Mg-Zn-Mn系变形镁合金强化机理研究
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摘要
本文研究了Zn、Mn含量对Mg-Zn-Mn系变形镁合金室温力学性能和显微组织的影响、单级和双级时效过程中时效析出相的演变和α-Mn析出相的晶体学特征;采用原位电阻法和硬度法研究了Mg-6wt.%Zn-1wt.%Mn (ZM61)合金在不同温度进行单、双级时效时的相变动力学,得到了Johnson-Mehl-Avrami(JMA)动力学方程和“温度-时间-转变量”(TTT)图;还构建了析出强化模型并对ZM61合金单级时效早期的力学性能演变进行了模拟。
研究Zn含量的影响时发现:①挤压态合金的力学性能对Zn含量的变化不敏感,随Zn含量的增加,屈服强度σ0.2和抗拉强度σb的变动幅度均不大,延伸率δ保持在13%左右。T6(单级和双级)处理后,Zn含量从4%增到6%时,σ0.2和σb均大幅增加且δ没有显著降低,当Zn含量从6%增到9%时,σ0.2和σb的增幅不大但δ会显著降低。双级时效的强化效果优于单级时效但δ更低。挤压态ZM61经过“固溶+双级时效”(420℃/2h+90℃/24h+180℃/16h)处理后具有最佳的综合力学性能,即:σ0.2=340MPa,σb=366MPa,δ=5%。②Mg-Zn-Mn合金在时效过程中析出两种类型的析出相:一种是沿基体[001]Mg方向的杆状相β_1~′,一种是平躺在基体(001)Mg晶面上的盘状相β2′。ZM61在180℃进行单级时效时,硬度在3.5h接近峰值,峰时效之前主要发生杆状相数量密度的增加和杆的伸长,峰时效时杆状相的数量密度达到最大值,过时效阶段主要发生杆状相的粗化和盘状相的增多,严重粗化的杆状相常以α-Mn颗粒为异质核心。③ZM61在180℃进行双级时效时,硬度在1h(86HV)就接近峰值,预时效(90℃/24h)态组织中弥散分布着直径约5nm的Guinier-Preston (G.P.)区,前20min的组织中只能观察到杆状相而看不到盘状相,说明G.P.区只作为杆状相的异质形核核心,过时效阶段盘状相才逐渐增多。④ZM61在230℃进行单、双级时效时,达到峰时效的时间明显缩短(单级:2h,双级:0.5h)。双级时效7h时,合金虽已发生过时效,但组织中绝大部分的析出相仍为短杆状,盘状相的数量极少,说明高温时效和G.P.区形核的共同作用抑制了盘状相的析出。⑤单、双级时效态组织中,位错形核导致大量的析出相沿位错线整齐排列。
研究Mn含量的影响时发现:①均匀化、挤压和固溶处理时会析出α-Mn相,α-Mn相的截面形状包括:球状、平行多边形和棒状。②对一个正六边形α-Mn析出相的晶体学特征进行研究后发现:六边形相的六个刻面均属于｛110｝α-Mn晶面族。当所有界面均为｛110｝α-Mn时,α-Mn相的立体形貌为二十面体;α-Mn相与基体之间存在如下位向关系: (1 00)_(Mg)~// ( 321)_(Mn); [ 041]_(Mg) //[111]_(Mn)。③对一个棒状α-Mn析出相的晶体学特征进行分析后发现:棒状相躺在基面上,其长轴沿着基体晶格的最密排方向<100>α-Mg。④时效态组织中,α-Mn相会作为β_1~′相的异质形核核心,对异质形核的晶体学特征进行研究后发现:β_1~′相与α-Mn相之间存在能够共格匹配的低指数晶面,β_1~′相在α-Mn相上异质形核可以形成共格界面,取代之前α-Mn相与基体之间的非共格界面,从而大幅降低体系的界面能。
对ZM61单、双级时效的等温相变动力学进行研究后发现:①原位电阻法表明:对于单级时效,长大阶段的n约为1,粗化阶段的n约为0.5,说明长大阶段的相变机理为β1'杆状相的伸长,而粗化阶段的相变机理为β_2~'盘状相的粗化。单级时效的TTT图表明:在90~250℃范围内没有出现“鼻子”,说明250℃以下的相变动力学由Zn在Mg中的扩散速度决定。双级时效的相变机制与单级时效一致,双级时效的TTT图表明:在130~250℃范围内也没有出现“鼻子”,相变动力学仍由Zn原子在Mg中的扩散速度控制。②硬度法的研究表明:不同温度下,单级和双级时效的n大部分都接近1,说明峰时效之前的相变机制为β1'杆状相的伸长。单级和双级时效早期的相变激活能都接近80KJ/mol。TTT图表明:“鼻子”仍未出现,双级时效大幅度地加快了相变速率。
采用模型法研究ZM61合金单级时效早期的力学性能演变时发现:①“强化公式2”(假设析出相在滑移面上随机分布时推导出的Orowan强化公式)的预测结果表明:用JMA方程表达fv时,屈服强度曲线上存在极大值,用均匀形核理论表达fv时,屈服强度在时效早期缓慢增加,接近峰时效时增速加快,不存在极大值点。对屈服强度出现极大值的分析表明:屈服强度由杆状相的体积分数和直径共同决定,体积分数增加不一定带来屈服强度的提升,因为杆状相直径的增加会迅速地降低屈服强度。②对比“强化公式1”(假设析出相在滑移面上呈正三角形阵列规则排列时推导出的Orowan强化公式)和“强化公式2”的预测结果发现:“强化公式1”和“强化公式2”所得出的曲线形态是一致的,但“强化公式1”对屈服强度的预测值整体上远远大于“强化公式2”的预测值,这说明:两种强化公式反映相同的屈服强度演变特征,但杆状相以三角形阵列规则排列时带来的强化效果显著地优于随机排列的杆状相带来的强化效果。然而,“强化公式2”得出屈服强度演变与实测结果吻合较好,说明:Mg-Zn-Mn合金经“挤压+固溶+时效”处理后,杆状相以随机排列为主。
Effects of Zn and Mn content on the tensile properties and microstructure of Mg-Zn-Mn wrought magnesium alloys, precipitate evolution during one- and two-step aging and crystallographic characteristics ofα-Mn phases have been systematically ivestigated by means of optical microscopy (OM), scanning electron microscopy (SEM) equipped with energy dispersive spectronmetry (EDS), X-ray diffraction (XRD) and Transmission electron microscopy (TEM). In order to getting a far better understanding of precipitation feature, in-situ resistivity measurement and hardness test were used to quantitatively determine the phase transformation kinetics in Mg-6wt.% Zn-1wt.%Mn(ZM61) alloy during one- and two-step aging , in which Johnson-Mehl-Avrami (JMA) equations and‘Time-Temperature-Transformation’(TTT) curves are deduced. Moreover, yield strength evolution of ZM61 alloy during the early stage of one-step aging was simulated by modelling.
Research on the effect of Zn content shows that:①the tensile properties of as-extruded alloys are not sensitive to Zn content, both yield strengthσ0.2 and tensile strengthσb show slight variation and elongation is maintained at 13% with the increase in Zn content. After T6 treatment,σ0.2 andσb increase largely andδfalls slightly as Zn content rises from 4wt.% to 6wt.%,however, as Zn content rises from 6wt.% to 9wt.%, only a small increase inσ0.2 andσb occurs butδfalls largely. In contrast to one-step aging, two-step aging has better strengthening effect but lowerδ. Consequently, 6 wt. % is the best Zn content for the Mg-xZn-1Mn alloys to possess the optimum combination property.②While ZM61 is treated by one-step aging at 180℃, hardness reaches to peak value at 3.5h, the main phase transformation before peak aging is the increase in number density and length of rod-like particles,the number density rises to maximum at peak aging, the main phase transformation during over-aging is the coarsening of rod-like particles and increase in the number of disc-like particles, it is worth noting that severely coarsened rod-like particles always heterogeneously nucleated onα-Mn particles.③While ZM61 is treated by two-step aging at 180, only 1 hour is needed for hardness to approach peak value, a vast number of G.P. zones with 5nm in diameter are present in as-pre-aged microstructure, no disc-like particle can be seen in microstructure as aging time is less than 20min, indicating that G.P. zones can only act as the heterogeneous nuclei towards rod-like particles, disc-like particles gradually increase during over aging.④As ZM61 is treated by one- and two-step aging at 230℃, time needed to rearch peak aging is shortened obviously (one-step aging: 2h, two-step aging 0.5h). As two-step aging runs for 7h, although the alloy has been under over aging, almost all precipitates are short rods, meanwhile, disc-like particles are rare, indicating that both high temperature and G.P.-zone-nucleation-mechanism retard the precipitation of disc-like particles.⑤In the as-one- and two-step-aged microstructure, dislocation-nucleation-mechanism results in regular alignment of precipitates along dislocations.
Research on the effect of Mn content shows that:①α-Mn particles can be precipitated out during homogenization, hot-extrusion and solutionization; the cross-section morphologies ofα-Mn precipitates include spheric shape, polygon and rod.②It has been found by investigating the crystallographic characteristics of anα-Mn particle with regular hexagon morphology that: the six facets of thisα-Mn particle all belong to｛110｝α-Mn crystal plane family, if all exterior surfaces belong to｛110｝α-Mn, the three-dimensional morphology of thisα-Mn particle will be a icosahedron. The orientation relationship between thisα-Mn particle and matrix is (1 00)_(Mg)~// ( 321)_(Mn); [ 041]_(Mg) //[111]_(Mn).③It has been found by investigating the crystallographic characteristics of a rod-likeα-Mn particle that: the rod lies on the base plane of matrix, the long axis is along the close packed direction of matrix.④In as-aged microstructure, it is common thatα-Mn can act as the heterogeneous nuclei ofβ_1~′rods, it has been found by investigating the crystallographic characteristics of heterogeneous nucleation that: there exist low-index crystal planes betweenβ_1~′andα-Mn that can form coherent interface, consequently, if heterogeneous nucleation occurs, initial incoherent interface betweenα-Mn and matrix will be replaced by coherent interface, which can largely reduce surface energy.
The investigation in isothermal phase transformation kinetics of ZM61 alloy during one- and two-step aging shows that:①by means of in-situ resistivity measurement, the Avrami indexes of nucleation, growth and coarsening stages during one-step aging are about 0.3, 1 and 0.5, respectively, indicating that the phase transformation mechanism during growth stage is the elongation ofβ1' rods and that during coarsening stage is the coarsening ofβ_2~' discs.“Temperature-Time-Transformation”(TTT)curve of one-step aging indicates that:‘Nose’does not appear in the temperature range 90~250℃, the precipitation kinetics under 250℃is controlled by diffusibility of Zn in Mg and nucleation stage is largely shortened while aging temperature is higher than 150℃. The Avrami indexes of growth and coarsen stage of two-step aging are 1 and 0.5, indicating that two-step aging does not change the phase transformation mechanism. TTT curve of two-step aging shows that‘nose’still does not appear in the temperature range 130~250℃and precipitation kinetics is still controlled by the diffusibility of Zn.②By means of hardness test, most Avrami indexes of one- and two-step aging at different temperature are near to 1, indicating that the phase transformation mechanism before peak aging is the elongation ofβ1' rods. The phase transformation activation energy of early stage of one- and two-step aging are all near 80KJ/mol. TTT curve shows that‘nose’is not present; two-step aging largely accelerates the phase transformation rate.
Mechanical properties evolution of ZM61 during the early stage of one-step aging is investigated by modeling, the results show that:①the predicted results of model using‘strengthening equation 2’(Orowan strengthening equation presuming a random distribution of precipitates on gliding planes) indicate that:the increasing velocity of the rod length is much faster than that of rod diameter; the‘fv-t’curve deduced by‘homogeneous nucleation theory’(HNT) rises by exponential form, while‘fv-t’curve deduced by JMA equation rises by‘S’form. As fv is deduced by JMA equation, yield strength curve has a maximal point, as fv is deduced by HNT, yield strength rises much slowly in the early stage of aging but much faster while peak aging is approached and no maximal point appear. Analysis of the formation of maximal point shows that: both volume fraction and diameter ofβ1' rods determine the yield strength, increase in volume fraction ofβ1' rods is not certain to raise yield strength, since increase in rod diameter will reduce yield strength.②By contrasting the predicted results of model using‘strengthening equation 2’and model using‘strengthening equation 1’(Orowan strengthening equation presuming that precipitates are arranged to form regular-triangle arrays), it can be found that: the yield strength values predicted by‘strengthening equation 1’are entirely larger than those predicted by‘strengthening equation 2’, indicating that precipitates arranged as regular-triangle arrays bring about extremely large strengthening effect.
研究Zn含量的影响时发现:①挤压态合金的力学性能对Zn含量的变化不敏感,随Zn含量的增加,屈服强度σ0.2和抗拉强度σb的变动幅度均不大,延伸率δ保持在13%左右。T6(单级和双级)处理后,Zn含量从4%增到6%时,σ0.2和σb均大幅增加且δ没有显著降低,当Zn含量从6%增到9%时,σ0.2和σb的增幅不大但δ会显著降低。双级时效的强化效果优于单级时效但δ更低。挤压态ZM61经过“固溶+双级时效”(420℃/2h+90℃/24h+180℃/16h)处理后具有最佳的综合力学性能,即:σ0.2=340MPa,σb=366MPa,δ=5%。②Mg-Zn-Mn合金在时效过程中析出两种类型的析出相:一种是沿基体[001]Mg方向的杆状相β_1~′,一种是平躺在基体(001)Mg晶面上的盘状相β2′。ZM61在180℃进行单级时效时,硬度在3.5h接近峰值,峰时效之前主要发生杆状相数量密度的增加和杆的伸长,峰时效时杆状相的数量密度达到最大值,过时效阶段主要发生杆状相的粗化和盘状相的增多,严重粗化的杆状相常以α-Mn颗粒为异质核心。③ZM61在180℃进行双级时效时,硬度在1h(86HV)就接近峰值,预时效(90℃/24h)态组织中弥散分布着直径约5nm的Guinier-Preston (G.P.)区,前20min的组织中只能观察到杆状相而看不到盘状相,说明G.P.区只作为杆状相的异质形核核心,过时效阶段盘状相才逐渐增多。④ZM61在230℃进行单、双级时效时,达到峰时效的时间明显缩短(单级:2h,双级:0.5h)。双级时效7h时,合金虽已发生过时效,但组织中绝大部分的析出相仍为短杆状,盘状相的数量极少,说明高温时效和G.P.区形核的共同作用抑制了盘状相的析出。⑤单、双级时效态组织中,位错形核导致大量的析出相沿位错线整齐排列。
研究Mn含量的影响时发现:①均匀化、挤压和固溶处理时会析出α-Mn相,α-Mn相的截面形状包括:球状、平行多边形和棒状。②对一个正六边形α-Mn析出相的晶体学特征进行研究后发现:六边形相的六个刻面均属于｛110｝α-Mn晶面族。当所有界面均为｛110｝α-Mn时,α-Mn相的立体形貌为二十面体;α-Mn相与基体之间存在如下位向关系: (1 00)_(Mg)~// ( 321)_(Mn); [ 041]_(Mg) //[111]_(Mn)。③对一个棒状α-Mn析出相的晶体学特征进行分析后发现:棒状相躺在基面上,其长轴沿着基体晶格的最密排方向<100>α-Mg。④时效态组织中,α-Mn相会作为β_1~′相的异质形核核心,对异质形核的晶体学特征进行研究后发现:β_1~′相与α-Mn相之间存在能够共格匹配的低指数晶面,β_1~′相在α-Mn相上异质形核可以形成共格界面,取代之前α-Mn相与基体之间的非共格界面,从而大幅降低体系的界面能。
对ZM61单、双级时效的等温相变动力学进行研究后发现:①原位电阻法表明:对于单级时效,长大阶段的n约为1,粗化阶段的n约为0.5,说明长大阶段的相变机理为β1'杆状相的伸长,而粗化阶段的相变机理为β_2~'盘状相的粗化。单级时效的TTT图表明:在90~250℃范围内没有出现“鼻子”,说明250℃以下的相变动力学由Zn在Mg中的扩散速度决定。双级时效的相变机制与单级时效一致,双级时效的TTT图表明:在130~250℃范围内也没有出现“鼻子”,相变动力学仍由Zn原子在Mg中的扩散速度控制。②硬度法的研究表明:不同温度下,单级和双级时效的n大部分都接近1,说明峰时效之前的相变机制为β1'杆状相的伸长。单级和双级时效早期的相变激活能都接近80KJ/mol。TTT图表明:“鼻子”仍未出现,双级时效大幅度地加快了相变速率。
采用模型法研究ZM61合金单级时效早期的力学性能演变时发现:①“强化公式2”(假设析出相在滑移面上随机分布时推导出的Orowan强化公式)的预测结果表明:用JMA方程表达fv时,屈服强度曲线上存在极大值,用均匀形核理论表达fv时,屈服强度在时效早期缓慢增加,接近峰时效时增速加快,不存在极大值点。对屈服强度出现极大值的分析表明:屈服强度由杆状相的体积分数和直径共同决定,体积分数增加不一定带来屈服强度的提升,因为杆状相直径的增加会迅速地降低屈服强度。②对比“强化公式1”(假设析出相在滑移面上呈正三角形阵列规则排列时推导出的Orowan强化公式)和“强化公式2”的预测结果发现:“强化公式1”和“强化公式2”所得出的曲线形态是一致的,但“强化公式1”对屈服强度的预测值整体上远远大于“强化公式2”的预测值,这说明:两种强化公式反映相同的屈服强度演变特征,但杆状相以三角形阵列规则排列时带来的强化效果显著地优于随机排列的杆状相带来的强化效果。然而,“强化公式2”得出屈服强度演变与实测结果吻合较好,说明:Mg-Zn-Mn合金经“挤压+固溶+时效”处理后,杆状相以随机排列为主。
Effects of Zn and Mn content on the tensile properties and microstructure of Mg-Zn-Mn wrought magnesium alloys, precipitate evolution during one- and two-step aging and crystallographic characteristics ofα-Mn phases have been systematically ivestigated by means of optical microscopy (OM), scanning electron microscopy (SEM) equipped with energy dispersive spectronmetry (EDS), X-ray diffraction (XRD) and Transmission electron microscopy (TEM). In order to getting a far better understanding of precipitation feature, in-situ resistivity measurement and hardness test were used to quantitatively determine the phase transformation kinetics in Mg-6wt.% Zn-1wt.%Mn(ZM61) alloy during one- and two-step aging , in which Johnson-Mehl-Avrami (JMA) equations and‘Time-Temperature-Transformation’(TTT) curves are deduced. Moreover, yield strength evolution of ZM61 alloy during the early stage of one-step aging was simulated by modelling.
Research on the effect of Zn content shows that:①the tensile properties of as-extruded alloys are not sensitive to Zn content, both yield strengthσ0.2 and tensile strengthσb show slight variation and elongation is maintained at 13% with the increase in Zn content. After T6 treatment,σ0.2 andσb increase largely andδfalls slightly as Zn content rises from 4wt.% to 6wt.%,however, as Zn content rises from 6wt.% to 9wt.%, only a small increase inσ0.2 andσb occurs butδfalls largely. In contrast to one-step aging, two-step aging has better strengthening effect but lowerδ. Consequently, 6 wt. % is the best Zn content for the Mg-xZn-1Mn alloys to possess the optimum combination property.②While ZM61 is treated by one-step aging at 180℃, hardness reaches to peak value at 3.5h, the main phase transformation before peak aging is the increase in number density and length of rod-like particles,the number density rises to maximum at peak aging, the main phase transformation during over-aging is the coarsening of rod-like particles and increase in the number of disc-like particles, it is worth noting that severely coarsened rod-like particles always heterogeneously nucleated onα-Mn particles.③While ZM61 is treated by two-step aging at 180, only 1 hour is needed for hardness to approach peak value, a vast number of G.P. zones with 5nm in diameter are present in as-pre-aged microstructure, no disc-like particle can be seen in microstructure as aging time is less than 20min, indicating that G.P. zones can only act as the heterogeneous nuclei towards rod-like particles, disc-like particles gradually increase during over aging.④As ZM61 is treated by one- and two-step aging at 230℃, time needed to rearch peak aging is shortened obviously (one-step aging: 2h, two-step aging 0.5h). As two-step aging runs for 7h, although the alloy has been under over aging, almost all precipitates are short rods, meanwhile, disc-like particles are rare, indicating that both high temperature and G.P.-zone-nucleation-mechanism retard the precipitation of disc-like particles.⑤In the as-one- and two-step-aged microstructure, dislocation-nucleation-mechanism results in regular alignment of precipitates along dislocations.
Research on the effect of Mn content shows that:①α-Mn particles can be precipitated out during homogenization, hot-extrusion and solutionization; the cross-section morphologies ofα-Mn precipitates include spheric shape, polygon and rod.②It has been found by investigating the crystallographic characteristics of anα-Mn particle with regular hexagon morphology that: the six facets of thisα-Mn particle all belong to｛110｝α-Mn crystal plane family, if all exterior surfaces belong to｛110｝α-Mn, the three-dimensional morphology of thisα-Mn particle will be a icosahedron. The orientation relationship between thisα-Mn particle and matrix is (1 00)_(Mg)~// ( 321)_(Mn); [ 041]_(Mg) //[111]_(Mn).③It has been found by investigating the crystallographic characteristics of a rod-likeα-Mn particle that: the rod lies on the base plane of matrix, the long axis is along the close packed direction of matrix.④In as-aged microstructure, it is common thatα-Mn can act as the heterogeneous nuclei ofβ_1~′rods, it has been found by investigating the crystallographic characteristics of heterogeneous nucleation that: there exist low-index crystal planes betweenβ_1~′andα-Mn that can form coherent interface, consequently, if heterogeneous nucleation occurs, initial incoherent interface betweenα-Mn and matrix will be replaced by coherent interface, which can largely reduce surface energy.
The investigation in isothermal phase transformation kinetics of ZM61 alloy during one- and two-step aging shows that:①by means of in-situ resistivity measurement, the Avrami indexes of nucleation, growth and coarsening stages during one-step aging are about 0.3, 1 and 0.5, respectively, indicating that the phase transformation mechanism during growth stage is the elongation ofβ1' rods and that during coarsening stage is the coarsening ofβ_2~' discs.“Temperature-Time-Transformation”(TTT)curve of one-step aging indicates that:‘Nose’does not appear in the temperature range 90~250℃, the precipitation kinetics under 250℃is controlled by diffusibility of Zn in Mg and nucleation stage is largely shortened while aging temperature is higher than 150℃. The Avrami indexes of growth and coarsen stage of two-step aging are 1 and 0.5, indicating that two-step aging does not change the phase transformation mechanism. TTT curve of two-step aging shows that‘nose’still does not appear in the temperature range 130~250℃and precipitation kinetics is still controlled by the diffusibility of Zn.②By means of hardness test, most Avrami indexes of one- and two-step aging at different temperature are near to 1, indicating that the phase transformation mechanism before peak aging is the elongation ofβ1' rods. The phase transformation activation energy of early stage of one- and two-step aging are all near 80KJ/mol. TTT curve shows that‘nose’is not present; two-step aging largely accelerates the phase transformation rate.
Mechanical properties evolution of ZM61 during the early stage of one-step aging is investigated by modeling, the results show that:①the predicted results of model using‘strengthening equation 2’(Orowan strengthening equation presuming a random distribution of precipitates on gliding planes) indicate that:the increasing velocity of the rod length is much faster than that of rod diameter; the‘fv-t’curve deduced by‘homogeneous nucleation theory’(HNT) rises by exponential form, while‘fv-t’curve deduced by JMA equation rises by‘S’form. As fv is deduced by JMA equation, yield strength curve has a maximal point, as fv is deduced by HNT, yield strength rises much slowly in the early stage of aging but much faster while peak aging is approached and no maximal point appear. Analysis of the formation of maximal point shows that: both volume fraction and diameter ofβ1' rods determine the yield strength, increase in volume fraction ofβ1' rods is not certain to raise yield strength, since increase in rod diameter will reduce yield strength.②By contrasting the predicted results of model using‘strengthening equation 2’and model using‘strengthening equation 1’(Orowan strengthening equation presuming that precipitates are arranged to form regular-triangle arrays), it can be found that: the yield strength values predicted by‘strengthening equation 1’are entirely larger than those predicted by‘strengthening equation 2’, indicating that precipitates arranged as regular-triangle arrays bring about extremely large strengthening effect.
引文
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