中强可焊铝镁钪合金制备及其相关基础研究
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摘要
在工业化生产条件下，采用半连续铸造、热轧、冷轧和稳定化处理技术制备了厚度为2．0mm、宽度为1200mm的铝镁钪合金板材。采用热加工模拟、热塑性、硬度和电导率测试方法，室温拉伸、金相和电子显微分析方法研究了铝镁钪合金在不同均匀化处理、不同热加工工艺和稳定化处理工艺条件下的力学性能、腐蚀性能和显微组织结构及其变化。在此基础上，还研制成功了铝镁钪合金板材配用焊丝和研究了合金成品板材的焊接性能。论文研究获得以下主要结论：
(1)铝镁钪合金的成分范围为Al-(5．5～6．5)Mg-(0．15～0．40)Mn-(0．2-0．4)Sc-(0．1～0．15)Zr-0．02Ti-0．0025Be，成分优化结果表明，Mg应当控制在中上限，取6．0％～6．2％，Mn应当控制在中限，取0．3％，Sc和Zr含量应当分别控制在0．25％和0．12％。
(2)Mn以Al-10％Mn中间合金的形式随铝锭一道加入，装在铝锭的上层；Sc以Al-2％Sc中间合金、Zr以Al-4％Zr中间合金的形式在铝锭熔化后熔体温度达到800℃以上时加入；Ti以块状Al-4％Ti和线状Al-5％Ti-1％B中间合金两种形式加入，其中块状Al-4％Ti中间合金在炉前取样分析前加入，线状Al-5％Ti-1％B中间合金则是在半连续铸造时通过专用送线机构加入到静止炉与铸造机之间的流槽熔体中。
(3)铝镁钪合金最佳精炼工艺由炉内熔体精炼净化和炉外在线精炼净化组成。炉外在线精炼净化需要在精炼净化装置中始终通入惰性气体，且保证气泡均匀细小。
(4)设计并改进了结晶器二次冷却水出水孔的角度，将原来的45°改为30°，可避免大规格铸锭冷隔和裂纹的产生。铝镁钪合金最佳的熔铸工艺参数如下：
(5)半连续激冷铸造条件下生产的铝镁钪合金铸锭在均匀化过程中有类似于传统铝合金固溶后时效过程中的析出特性，即半连续急冷铸造过程中形成的过饱和固溶体会分解析出纳米级的Al_3(Sc，Zr)相。
(6)铝镁钪合金铸锭均匀化的目的除了消除铸锭的宏观应力从而降低铸锭热轧过程中的变形抗力外，主要是调控过饱和固溶体分解析出Al_3(Sc,Zr)的特性，使其均匀弥散分布在铝基固溶体基体上。
(7)综合考虑析出粒子的特性和适当降低铸锭热轧过程中的变形抗力以及热轧后板材的最终拉伸力学性能，铝镁钪合金铸锭均匀化的最佳工艺为300～350℃／8h。
(8)铝镁钪合金高温压缩变形时，应变速率的对数lnε和流变应力、lnσ、ln[sinh(ασ)]之间，ln[sinh(ασ)]和温度T的倒数1／T之间满足线性关系，说明该合金变形过程是一种类似于高温蠕变的热激活过程。据此求得该合金的高温变形材料常数为：
铝镁钪合金热压缩变形的流变应力方程为：
(9)随热塑性试验温度升高，铝镁钪合金高温瞬时强度降低，塑性升高，350℃-400℃铸锭合金变形抗力适中，热塑性较好，合宜的热轧温度为400℃-420℃。大生产条件下，应严格控制道次和道次变形量，开始轧制时道次压下量和轧制速度不宜过大，轧制变形量超过25％后，应逐渐加大道次压下量和提高轧制速度，使变形深透到整个轧件厚度。
(10)铝镁钪合金的再结晶温度比较高，合金可以在较高温度下进行稳定化退火处理。冷轧板材在200℃以下稳定化退火，腐蚀速率、剥落腐蚀反而增加和变差，200℃／1h稳定化退火后腐蚀速率最大、剥落腐蚀最严重；300℃／1h以上稳定化退火，腐蚀速率变小，剥落腐蚀性能由EB级逐步向N级和P级转化。综合考虑合金的力学性能和抗腐蚀性能，铝镁钪合金冷轧板材最佳稳定化退火处理工艺为300℃／1h。
(11)设计和制备了铝镁钪合金板材配用焊丝，这种焊丝与基材有很好的焊接相容性，焊接接头强度系数为85％，微量Sc、Zr对焊接接头的强化作用主要来源于两个方面，一是微量Sc、Zr对焊缝凝固组织的晶粒细化强化和含Sc、Zr化合物的析出强化，二是Al_3(Sc、Zr)析出粒子的存在显著提高了成品板材在焊接热循环过程中的抗再结晶软化能力。
(12)研制的铝镁钪合金板材拉伸力学性能σ_b≥415 MPa，σ_(0.2)≥302MPa，δ_5≥15％，剥落腐蚀性能达到P级，焊接接头强度系数≥0．85，全面达到项目攻关要求。
The Al-Mg-Sc alloy sheets were prepared by semi-continuous casting、hot rollings cold rolling and stabilizing under the condition of industrialization production which dimension was thickness 2mm,by width 1200mm. Using thermal processing simulation and the research of plasticity、hardness measurement and electrical resistance test、tensile test at room temperature and metallographic analysis and electronic microscopy , the mechanical properties、corrosion resistance、microstructure and the variation disciplinarian of microstructure as well as weld properties of Al-Mg-Sc alloy sheets were investigated when the processing technical condition homogenizing and stabilizing treatment technical conditions are different. On the base, the welding properties of Al-Mg-Sc alloy finished sheets were researched. The results show that:
(1) The optimum chemical components range of Al-Mg-Mn-Sc-Zr alloy is Al-5.5-6.5Mg-0.15-0.40Mn-0.2-0.4Sc-0.1-0.15Zr-0.02Ti-Be, in which the content of Mg should be controlled above the medium value and the concentration of Mn is limited to the interspace of the range, while that of Sc and Zr can be controlled in 0.25 and 0.12%, respectively.
(2) Mn is entered together with aluminum bulks in the form of Al-10%Mn master alloys, being placed upper layer of aluminum bulks. Sc is joined in the form of Al-2%Sc master alloys agent, and Zr is joined in the form of Al-4%Zr master alloys, and both of them are carried when temperature of the melted materiel is over 800℃after aluminum bulks are melted. Ti is joined in the form of Al-4%Ti and Al-5%Ti-l%B master alloys, Al-4%Ti master alloys is joined before analyzing sample, inline in chute the form of Al-5%Ti-l%B master alloys at semi-continuous casting.
(3)The best refined processing is made up of the melted refining in furnace and the melted refined online out furnace. During the whole of the latter process, the inert gases with small uniform air bladder are pumped continuously in filter.
(4) The angle of mold draining hole for secondary cooling water is redesigned, and the original 45°is changed to 30°. The optimal parameter of melt-cast technical of Al-Mg-Sc alloy is show in the following table:
(5) During the homogenization process of the as-cast, there is the precipitation property which is similar with the property of traditional aluminium alloy during the process of aging after solid solution, i.e. oversaturated solid solution formed during the process of semi-continuous sharp quenching casting can be decomposed to precipitate Al_3(Sc,Zr) phase of nanometer size.
(6) Besides eliminating the macroscopical stress of the as-cast which decrease the deformation resistance in the process of hot rolling, the main purpose of homogenization is regulating the precipitation property mentioned above, in order to achieve the homogeneous distribution of the particles in the aluminum solid solution matrix.
(7) Overall evaluating the property of precipitated particles, decrease of the deformation resistance in the process of hot rolling and the final mechanical property, the best homogenization temperature is 300-350℃, keeping for 8 hours.
(8) When Sc-Al-Mg alloy is deformed by compression at high temperature, the natural logarithm of strain rate lnεand flow stress, lnσ, ln[sinh(ασ)] ,ln[sinh(ασ)] and the reciprocal of tempurture 1/T satisfy linear relationship. That's to say, the deformation process of this alloy is similar to a thermal activation process of high-temperature creep process. Thus, the high temperature deformation material constant of this alloy is:
we can obtain the equation of flow stress of Al-Mg-Sc alloy deformed by reason of thermal compression as follows :ε= 8.75×10~(12)[sinh(0.1336σ)]~(5.25)exp(-183.201/RT)
(9) With the increase of temperature in thermosplastic experiment, the the short time tensile strength of received-alloy is decreased, and the plasticity is increased. The cast at 350℃-400℃has a proper deformation resistance and a good thermal plasticity, so the proper temperature for hot rolling is 400℃-420℃. Under the manufacture conditions, the pass and reduction in pass should be controlled strictly. Reduction in pass and rolling speed should not be oversized at the beginning of rolling. And after the displacement is over 25%, the reduction in pass and rolling speed should be enhanced generally to make sure the deformation distributing in the whole workpiece.
(10) The recrystallization temperature of Al-Mg-Sc alloy is higher and may be stabilizing annealinged under higher temperature. The corrosion resistance is worse when the stabilizing annealing temperature is lower then 200℃, and the corrosion resistance of cool-roll plane stabilizing annealinged under the conditions of 200℃/1h is the worst one. Correspondingly, the corrosion resistance becomes better and changes from EB degree to N and P degree, when the stabilizing annealing under the conditions of 300℃/1h. Considering the mechanical properties and the corrosion resistance, the best stabilizing annealing process parameters for the cool-roll planes are 300℃/1h.
(11) The matched welding wire is also designed and prepared, which have a very good welding compatibility with the matrix, and the intensity coefficient of the welded joints achieves 86%. The effect of minor Sc and Zr on the joint strength includes two aspect. One is that the minor Sc and Zr refine and strengthen the welded joint structure. The other is the precipitate Al3(Sc,Zr) particles increase the recrystallization softening resistance during the welding thermal-cycle process.
(12) The mechanical properties of the as-researched Al-Mg-Sc alloy plane areσb≥415MPa,σ0.2≥302MPa,δ5≥15%, and the exfoliation corrosion property achieves P degree, and the intensity coefficient of the welded joints is more than 0.85. The results meets the requirements roundly.
(1)铝镁钪合金的成分范围为Al-(5．5～6．5)Mg-(0．15～0．40)Mn-(0．2-0．4)Sc-(0．1～0．15)Zr-0．02Ti-0．0025Be，成分优化结果表明，Mg应当控制在中上限，取6．0％～6．2％，Mn应当控制在中限，取0．3％，Sc和Zr含量应当分别控制在0．25％和0．12％。
(2)Mn以Al-10％Mn中间合金的形式随铝锭一道加入，装在铝锭的上层；Sc以Al-2％Sc中间合金、Zr以Al-4％Zr中间合金的形式在铝锭熔化后熔体温度达到800℃以上时加入；Ti以块状Al-4％Ti和线状Al-5％Ti-1％B中间合金两种形式加入，其中块状Al-4％Ti中间合金在炉前取样分析前加入，线状Al-5％Ti-1％B中间合金则是在半连续铸造时通过专用送线机构加入到静止炉与铸造机之间的流槽熔体中。
(3)铝镁钪合金最佳精炼工艺由炉内熔体精炼净化和炉外在线精炼净化组成。炉外在线精炼净化需要在精炼净化装置中始终通入惰性气体，且保证气泡均匀细小。
(4)设计并改进了结晶器二次冷却水出水孔的角度，将原来的45°改为30°，可避免大规格铸锭冷隔和裂纹的产生。铝镁钪合金最佳的熔铸工艺参数如下：
(5)半连续激冷铸造条件下生产的铝镁钪合金铸锭在均匀化过程中有类似于传统铝合金固溶后时效过程中的析出特性，即半连续急冷铸造过程中形成的过饱和固溶体会分解析出纳米级的Al_3(Sc，Zr)相。
(6)铝镁钪合金铸锭均匀化的目的除了消除铸锭的宏观应力从而降低铸锭热轧过程中的变形抗力外，主要是调控过饱和固溶体分解析出Al_3(Sc,Zr)的特性，使其均匀弥散分布在铝基固溶体基体上。
(7)综合考虑析出粒子的特性和适当降低铸锭热轧过程中的变形抗力以及热轧后板材的最终拉伸力学性能，铝镁钪合金铸锭均匀化的最佳工艺为300～350℃／8h。
(8)铝镁钪合金高温压缩变形时，应变速率的对数lnε和流变应力、lnσ、ln[sinh(ασ)]之间，ln[sinh(ασ)]和温度T的倒数1／T之间满足线性关系，说明该合金变形过程是一种类似于高温蠕变的热激活过程。据此求得该合金的高温变形材料常数为：
铝镁钪合金热压缩变形的流变应力方程为：
(9)随热塑性试验温度升高，铝镁钪合金高温瞬时强度降低，塑性升高，350℃-400℃铸锭合金变形抗力适中，热塑性较好，合宜的热轧温度为400℃-420℃。大生产条件下，应严格控制道次和道次变形量，开始轧制时道次压下量和轧制速度不宜过大，轧制变形量超过25％后，应逐渐加大道次压下量和提高轧制速度，使变形深透到整个轧件厚度。
(10)铝镁钪合金的再结晶温度比较高，合金可以在较高温度下进行稳定化退火处理。冷轧板材在200℃以下稳定化退火，腐蚀速率、剥落腐蚀反而增加和变差，200℃／1h稳定化退火后腐蚀速率最大、剥落腐蚀最严重；300℃／1h以上稳定化退火，腐蚀速率变小，剥落腐蚀性能由EB级逐步向N级和P级转化。综合考虑合金的力学性能和抗腐蚀性能，铝镁钪合金冷轧板材最佳稳定化退火处理工艺为300℃／1h。
(11)设计和制备了铝镁钪合金板材配用焊丝，这种焊丝与基材有很好的焊接相容性，焊接接头强度系数为85％，微量Sc、Zr对焊接接头的强化作用主要来源于两个方面，一是微量Sc、Zr对焊缝凝固组织的晶粒细化强化和含Sc、Zr化合物的析出强化，二是Al_3(Sc、Zr)析出粒子的存在显著提高了成品板材在焊接热循环过程中的抗再结晶软化能力。
(12)研制的铝镁钪合金板材拉伸力学性能σ_b≥415 MPa，σ_(0.2)≥302MPa，δ_5≥15％，剥落腐蚀性能达到P级，焊接接头强度系数≥0．85，全面达到项目攻关要求。
The Al-Mg-Sc alloy sheets were prepared by semi-continuous casting、hot rollings cold rolling and stabilizing under the condition of industrialization production which dimension was thickness 2mm,by width 1200mm. Using thermal processing simulation and the research of plasticity、hardness measurement and electrical resistance test、tensile test at room temperature and metallographic analysis and electronic microscopy , the mechanical properties、corrosion resistance、microstructure and the variation disciplinarian of microstructure as well as weld properties of Al-Mg-Sc alloy sheets were investigated when the processing technical condition homogenizing and stabilizing treatment technical conditions are different. On the base, the welding properties of Al-Mg-Sc alloy finished sheets were researched. The results show that:
(1) The optimum chemical components range of Al-Mg-Mn-Sc-Zr alloy is Al-5.5-6.5Mg-0.15-0.40Mn-0.2-0.4Sc-0.1-0.15Zr-0.02Ti-Be, in which the content of Mg should be controlled above the medium value and the concentration of Mn is limited to the interspace of the range, while that of Sc and Zr can be controlled in 0.25 and 0.12%, respectively.
(2) Mn is entered together with aluminum bulks in the form of Al-10%Mn master alloys, being placed upper layer of aluminum bulks. Sc is joined in the form of Al-2%Sc master alloys agent, and Zr is joined in the form of Al-4%Zr master alloys, and both of them are carried when temperature of the melted materiel is over 800℃after aluminum bulks are melted. Ti is joined in the form of Al-4%Ti and Al-5%Ti-l%B master alloys, Al-4%Ti master alloys is joined before analyzing sample, inline in chute the form of Al-5%Ti-l%B master alloys at semi-continuous casting.
(3)The best refined processing is made up of the melted refining in furnace and the melted refined online out furnace. During the whole of the latter process, the inert gases with small uniform air bladder are pumped continuously in filter.
(4) The angle of mold draining hole for secondary cooling water is redesigned, and the original 45°is changed to 30°. The optimal parameter of melt-cast technical of Al-Mg-Sc alloy is show in the following table:
(5) During the homogenization process of the as-cast, there is the precipitation property which is similar with the property of traditional aluminium alloy during the process of aging after solid solution, i.e. oversaturated solid solution formed during the process of semi-continuous sharp quenching casting can be decomposed to precipitate Al_3(Sc,Zr) phase of nanometer size.
(6) Besides eliminating the macroscopical stress of the as-cast which decrease the deformation resistance in the process of hot rolling, the main purpose of homogenization is regulating the precipitation property mentioned above, in order to achieve the homogeneous distribution of the particles in the aluminum solid solution matrix.
(7) Overall evaluating the property of precipitated particles, decrease of the deformation resistance in the process of hot rolling and the final mechanical property, the best homogenization temperature is 300-350℃, keeping for 8 hours.
(8) When Sc-Al-Mg alloy is deformed by compression at high temperature, the natural logarithm of strain rate lnεand flow stress, lnσ, ln[sinh(ασ)] ,ln[sinh(ασ)] and the reciprocal of tempurture 1/T satisfy linear relationship. That's to say, the deformation process of this alloy is similar to a thermal activation process of high-temperature creep process. Thus, the high temperature deformation material constant of this alloy is:
we can obtain the equation of flow stress of Al-Mg-Sc alloy deformed by reason of thermal compression as follows :ε= 8.75×10~(12)[sinh(0.1336σ)]~(5.25)exp(-183.201/RT)
(9) With the increase of temperature in thermosplastic experiment, the the short time tensile strength of received-alloy is decreased, and the plasticity is increased. The cast at 350℃-400℃has a proper deformation resistance and a good thermal plasticity, so the proper temperature for hot rolling is 400℃-420℃. Under the manufacture conditions, the pass and reduction in pass should be controlled strictly. Reduction in pass and rolling speed should not be oversized at the beginning of rolling. And after the displacement is over 25%, the reduction in pass and rolling speed should be enhanced generally to make sure the deformation distributing in the whole workpiece.
(10) The recrystallization temperature of Al-Mg-Sc alloy is higher and may be stabilizing annealinged under higher temperature. The corrosion resistance is worse when the stabilizing annealing temperature is lower then 200℃, and the corrosion resistance of cool-roll plane stabilizing annealinged under the conditions of 200℃/1h is the worst one. Correspondingly, the corrosion resistance becomes better and changes from EB degree to N and P degree, when the stabilizing annealing under the conditions of 300℃/1h. Considering the mechanical properties and the corrosion resistance, the best stabilizing annealing process parameters for the cool-roll planes are 300℃/1h.
(11) The matched welding wire is also designed and prepared, which have a very good welding compatibility with the matrix, and the intensity coefficient of the welded joints achieves 86%. The effect of minor Sc and Zr on the joint strength includes two aspect. One is that the minor Sc and Zr refine and strengthen the welded joint structure. The other is the precipitate Al3(Sc,Zr) particles increase the recrystallization softening resistance during the welding thermal-cycle process.
(12) The mechanical properties of the as-researched Al-Mg-Sc alloy plane areσb≥415MPa,σ0.2≥302MPa,δ5≥15%, and the exfoliation corrosion property achieves P degree, and the intensity coefficient of the welded joints is more than 0.85. The results meets the requirements roundly.
引文
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