Mg-Nd-Zn-Zr合金微观组织、力学性能和强化机制的研究
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摘要
镁稀土合金因其优良的力学性能，特别是高温性能引起国内外越来越多的重视。以Mg-Gd系合金为代表的镁重稀土合金因其具有出众的时效硬化特性和优良的耐热性能成为研究热门合金；这类合金的室温和高温力学性能虽然良好，但高的稀土含量(>8wt.%)大大的提高了合金的成本，成本的提高势必阻碍合金的应用。稀土元素Nd在镁中的最大固溶度为3.6wt.%，而且在200℃时的固溶度几乎为零(0.08wt.%)，Mg-Nd两元合金即具有明显的时效强化效果，因此以Mg-Nd系合金为基础有望开发出高强度低成本镁稀土合金，我国ZM6和前苏联ML10合金即是通过在镁中添加富Nd混合稀土和少量Zn元素形成的商业镁合金。少量Zn元素加入Mg-Nd合金中可以提高合金时效时的峰值硬度和蠕变强度，进一步添加Zn元素反而会降低合金的峰值硬度，Zn元素在Mg-Nd合金中的作用机制尚不清楚，因此有必要对Mg-Nd-Zn系合金进行系统深入的研究，以达到优化合金力学性能、揭示合金强化机制的目的。
本文主要以Mg-Nd-Zn-Zr铸造合金(Zr元素作为晶粒细化剂)为基础，采用电感耦合等离子直读光谱仪(ICP)、光学显微镜(OM)、X射线衍射仪(XRD)、扫描电子显微镜(SEM)和透射电子显微镜(TEM)等分析手段，通过硬度、室温高温拉伸、室温压缩和冲击、蠕变试验，分别研究了不同Zn含量和不同Nd含量对铸造Mg-2.75Nd-xZn-Zr(x=0,0.2,0.5,1.0,2.0)和Mg-yNd-0.2Zn-Zr(y=1.25,1.75,2.25,2.75,3.0,3.25)(wt.%)合金组织与力学性能的影响，得到优化的合金化学成分配比；重点研究了合金中微量Zn元素对合金塑性变形机制的影响，优化后铸造合金典型时效态下的析出相、力学行为和强化机制，以及热挤压工艺对合金显微组织和室温力学行为的影响。研究结果表明:
当x=0.2，y=3.0wt.%时，铸造Mg-yNd-xZn-Zr合金在铸态、固溶处理态和200℃峰值时效态下具有最佳的室温强度和延伸率配比，为优化的合金成分。该成分铸造和挤压合金最佳的室温屈服强度、抗拉强度与延伸率组合分别为：140MPa-300MPa-11%和314MPa-325MPa-19.3%。
微量Zn元素(0.2wt.%)可以明显改善Mg-Nd-Zn-Zr合金在铸态、固溶处理态和200℃峰值时效态下合金的塑性并提高合金的抗拉强度。通过对比研究固溶处理态Mg-2.75Nd-Zr(NK-T4)和Mg-2.75Nd-0.2Zn-Zr (NZK-T4)合金室温原位拉伸(in-situ tensiletest)过程中试样表面形貌的变化，发现与NK-T4合金相比，NZK-T4合金塑性的提高很可能是波浪形滑移条纹所对应的塑性变形机制的大量开动引起的。对两种合金5%室温拉伸变形后的显微组织观察表明，除基面滑移外，非基面位错在NK-T4和NZK-T4两种合金中都可以观察到，但NZK-T4合金中非基面位错的密度更大，特别是在晶界附近；此外，在NZK-T4合金中，或者位错也可以在某些晶粒内大量观察到。所以原位拉伸观察到的大量波浪形滑移条纹很可能是由非基面滑移产生的。Nd元素以溶质原子的形式存在于合金中会促进非基面滑移系(主要为非基面位错)的开动，微量Zn元素的加入会进一步促进非基面滑移(包括非基面位错、或者位错)的开动，从而明显改善合金的室温塑性，提高合金的抗拉强度。
铸造Mg-3.0Nd-0.2Zn-Zr(NZ30K)(wt.%)合金250℃下时效0.5～500h，析出相均为β’亚稳相，随着时效时间的增加，β’亚稳相粗化，析出相密度下降；200℃峰值时效10～14h，析出相在{1100}α和{1120}α棱柱面上均有分布，此时析出相主要为β”亚稳相。铸造合金200℃峰值时效态下具有最佳的室温力学性能。
析出相的强化作用占铸造时效态NZ30K合金屈服强度的60%左右；而挤压时效后，细晶和挤压过程中产生的第二相的总体强化作用占到50%以上，析出相强化作用的绝对贡献值与铸造时效态合金相当，但相对值下降到30%左右。
挤压态NZ30K合金主要由再结晶晶粒、未完全再结晶组织和热挤压过程中析出的第二相组成，其中再结晶晶粒呈双峰分布，大晶粒尺寸在微米级，小晶粒尺寸在亚微米级，未完全再结晶组织的(0001)面平行于挤压方向。挤压态NZ30K合金室温拉伸时表现出明显的韧性断裂特征：出现了明显的屈服降(Yield Drop)和下屈服平台、拉伸后期产生明显的缩颈、拉伸断口由大量韧窝组成。合金屈服降是由合金拉伸时局部塑性变形引起的，局部塑性变形的产生与挤压态合金中未完全再结晶组织和小晶粒分布不均匀、晶粒的双峰分布、晶粒自身塑性变形能力提高和初始可动位错密度较低等因素密切相关。局部塑性变形在拉伸试样标距段的扩展产生下屈服平台，在此阶段，合金的塑性变形主要由基面与非基面位错提供。局部塑性变形扩展完成后，合金进入均匀塑性变形阶段，仍主要由基面与非基面位错提供，此时晶粒内部出现局部塑性变形带和位错墙；合金应力达到最大后产生缩颈，此时含矢量位错大量参与塑性变形，合金具备了五个独立滑移系，发生韧性断裂。在整个塑性变形阶段，孪晶数量较少(位于部分大晶粒内部)，仅起到辅助变形的作用。
The extremely low density, high specific strength and stiffness of Mg alloy make itattractive for engineering applications. It has been demonstrated that rare earth metals(RE) are the most effective elements to improve the strength properties of magnesiumalloys especially at elevated temperatures. More recently, a lot of work has been focusedon magnesium alloys containing heavy rare earth elements, such as Mg-Gd based alloys.Though these alloys show high strength, high content of heavy rare earth elementsenhances alloys’ cost, which would probably limit their engineering application. Rationaluse of Neodynium (Nd) could make it possible to develop a high strength and low costmagnesium alloy. Nd is one of light rare earth elements, with maximum solubility in solidMg of3.6wt.%at eutectic temperature545℃. Mg-Nd binary alloys have already hadsignificant strengthening effect. The commercial Russia ML10and Chinese ZM6alloys aredeveloped from Mg-MM alloy, in which MM is Nd rich Misch Metal. Addition of smallamount Zn to Mg-Nd alloy can further increase its peak-aged hardness and creepstrength, but more addition can reduce the peak-aged hardness. The strengthenmechanisms of Zn addition in Mg-Nd alloy are unclear yet. Therefore, it is necessary to dosystematic research on Mg-Nd-Zn alloys in order to optimize the alloy’s strength andreveal the strengthen mechanisms.
By inductively coupled plasma analyzer (ICP), optical microscopy (OM), X-raydiffractometer (XRD), scanning electron microscopy (SEM) and transmission electronmicroscopy (TEM), hardness, tensile, compression and creep test, the microstructure andmechanical properties of gravity cast Mg-2.75Nd-xZn-Zr (x=0,0.2,0.5,1.0,2.0wt.%) andMg-yNd-0.2Zn-Zr (y=1.25,1.75,2.25,2.75,3.0,3.25wt.%) alloys in as-cast,solution-treated and200℃peak-aged conditions are investigated at room temperatureand the optimal chemical compositions are determined. The effect of trace amount of Znaddition on the plastic deformation mechanism of the alloy at room temperature, theprecipitates, mechanical behavior and strengthen mechanism in typical aged optimized alloy, and the effect of hot extrusion on the optimized alloy are investigated anddiscussed. The results show:
When x=0.2, y=3.0wt.%, the cast Mg-yNd-xZn-Zr alloy has the best combination ofroom temperature strength and elongation in as-cast, solution-treated and200℃peak-aged conditions, and is considered as optimized cast alloy. The best mechanicalproperties of optimized cast alloy at room temperature are: yield strength (YS)140MPa,ultimate tensile strength (UTS)300MPa, elongation11%. The best mechanical propertiesof hot extruded alloy, whose chemical composition are the same as the optimized castalloy, at room temperature are: YS314MPa, UTS325MPa, elongation19.3%.
Trace amount of Zn addition can significantly enhance Mg-Nd-Zn-Zr alloys’ ductility andincrease the UTS in as-cast, solution-treated and200℃peak-aged conditions at roomtemperature. By comparison the surface morphology variation of solution-treatedMg-2.75Nd-Zr (NK-T4) and Mg-2.75Nd-0.2Zn-Zr (NZK-T4) alloy tensile samples in in-situtensile test in SEM at room temperature, it is found that the enhancement of ductility ofNZK-T4alloy is probably due to the frequent activity of plastic deformation mechanismrepresented by the wave slip lines. The investigation of dislocation distribution in5%tensile deformed NK-T4and NZK-T4samples in TEM shows that, besides basal dislocations, non-basal basal dislocations are investigated in both NK-T4and NZK-T4alloys, however, the dislocation density is much higher in NZK-T4alloy than that in NK-T4alloy, specially near the grain boundaries. Also, in some grains in NZK-T4alloy, or dislocations are investigated and their density are high. Therefore, the wave slip linesinvestigated on the surface of tensile samples in in-situ tensile test are probably causedby the non-basal dislocations investigated in TEM. Nd solute atoms in magnesium alloycan enhance the activity of non-basal dislocations (mainly non-basal dislocations).Trace amount of Zn addition can further promote the activity of non-basal dislocations,inclusion non-basal dislocations and or dislocations, which improve thealloys’ both ductility and UTS at room temperature.
Cast Mg-3.0Nd-0.2Zn-Zr (NZ30K)(wt.%) alloy has different precipitates under differentaging process: the precipitates are the β’ metastable phase when aged at250℃for0.5to500h; the precipitates are mainly the β” metastable phase when aged at200℃for10to14h (peak-aged). The200℃peak-aged alloy has the best mechanical properties atroom temperature.
The contribution of precipitate strengthening in cast-T6alloy is about60%. After hot extrusion and200℃peak-aging, the absolute strengthening contribution of precipitatestays about90MPa as cast-T6alloy, but the contribution percentage reduces to30%. Thestrengthening contribution of grain refinement and secondary phase produced during hotextrusion is more than50%in hot extruded alloy.
As-extruded NZ30K alloy composes of recrystallized grains, un-recrystallized area andsecond phases precipitated during hot extrusion. The recrystallized grains show thebimodal grain size distribution. The fine grains are less than1μm, while the coarse grainsare several micrometers in size. The (0001) planes of the un-recrystallized area areparallel to the extrusion direction, which is probably the main reason of the ring fibertexture. As-extruded NZ30K alloy shows typical ductile fracture characteristics during thetensile test at room temperature: the yield drop phenomenon, the yield point elongation,necking in the late period of tensile test and dimple fracture surface. The yield dropphenomenon is caused by the localized plastic deformation at the beginning of tensiletest. The localized plastic deformation is closely associated with the non-homogeneousdistribution of the un-recrystallized area and fine grains, the bimodal grain sizedistribution, the enhanced plastic deformation ability of the individual grains by Nd andZn solute atoms and the low density of mobile dislocation in as-extruded alloy. Thepropagation of localized plastic deformation on the gauge length of tensile samples leadsto the yield point elongation, which are mainly caused by the basal and non-basal dislocations. The homogeneous plastic deformation follows the yield point elongation,which are also mainly caused by the basal and non-basal dislocations. Localizeddeformation zone and dislocation walls are investigated in the grain interiors in this stage.After UTS, necking happens and lots of dislocations containing component areinvestigated. In this stage, the alloy has five individual slip systems and ductile fracturehappens. During the whole tensile deformation, twinning is only investigated in somecoarse grains, hence, only takes small part of the whole plastic deformation.
本文主要以Mg-Nd-Zn-Zr铸造合金(Zr元素作为晶粒细化剂)为基础，采用电感耦合等离子直读光谱仪(ICP)、光学显微镜(OM)、X射线衍射仪(XRD)、扫描电子显微镜(SEM)和透射电子显微镜(TEM)等分析手段，通过硬度、室温高温拉伸、室温压缩和冲击、蠕变试验，分别研究了不同Zn含量和不同Nd含量对铸造Mg-2.75Nd-xZn-Zr(x=0,0.2,0.5,1.0,2.0)和Mg-yNd-0.2Zn-Zr(y=1.25,1.75,2.25,2.75,3.0,3.25)(wt.%)合金组织与力学性能的影响，得到优化的合金化学成分配比；重点研究了合金中微量Zn元素对合金塑性变形机制的影响，优化后铸造合金典型时效态下的析出相、力学行为和强化机制，以及热挤压工艺对合金显微组织和室温力学行为的影响。研究结果表明:
当x=0.2，y=3.0wt.%时，铸造Mg-yNd-xZn-Zr合金在铸态、固溶处理态和200℃峰值时效态下具有最佳的室温强度和延伸率配比，为优化的合金成分。该成分铸造和挤压合金最佳的室温屈服强度、抗拉强度与延伸率组合分别为：140MPa-300MPa-11%和314MPa-325MPa-19.3%。
微量Zn元素(0.2wt.%)可以明显改善Mg-Nd-Zn-Zr合金在铸态、固溶处理态和200℃峰值时效态下合金的塑性并提高合金的抗拉强度。通过对比研究固溶处理态Mg-2.75Nd-Zr(NK-T4)和Mg-2.75Nd-0.2Zn-Zr (NZK-T4)合金室温原位拉伸(in-situ tensiletest)过程中试样表面形貌的变化，发现与NK-T4合金相比，NZK-T4合金塑性的提高很可能是波浪形滑移条纹所对应的塑性变形机制的大量开动引起的。对两种合金5%室温拉伸变形后的显微组织观察表明，除基面滑移外，非基面位错在NK-T4和NZK-T4两种合金中都可以观察到，但NZK-T4合金中非基面位错的密度更大，特别是在晶界附近；此外，在NZK-T4合金中，
铸造Mg-3.0Nd-0.2Zn-Zr(NZ30K)(wt.%)合金250℃下时效0.5～500h，析出相均为β’亚稳相，随着时效时间的增加，β’亚稳相粗化，析出相密度下降；200℃峰值时效10～14h，析出相在{1100}α和{1120}α棱柱面上均有分布，此时析出相主要为β”亚稳相。铸造合金200℃峰值时效态下具有最佳的室温力学性能。
析出相的强化作用占铸造时效态NZ30K合金屈服强度的60%左右；而挤压时效后，细晶和挤压过程中产生的第二相的总体强化作用占到50%以上，析出相强化作用的绝对贡献值与铸造时效态合金相当，但相对值下降到30%左右。
挤压态NZ30K合金主要由再结晶晶粒、未完全再结晶组织和热挤压过程中析出的第二相组成，其中再结晶晶粒呈双峰分布，大晶粒尺寸在微米级，小晶粒尺寸在亚微米级，未完全再结晶组织的(0001)面平行于挤压方向。挤压态NZ30K合金室温拉伸时表现出明显的韧性断裂特征：出现了明显的屈服降(Yield Drop)和下屈服平台、拉伸后期产生明显的缩颈、拉伸断口由大量韧窝组成。合金屈服降是由合金拉伸时局部塑性变形引起的，局部塑性变形的产生与挤压态合金中未完全再结晶组织和小晶粒分布不均匀、晶粒的双峰分布、晶粒自身塑性变形能力提高和初始可动位错密度较低等因素密切相关。局部塑性变形在拉伸试样标距段的扩展产生下屈服平台，在此阶段，合金的塑性变形主要由基面与非基面位错提供。局部塑性变形扩展完成后，合金进入均匀塑性变形阶段，仍主要由基面与非基面位错提供，此时晶粒内部出现局部塑性变形带和位错墙；合金应力达到最大后产生缩颈，此时含
The extremely low density, high specific strength and stiffness of Mg alloy make itattractive for engineering applications. It has been demonstrated that rare earth metals(RE) are the most effective elements to improve the strength properties of magnesiumalloys especially at elevated temperatures. More recently, a lot of work has been focusedon magnesium alloys containing heavy rare earth elements, such as Mg-Gd based alloys.Though these alloys show high strength, high content of heavy rare earth elementsenhances alloys’ cost, which would probably limit their engineering application. Rationaluse of Neodynium (Nd) could make it possible to develop a high strength and low costmagnesium alloy. Nd is one of light rare earth elements, with maximum solubility in solidMg of3.6wt.%at eutectic temperature545℃. Mg-Nd binary alloys have already hadsignificant strengthening effect. The commercial Russia ML10and Chinese ZM6alloys aredeveloped from Mg-MM alloy, in which MM is Nd rich Misch Metal. Addition of smallamount Zn to Mg-Nd alloy can further increase its peak-aged hardness and creepstrength, but more addition can reduce the peak-aged hardness. The strengthenmechanisms of Zn addition in Mg-Nd alloy are unclear yet. Therefore, it is necessary to dosystematic research on Mg-Nd-Zn alloys in order to optimize the alloy’s strength andreveal the strengthen mechanisms.
By inductively coupled plasma analyzer (ICP), optical microscopy (OM), X-raydiffractometer (XRD), scanning electron microscopy (SEM) and transmission electronmicroscopy (TEM), hardness, tensile, compression and creep test, the microstructure andmechanical properties of gravity cast Mg-2.75Nd-xZn-Zr (x=0,0.2,0.5,1.0,2.0wt.%) andMg-yNd-0.2Zn-Zr (y=1.25,1.75,2.25,2.75,3.0,3.25wt.%) alloys in as-cast,solution-treated and200℃peak-aged conditions are investigated at room temperatureand the optimal chemical compositions are determined. The effect of trace amount of Znaddition on the plastic deformation mechanism of the alloy at room temperature, theprecipitates, mechanical behavior and strengthen mechanism in typical aged optimized alloy, and the effect of hot extrusion on the optimized alloy are investigated anddiscussed. The results show:
When x=0.2, y=3.0wt.%, the cast Mg-yNd-xZn-Zr alloy has the best combination ofroom temperature strength and elongation in as-cast, solution-treated and200℃peak-aged conditions, and is considered as optimized cast alloy. The best mechanicalproperties of optimized cast alloy at room temperature are: yield strength (YS)140MPa,ultimate tensile strength (UTS)300MPa, elongation11%. The best mechanical propertiesof hot extruded alloy, whose chemical composition are the same as the optimized castalloy, at room temperature are: YS314MPa, UTS325MPa, elongation19.3%.
Trace amount of Zn addition can significantly enhance Mg-Nd-Zn-Zr alloys’ ductility andincrease the UTS in as-cast, solution-treated and200℃peak-aged conditions at roomtemperature. By comparison the surface morphology variation of solution-treatedMg-2.75Nd-Zr (NK-T4) and Mg-2.75Nd-0.2Zn-Zr (NZK-T4) alloy tensile samples in in-situtensile test in SEM at room temperature, it is found that the enhancement of ductility ofNZK-T4alloy is probably due to the frequent activity of plastic deformation mechanismrepresented by the wave slip lines. The investigation of dislocation distribution in5%tensile deformed NK-T4and NZK-T4samples in TEM shows that, besides basal dislocations, non-basal basal dislocations are investigated in both NK-T4and NZK-T4alloys, however, the dislocation density is much higher in NZK-T4alloy than that in NK-T4alloy, specially near the grain boundaries. Also, in some grains in NZK-T4alloy,
Cast Mg-3.0Nd-0.2Zn-Zr (NZ30K)(wt.%) alloy has different precipitates under differentaging process: the precipitates are the β’ metastable phase when aged at250℃for0.5to500h; the precipitates are mainly the β” metastable phase when aged at200℃for10to14h (peak-aged). The200℃peak-aged alloy has the best mechanical properties atroom temperature.
The contribution of precipitate strengthening in cast-T6alloy is about60%. After hot extrusion and200℃peak-aging, the absolute strengthening contribution of precipitatestays about90MPa as cast-T6alloy, but the contribution percentage reduces to30%. Thestrengthening contribution of grain refinement and secondary phase produced during hotextrusion is more than50%in hot extruded alloy.
As-extruded NZ30K alloy composes of recrystallized grains, un-recrystallized area andsecond phases precipitated during hot extrusion. The recrystallized grains show thebimodal grain size distribution. The fine grains are less than1μm, while the coarse grainsare several micrometers in size. The (0001) planes of the un-recrystallized area areparallel to the extrusion direction, which is probably the main reason of the ring fibertexture. As-extruded NZ30K alloy shows typical ductile fracture characteristics during thetensile test at room temperature: the yield drop phenomenon, the yield point elongation,necking in the late period of tensile test and dimple fracture surface. The yield dropphenomenon is caused by the localized plastic deformation at the beginning of tensiletest. The localized plastic deformation is closely associated with the non-homogeneousdistribution of the un-recrystallized area and fine grains, the bimodal grain sizedistribution, the enhanced plastic deformation ability of the individual grains by Nd andZn solute atoms and the low density of mobile dislocation in as-extruded alloy. Thepropagation of localized plastic deformation on the gauge length of tensile samples leadsto the yield point elongation, which are mainly caused by the basal and non-basal dislocations. The homogeneous plastic deformation follows the yield point elongation,which are also mainly caused by the basal and non-basal dislocations. Localizeddeformation zone and dislocation walls are investigated in the grain interiors in this stage.After UTS, necking happens and lots of dislocations containing
引文
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