EW75合金的组织结构及在制备加工中的演化
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摘要
稀土元素Gd、Y在镁合金中具有显著的时效强化效应,在此基础上通过成分优化设计研发的EW75合金(Mg-7Gd-5Y-1Nd-0.5Zr)室温高温力学性能优良,发展应用前景广阔。虽然目前关于Mg-Gd-Y系合金组织和性能的研究较多,但是亚稳时效析出相的晶体学特征还存在争议。此外,均匀化热处理之后进行预析出热处理,在合金中形成第二相颗粒,研究其对合金高温变形行为特别是动态再结晶的影响较少。本论文以此为立题依据,系统研究EW75合金不同热处理和加工状态下相的形貌、结构及强化机制,并通过合理的预析出热处理工艺控制第二相颗粒的形成,研究第二相对合金热压缩和多向锻造变形过程的影响作用,为研制高性能稀土镁合金提供实验基础和理论依据。
确定铸态EW75合金组织由基体、骨骼状相(fc.c., a=2.22nm)、方块状H(f.c.c., a=0.53nm)和Zr颗粒组成。其中骨骼状相化学成分为Mg5(Y0.4Gd0.4Nd0.2),方块状相化学成分为Mg(Y3Gd)。经过均匀化处理后,骨骼状相基本消失,合金的组织主要由基体和方块状相Mg(Y3Gd)组成,Mg(Y3Gd)相的结构、成分与铸态合金中的相同。
对均匀化EW75合金在520℃／480℃／440℃／400℃温度进行30min的等温预析出热处理,形成尺寸大于1μm的第二相颗粒。520℃、480℃等温预析出热处理的相为方块状的Mg(Y3Gd)相,而在440℃、400℃预析出热处理时出现杆状Mg5(Y0.4Gd0.4Nd0.2)相。将经过预析出热处理的合金(预析出处理合金)和均匀化合金分别进行后续的高温热压缩和多向锻造变形。
研究了EW75合金的时效沉淀相及其强化机制。EW75合金在210℃等温时效过程中的主要沉淀相为β’相,以及沿(0001)。析出的沉淀相和β相。β’相的结构为底心正交(b.c.o.)结构,晶格常数a=0.64nm,b=2.22nm,c=0.52nm。β’相与Mg基体完全共格,以(1120)α为惯习面,与基体的取向关系为：[001]β,／／[0001]α,(100)β／／(1120)αβ’相在空间的形貌为椭球状。通过高角度环形暗场扫描透射电子显微技术(HAADF-STEM)观察结果,确定β’相的原子结构模型为Mg7RE型。β’相与基体的共格关系及其不同变体间相互交错成网状是其在210℃时效具有较高的热稳定性的主要原因。沿(0001)。析出的沉淀相以(0001)。为惯习面,与基体完全共格,为板状形貌,沿[0001]。方向的尺寸为2nm,沿[1120]。和[1010]。方向的尺寸为5nm,在之前文献中未见报道。过时效阶段的沉淀相为β相,其品格常数a=2.22nm,与基体的取向关系为：(111)β//(1120)α,[11]β//[0001]α,化学成分为Mg5(Y0.4Gd0.4Nd0.2)。一个β相通常由具有(111)β孪晶关系的几个部分组成。考虑β相的板状形貌及其[0001]α方向的长度,建立了β相的强化机制模型,在本合金中当β相沿[1120]α方向长度应当控制在2μm以内。
研究了均匀化EW75合金在热压缩变形过程中的组织演变。晶界是主要的动态再结晶形核位置,并且再结晶晶粒与原始变形晶粒的取向存在一定关系。变形量较小时,晶界发生迁移形成锯齿状,具有非连续动态再结晶特征。变形量较大时,小角度晶界通过连续吸收位错形成大角度晶界,属于连续动态再结晶的特征。合金在热压缩过程中晶粒发生了明显的转动使基面法向趋于与压缩方向一致,具有典型的基面纤维织构特征。
研究了预析出处理EW75合金中第二相对合金热压缩变形行为及组织演变的影响。建立了动态再结晶动力学模型,预析出处理合金的动态再结晶激活能低于均匀化合金,完成再结晶所需变形量较小。预析出处理合金在变形过程中,第二相附近产生具有一定取向差梯度的变形区,因此除晶界以外,第二相颗粒也是动态再结晶形核的有利位置,并且第二相附近的动态再结晶晶粒取向随机。预析出处理合金中的第二相可以起到促进动态再结晶的作用。
研究了均匀化EW75合金在多向锻造变形过程中的显微组织、变形织构及变形析出相。动态再结晶是合金主要的晶粒细化方式,原始晶界是动态再结晶的主要形核位置。EW75合金在第一道次锻压之后形成了较强的(0001)基面纤维织构,由于外加应力轴的不断变化和动态再结晶体积分数的增加,在后续变形道次基面织构不断弱化。多向锻造过程中的变形析出相为Mg5(Gd0.4Y0.4Nd0.2),结构为f.c.c.,晶格常数a=2.22nm,变形析出相多分布于动态再结晶晶界,起到了阻碍动态再结晶晶粒长大的作用。
研究了预析出处理EW75合金中第二相对多向锻造变形过程中的显微组织及变形织构的影响。预析出处理合金的动态再结晶形核位置为原始晶界和第二相颗粒。由于第二相颗粒对位错的阻碍作用,更容易在再结晶晶粒内发生多重再结晶。第二相附近的动态再结晶晶粒取向随机,对弱化合金织构有一定作用。对预析出处理合金进行六道次多向锻造变形,最终得到了平均晶粒尺寸为5.15μm,织构较弱,垂直于压缩方向抗拉强度、屈服强度和延伸率分别为347MPa、305.5MPa和3.5%的合金。
Magnesium alloys with the addition of rare earth metals(RE) Gd, Y have significant precipitation hardening effect. EW75(Mg-7Gd-5Y-1Nd-0.5Zr) alloy have great potential to be used widely due to their high specific strength at both room and elevated temperatures. Although there has been a lot of research work about the microstructure and mechanical properties of Mg-Gd-Y series alloys, there is still a debate about the characterization of metastable phase formed during ageing. Besides, the understand about the particle effects on the flow stress behavior and microstructure evolution during hot deformation is limited. Thus, in this study, the morphology, structure, and strengthening mechanism of phases formed in EW75alloy will be systemically researched. Also, the effect of particles on the deformation behavior and microstructure evolution during hot compression and multi-axial forging will be investigated. The aim of the present work is to provide experimental and theoretical results for the development and application of high performance Mg-RE alloys.
As-cast microstructure of EW75alloy consists of α-Mg matrix, skeletal phase(f.c.c., a=2.22nm), block-shaped phase(f.c.c., a=0.53nm) and Zr particles. A composition of Mg5(Y0.4Gd0.4Nd0.2) is suggested for the skeletal phase, and a composition of Mg(YdGd) is for the block-shaped phase. After homogenized heat treatment, the skeletal phase in the as-cast alloy have been completely dissolved, the microstructure of as-homogenized alloy consists of α-Mg matrix and block-shaped Mg(Y3Gd) phase. The structure and composition of Mg(Y3Gd) phase is identical with that in the as-cast alloy.
After homogenized heat treatment, the pre-treated heat treatment(water quenching at room temperature and ageing at520℃/480℃/440℃/400℃for30min) for alloys were carried out. After isothermal pre-treated heat treatment, the particles with size larger than1μm are observed in the alloy. The block-shaped Mg(Y3Gd) phase formed in the520℃and480℃isothermal pre-treated alloys. However, the bacilliform Mg5(Y0.4Gd0.4Nd0.2) phase formed in the440℃and400℃pre-treated alloys.
The precipitates in EW75alloy during ageing have been investigated. The precipitates of EW75alloy aged at210℃are β' phase, a new type of phase precipitated on the (0001)α habit plane and β phase. A b.c.o. structure with lattice parameters of a=0.64nm, b=2.22nm and c=0.52nm can be identified for β''phase. The β' precipitates are totally coherent with the matrix. The orientation relationship between the β' precipitates and the matrix satisfies [001]β'//[0001]α and (100)β'//(1120)α. Atomic-scaled HAADF-STKM observations along the [0001]α and [1120]α, zone axes suggest an Mg7RK-type structural model for the β' phase. Coherent relationship and joining of β' precipitates are responsible for the good thermal stability of alloy ageing at210℃. A new type of phase precipitated on the (0001α habit plane was observed in the21()℃718h and210℃/180h ageing samples. A completely coherent relationship between the precipitates and the matrix can be found. The new precipitates are plate-shaped with approximately2nm wide along the [0001|α direction of the matrix and5nm long along the [1120]α and [1010]α directions. None of the phases precipitated on the (0001)α plane was reported in Mg-Gd or Mg-Y series alloys during ageing heat treatment. The β phase formed in the over-aged EW75alloy. The β precipitate has a f.c.c. structure with a lattice parameter of a＝2.22nm, a composition of Mg5(Y0.4Gd0.4Nd0.2) is suggested for the β phase. Furthermore, the β precipitate forms as plates with a habit plane parallel to (1100)α The orientation relationship between the β phase and a-Mg matrix is(112)β(l100)α|110]β//[0001α. A single β plate often contains several domains of (lll)β twin-related variants. Assuming the plate shape and the length along [0001]α direction of β phase, an appropriate versions of the Orowan equation for β phase have been developed.
Microstructure evolution during hot compression of as-homogenized EW75alloy has been investigated. New dynamic recrystallization grains formed near origin grain boundaries. The orientation of new grains is related to the original grains. At low strains, the original grain boundaries are serrated and bulging at grain boundary regions can be recognized, which indicate that discontinuous dynamic recrystallization is operative. At higher strains, new grains result from the gradual increase in mis-orientation between subgrains during plastic deformation. Continuous absorption of dislocations in the low-angle boundaries results in continuous dynamic recrystallization. During hot compression, there is a tendency to exhibit a basal fiber texture in which the majority of grains are oriented to such that their [0001]α direction are nearly parallel to the compression direction.
The effect of particles on flow stress behavior and microstructure evolution has been investigated. According to the DRX kinetics model, Qrex for the pre-treated alloys is smaller compared with the as-homogenized alloys. The deformation time required for the same amount of DRX volume fraction is shorter for the pre-treated alloys. In pre-treated alloys, the misorientation gradient surrounding particles is large enough that DRX grains formed both near the origin grain boundaries and large particles. The orientation of DRX grains formed around the particles is quite random. The DRX promoting effect of particles in pre-treated alloys during hot compression can be deduced.
Microstructure, texture evolution and dynamic precipitation during multi-axial forging(MAF) of as-homogenized EW75alloy have been investigated. DRX is the dominant grain refinement mechanism in the as-homogenized alloy during MAF process. DRX grains are primely formed near origin grain boundaries. A pronounced basal texture can be observed in the EW75alloy after the first pass of MAF. However, the basal texture have been weakened during the subsequent passes, due to the various loading directions and increasing of DRX volume fractions. The dynamic precipitates formed during MAF processing has an f.c.c. structure with a lattice parameter of a=2.22nm. Most of the dynamic precipitates locate on the dynamic recrystallization grain boundaries.
The effect of particles on microstructure and texture evolution during MAF process has been investigated. In the pre-treated alloys, DRX grains can be formed both near origin grain boundaries and large particles. The orientation of DRX grains formed around the particles is quite random, which is beneficial to the texture weaken. After6passes of MAF, simultaneously average grain size of5.15μm and weak texture have been achieved in the pre-treated EW75alloy. The ultimate tensile strength, yield strength and elongation are347MPa,305.5MPa and3.5%, respectively.
确定铸态EW75合金组织由基体、骨骼状相(fc.c., a=2.22nm)、方块状H(f.c.c., a=0.53nm)和Zr颗粒组成。其中骨骼状相化学成分为Mg5(Y0.4Gd0.4Nd0.2),方块状相化学成分为Mg(Y3Gd)。经过均匀化处理后,骨骼状相基本消失,合金的组织主要由基体和方块状相Mg(Y3Gd)组成,Mg(Y3Gd)相的结构、成分与铸态合金中的相同。
对均匀化EW75合金在520℃／480℃／440℃／400℃温度进行30min的等温预析出热处理,形成尺寸大于1μm的第二相颗粒。520℃、480℃等温预析出热处理的相为方块状的Mg(Y3Gd)相,而在440℃、400℃预析出热处理时出现杆状Mg5(Y0.4Gd0.4Nd0.2)相。将经过预析出热处理的合金(预析出处理合金)和均匀化合金分别进行后续的高温热压缩和多向锻造变形。
研究了EW75合金的时效沉淀相及其强化机制。EW75合金在210℃等温时效过程中的主要沉淀相为β’相,以及沿(0001)。析出的沉淀相和β相。β’相的结构为底心正交(b.c.o.)结构,晶格常数a=0.64nm,b=2.22nm,c=0.52nm。β’相与Mg基体完全共格,以(1120)α为惯习面,与基体的取向关系为：[001]β,／／[0001]α,(100)β／／(1120)αβ’相在空间的形貌为椭球状。通过高角度环形暗场扫描透射电子显微技术(HAADF-STEM)观察结果,确定β’相的原子结构模型为Mg7RE型。β’相与基体的共格关系及其不同变体间相互交错成网状是其在210℃时效具有较高的热稳定性的主要原因。沿(0001)。析出的沉淀相以(0001)。为惯习面,与基体完全共格,为板状形貌,沿[0001]。方向的尺寸为2nm,沿[1120]。和[1010]。方向的尺寸为5nm,在之前文献中未见报道。过时效阶段的沉淀相为β相,其品格常数a=2.22nm,与基体的取向关系为：(111)β//(1120)α,[11]β//[0001]α,化学成分为Mg5(Y0.4Gd0.4Nd0.2)。一个β相通常由具有(111)β孪晶关系的几个部分组成。考虑β相的板状形貌及其[0001]α方向的长度,建立了β相的强化机制模型,在本合金中当β相沿[1120]α方向长度应当控制在2μm以内。
研究了均匀化EW75合金在热压缩变形过程中的组织演变。晶界是主要的动态再结晶形核位置,并且再结晶晶粒与原始变形晶粒的取向存在一定关系。变形量较小时,晶界发生迁移形成锯齿状,具有非连续动态再结晶特征。变形量较大时,小角度晶界通过连续吸收位错形成大角度晶界,属于连续动态再结晶的特征。合金在热压缩过程中晶粒发生了明显的转动使基面法向趋于与压缩方向一致,具有典型的基面纤维织构特征。
研究了预析出处理EW75合金中第二相对合金热压缩变形行为及组织演变的影响。建立了动态再结晶动力学模型,预析出处理合金的动态再结晶激活能低于均匀化合金,完成再结晶所需变形量较小。预析出处理合金在变形过程中,第二相附近产生具有一定取向差梯度的变形区,因此除晶界以外,第二相颗粒也是动态再结晶形核的有利位置,并且第二相附近的动态再结晶晶粒取向随机。预析出处理合金中的第二相可以起到促进动态再结晶的作用。
研究了均匀化EW75合金在多向锻造变形过程中的显微组织、变形织构及变形析出相。动态再结晶是合金主要的晶粒细化方式,原始晶界是动态再结晶的主要形核位置。EW75合金在第一道次锻压之后形成了较强的(0001)基面纤维织构,由于外加应力轴的不断变化和动态再结晶体积分数的增加,在后续变形道次基面织构不断弱化。多向锻造过程中的变形析出相为Mg5(Gd0.4Y0.4Nd0.2),结构为f.c.c.,晶格常数a=2.22nm,变形析出相多分布于动态再结晶晶界,起到了阻碍动态再结晶晶粒长大的作用。
研究了预析出处理EW75合金中第二相对多向锻造变形过程中的显微组织及变形织构的影响。预析出处理合金的动态再结晶形核位置为原始晶界和第二相颗粒。由于第二相颗粒对位错的阻碍作用,更容易在再结晶晶粒内发生多重再结晶。第二相附近的动态再结晶晶粒取向随机,对弱化合金织构有一定作用。对预析出处理合金进行六道次多向锻造变形,最终得到了平均晶粒尺寸为5.15μm,织构较弱,垂直于压缩方向抗拉强度、屈服强度和延伸率分别为347MPa、305.5MPa和3.5%的合金。
Magnesium alloys with the addition of rare earth metals(RE) Gd, Y have significant precipitation hardening effect. EW75(Mg-7Gd-5Y-1Nd-0.5Zr) alloy have great potential to be used widely due to their high specific strength at both room and elevated temperatures. Although there has been a lot of research work about the microstructure and mechanical properties of Mg-Gd-Y series alloys, there is still a debate about the characterization of metastable phase formed during ageing. Besides, the understand about the particle effects on the flow stress behavior and microstructure evolution during hot deformation is limited. Thus, in this study, the morphology, structure, and strengthening mechanism of phases formed in EW75alloy will be systemically researched. Also, the effect of particles on the deformation behavior and microstructure evolution during hot compression and multi-axial forging will be investigated. The aim of the present work is to provide experimental and theoretical results for the development and application of high performance Mg-RE alloys.
As-cast microstructure of EW75alloy consists of α-Mg matrix, skeletal phase(f.c.c., a=2.22nm), block-shaped phase(f.c.c., a=0.53nm) and Zr particles. A composition of Mg5(Y0.4Gd0.4Nd0.2) is suggested for the skeletal phase, and a composition of Mg(YdGd) is for the block-shaped phase. After homogenized heat treatment, the skeletal phase in the as-cast alloy have been completely dissolved, the microstructure of as-homogenized alloy consists of α-Mg matrix and block-shaped Mg(Y3Gd) phase. The structure and composition of Mg(Y3Gd) phase is identical with that in the as-cast alloy.
After homogenized heat treatment, the pre-treated heat treatment(water quenching at room temperature and ageing at520℃/480℃/440℃/400℃for30min) for alloys were carried out. After isothermal pre-treated heat treatment, the particles with size larger than1μm are observed in the alloy. The block-shaped Mg(Y3Gd) phase formed in the520℃and480℃isothermal pre-treated alloys. However, the bacilliform Mg5(Y0.4Gd0.4Nd0.2) phase formed in the440℃and400℃pre-treated alloys.
The precipitates in EW75alloy during ageing have been investigated. The precipitates of EW75alloy aged at210℃are β' phase, a new type of phase precipitated on the (0001)α habit plane and β phase. A b.c.o. structure with lattice parameters of a=0.64nm, b=2.22nm and c=0.52nm can be identified for β''phase. The β' precipitates are totally coherent with the matrix. The orientation relationship between the β' precipitates and the matrix satisfies [001]β'//[0001]α and (100)β'//(1120)α. Atomic-scaled HAADF-STKM observations along the [0001]α and [1120]α, zone axes suggest an Mg7RK-type structural model for the β' phase. Coherent relationship and joining of β' precipitates are responsible for the good thermal stability of alloy ageing at210℃. A new type of phase precipitated on the (0001α habit plane was observed in the21()℃718h and210℃/180h ageing samples. A completely coherent relationship between the precipitates and the matrix can be found. The new precipitates are plate-shaped with approximately2nm wide along the [0001|α direction of the matrix and5nm long along the [1120]α and [1010]α directions. None of the phases precipitated on the (0001)α plane was reported in Mg-Gd or Mg-Y series alloys during ageing heat treatment. The β phase formed in the over-aged EW75alloy. The β precipitate has a f.c.c. structure with a lattice parameter of a＝2.22nm, a composition of Mg5(Y0.4Gd0.4Nd0.2) is suggested for the β phase. Furthermore, the β precipitate forms as plates with a habit plane parallel to (1100)α The orientation relationship between the β phase and a-Mg matrix is(112)β(l100)α|110]β//[0001α. A single β plate often contains several domains of (lll)β twin-related variants. Assuming the plate shape and the length along [0001]α direction of β phase, an appropriate versions of the Orowan equation for β phase have been developed.
Microstructure evolution during hot compression of as-homogenized EW75alloy has been investigated. New dynamic recrystallization grains formed near origin grain boundaries. The orientation of new grains is related to the original grains. At low strains, the original grain boundaries are serrated and bulging at grain boundary regions can be recognized, which indicate that discontinuous dynamic recrystallization is operative. At higher strains, new grains result from the gradual increase in mis-orientation between subgrains during plastic deformation. Continuous absorption of dislocations in the low-angle boundaries results in continuous dynamic recrystallization. During hot compression, there is a tendency to exhibit a basal fiber texture in which the majority of grains are oriented to such that their [0001]α direction are nearly parallel to the compression direction.
The effect of particles on flow stress behavior and microstructure evolution has been investigated. According to the DRX kinetics model, Qrex for the pre-treated alloys is smaller compared with the as-homogenized alloys. The deformation time required for the same amount of DRX volume fraction is shorter for the pre-treated alloys. In pre-treated alloys, the misorientation gradient surrounding particles is large enough that DRX grains formed both near the origin grain boundaries and large particles. The orientation of DRX grains formed around the particles is quite random. The DRX promoting effect of particles in pre-treated alloys during hot compression can be deduced.
Microstructure, texture evolution and dynamic precipitation during multi-axial forging(MAF) of as-homogenized EW75alloy have been investigated. DRX is the dominant grain refinement mechanism in the as-homogenized alloy during MAF process. DRX grains are primely formed near origin grain boundaries. A pronounced basal texture can be observed in the EW75alloy after the first pass of MAF. However, the basal texture have been weakened during the subsequent passes, due to the various loading directions and increasing of DRX volume fractions. The dynamic precipitates formed during MAF processing has an f.c.c. structure with a lattice parameter of a=2.22nm. Most of the dynamic precipitates locate on the dynamic recrystallization grain boundaries.
The effect of particles on microstructure and texture evolution during MAF process has been investigated. In the pre-treated alloys, DRX grains can be formed both near origin grain boundaries and large particles. The orientation of DRX grains formed around the particles is quite random, which is beneficial to the texture weaken. After6passes of MAF, simultaneously average grain size of5.15μm and weak texture have been achieved in the pre-treated EW75alloy. The ultimate tensile strength, yield strength and elongation are347MPa,305.5MPa and3.5%, respectively.
引文
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