镁铝合金中连续析出沉淀相的电子显微学研究
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摘要
镁合金具有比强度比刚度高、导热导电性能好、阻尼减震、电磁屏蔽、易于加工成形和容易回收等优点。在汽车、电子、航空、航天、国防等领域具有重要的应用价值和广阔的应用前景。
在镁合金系列中,运用最广泛的是Al作为主要合金元素的镁合金。AZ91是目前开发最为成功、工业应用中最多的Mg-Al系合金之一。本文以AZ91作为主要实验材料,同时由于Mg-Sn合金具有良好的力学性能,在高温下有稳定的显微结构,以及良好的铸造性能,而且成本要相对低廉,我们设计了成分为Mg-9wt%Al-1wt%Zn-0.2wt%Mn-4wt%Sn新一类镁合金。主要通过透射电子显微镜并结合其他表征手段,系统地研究了这两类时效合金的连续析出相,包括组织相态和晶体学特征,试图找出提高它们的时效强化效果的有效途径,也为开发和应用镁合金提供一定的理论依据。
首先对固溶过后AZ91合金样品和MgAl-Zn-Sn铸锭样品在透射电镜里面进行了实时的原位时效观察,实验结果表明,两类合金样品的析出相均是随着时效时间而逐渐长大,形状趋于规则,轮廓也逐渐明显,大多数析出相是沿着基体(0001)α的板条状析出相。在这两类样品中都没有发现G.P.区。
接下来,对电镜外200℃时效8小时的AZ91合金样品,进行了透射电子显微观察,分析了合金中连续析出相γ-Mg17Al12与基体之间的的各种位向关系(OR)。首先根据拍摄的不同方向TEM照片,统计了AZ91析出相的三维尺度分布,长度(1St_D)、宽度(2nd-D)和厚度(3rd-D)的尺寸分布分别集中在750±300 nm,45±35nm和200±100 nm的范围内。接着,结合前人的工作,确定绝大多数析出相是板条状的第一类析出相,该类析出相与基体保持Burgers OR,惯习面是(0001)α；通过高分辨电子显微学方法,还确定了与Burgers关系非常接近的Potter OR;在数量上来说,不是优先析出形态,但是具有最优的位向关系与对称性形态的CrawleyOR,还有另外一种Porter OR也在实验中也得以证实,同时存在少量的Pitsch-Schrader OR;在我们实验中还发现了一种从未报道过的析出相位向关系,[0001]α//[131]γ,(1210)α//(303)γ。结合运动学理论,对以上提到的几种位向关系进行了SAED模拟,和实验符合得很好。我们还模拟了以上几种(包括Gjonnes-OstmoeOR)析出相位向关系两相重叠的极射赤面投影图。然后结合O点阵与不变线理论,由Pitsch-Schrader OR解释了Crawley OR。
快速凝固属于非平衡凝固,具有细化晶粒及减小第二相尺寸、扩大合金元素在基体的固溶度极限、减小偏析、出现亚稳相、获得更为均匀的组织等一系列优点、为合金提供了不同于常规凝固方式的组织结构的多种可能性。为此,我们分别制备了Mg-Al-Zn-Sn合金快速凝固的条带样品和常规凝固方式的铸态样品。通过综合热分析(DTA和DSC),先确定了这类合金的固溶温度为400℃；根据金相显微镜对铸态样品显微组织的观察结果,Sn元素的加入有细化晶粒的效果；利用X射线衍射仪和扫描电子显微镜及附带的能谱仪(EDS)对样品综合分析得到样品的主要成分除了α-Mg,γ-Mg17Al12,还有Mg2Sn, Sn元素主要分布在晶界处；对铸态样品分别进行了低温(130℃)时效和高温(250℃)时效,在低温时效样品中只确定了γ-Mg17Al12相,没有找到Mg2Sn相；在高温时效样品中找到了两类不同位向关系的Mg2Sn析出相,一类为(0001)α//(110)Mg2Sn,[1120]α//[111]Mg2Sn,还有一类为(0001)α//(110)Mg2Sn,[1120]α//[001]Mg2Sn；对于0.2mm厚条带样品中,通过TEM方法与附带的EDS分析得到样品表面分布着大量球状的析出相,这是在平衡凝固的铸态样品中所没有出现的。同时析出相组成成分为Mg、Al与Sn三种元素。在0.3mm厚的条带样品中观察到了Mg2Sn相,拍摄了其高分辨像并进行了标定与模拟。
Magnesium alloys have great potential for application in structure parts in automobiles, computers, airplanes, spaceflight and national defence due to their excellent propoties such as low density, high specific strength, superior damping characteristics, good electromagnetic shielding performance, etc.
The most commonly used magnesium alloys are those based on the Mg-Al system. Principally, AZ91 is the most widely used commercial magnesium alloy. The study will concentrate on this kind of alloy. Concerning the Mg-Sn alloys have lots of advantages, such as good shielding performance and mechanical strength, stable microstructure in elevated temperature, and low price, we developed a new kind of magnesium alloy-Mg-9wt%Al-lwt%Zn-0.2wt%Mn-4wt%Sn. Transmission electron microscopy (TEM), optical microscopy(OM), X-ray diffraction(XRD), scanning electron microscopy with energy dispersive spectrometer(SEM/EDS) were employed to characterize the crystallography of continuous precipitations of these two kind of magnesium alloys, including microstructure, phase constitution, dimension, and orientation relationships. This study would help to provide a scientific basis for the development and applications of magnesium alloys.
Firstly, die-cast AZ91 and Mg-Al-Zn-Sn were solution treated.Then An in-situ observation of the precipitating process of continuous precipitations in these two kinds of magnesium alloys, were carried out with a transmission electron microscope equipped with a heating stage maintained. The results showed that the size of the continuous precipitates in both alloys grew with the aging time, the figure turned regular and the shape became vivider than before. Most of continuous precipitations were lath-shaped lying along the (0001)αof the magnesium matrix phase. No G.P.zones were observed during the process of aging.
Secondly, AZ91 specimen which aged at 200℃for 8h was observed in the transmission electron microscope. We surveyed the 3-D size as overall information by utilizing various samples along various directions. The statistical results showed that the 1st-D(along[1010]αor length),2nd-D(along [0001]αor width) and 3rd-D([1210]α or thickness) sizes are concentrated on 750±300 nm,45±35 nm and 200±100 nm, respectively. By using the selected-area electron diffraction (SAED)method with the tilting technique, the reported orientation relationships and morphologies of the continuous precipitates have been reconfirmed as follows. The predominant fraction of continuous precipitates is thin lath, with the primary habit plane parallel to the basal plane of the matrix (0001)α, and possesses the Burgers OR. We had also observed the Pitsch-Schrader OR among these thin lath-shaped precipitates. Another type, comprising only a small fraction, has the primary growth direction perpendicular to the basal plane (0001)a and has the Crawley OR. The Porter OR precipitates have the primary growth direction lying at an angle of about 16°to the normal of the (0001)a which is even less common. We had observed continuous precipitate particles with the Potter OR in an AZ91 alloy using HRTEM. However, precipitate particles with the Gjonnes-Ostmoe OR were not found in our experiment. In this study, a new orientation relationship of continuous precipitates was observed in the AZ91 alloy. By using the SAED method with the tilting technique, it was confirmed that the new orientation relationship is in the form of [0001]α//[131]γ, (1120)α//(303)γ. We had also calculated six stereographic projections for the reported orientation relationships. And the Crawley OR can be obtained from Pitsch-Schrader OR by the interpretation of O-Lattice theory and Invariant-Line theory.
Rapid solidification is non-equilibrium solidification, which can effectively fine grains and secondary phases, increase the solid solubility of alloy elements in matrix, improve phase constitution and form new metastable phases and so on. Based on these adavantages, we made die-case Mg-Al-Zn-Sn specimen by conventional solidification and thin ribbon specimen by rapid solification. By using DTA and DSC, we confirmed the solution temperature (400℃) of the Mg-Al-Zn-Sn alloy and by using OM, and we found that the grains were fined because of addition of Sn. The constitution of the alloy includedα-Mg,γ-Mg17Al12 and Mg2Sn based on the results of XRD and EDS. Die-cast Mg-Al-Zn-Sn alloy specimen was aged at two different temperature,130℃and 250℃. No Mg2Sn phase was found in the low temperature aging specimen, but we confirmed two different orientation relationships of Mg2Sn phase at the high temperature aging specimen. Transmission electron microscopy on the ribbon specimen with 0.2nm thickness revealed lots of ball-shaped continuous precipitations on the Mg-matrix which were not observed in the conventional solidification die-cast specimen. Beside, we investigated that the ball-shaped continuous precipitates are three-element compound with Mg, Al and Sn by EDS method. Both y-Mg17Al12 phase and Mg2Sn phase were observed in the 0.3 mm thickness ribbon specimen, which were confirmed by HRTEM and simulation.
在镁合金系列中,运用最广泛的是Al作为主要合金元素的镁合金。AZ91是目前开发最为成功、工业应用中最多的Mg-Al系合金之一。本文以AZ91作为主要实验材料,同时由于Mg-Sn合金具有良好的力学性能,在高温下有稳定的显微结构,以及良好的铸造性能,而且成本要相对低廉,我们设计了成分为Mg-9wt%Al-1wt%Zn-0.2wt%Mn-4wt%Sn新一类镁合金。主要通过透射电子显微镜并结合其他表征手段,系统地研究了这两类时效合金的连续析出相,包括组织相态和晶体学特征,试图找出提高它们的时效强化效果的有效途径,也为开发和应用镁合金提供一定的理论依据。
首先对固溶过后AZ91合金样品和MgAl-Zn-Sn铸锭样品在透射电镜里面进行了实时的原位时效观察,实验结果表明,两类合金样品的析出相均是随着时效时间而逐渐长大,形状趋于规则,轮廓也逐渐明显,大多数析出相是沿着基体(0001)α的板条状析出相。在这两类样品中都没有发现G.P.区。
接下来,对电镜外200℃时效8小时的AZ91合金样品,进行了透射电子显微观察,分析了合金中连续析出相γ-Mg17Al12与基体之间的的各种位向关系(OR)。首先根据拍摄的不同方向TEM照片,统计了AZ91析出相的三维尺度分布,长度(1St_D)、宽度(2nd-D)和厚度(3rd-D)的尺寸分布分别集中在750±300 nm,45±35nm和200±100 nm的范围内。接着,结合前人的工作,确定绝大多数析出相是板条状的第一类析出相,该类析出相与基体保持Burgers OR,惯习面是(0001)α；通过高分辨电子显微学方法,还确定了与Burgers关系非常接近的Potter OR;在数量上来说,不是优先析出形态,但是具有最优的位向关系与对称性形态的CrawleyOR,还有另外一种Porter OR也在实验中也得以证实,同时存在少量的Pitsch-Schrader OR;在我们实验中还发现了一种从未报道过的析出相位向关系,[0001]α//[131]γ,(1210)α//(303)γ。结合运动学理论,对以上提到的几种位向关系进行了SAED模拟,和实验符合得很好。我们还模拟了以上几种(包括Gjonnes-OstmoeOR)析出相位向关系两相重叠的极射赤面投影图。然后结合O点阵与不变线理论,由Pitsch-Schrader OR解释了Crawley OR。
快速凝固属于非平衡凝固,具有细化晶粒及减小第二相尺寸、扩大合金元素在基体的固溶度极限、减小偏析、出现亚稳相、获得更为均匀的组织等一系列优点、为合金提供了不同于常规凝固方式的组织结构的多种可能性。为此,我们分别制备了Mg-Al-Zn-Sn合金快速凝固的条带样品和常规凝固方式的铸态样品。通过综合热分析(DTA和DSC),先确定了这类合金的固溶温度为400℃；根据金相显微镜对铸态样品显微组织的观察结果,Sn元素的加入有细化晶粒的效果；利用X射线衍射仪和扫描电子显微镜及附带的能谱仪(EDS)对样品综合分析得到样品的主要成分除了α-Mg,γ-Mg17Al12,还有Mg2Sn, Sn元素主要分布在晶界处；对铸态样品分别进行了低温(130℃)时效和高温(250℃)时效,在低温时效样品中只确定了γ-Mg17Al12相,没有找到Mg2Sn相；在高温时效样品中找到了两类不同位向关系的Mg2Sn析出相,一类为(0001)α//(110)Mg2Sn,[1120]α//[111]Mg2Sn,还有一类为(0001)α//(110)Mg2Sn,[1120]α//[001]Mg2Sn；对于0.2mm厚条带样品中,通过TEM方法与附带的EDS分析得到样品表面分布着大量球状的析出相,这是在平衡凝固的铸态样品中所没有出现的。同时析出相组成成分为Mg、Al与Sn三种元素。在0.3mm厚的条带样品中观察到了Mg2Sn相,拍摄了其高分辨像并进行了标定与模拟。
Magnesium alloys have great potential for application in structure parts in automobiles, computers, airplanes, spaceflight and national defence due to their excellent propoties such as low density, high specific strength, superior damping characteristics, good electromagnetic shielding performance, etc.
The most commonly used magnesium alloys are those based on the Mg-Al system. Principally, AZ91 is the most widely used commercial magnesium alloy. The study will concentrate on this kind of alloy. Concerning the Mg-Sn alloys have lots of advantages, such as good shielding performance and mechanical strength, stable microstructure in elevated temperature, and low price, we developed a new kind of magnesium alloy-Mg-9wt%Al-lwt%Zn-0.2wt%Mn-4wt%Sn. Transmission electron microscopy (TEM), optical microscopy(OM), X-ray diffraction(XRD), scanning electron microscopy with energy dispersive spectrometer(SEM/EDS) were employed to characterize the crystallography of continuous precipitations of these two kind of magnesium alloys, including microstructure, phase constitution, dimension, and orientation relationships. This study would help to provide a scientific basis for the development and applications of magnesium alloys.
Firstly, die-cast AZ91 and Mg-Al-Zn-Sn were solution treated.Then An in-situ observation of the precipitating process of continuous precipitations in these two kinds of magnesium alloys, were carried out with a transmission electron microscope equipped with a heating stage maintained. The results showed that the size of the continuous precipitates in both alloys grew with the aging time, the figure turned regular and the shape became vivider than before. Most of continuous precipitations were lath-shaped lying along the (0001)αof the magnesium matrix phase. No G.P.zones were observed during the process of aging.
Secondly, AZ91 specimen which aged at 200℃for 8h was observed in the transmission electron microscope. We surveyed the 3-D size as overall information by utilizing various samples along various directions. The statistical results showed that the 1st-D(along[1010]αor length),2nd-D(along [0001]αor width) and 3rd-D([1210]α or thickness) sizes are concentrated on 750±300 nm,45±35 nm and 200±100 nm, respectively. By using the selected-area electron diffraction (SAED)method with the tilting technique, the reported orientation relationships and morphologies of the continuous precipitates have been reconfirmed as follows. The predominant fraction of continuous precipitates is thin lath, with the primary habit plane parallel to the basal plane of the matrix (0001)α, and possesses the Burgers OR. We had also observed the Pitsch-Schrader OR among these thin lath-shaped precipitates. Another type, comprising only a small fraction, has the primary growth direction perpendicular to the basal plane (0001)a and has the Crawley OR. The Porter OR precipitates have the primary growth direction lying at an angle of about 16°to the normal of the (0001)a which is even less common. We had observed continuous precipitate particles with the Potter OR in an AZ91 alloy using HRTEM. However, precipitate particles with the Gjonnes-Ostmoe OR were not found in our experiment. In this study, a new orientation relationship of continuous precipitates was observed in the AZ91 alloy. By using the SAED method with the tilting technique, it was confirmed that the new orientation relationship is in the form of [0001]α//[131]γ, (1120)α//(303)γ. We had also calculated six stereographic projections for the reported orientation relationships. And the Crawley OR can be obtained from Pitsch-Schrader OR by the interpretation of O-Lattice theory and Invariant-Line theory.
Rapid solidification is non-equilibrium solidification, which can effectively fine grains and secondary phases, increase the solid solubility of alloy elements in matrix, improve phase constitution and form new metastable phases and so on. Based on these adavantages, we made die-case Mg-Al-Zn-Sn specimen by conventional solidification and thin ribbon specimen by rapid solification. By using DTA and DSC, we confirmed the solution temperature (400℃) of the Mg-Al-Zn-Sn alloy and by using OM, and we found that the grains were fined because of addition of Sn. The constitution of the alloy includedα-Mg,γ-Mg17Al12 and Mg2Sn based on the results of XRD and EDS. Die-cast Mg-Al-Zn-Sn alloy specimen was aged at two different temperature,130℃and 250℃. No Mg2Sn phase was found in the low temperature aging specimen, but we confirmed two different orientation relationships of Mg2Sn phase at the high temperature aging specimen. Transmission electron microscopy on the ribbon specimen with 0.2nm thickness revealed lots of ball-shaped continuous precipitations on the Mg-matrix which were not observed in the conventional solidification die-cast specimen. Beside, we investigated that the ball-shaped continuous precipitates are three-element compound with Mg, Al and Sn by EDS method. Both y-Mg17Al12 phase and Mg2Sn phase were observed in the 0.3 mm thickness ribbon specimen, which were confirmed by HRTEM and simulation.
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