变质细化和热处理对挤压铸造成形A356铝合金构件性能的影响
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Influence of Modification, Refinement and Heat Treatment on Mechanical Properties of A356 Al-alloy Components Prepared by Squeeze Casting
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通讯作者: 姜巨福,jiangjufu@hit.edu.cn,研究方向为合金及复合材料挤压铸造理论与技术、合金及其复合材料半固态加工理论与技术
收稿日期: 2020-05-29 修回日期: 2020-09-09 网络出版日期: 2021-01-04
基金资助: |
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Corresponding authors: JIANG Jufu, Tel:
Received: 2020-05-29 Revised: 2020-09-09 Online: 2021-01-04
作者简介 About authors
姜巨福,男,1976年生,教授
用Al-10Sr变质剂和Al-5Ti-B细化剂处理A356铝合金熔体,并结合挤压铸造和T6热处理工艺,研究变质细化与热处理对A356铝合金挤压铸造件的组织和性能的影响规律。结果表明,随着Al-10Sr变质剂加入量的增加,共晶Si的形貌由片状和长杆状变为颗粒状和蠕虫状,α-Al的晶粒尺寸先减少后增大。当Al-10Sr的加入量(质量分数)为0.3%时,挤压铸造成形件的最优抗拉强度、屈服强度和延伸率分别为221.3 MPa、104.5 MPa和10.3%。Al-10Sr变质能提高形核率、细化α-Al晶粒尺寸和改变共晶硅形貌,使铸造件的力学性能提高。随着A-5Ti-B的增加,晶粒尺寸先降后增,力学性能先增后降。Al-5Ti-B的加入量为0.6%时,最优抗拉强度、屈服强度和延伸率分别为215.6 MPa、106.6 MPa和9.0%。T6热处理(固溶540℃/4 h+时效190℃/4 h)使屈服强度和抗拉强度显著提高和延伸率降低。经过0.6% 的Al-5Ti-B细化处理,T6处理挤压铸造件的最优的抗拉强度、屈服强度和延伸率分别为297.5 MPa、239.3 MPa和8.0%。共晶硅的球化和细化、成形件成分的均匀化以及Mg2Si强化相在基体中弥散析出,是热处理后构件力学性能提高的主要原因。
关键词:
Influence of modification, refinement and heat treatment on the microstructure and mechanical properties of A356 Al-alloy components prepared by squeeze casting was investigated. The results show that with increase of Al-10Sr modification agent, the morphology of eutectic Si changed from lamellar, rod-like shape to granular and wormlike shape, and the grain size of α-Al increased first and then decreased. When 0.3% Al-10Sr modification agent was added, the optimal mechanical properties of squeeze casting components including ultimate tensile strength of 221.3 MPa, yield strength of 104.5 MPa and elongation of 10.3% were achieved. The improvement of mechanical properties can be attributed to the increase of nucleation rate, the decrease of α-Al grain size and the change of eutectic Si morphology by adding 0.3% Al-10Sr modification agent. With the increase of A-5Ti-B refiner, the α-Al grain size first decreased and then increased, but the changing trend of mechanical properties is inverse. When 0.6% Al-5Ti-B refiner was added, the optimal ultimate tensile strength, yield strength and elongation were 215.6 MPa, 106.6 MPa and 9.0%, respectively. T6 heat treatment including solid solution at 540℃ for 4 h and artificial aging at 190℃ for 4 h led to the improvement of yield strength and ultimate tensile strength, but it led to the decrease of elongation. The optimal mechanical properties such as yield strength of 239.3 MPa, ultimate tensile strength of 297.5 MPa and elongation of 8.0% were obtained for the squeeze casting component with T6 treatment and an addition of 0.6% A-5Ti-B refiner. The globularization of eutectic Si, the refinement of eutectic Si, the homogenization of composition for the prepared component and the precipitation of Mg2Si phase in α-Al matrix all lead to the improvement of mechanical properties of squeeze casting component with T6 treatment.
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本文引用格式
姜巨福, 王迎, 肖冠菲, 邓腾, 刘英泽, 张颖.
JIANG Jufu, WANG Ying, XIAO Guanfei, DENG Teng, LIU Yingze, ZHANG Ying.
挤压铸造技术的优越性,使各国投入了很大的精力研究金属挤压铸造技术。前苏联[8,9]、美国[10,11]、日本[12,13]、中国[14~17]、英国[18,19]、意大利[20]和韩国[21,22]在钢铁材料、铝合金、铜合金、镁合金以及铝基复合材料等方面,开展了挤压铸造理论、工艺以及装备的研究和开发。随着轻量化技术的发展,铝合金结构件的挤压铸造成形工艺受到了极大的关注。挤压铸造工艺在轿车和重载汽车铝轮毂的成形制造等方面,有较好的应用前景[24,25]。挤压铸造,是成形汽车空调压缩机铝合金连杆和摇盘的重要技术选择[25~27]。研究发现,挤压铸造技术在成形轿车转向节、控制臂、发动机拉杆弯臂和副车架等底盘承载结构件等方面有明显的优势[28~32]。挤压铸造,也是Al-Cu系高强特种装备铝合金负重轮的主要成形方法[33,34]。
1 实验方法
实验用材料为A356铸造铝合金。使用X射线荧光光谱仪测试其成分(质量分数)为: 6.93% Si、0.49% Mg、0.054% Ti、0.02% Fe、0.33% Mn、0.011% Cu、0.043% Zn和基体Al。A356铝合金的变质剂和细化剂为Al-10Sr合金和Al-5Ti-B合金。
分别取不同质量分数的Al-10Sr变质剂或Al-5Ti-B细化剂加入到金属液中,研究不同质量分数的变质剂和细化剂对成形件微观组织和力学性能的影响规律。在挤压铸造成形实验方案中,保持浇注温度、模具温度和比压不变,改变变质剂、细化剂的加入量,并将未加变质剂和细化剂的试样、Al-10Sr变质剂加入量为0.3%的试样和Al-5Ti-B细化剂加入量为0.6%的的试样进行热处理。具体挤压铸造成形实验方案,如表1所示。
表1 本文的挤压铸造成形实验方案
Table 1
Sample No. | Pouring temperature/℃ | Die temperature /℃ | Specific pressure /MPa | Dwell time/s | Added master alloy | Quantity /% | Heat treatment status |
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1 | 700 | 250 | 398 | 30 | No | 0 | No T6 |
2 | 700 | 250 | 398 | 30 | Al-10Sr | 0.1 | No T6 |
3 | 700 | 250 | 398 | 30 | Al-10Sr | 0.3 | No T6 |
4 | 700 | 250 | 398 | 30 | Al-10Sr | 3 | No T6 |
5 | 700 | 250 | 398 | 30 | Al-5Ti-B | 0.1 | No T6 |
6 | 700 | 250 | 398 | 30 | Al-5Ti-B | 0.6 | No T6 |
7 | 700 | 250 | 398 | 30 | Al-5Ti-B | 3 | No T6 |
8 | 700 | 250 | 398 | 30 | No | 0 | T6 |
9 | 700 | 250 | 398 | 30 | Al-10Sr | 0.3 | T6 |
10 | 700 | 250 | 398 | 30 | Al-5Ti-B | 0.6 | T6 |
对A356挤压铸造成形件进行T6处理: 固溶温度和时间分别为540℃和4 h,人工时效温度和时间分别为195℃和4 h[40]。
图1给出了A356合金轮毂模拟件的挤压铸造三维结构图和取样位置。将金相试样依次用600 #至2000 #砂纸进行粗磨和精磨,然后用0.5 μm金刚石抛光剂辅助抛光,最后用0.5%的HF水溶液腐蚀试样。用金相显微镜(Olympus GX71)进行金相观察,用岛津电子万能试验机(AG-X plus 20kN)进行拉伸试验,拉伸速度为2 mm/min。使用图像处理软件Image Pro Plus计算金相图的晶粒面积,晶粒的平均直径为
式中
图1
图1
挤压铸造成形件的三维造型图、微观组织和测量力学性能取样位置
Fig.1
Three dimension model of squeeze casting component and locations of samples
2 实验结果
2.1 变质剂对成形件组织性能的影响
图2给出了熔炼时Al-10Sr变质剂的加入量分别为0%、0.1%、0.3%和3%的铝合金液挤压铸造成形制件的微观组织。未加变质剂时共晶硅的形貌为片状和长杆状,构件组织有细小的等轴晶和尺寸较大的蔷薇晶(图2a和图2e)。加入0.1%的Al-10Sr变质剂时共晶硅组织开始细化,部分区域共晶硅细化成蠕虫状,共晶硅尺寸显著减小,但是大部分是短杆状和片状。在硅相被细化的区域附近,出现了细小的球状晶粒(图2b)。加入0.3%的Al-10Sr变质剂时变质效果最好,共晶硅都变质细化为蠕虫状和颗粒状,晶粒的圆整度也比较高;一部分α(Al)晶粒是接近半固态的球晶,晶粒细小圆整,组织致密均匀(图2c和2f)。加入3%的Al-10Sr变质剂时共晶硅的形貌变化不大,但是晶粒严重粗化且尺寸差异很大,发生了过变质,但是共晶硅仍然比未加变质剂时细小(图2d)。图2g给出了晶粒平均尺寸的定量描述。可以看出,未加变质剂前平均晶粒直径为33.7 μm,加入量为0.1%的平均晶粒直径减少到29.7 μm,加入量为0.3%时平均晶粒直径最小(25.8 μm);但是,当加入量为3%时平均晶粒直径增大到32.9 μm;比0.3%时明显增大,但是比未变质构件的平均晶粒尺寸小。
图2
图2
加入不同量变质剂挤压铸造件的微观组织和平均晶粒尺寸
Fig.2
Microstructure and average grain size of squeeze casting component with different addition quantity of Al-10Sr modifier (a) 0, (b) 0.1%, (c) 0.3%, (d) 3%, (e) 0 (1000x), (f) 0.3% (1000x), (g) average grain size
图3给出了熔炼时Al-10Sr变质剂的加入量分别为0、0.1%、0.3%和3%的金属液在浇注温度为700℃、模具温度为250℃、保压30s条件下挤压铸造成形制件的力学性能。由图3可见,加入量为0.1%时制件的力学性能稍有降低。其原因可能是,铝锶变质剂较长的孕育期使合金的元素烧损增多,使力学性能降低。而加入少量变质剂时力学性能提高得不多。加入0.3%的Al-10Sr变质剂时挤压铸造成形件的最优抗拉强度、屈服强度和延伸率分别为221.3 MPa、104.5 MPa和10.3%,分别提高了5.9%、1.5%和20.4%。变质剂加入量为3%的制件其力学性能不如加入量为0.3%的制件,但是与比未加变质剂的制件相比明显提高。
图3
图3
加入不同量Al-10Sr变质剂制件的力学性能
Fig.3
Mechanical properties of squeeze casting component with different addition quantity of Al-10Sr modifier
2.2 细化剂对制件微观组织的影响
图4
图4
加入不同量Al-5Ti-B细化剂挤压铸造件的微观组织和平均晶粒直径
Fig.4
Microstructure and average grain size of squeeze casting component with different addition quantity of Al-5Ti-B refiner (a) 0.1%, (b) 0.6%, (c) 3%, (d) average size of grains
图5
图5
加入不同量细化剂制件的力学性能
Fig.5
Mechanical properties of squeeze casting component with different quantity of Al-5Ti-B refiner
2.3 热处理对制件微观组织和力学性能的影响
图6
图6
热处理前后工程应力-工程应变曲线
Fig.6
Engineering stress-strain curve of squeeze casting component before and after T6
图7
图7
挤压铸造件热处理后的微观组织
Fig.7
Microstructure of squeeze casting component with T6 (a) No.8 sample, (b) No.9 sample, (c) No.10 sample
3 讨论
此外,铝锶合金变质的孕育期较长,加入金属液内后经过20~30 min的孕育期才能发挥作用。其原因是,铝锶合金加入金属液后熔解释放的Sr4Al化合物在金属液内扩散,与Si原子形成新的化合物相Sr2Si2Al,Sr2Si2Al再向金属液释放Sr原子,此时才能起变质作用。如图8的线扫描能谱图所示,多余的Sr存在于晶界中,晶内的含量很小。过多的Sr则以Al4SrSi2的形式存在晶界中,对组织性能的危害较小,可见铝锶变质剂的过变质现象不明显。图8给出了Sr变质对共晶硅形貌的影响。如图8所示,加入Sr变质剂可使共晶硅由变质前的针状或者层片状演变成有大部分颗粒状和少部分蠕虫状的形貌。其中颗粒状共晶硅的尺寸大都小于1 μm,颗粒明显细化,有利于提高挤压铸造件的力学性能。Al-10Sr变质剂能有效细化共晶硅组织,使其由片状和长杆状细化成颗粒状和蠕虫状(图9)。这是变质剂能提高制件力学性能的主要原因,因为变质剂改善了硅相的形貌和分布。
图8
图8
Al-10Sr变质剂加入量为3%制件的组织扫描能谱
Fig.8
SEM image and EDS of squeeze casting component with 3% addition of Al-10Sr modifier (a) SEM image with scanning line, (b) line scanning of Sr element
图9
图9
Al-10Sr变质剂加入量为3%制件的组织点扫描能谱
Fig.9
SEM image and point scanning EDS of squeeze casting component with 3% addition of Al-10Sr modifier (a) SEM image, (b) point A scanning EDS
加入变质剂对抗拉强度没有显著的影响,但是使延伸率显著提高(图3)。加入少量的变质剂时只有部分共晶硅组织细化,所以力学性能提高的幅度小;而过量的变质剂使α-Al组织粗大(图2d、2g),降低变质的效果,并且产生较多的锶化物而降低制件的力学性能。加入质量分数为0.3%的Al-10Sr变质剂,对制件的组织和力学性能有良好作用。加入过量细化剂,使平均晶粒尺寸增大到32.9 μm(图2g)。Al-5Ti-B细化剂对挤压铸造件的细化效果不明显,其原因可能是Al-5Ti-B细化剂的主要作用是细化α-Al。TiB2、TiAl3等粒子作为异质形核核心且细化剂使α-Al相的过冷度提高,两者的共同作用提高了α-Al的形核率[46],因此也细化了晶粒(图4)。铝钛硼细化剂提高制件力学性能的机理是使晶粒细化。晶粒细化使晶界面积增大,有效阻碍位错运动。因为位错难以穿过晶界而只能在晶界前塞积,形成位错墙阻碍后续的位错运动,从而使制件的力学性能提高。晶粒数量增多、尺寸变小使晶界增多且分布更加均匀,提高了阻碍位错的能力,位错墙也增多,因此力学性能提高[47]。Al-5Ti-B细化剂的细化机理是,加入Al-5Ti-B细化剂使TiB2粒子弥散分布在金属液中而TiAl3粒子在TiB2上沉淀析出,然后Al通过包晶反应在TiAl3表面形核。TiAl3粒子容易团聚沉淀从而失去细化作用[48],因此加入过多的细化剂使细化粒子更容易团聚沉淀,其细化效果反而下降。这直接影响挤压铸造成形件的力学性能(图5)。
本文T6处理的A356铝合金挤压铸造件的抗拉强度和延伸率(图6),大于A356压铸件T6处理的261.8 MPa的抗拉强度和4.98%的延伸率[49],也大于低压铸造T6状态的247.5 MPa的抗拉强度和4.72%的延伸率[50],更明显大于T6状态重力铸造的225 MPa的抗拉强度和1%的延伸率[40]。热处理能有效提高制件的强度。其原因是,T6热处理使强化相弥散地分布在基体内,使制件由位错强化转变为弥散强化。热处理前的微观组织中共晶硅形貌是片状和针状(图2a、图2c和图4b),热处理后晶粒粗化明显,共晶硅的形貌也发生显著变化。共晶硅相的尺寸明显减小,并且逐渐球化,呈现出粒状,分布较为均匀,如图7所示。T6热处理中的固溶将Mg2Si强化相溶解于α-Al基体形成过饱和固溶体,再通过时效重新析出。而共晶硅在热处理时不会溶解于基体内再析出,而是聚集球化。共晶硅在热处理时经历熔断和粒化两个阶段,熔断发生在共晶硅分枝、凹陷这些畸变能较高的部位,粒化就是共晶硅逐渐圆钝化,对于重力铸造组织该过程比较长。固溶温度较高时共晶硅中的Al溶解,使共晶硅变成β-Si [51,52]。热处理使Mg2Si强化相均匀地分布在基体内,使制件的强化机制由热处理前的位错强化变成弥散强化,从而使性能显著提高。
图10
图10
挤压铸造成形件热处理后断口的形貌
Fig.10
Fracture morphology of squeeze casting component (a) low-resolution sample 9, (b) high-resolution sample 9, (c) low-resolution sample 10, (d) high-resolution sample 10
图11给出了热处理后制件第二相的透射形貌面扫描能谱图。图11a中白色条状物,就是热处理后的第二相。图11b到f分别给出了Al、Si、Mn、Mg、Fe元素的分布图。可以看到,在第二相上Si元素的含量提高而Al元素则较少,Fe、Mn、Mg元素没有明显的变化,说明第二相的主要元素是Si。A356铸造铝合金时效经历四个阶段: 由固溶后的过饱和固溶体α-Al相转变为G.P区,G.P区为强化相析出的异质形核,是溶解元素的富集区。β″、 β′和β分别是在G.P区析出的强化相,其中针状β″相是主要析出相,对力学性能的强化效果最好;杆状β′相是过时效时析出的亚稳相,其强化效果略差;盘状β相是平衡相,使强化效果减弱。图12a给出了强化相的透射形貌,可见析出的强化相其尺寸只有5 nm左右。图12b给出了强化相的选区电子衍射斑点,可见排列整齐的十字花样。对该花样斑点进行标定,晶面距离为0.1348 nm,其晶带轴为[0 0 1],确定该强化相为Mg2Si。
图11
图11
热处理后制件晶界的透射电镜形貌
Fig.11
TEM image (a) and EDS mapping images (b) Al, (c) Si, (d) Mn, (e) Mg, (f) Fe
图12
图12
强化相透射电镜形貌和选区电子衍射斑点
Fig.12
TEM image and selected area electron diffraction (SAED) (a) TEM dark field image, (b) SAED
4 结论
(1) Al-10Sr变质剂对挤压铸造件的共晶Si的形貌、α(Al)的尺寸和力学性能有明显的影响。当Al-10Sr变质剂加入量分别为0.1%、0.3%和3%时,共晶Si的形貌由片状和长杆状变为颗粒状和蠕虫状,α-Al的晶粒尺寸先减少后增大。Al-10Sr变质剂的加入量为0.3%时铸造件最佳的抗拉强度、屈服强度和延伸率分别为221.3 MPa、104.5 MPa和10.3%,比未加入变质剂分别提高了5.9%、1.5%和20.4%。其主要原因是: Al-10Sr变质剂使铝合金的熔点、增大熔体的过冷和形核率提高,使α-Al的晶粒细化;Al-10Sr变质剂还使Si的生长方向改变,影响了共晶硅的形貌。
(2) 加入0.1%、0.6%和3%的Al-5Ti-B细化剂时,铸造件的晶粒平均直径分别为32. 9 μm、31.6 μm和51.7 μm。当加入0.6%的Al-5Ti-B细化剂时,铸造件的晶粒尺寸比于未加细化剂时减小了2.3%和6.2%。随着Al-5Ti-B细化剂加入量的增加,挤压铸造成形件的力学性能先增加后降低。加入量为0.6%时最优的抗拉强度、屈服强度和延伸率分别为215.6 MPa、106.6 MPa和9.0%,比未加入变质剂分别提高了3.3%、3.6%和5.1%。Al-5Ti-B细化剂对力学性能的影响,是通过对α-Al晶粒尺寸的影响实现的。但是,加入过量的细化剂使α-Al的晶粒尺寸的增加和力学性能的下降,这与TiAl3粒子的析出和团聚沉淀有关。
(3) 经过T6热处理(固溶540℃/4 h+时效190℃/4 h)、未变质细化和已变质细化的A356挤压铸造件,其强度显著提高、延伸率稍有降低。用Al-5Ti-B细化处理的挤压铸造件热处理后其力学性能为: 屈服强度为239.3 MPa,抗拉强度为297.5 MPa,延伸率为8.0%。共晶硅的球化和细化、构件成分均匀化以及Mg2Si强化相在基体中弥散析出,是T6热处理使挤压铸造成形件力学性能提高的主要原因。
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