含稀土镁合金细晶化、塑性变形再结晶、时效脱溶及焊接性研究
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摘要
含稀土元素的镁合金具有铸造性能佳，塑性变形潜力大，比强度高，力学性能优良等诸多优点。作者以Mg-Al-Zn(AZ31、AZ61、AZ91)、ZK60、Mg-0.5％Zn-0.5％Zr系列为基础合金，进行稀土合金化研究，用X射线衍射和扫描电子显微分析方法对含稀土元素的合金进行了物相鉴定，用稀土元素和锆对试验合金铸锭进行细晶化处理，在热／力模拟试验的基础上，对含稀土元素的镁合金进行了轧制、挤压塑性变形，对变形后的合金进行了时效强化研究以及电弧焊焊接性试验。利用光学显微镜、扫描电子显微镜以及透射电子显微镜对试验合金在铸态、塑性变形过程状态以及热处理前后的微观组织进行了观察和分析。
1、添加稀土元素的镁及镁合金除了基体相α(Mg)和Mg-Al-Zn合金中的Mg_(17)Al_(12)相、Mg-Zn-Zr中的MgZn等相外，还有稀土元素与镁、锌生成的稀土化合物，这些中间相在铸态时主要分布在晶界，挤压变形后沿着挤压方向分布；加入稀土Ce可以明显细化AZ31合金铸态晶粒，加入Nd、Y分别细化了Mg-0.5％Zn-0.5％Zr合金和ZK60合金铸态晶粒。作者认为镁合金凝固过程中，受凝固时扩散动力学条件限制，稀土元素在固／液界面前沿富集，增大了合金的成分过冷，使树枝晶的生长更发达，二次枝晶增多，枝晶间距减小，晶粒细化。凝固过程中溶质再分配造成固／液界面前沿成分过冷度增大是稀土元素细化镁合金的主要机理。
2、轧制变形使含稀土的Mg-Al-Zn-Ce合金产生了明显的加工硬化，提高了合金强度，轧制变形时被破碎的β相和Al_4Ce稀土相是强化合金的主要原因；Mg-Al-Zn-Ce合金在热塑性变形时有多种变形机制共同作用，大尺寸晶粒产生位错滑移和晶体孪生，小尺寸晶粒产生晶界滑动协调大尺寸晶粒的变形，适量Ce的加入有助于在热轧变形过程中产生大量的动态再结晶小尺寸晶粒，更有效地提高了含稀土镁合金的塑性变形能力。
3、含1.0％Ce的AZ31、AZ61、AZ91合金在673K温度下的变形激活能均比不含Ce的AZ31、AZ61、AZ91合金低，使得合金在673K温度下的塑性变形能力增加，因而有利于合金的塑性变形；在Mg-0.5％Zn-0.5％Zr合金中添加稀土元素Nd和Y、在ZK60合金中添加稀土元素Y后，形成的含稀土化合物在镁合金基体中弥散分布，阻碍合金塑性变形过程中的位错滑移，使位错发生交滑移和攀移所需能量提高，从而提高了合金发生动态再结晶的温度。
4、Mg-0.5％Zn-0.5％Zr～2.2％Nd-4.0％Y合金有良好的挤压变形能力和热处理强化能力，挤压后T5处理态的室温力学性能为：σ_b=293.5MPa，σ_(0.2)=281.2MPa，δ=11％；高温瞬时拉伸力学性能250℃为σ_b=228.78MPa，δ=14.8％；330℃为σ_b=211.2MPa，δ=16.4％。作者的研究工作表明，Mg-0.5％Zn-0.5％Zr-2.2％Nd-4.0％Y合金具有良好的室温和高温综合力学性能。
5、含稀土的镁合金淬火获得镁基过饱和固溶体，在时效脱溶时，Mg-Al-Zn系合金直接析出Mg_(17)Al_(12)平衡相，Mg_(17)Al_(12)相脱溶以两种方式进行，即晶内连续脱溶和晶界不连续脱溶。含稀土的ZK60合金脱溶过程存在预脱溶阶段，在150℃时效时，先析出MgZn′(β′)过渡亚稳相，ZK60合金的时效强化主要来源于过渡相β′对位错运动的阻碍作用，稀土元素Nd、Y对ZK60合金晶粒的细化有利于提高合金中β′相的析出密度，使合金的强化值增大。ZK60-RE合金在150℃时效时的脱溶过程为：SSSS→β′→β(平衡相)，Mg-0.5％Zn-0.5％Zr-2.2％Nd-4.0％Y合金在200℃时效时的脱溶过程为：SSSS→β″→β′→β(平衡相)。
6、GTAW焊接试验表明，AZ31、AZ61Ce合金焊缝金属熔池边缘区域依托母材未熔晶粒形核、长大，即联生生长；稀土Ce能改善AZ31、AZ61合金焊接接头强度及提高焊接接头有效系数，Ce改善Mg-Al-Zn合金焊接性的原因是由于Ce与Al形成了高熔点的Al_4Ce相，减少了粗大的Mg_(17)Al_(12)相的数量和细化了焊缝区的晶粒。ZK60-2.0％Nd-1.0％Y合金焊接接头有效系数比ZK60合金提高明显，原因是稀土元素Nd、Y与镁、锌形成了热稳定性高的第二相稀土化合物，减少了分布在晶界上的粗大MgZn数量。
Magnesium alloys containing rare-earth (RE) are among the bestlightweight structural materials with a good castablity, significant latentplastic deformability, high strength-to-weight ratio and excellentmechanical properties. The author did a lot of researches in rare-earthalloying with Mg-Al-Zn (AZ31 AZ61 AZ91), ZK60 and Mg-RE alloys.The intermetallic phase was identified by X-rays diffraction analysis(XRD) and scan electron microscopy (SEM). The refinement of grainswas carried out by adding RE and Zr. The hot-force compressionsimulation experiment of the investigated alloys was performed beforerolling or extrusion plastic deformation. The aging precipitation andweldability of the investigated alloys was studied and the microstructurewere took observation by optical microscopy (OM), SEM andtransmission electron microscopy (TEM) at casting, during plasticdeformation, before and after heat-treatment. The experimental resultswere analysed and generalized.
1. The author made three series of Mg-Al-Zn-Ce; ZK60-RE andMg-0.5%Zn-0.5%Zr-RE alloys. The intermetallic phase has Mg-REcompounds besidesα-Mg, Mg_(17)Al_(12) of the Mg-Al-Zn alloys,α-Mg, MgZn of the ZK60-RE andα-Mg of the Mg-0.5%Zn-0.5%Zr-RE alloys.The intermetallic phase distributed on the crystal boundary as-casting and aligned along extrusion direction after extruding. The crystal-size ofAZ31Ce as-casting was refined by adding Ce. The crystal-size of theMg-0.5%Zn-0.5%Zr and ZK60 alloys were refined by adding Nd and Y.The essences of refinement of grains of the Mg alloy were systematicallystudied. It revealed that adding RE can improve the refinement of grains.Through principle of solute elements division principle, the mechanism ofrefinement of grains of Mg alloys containing RE is caused by thecomposition undercooling as solute elements (RE) division again.
2. After rolling, significant strengthening was emerged fromMg-Al-Zn-Ce alloys. The ultimate tensile strength was improved. Theinvestigated alloys were strengthened chiefly by Al_4Ce andβ-Mg_(17)Al_(12)broken during rolling. The mechanism of plastic deformation of theMg-Al-Zn-Ce alloys is versatile. The slip of dislocation and twinningwere carried on large-size grains. The deformation of large-size grainswere coordinated by the small-size grains. A lot of small-size: dynamicrecrystallization grains were produced during rolling since addingadequate Ce. The deformability of the investigated alloys was increasedmassively.
3. The deformation activation energy of the AZ31, AZ61, AZ91containing 1.0%Ce are lower than that of AZ31, AZ61, AZ91 alloyswithout Ce. The deformability of the former was improved at 673K. AfterMg-0.5%Zn-0.5%Zr alloys added Nd and Y, ZK60 added Y, the compounds containing RE distributed pervasively on the Mg matrix. Theslip of dislocation was hindered by the compounds particle during plasticdeformation. The energy of dislocation slip increased and the dynamicrecrystallization temperature increased.
4. Mg-0.5%Zn-0.5%Zr-2.2%Nd-4.0%Y alloy possesses goodextrusion deformability and strengthening ability after heat-treatment.The mechanical properties of this alloy at T5-treatment after extrusion areσ_b=293.5MPa,σ_(0.2)=281.2MPa,δ=11%. The ultimate tensile strengthat 250℃areσ_b=228.78MPa,δ=14.8% andσ_b=211.2MPa,δ=16.4% at 330℃. Mg-0.5%Zn-0.5%Zr-2.2%Nd-4.0%Y alloy possesseshigh mechanical properties comprehensively.
5. The equilibriumβ-Mg_(17)Al_(12) precipitated directly fromsupersaturated solid solution in Mg-Al-Zn-Ce alloys. Theβphaseprecipitated continuously within crystal grain and precipitateduncontinuously on the crystal boundary. It was found that ZK60 alloysprecipitated beforehand. The transition phase MgZn′(β′) precipitated firstat 150℃treatment. The strengthening of ZK60 alloys originates fromthat hindrance ofβ′to dislocation. The refinement of grains since Zrand RE Nd, Y are beneficial to increase the density ofβ′in Mg matrix.The value of strengthening improved markedly. The precipitation order ofZK60-RE alloys are SSSS→β′→βat 150℃and that ofMg-0.5%Zn-0.5%Zr-RE alloys are SSSS→β″→β′→βat 200℃.
6. After doing gas tungsten arc welding (GTAW/MIG) experimentwith AZ-Ce, ZK60-RE alloy, the formation of crystal nucleus andcrystalline growth of the welding line melted metal of the investigatedalloy were found. In other word, the new nucleus growth was allied to thegrain of mother stuff crystal, and the heterogeneous nucleation occured inthe centre of the welding line melted metal. RE can improve thetransverse ultimate tensile strength of AZ31 and ZK60 alloys. Theeffectual coefficient of the welding connect increased obviously. Thestrengthening mechanism of the welding connect of AZ31Ce alloys is thatCe and Al combined Al_4Ce compound. Nd and Y reduced the harm of Znto grain boundary while Zn and Mg compound of bulky MgZn phaseduring crystallizing.
1、添加稀土元素的镁及镁合金除了基体相α(Mg)和Mg-Al-Zn合金中的Mg_(17)Al_(12)相、Mg-Zn-Zr中的MgZn等相外，还有稀土元素与镁、锌生成的稀土化合物，这些中间相在铸态时主要分布在晶界，挤压变形后沿着挤压方向分布；加入稀土Ce可以明显细化AZ31合金铸态晶粒，加入Nd、Y分别细化了Mg-0.5％Zn-0.5％Zr合金和ZK60合金铸态晶粒。作者认为镁合金凝固过程中，受凝固时扩散动力学条件限制，稀土元素在固／液界面前沿富集，增大了合金的成分过冷，使树枝晶的生长更发达，二次枝晶增多，枝晶间距减小，晶粒细化。凝固过程中溶质再分配造成固／液界面前沿成分过冷度增大是稀土元素细化镁合金的主要机理。
2、轧制变形使含稀土的Mg-Al-Zn-Ce合金产生了明显的加工硬化，提高了合金强度，轧制变形时被破碎的β相和Al_4Ce稀土相是强化合金的主要原因；Mg-Al-Zn-Ce合金在热塑性变形时有多种变形机制共同作用，大尺寸晶粒产生位错滑移和晶体孪生，小尺寸晶粒产生晶界滑动协调大尺寸晶粒的变形，适量Ce的加入有助于在热轧变形过程中产生大量的动态再结晶小尺寸晶粒，更有效地提高了含稀土镁合金的塑性变形能力。
3、含1.0％Ce的AZ31、AZ61、AZ91合金在673K温度下的变形激活能均比不含Ce的AZ31、AZ61、AZ91合金低，使得合金在673K温度下的塑性变形能力增加，因而有利于合金的塑性变形；在Mg-0.5％Zn-0.5％Zr合金中添加稀土元素Nd和Y、在ZK60合金中添加稀土元素Y后，形成的含稀土化合物在镁合金基体中弥散分布，阻碍合金塑性变形过程中的位错滑移，使位错发生交滑移和攀移所需能量提高，从而提高了合金发生动态再结晶的温度。
4、Mg-0.5％Zn-0.5％Zr～2.2％Nd-4.0％Y合金有良好的挤压变形能力和热处理强化能力，挤压后T5处理态的室温力学性能为：σ_b=293.5MPa，σ_(0.2)=281.2MPa，δ=11％；高温瞬时拉伸力学性能250℃为σ_b=228.78MPa，δ=14.8％；330℃为σ_b=211.2MPa，δ=16.4％。作者的研究工作表明，Mg-0.5％Zn-0.5％Zr-2.2％Nd-4.0％Y合金具有良好的室温和高温综合力学性能。
5、含稀土的镁合金淬火获得镁基过饱和固溶体，在时效脱溶时，Mg-Al-Zn系合金直接析出Mg_(17)Al_(12)平衡相，Mg_(17)Al_(12)相脱溶以两种方式进行，即晶内连续脱溶和晶界不连续脱溶。含稀土的ZK60合金脱溶过程存在预脱溶阶段，在150℃时效时，先析出MgZn′(β′)过渡亚稳相，ZK60合金的时效强化主要来源于过渡相β′对位错运动的阻碍作用，稀土元素Nd、Y对ZK60合金晶粒的细化有利于提高合金中β′相的析出密度，使合金的强化值增大。ZK60-RE合金在150℃时效时的脱溶过程为：SSSS→β′→β(平衡相)，Mg-0.5％Zn-0.5％Zr-2.2％Nd-4.0％Y合金在200℃时效时的脱溶过程为：SSSS→β″→β′→β(平衡相)。
6、GTAW焊接试验表明，AZ31、AZ61Ce合金焊缝金属熔池边缘区域依托母材未熔晶粒形核、长大，即联生生长；稀土Ce能改善AZ31、AZ61合金焊接接头强度及提高焊接接头有效系数，Ce改善Mg-Al-Zn合金焊接性的原因是由于Ce与Al形成了高熔点的Al_4Ce相，减少了粗大的Mg_(17)Al_(12)相的数量和细化了焊缝区的晶粒。ZK60-2.0％Nd-1.0％Y合金焊接接头有效系数比ZK60合金提高明显，原因是稀土元素Nd、Y与镁、锌形成了热稳定性高的第二相稀土化合物，减少了分布在晶界上的粗大MgZn数量。
Magnesium alloys containing rare-earth (RE) are among the bestlightweight structural materials with a good castablity, significant latentplastic deformability, high strength-to-weight ratio and excellentmechanical properties. The author did a lot of researches in rare-earthalloying with Mg-Al-Zn (AZ31 AZ61 AZ91), ZK60 and Mg-RE alloys.The intermetallic phase was identified by X-rays diffraction analysis(XRD) and scan electron microscopy (SEM). The refinement of grainswas carried out by adding RE and Zr. The hot-force compressionsimulation experiment of the investigated alloys was performed beforerolling or extrusion plastic deformation. The aging precipitation andweldability of the investigated alloys was studied and the microstructurewere took observation by optical microscopy (OM), SEM andtransmission electron microscopy (TEM) at casting, during plasticdeformation, before and after heat-treatment. The experimental resultswere analysed and generalized.
1. The author made three series of Mg-Al-Zn-Ce; ZK60-RE andMg-0.5%Zn-0.5%Zr-RE alloys. The intermetallic phase has Mg-REcompounds besidesα-Mg, Mg_(17)Al_(12) of the Mg-Al-Zn alloys,α-Mg, MgZn of the ZK60-RE andα-Mg of the Mg-0.5%Zn-0.5%Zr-RE alloys.The intermetallic phase distributed on the crystal boundary as-casting and aligned along extrusion direction after extruding. The crystal-size ofAZ31Ce as-casting was refined by adding Ce. The crystal-size of theMg-0.5%Zn-0.5%Zr and ZK60 alloys were refined by adding Nd and Y.The essences of refinement of grains of the Mg alloy were systematicallystudied. It revealed that adding RE can improve the refinement of grains.Through principle of solute elements division principle, the mechanism ofrefinement of grains of Mg alloys containing RE is caused by thecomposition undercooling as solute elements (RE) division again.
2. After rolling, significant strengthening was emerged fromMg-Al-Zn-Ce alloys. The ultimate tensile strength was improved. Theinvestigated alloys were strengthened chiefly by Al_4Ce andβ-Mg_(17)Al_(12)broken during rolling. The mechanism of plastic deformation of theMg-Al-Zn-Ce alloys is versatile. The slip of dislocation and twinningwere carried on large-size grains. The deformation of large-size grainswere coordinated by the small-size grains. A lot of small-size: dynamicrecrystallization grains were produced during rolling since addingadequate Ce. The deformability of the investigated alloys was increasedmassively.
3. The deformation activation energy of the AZ31, AZ61, AZ91containing 1.0%Ce are lower than that of AZ31, AZ61, AZ91 alloyswithout Ce. The deformability of the former was improved at 673K. AfterMg-0.5%Zn-0.5%Zr alloys added Nd and Y, ZK60 added Y, the compounds containing RE distributed pervasively on the Mg matrix. Theslip of dislocation was hindered by the compounds particle during plasticdeformation. The energy of dislocation slip increased and the dynamicrecrystallization temperature increased.
4. Mg-0.5%Zn-0.5%Zr-2.2%Nd-4.0%Y alloy possesses goodextrusion deformability and strengthening ability after heat-treatment.The mechanical properties of this alloy at T5-treatment after extrusion areσ_b=293.5MPa,σ_(0.2)=281.2MPa,δ=11%. The ultimate tensile strengthat 250℃areσ_b=228.78MPa,δ=14.8% andσ_b=211.2MPa,δ=16.4% at 330℃. Mg-0.5%Zn-0.5%Zr-2.2%Nd-4.0%Y alloy possesseshigh mechanical properties comprehensively.
5. The equilibriumβ-Mg_(17)Al_(12) precipitated directly fromsupersaturated solid solution in Mg-Al-Zn-Ce alloys. Theβphaseprecipitated continuously within crystal grain and precipitateduncontinuously on the crystal boundary. It was found that ZK60 alloysprecipitated beforehand. The transition phase MgZn′(β′) precipitated firstat 150℃treatment. The strengthening of ZK60 alloys originates fromthat hindrance ofβ′to dislocation. The refinement of grains since Zrand RE Nd, Y are beneficial to increase the density ofβ′in Mg matrix.The value of strengthening improved markedly. The precipitation order ofZK60-RE alloys are SSSS→β′→βat 150℃and that ofMg-0.5%Zn-0.5%Zr-RE alloys are SSSS→β″→β′→βat 200℃.
6. After doing gas tungsten arc welding (GTAW/MIG) experimentwith AZ-Ce, ZK60-RE alloy, the formation of crystal nucleus andcrystalline growth of the welding line melted metal of the investigatedalloy were found. In other word, the new nucleus growth was allied to thegrain of mother stuff crystal, and the heterogeneous nucleation occured inthe centre of the welding line melted metal. RE can improve thetransverse ultimate tensile strength of AZ31 and ZK60 alloys. Theeffectual coefficient of the welding connect increased obviously. Thestrengthening mechanism of the welding connect of AZ31Ce alloys is thatCe and Al combined Al_4Ce compound. Nd and Y reduced the harm of Znto grain boundary while Zn and Mg compound of bulky MgZn phaseduring crystallizing.
引文
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