元系中部分二元、三元系的相关系进行了研究,根据所建立的热力学数据库模拟了典型Mg-Zn-RE合金凝固过程中的组织演变,为镁合金的设计提供理论依据,主要研究工作如下：
(1)采用合金法,通过X-射线衍射分析(XRD)、扫描电子显微镜(SEM)和电子探针显微分析(EPMA)等检测分析手段,测定了Mg-Zn-Gd三元系673K富镁角的等温截面。实验证实了存在三元相X相(14H长程有序结构)、W相(面心立方结构)和I相(二十面体准晶结构),检测到三个两相区：(Mg)+X、(Mg)+W、(Mg)+I;四个三相区：(Mg)+X+Mg5Gd、(Mg)+X+W、(Mg)+W+I、L+(Mg)+I。其中Mg5Gd相、W和I相都有一定溶解度范围。
结合实验结果和文献信息,运用CALPHAD方法优化计算了Gd-Zn二元系和Mg-Zn-Gd三元系,其中液相采用替换溶液模型,有序相BCC_B2与无序相BCC_A2采用了同一个吉布斯自由能表达式,以处理BCC_B2与BCC A2之间的有序无序转变关系。计算结果与实验数据吻合。
(2)采用同(1)实验方法测定了Mg-Gd-Nd三元系673K富镁角的等温截面。实验检测到三元相p,检测到两个三相区：(Mg)+Mg41Nd5+β Mg5Gd+Mg41Nd5+β;两个两相区：(Mg)+Mg5Gd、(Mg)+Mg41Nd5。二元化合物Mg5Gd、Mg41Nd5有较大的溶解度范围。
结合实验结果和文献信息,运用CALPHAD方法优化计算了Gd-Nd二元系和Gd-Mg-Nd三元系。计算结果与实验信息吻合。
(3)结合实验信息,选择合理的热力学模型,采用CALPHAD方法优化计算了Mg-Zn-La、Mg-Zn-Ce、Mg-Zn-Nd、Mg-Zn-Pr和Mg-Zn-Sm三元系,其中所有有序相BCC_B2与无序相BCC_A2都采用了同一个吉布斯自由能表达式来处理BCC_B2和BCC_A2之间的有序无序转变。每一个三元合金体系都得到一套自洽的热力学参数。
(4)建立了Mg-Ce-Gd-La-Nd-Pr-Sm-Zn多元系的热力学数据库,可应用于稀土镁合金的成分和热处理工艺设计。
(5)采用扫描电子显微镜和X-射线衍射分析等检测分析手段,观察了几个典型的Mg-Zn-RE (RE=Ce、Nd、Gd和Sm),Mg-Gd-Nd合金的铸态组织。采用所建立的热力学数据库,模拟了这些合金的平衡凝固和Scheil凝固过程,并与实验观察到的相关合金铸态微观组织进行了对比分析,合理地解释了实验合金在凝固过程中的组织演化过程。
ABSTRACT:As the lightest metal structure material, magnesium alloys have been widely applied in automotive, aerospace and electronic industries because of a number of desirable features, such as light weight, high specific strength and stiffness, excellent electro-magnetic shielding, good damping characteristic, good machinability, etc. Magnesium alloys have great application prospect, known as the "21st Century Green Engineering Materials". However, the limited mechanical strength of magnesium alloys, especially at elevated temperature, has retarded their application. It has been demonstrated that rare earth metals (RE) are the most effective elements to improve the strength of magnesium especially at high temperatures. The RE addition in Mg-Zn based alloys would enhance the high-temperature strength and creep resistance. The precision thermodynamic description of the multi-component magnesium system is crucially necessary for the design and optimization of alloy compositions and manufacturing processes. Associated with the project "Study on the phase diagrams and alloying of Mg-based alloy systems" financed by National Science Foundation of China (No.50731002), experimental investigation and thermodynamic calculation (CALPHAD) were carried out on partial phase equilibria of Mg-Ce-Gd-La-Nd-Pr-Sm-Zn system. Based on the database, the equilibrium solidification and the solidification according to the Scheil model were calculated for some typical Mg-Zn-RE alloys. The major work of this study is as follows:
(1) The phase relations of the Mg-Zn-Gd ternary system in the Mg-rich corner at673K were determined by means of alloying method, X-ray diffraction analysis (XRD), scanning electron microscopy (SEM) and electron-probe microanalysis (EPMA). Three ternary phases, X-(Mg]2ZnGd,14H long period stacking ordered structure), W-(Mg3Zn3Gd2, fcc) and I-(Mg3Zn6Gd1, icosahedral quasicrystal structure), were identified. The experimental results showed that there are three two-phase regions,(Mg)+X,(Mg)+W,(Mg)+I, and four three-phase regions,(Mg)+X+Mg5Gd,(Mg)+X+W,(Mg)+W+I, L+(Mg)+I. Mg5Gd, W and I have extended homogeneities along Gd to Zn.
Based on the experimental results and literature information, the Gd-Zn binary system and Mg-Zn-Gd ternary system were optimized by means of CALculation of PHAse Diagram (CALPHAD) method. In particular, the order/disorder transition between BCC_B2and BCC_A2in the system has been taken into account and their Gibbs energies were expressed with a single expression. Reasonable agreement between the calculated and experimental data was achieved.
(2) The phase relations of the Mg-Gd-Nd system in the Mg-rich corner at673K were determined using the same method as above. Ternary phase (3was identified. The experimental results showed that there are two three-phase regions,(Mg)+Mg5Gd+Mg41Nd5, Mg5Gd+Mg41Nd5+β, and three two-phase regions,(Mg)+Mg5Gd, Mg41Nd5+Mg5Gd,(Mg)+Mg41Nd5. Mg5Gd and Mg41Nd5have largely extended homogeneities along Gd to Nd.
Based on the experimental results and literature information, the Gd-Nd binary system and Mg-Gd-Nd ternary system were optimized by means of CALculation of PHAse Diagram (CALPHAD) method. The calculated phase diagrams were in good agreement with available experimental data.
(3) Based on available experimental data and literature information, the ternary systems, Mg-Zn-La, Mg-Zn-Ce, Mg-Zn-Nd, Mg-Zn-Pr and Mg-Zn-Sm ternary systems have been optimized using CALPHAD method. In order to treat the order/disorder transition between BCC B2and BCC_A2, the Gibbs energy of the ordered BCC_B2phase in all these systems was deseribed with a2-sublattice model and the same to the one of the disordered BCC_A2phase. A set of self-consistent thermodynamic parameters of individual ternary system was obtained.
(4) The thermodynamic database of Mg-Ce-Gd-La-Nd-Pr-Sm-Zn has been established, using to design the composition and heat treatment process of magnesium alloys.
(5) Using scanning electron microscopy (SEM) and X-ray diffraction analysis (XRD), the cast samples of some typical Mg-Zn-RE(RE=Ce, Nd, Gd and Sm), Mg-Gd-Nd alloys were observed. Based on the thermodynamic database, the equilibrium solidification and the solidification according to the Scheil model were calculated for these alloys to understand the experimental microstructures during solidification.
(1)采用合金法,通过X-射线衍射分析(XRD)、扫描电子显微镜(SEM)和电子探针显微分析(EPMA)等检测分析手段,测定了Mg-Zn-Gd三元系673K富镁角的等温截面。实验证实了存在三元相X相(14H长程有序结构)、W相(面心立方结构)和I相(二十面体准晶结构),检测到三个两相区：(Mg)+X、(Mg)+W、(Mg)+I;四个三相区：(Mg)+X+Mg5Gd、(Mg)+X+W、(Mg)+W+I、L+(Mg)+I。其中Mg5Gd相、W和I相都有一定溶解度范围。
结合实验结果和文献信息,运用CALPHAD方法优化计算了Gd-Zn二元系和Mg-Zn-Gd三元系,其中液相采用替换溶液模型,有序相BCC_B2与无序相BCC_A2采用了同一个吉布斯自由能表达式,以处理BCC_B2与BCC A2之间的有序无序转变关系。计算结果与实验数据吻合。
(2)采用同(1)实验方法测定了Mg-Gd-Nd三元系673K富镁角的等温截面。实验检测到三元相p,检测到两个三相区：(Mg)+Mg41Nd5+β Mg5Gd+Mg41Nd5+β;两个两相区：(Mg)+Mg5Gd、(Mg)+Mg41Nd5。二元化合物Mg5Gd、Mg41Nd5有较大的溶解度范围。
结合实验结果和文献信息,运用CALPHAD方法优化计算了Gd-Nd二元系和Gd-Mg-Nd三元系。计算结果与实验信息吻合。
(3)结合实验信息,选择合理的热力学模型,采用CALPHAD方法优化计算了Mg-Zn-La、Mg-Zn-Ce、Mg-Zn-Nd、Mg-Zn-Pr和Mg-Zn-Sm三元系,其中所有有序相BCC_B2与无序相BCC_A2都采用了同一个吉布斯自由能表达式来处理BCC_B2和BCC_A2之间的有序无序转变。每一个三元合金体系都得到一套自洽的热力学参数。
(4)建立了Mg-Ce-Gd-La-Nd-Pr-Sm-Zn多元系的热力学数据库,可应用于稀土镁合金的成分和热处理工艺设计。
(5)采用扫描电子显微镜和X-射线衍射分析等检测分析手段,观察了几个典型的Mg-Zn-RE (RE=Ce、Nd、Gd和Sm),Mg-Gd-Nd合金的铸态组织。采用所建立的热力学数据库,模拟了这些合金的平衡凝固和Scheil凝固过程,并与实验观察到的相关合金铸态微观组织进行了对比分析,合理地解释了实验合金在凝固过程中的组织演化过程。
ABSTRACT:As the lightest metal structure material, magnesium alloys have been widely applied in automotive, aerospace and electronic industries because of a number of desirable features, such as light weight, high specific strength and stiffness, excellent electro-magnetic shielding, good damping characteristic, good machinability, etc. Magnesium alloys have great application prospect, known as the "21st Century Green Engineering Materials". However, the limited mechanical strength of magnesium alloys, especially at elevated temperature, has retarded their application. It has been demonstrated that rare earth metals (RE) are the most effective elements to improve the strength of magnesium especially at high temperatures. The RE addition in Mg-Zn based alloys would enhance the high-temperature strength and creep resistance. The precision thermodynamic description of the multi-component magnesium system is crucially necessary for the design and optimization of alloy compositions and manufacturing processes. Associated with the project "Study on the phase diagrams and alloying of Mg-based alloy systems" financed by National Science Foundation of China (No.50731002), experimental investigation and thermodynamic calculation (CALPHAD) were carried out on partial phase equilibria of Mg-Ce-Gd-La-Nd-Pr-Sm-Zn system. Based on the database, the equilibrium solidification and the solidification according to the Scheil model were calculated for some typical Mg-Zn-RE alloys. The major work of this study is as follows:
(1) The phase relations of the Mg-Zn-Gd ternary system in the Mg-rich corner at673K were determined by means of alloying method, X-ray diffraction analysis (XRD), scanning electron microscopy (SEM) and electron-probe microanalysis (EPMA). Three ternary phases, X-(Mg]2ZnGd,14H long period stacking ordered structure), W-(Mg3Zn3Gd2, fcc) and I-(Mg3Zn6Gd1, icosahedral quasicrystal structure), were identified. The experimental results showed that there are three two-phase regions,(Mg)+X,(Mg)+W,(Mg)+I, and four three-phase regions,(Mg)+X+Mg5Gd,(Mg)+X+W,(Mg)+W+I, L+(Mg)+I. Mg5Gd, W and I have extended homogeneities along Gd to Zn.
Based on the experimental results and literature information, the Gd-Zn binary system and Mg-Zn-Gd ternary system were optimized by means of CALculation of PHAse Diagram (CALPHAD) method. In particular, the order/disorder transition between BCC_B2and BCC_A2in the system has been taken into account and their Gibbs energies were expressed with a single expression. Reasonable agreement between the calculated and experimental data was achieved.
(2) The phase relations of the Mg-Gd-Nd system in the Mg-rich corner at673K were determined using the same method as above. Ternary phase (3was identified. The experimental results showed that there are two three-phase regions,(Mg)+Mg5Gd+Mg41Nd5, Mg5Gd+Mg41Nd5+β, and three two-phase regions,(Mg)+Mg5Gd, Mg41Nd5+Mg5Gd,(Mg)+Mg41Nd5. Mg5Gd and Mg41Nd5have largely extended homogeneities along Gd to Nd.
Based on the experimental results and literature information, the Gd-Nd binary system and Mg-Gd-Nd ternary system were optimized by means of CALculation of PHAse Diagram (CALPHAD) method. The calculated phase diagrams were in good agreement with available experimental data.
(3) Based on available experimental data and literature information, the ternary systems, Mg-Zn-La, Mg-Zn-Ce, Mg-Zn-Nd, Mg-Zn-Pr and Mg-Zn-Sm ternary systems have been optimized using CALPHAD method. In order to treat the order/disorder transition between BCC B2and BCC_A2, the Gibbs energy of the ordered BCC_B2phase in all these systems was deseribed with a2-sublattice model and the same to the one of the disordered BCC_A2phase. A set of self-consistent thermodynamic parameters of individual ternary system was obtained.
(4) The thermodynamic database of Mg-Ce-Gd-La-Nd-Pr-Sm-Zn has been established, using to design the composition and heat treatment process of magnesium alloys.
(5) Using scanning electron microscopy (SEM) and X-ray diffraction analysis (XRD), the cast samples of some typical Mg-Zn-RE(RE=Ce, Nd, Gd and Sm), Mg-Gd-Nd alloys were observed. Based on the thermodynamic database, the equilibrium solidification and the solidification according to the Scheil model were calculated for these alloys to understand the experimental microstructures during solidification.
引文
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