镁铝及镁稀土合金中析出相的电子显微学研究
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摘要
在轻质高强镁合金中,镁铝系合金特别是Mg-9.0wt.%A1-1.0wt.%Zn镁合金,以其在可铸性、机械强度和延展性各方面的优势赢得愈来愈广阔的应用前景,材料研究工作者愈来愈重视对它的研究,特别是研究影响其强度和韧性的微观机理。本论文采用X射线衍射(XRD),扫描电子显微术(SEM)和透射电子显微术(TEM),研究了几种镁合金在固溶处理后时效过程中沉淀相的析出规律、晶体学特征及其时效强化机理。
采用加热样品台,在透射电子显微镜内,对693K固溶后的铸态Mg-9.0wt.%Al-1.0wt.%Zn-4.0wt.%Sn合金的时效过程(403K温度下时效一个小时),进行了实时原位观察。实验中未观察到G.P.或过渡相的出现,此外实验结果表明Mg-9.0wt.%A1-1.0wt.%Zn-4.0wt.%Sn合金中的连续析出沉淀相(γ-Mg17Al12)的颗粒数密度值(Nv=4.92×1010/mm3)大于同样热处理条件下的Mg-9.0wt.%Al-1.0wt.%Zn(AZ91)镁铝合金的连续析出颗粒数密度(N,=2.7×X109/mm3).同时对比了Mg-9.0wt.%A1-1.0wt.%Zn-4.0wt.%Sn样品与AZ91合金样品在传统时效方式(马弗炉内)523K时效48小时的沉淀相(γ-Mg17Al12)连续析出颗粒数密度值,同样证实了这一结果。由此,添加少量的Sn元素促进了镁铝合金中沉淀相(γ-Mg17Al12)连续析出,因而将提高合金的时效硬化效果。
固溶处理(693K时效24小时)后采用传统时效方式(马弗炉内)在温度523K时效48小时的Mg-9.0wt.%Al-1.0wt.%Zn-4.0wt.%Sn合金中观测到连续析出γ-Mg17Al12颗粒与α-Mg基体间的一种新晶体学取向关系(0001)α//(321)γ,[1210]α//[133]γ。此外,还在该样品中观察到{1012}_α。类型的孪晶,并在该孪晶区域内观测到连续析出γ-Mg17Al12相与a-Mg基体间的另一种新晶体学取向关系：(0001)α//(T21)γ,[1210]α//[111]γ。孪晶区域中的这种晶体学取向关系的γ-Mg)7Al12颗粒的长轴取向沿着[0001]_α方向,在一定程度上阻碍基体α-Mg在(0001)。晶面上的滑移,因而对提高合金的强度有贡献。
对快速凝固技术制备的Mg-9.0wt.%A1-1.0wt.%Zn-4.0wt.%Sn合金样品进行研究,确定其微观组织主要由a-Mg基体相、γ-Mg17Al12相和β-Mg2Sn相组成,该方法制备的合金与传统方法浇铸的合金相比,晶粒尺寸大大减小：由几微米降至几百纳米,由霍尔佩奇关系式σ_s=σ_0+kd~(-1/2),因镁合金的k值较大,所以晶粒细化后镁合金的强韧性可大幅度提高。首次确定出晶界处的γ-Mg17Al12相以及弥散分布在晶内的γ-Mg17Al12相均与α-Mg基体之间呈Burgers取向关系。弥散分布在晶内的球形β-Mg2Sn相与α-Mg基体间的取向关系为(0001)_α//(110)_β,[1210]_α//[112]_β,这一取向关系与目前报道的铸态的Mg-Sn系合金样品中的取向关系都不相同。
在773K温度下固溶16小时后的Mg-9.05wt.%Gd-2.85wt.%Zn合金中,实验观察到存在14H类型的长周期结构。本文提出了Mg-9.05wt.%Gd-2.85wt.%Zn合金中14H类型的长周期结构模型,采用运动学理论模拟计算了电子衍射花样,与实验对比符合较好。采用实时原位透射电子显微术对固溶处理后(773K固溶16小时)的Mg-9.05wt.%Gd-2.85wt.%Zn样品的时效过程进行实时的原位观察(时效温度为523K),观察到早期的析出序列为：过饱和固溶体→G.P.区或γ″相→γ′相。在固溶处理(773K固溶16小时)后离位时效(马弗炉内623K时效0.5小时)的样品中,采用透射电子显微术(TEM)观察到少量的14H和18R类型的长周期结构交替存在区域。
Among lightweight and high-strength magnesium-based alloys, magnesium-aluminum alloys, especially the Mg-9.0wt.%Al-1.0wt.%Zn (AZ91) alloy, have been showing increasingly broad application aspects due to their various advantages in castability, mechanical strength and ductility. Now, much attention in the material researches has been paid to the alloys, and especially investigations of the microstructures and mechanism for improving their strength and toughness have been carried out. In this thesis, the precipitation process, the precipitates'crystallography and the age-hardening mechanism for several typical magnesium-based alloys have been investigated using X-ray diffraction (XRD) technology, scanning electron microscopy (SEM) and transmission electron microscopy (TEM).
The aging process of the solution-treated Mg-9.0wt.%Al-1.0wt.%Zn-4.0wt.%Sn alloy was carried out and observed in-situ on a transmission electron microscope (TEM) with a heating-stage for the specimen (403K for1hour). Either the G.P. zone or the transition phase was not observed during the aging process. Besides, the results show that the number of the continuous precipitates per unit volume (Nv=4.92×1010/mm3) for the above specimen is larger than that in AZ91(Nv=2.7×109/mm3) under the same condition. Meanwhile, the number of the continuous precipitated γ-Mg17Al12particles per unit volume in the Mg-9.0wt.%Al-1.0wt.%Zn-4.0wt.%Sn and AZ91alloy aged at523K for48hours under traditional aging condition (heated in a muffle furnace) had been measured and compared, and the similar conclusion was achieved. Therefore, a small amount addition of Sn to Mg-9.0wt.%Al-1.0wt.%Zn (AZ91) alloy will accelerate the continuous precipitation of the γ-Mg17Al12phase, and will devote to improving the age-hardening effect for the Mg-9.0wt.%Al-1.0wt.%Zn-4.0wt.%Sn alloy.
A new crystallographic orientation relationship (OR) between continuous precipitated γ-Mg17Al12particles and a-Mg matrix has been determined as (0001)α//(321)γ,[1210]α//[133]γ in the as-cast Mg-9.0wt.%Al-1.0wt.%Zn-4.0wt.%Sn alloy which was solution-treated at693K for24hours and then aged at523K for48hours in a traditional aging condition (heated in a muffle furnace). Besides, another new crystallographic OR between the y-Mg17Al12and the a-Mg matrix has been observed as (0001)α//(121)γ,[1210]α//[111]γ in a{1012}α type twin region in the same above alloy. The long axis of the continuous precipitated γ-Mg17Al12particles with this latter OR in this {1012}α type twin area is along the [0001]α direction, which will be as obstacles to the dislocation movements on the basal (0001)α plane of the a-Mg matrix. Consequently, this will contribute to the improvement of the mechanical strength of the alloy.
The microstructure investigation of rapidly solidified ribbons of Mg-9.0wt%Al-1.0wt%Zn-4.0wt%Sn alloy shows that the microstructure is constituted by α-Mg, γ-Mg17Al12and β-Mg2Sn phases. Compared to as-cast condition, the grain size with several hundred microns was significantly reduced to several hundred nanometers in rapidly solidified condition. According to the Hall-Petch relationship σs=σ0+kd-1/2and with a large value of k to the magnesium based alloys, the toughness of the magnesium based alloy will be improved greatly when the grain size is decreased as above. It is the first time to identify that, the OR between α-Mg phase and the y-Mg17Al12phase which exists at the grain boundaries is the Burgers OR, and the OR between α-Mg phase and a γ-Mg17Al12particle which exists in a grain is also the Burgers OR. In addition, the OR between α-Mg phase and a spherical particle of β-Mg2Sn phase distributed diffusely in α-Mg grains is in form of (0001)α//(110)β,[1210]α//[112]β, which is different from all the ORs reported in the as-cast Mg-Sn alloys.
In the solution-treated as-cast Mg-9.05wt.%Gd-2.85wt.%Zn alloy (at773K for16hours), the14H LPSO structure have been observed. By the proposed atomic structure model for the14H LPSO structure and kinetic theory, the electron diffraction patterns have been calculated, and the simulated have shown good agreement with the experimental results. The aging process of the solution-treated as-cast Mg-9.05wt.%Gd-2.85wt.%Zn alloy (at773K for16hours) was in-situ observed in a TEM with a heating-stage maintained at the temperature523K for the specimen. The experimental results show that the precipitation sequence at the early aging stage is that: supersaturated solid solution (SSS)→G.P. zone or γ" phase→γ' phase. In an as-cast Mg-9.05wt.%Gd-2.85wt.%Zn alloy, which have been solution treated at773K for16hours and then aged at623K for0.5hour in the muffle furnace, the14H and18R type long period stacking ordered (LPSO) structures have been observed by TEM methods.
采用加热样品台,在透射电子显微镜内,对693K固溶后的铸态Mg-9.0wt.%Al-1.0wt.%Zn-4.0wt.%Sn合金的时效过程(403K温度下时效一个小时),进行了实时原位观察。实验中未观察到G.P.或过渡相的出现,此外实验结果表明Mg-9.0wt.%A1-1.0wt.%Zn-4.0wt.%Sn合金中的连续析出沉淀相(γ-Mg17Al12)的颗粒数密度值(Nv=4.92×1010/mm3)大于同样热处理条件下的Mg-9.0wt.%Al-1.0wt.%Zn(AZ91)镁铝合金的连续析出颗粒数密度(N,=2.7×X109/mm3).同时对比了Mg-9.0wt.%A1-1.0wt.%Zn-4.0wt.%Sn样品与AZ91合金样品在传统时效方式(马弗炉内)523K时效48小时的沉淀相(γ-Mg17Al12)连续析出颗粒数密度值,同样证实了这一结果。由此,添加少量的Sn元素促进了镁铝合金中沉淀相(γ-Mg17Al12)连续析出,因而将提高合金的时效硬化效果。
固溶处理(693K时效24小时)后采用传统时效方式(马弗炉内)在温度523K时效48小时的Mg-9.0wt.%Al-1.0wt.%Zn-4.0wt.%Sn合金中观测到连续析出γ-Mg17Al12颗粒与α-Mg基体间的一种新晶体学取向关系(0001)α//(321)γ,[1210]α//[133]γ。此外,还在该样品中观察到{1012}_α。类型的孪晶,并在该孪晶区域内观测到连续析出γ-Mg17Al12相与a-Mg基体间的另一种新晶体学取向关系：(0001)α//(T21)γ,[1210]α//[111]γ。孪晶区域中的这种晶体学取向关系的γ-Mg)7Al12颗粒的长轴取向沿着[0001]_α方向,在一定程度上阻碍基体α-Mg在(0001)。晶面上的滑移,因而对提高合金的强度有贡献。
对快速凝固技术制备的Mg-9.0wt.%A1-1.0wt.%Zn-4.0wt.%Sn合金样品进行研究,确定其微观组织主要由a-Mg基体相、γ-Mg17Al12相和β-Mg2Sn相组成,该方法制备的合金与传统方法浇铸的合金相比,晶粒尺寸大大减小：由几微米降至几百纳米,由霍尔佩奇关系式σ_s=σ_0+kd~(-1/2),因镁合金的k值较大,所以晶粒细化后镁合金的强韧性可大幅度提高。首次确定出晶界处的γ-Mg17Al12相以及弥散分布在晶内的γ-Mg17Al12相均与α-Mg基体之间呈Burgers取向关系。弥散分布在晶内的球形β-Mg2Sn相与α-Mg基体间的取向关系为(0001)_α//(110)_β,[1210]_α//[112]_β,这一取向关系与目前报道的铸态的Mg-Sn系合金样品中的取向关系都不相同。
在773K温度下固溶16小时后的Mg-9.05wt.%Gd-2.85wt.%Zn合金中,实验观察到存在14H类型的长周期结构。本文提出了Mg-9.05wt.%Gd-2.85wt.%Zn合金中14H类型的长周期结构模型,采用运动学理论模拟计算了电子衍射花样,与实验对比符合较好。采用实时原位透射电子显微术对固溶处理后(773K固溶16小时)的Mg-9.05wt.%Gd-2.85wt.%Zn样品的时效过程进行实时的原位观察(时效温度为523K),观察到早期的析出序列为：过饱和固溶体→G.P.区或γ″相→γ′相。在固溶处理(773K固溶16小时)后离位时效(马弗炉内623K时效0.5小时)的样品中,采用透射电子显微术(TEM)观察到少量的14H和18R类型的长周期结构交替存在区域。
Among lightweight and high-strength magnesium-based alloys, magnesium-aluminum alloys, especially the Mg-9.0wt.%Al-1.0wt.%Zn (AZ91) alloy, have been showing increasingly broad application aspects due to their various advantages in castability, mechanical strength and ductility. Now, much attention in the material researches has been paid to the alloys, and especially investigations of the microstructures and mechanism for improving their strength and toughness have been carried out. In this thesis, the precipitation process, the precipitates'crystallography and the age-hardening mechanism for several typical magnesium-based alloys have been investigated using X-ray diffraction (XRD) technology, scanning electron microscopy (SEM) and transmission electron microscopy (TEM).
The aging process of the solution-treated Mg-9.0wt.%Al-1.0wt.%Zn-4.0wt.%Sn alloy was carried out and observed in-situ on a transmission electron microscope (TEM) with a heating-stage for the specimen (403K for1hour). Either the G.P. zone or the transition phase was not observed during the aging process. Besides, the results show that the number of the continuous precipitates per unit volume (Nv=4.92×1010/mm3) for the above specimen is larger than that in AZ91(Nv=2.7×109/mm3) under the same condition. Meanwhile, the number of the continuous precipitated γ-Mg17Al12particles per unit volume in the Mg-9.0wt.%Al-1.0wt.%Zn-4.0wt.%Sn and AZ91alloy aged at523K for48hours under traditional aging condition (heated in a muffle furnace) had been measured and compared, and the similar conclusion was achieved. Therefore, a small amount addition of Sn to Mg-9.0wt.%Al-1.0wt.%Zn (AZ91) alloy will accelerate the continuous precipitation of the γ-Mg17Al12phase, and will devote to improving the age-hardening effect for the Mg-9.0wt.%Al-1.0wt.%Zn-4.0wt.%Sn alloy.
A new crystallographic orientation relationship (OR) between continuous precipitated γ-Mg17Al12particles and a-Mg matrix has been determined as (0001)α//(321)γ,[1210]α//[133]γ in the as-cast Mg-9.0wt.%Al-1.0wt.%Zn-4.0wt.%Sn alloy which was solution-treated at693K for24hours and then aged at523K for48hours in a traditional aging condition (heated in a muffle furnace). Besides, another new crystallographic OR between the y-Mg17Al12and the a-Mg matrix has been observed as (0001)α//(121)γ,[1210]α//[111]γ in a{1012}α type twin region in the same above alloy. The long axis of the continuous precipitated γ-Mg17Al12particles with this latter OR in this {1012}α type twin area is along the [0001]α direction, which will be as obstacles to the dislocation movements on the basal (0001)α plane of the a-Mg matrix. Consequently, this will contribute to the improvement of the mechanical strength of the alloy.
The microstructure investigation of rapidly solidified ribbons of Mg-9.0wt%Al-1.0wt%Zn-4.0wt%Sn alloy shows that the microstructure is constituted by α-Mg, γ-Mg17Al12and β-Mg2Sn phases. Compared to as-cast condition, the grain size with several hundred microns was significantly reduced to several hundred nanometers in rapidly solidified condition. According to the Hall-Petch relationship σs=σ0+kd-1/2and with a large value of k to the magnesium based alloys, the toughness of the magnesium based alloy will be improved greatly when the grain size is decreased as above. It is the first time to identify that, the OR between α-Mg phase and the y-Mg17Al12phase which exists at the grain boundaries is the Burgers OR, and the OR between α-Mg phase and a γ-Mg17Al12particle which exists in a grain is also the Burgers OR. In addition, the OR between α-Mg phase and a spherical particle of β-Mg2Sn phase distributed diffusely in α-Mg grains is in form of (0001)α//(110)β,[1210]α//[112]β, which is different from all the ORs reported in the as-cast Mg-Sn alloys.
In the solution-treated as-cast Mg-9.05wt.%Gd-2.85wt.%Zn alloy (at773K for16hours), the14H LPSO structure have been observed. By the proposed atomic structure model for the14H LPSO structure and kinetic theory, the electron diffraction patterns have been calculated, and the simulated have shown good agreement with the experimental results. The aging process of the solution-treated as-cast Mg-9.05wt.%Gd-2.85wt.%Zn alloy (at773K for16hours) was in-situ observed in a TEM with a heating-stage maintained at the temperature523K for the specimen. The experimental results show that the precipitation sequence at the early aging stage is that: supersaturated solid solution (SSS)→G.P. zone or γ" phase→γ' phase. In an as-cast Mg-9.05wt.%Gd-2.85wt.%Zn alloy, which have been solution treated at773K for16hours and then aged at623K for0.5hour in the muffle furnace, the14H and18R type long period stacking ordered (LPSO) structures have been observed by TEM methods.
引文
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