CN103225028A - Al-Er-Zr-Si heat-resistant aluminum alloy and its heat treatment technology - Google Patents

Al-Er-Zr-Si heat-resistant aluminum alloy and its heat treatment technology Download PDF

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CN103225028A
CN103225028A CN2013100849305A CN201310084930A CN103225028A CN 103225028 A CN103225028 A CN 103225028A CN 2013100849305 A CN2013100849305 A CN 2013100849305A CN 201310084930 A CN201310084930 A CN 201310084930A CN 103225028 A CN103225028 A CN 103225028A
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聂祚仁
田舒
文胜平
高坤元
黄晖
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Beijing University of Technology
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Abstract

The invention relates to an Al-Er-Zr-Si heat-resistant aluminum alloy and its heat treatment technology, and belongs to the technical field of alloys. 0.05-0.25wt% of Er, 0.2-0.3wt% of Zr, 0.01-0.2wt% of Si and other inevitable impurities are added to a pure aluminum matrix. The solid solution ageing heat treatment technology of the alloy comprises a step of solid solution at 630-650DEG C for 20-30h, a step of water quenching to room temperature, and a step of isothermal ageing at 350DEG C. The Al-Er-Zr-Si heat-resistant aluminum alloy has a very substantial ageing reinforcement effect because of the composite micro-alloying of Er, Zr and Si, has a higher ageing reinforcement speed and a higher peak value hardness than an Al-Er-Zr alloy, and has a good heat resistance.

Description

一种Al-Er-Zr-Si耐热铝合金及其热处理工艺A kind of Al-Er-Zr-Si heat-resistant aluminum alloy and its heat treatment process

技术领域technical field

本发明涉及一种微合金化的铝合金材料及其热处理工艺,属于金属合金技术领域。The invention relates to a micro-alloyed aluminum alloy material and a heat treatment process thereof, belonging to the technical field of metal alloys.

技术背景technical background

耐热铝合金是指在高温下有足够的抗氧化性和在温度和载荷(动态和静态)的长时间作用下,具有抗塑性变形(蠕变)和破坏能力及导热性好和密度低等特点。在兵器、船舶、航空、航天、汽车等行业得到广泛应用,如坦克装甲车辆发动机的活塞、缸套、连杆、箱体、缸盖,导弹壳体、尾翼、航空发动机汽缸、叶片、飞机蒙皮等。Heat-resistant aluminum alloy means that it has sufficient oxidation resistance at high temperature and has resistance to plastic deformation (creep) and damage, good thermal conductivity and low density under long-term action of temperature and load (dynamic and static). features. It is widely used in weapons, ships, aviation, aerospace, automobile and other industries, such as pistons, cylinder liners, connecting rods, boxes, cylinder heads of tank armored vehicle engines, missile shells, empennages, aeroengine cylinders, blades, aircraft covers leather etc.

提高铝合金的耐热性能关键是要使合金中析出形成大量弥散分布的热稳定性析出相(在较高的温度条件下长大和粗化缓慢,而且部分发生结构转变)。近年来,国内外大量学者对稀土元素在铝合金的耐热性能的作用做了大量的研究。这些研究主要集中在La、Ce、Y、Sc、Zr和混合稀土对铝合金的影响,其中对稀土元素Sc研究最为深入,在Al-Si系、Al-Zn-Mg系及Al-Mg系等铝合金中添加Sc均取得了令人满意的研究结果。然而,添加Sc大大增加了铝合金的生产成本,使含Sc铝合金在工业中的应用受到了限制。将Er加入到铝合金中,能生成与Al3Sc作用相同的L12结构的Al3Er相,可以提高铝合金的再结晶温度,更能有效的起到细晶强化和弥散强化等积极作用,提高铝合金的综合使用性能。而且Er的价格比较便宜,在铝合金中添加少量的Er元素不会大幅度提高生产成本,能够广泛应用于工业生产中。The key to improving the heat resistance of aluminum alloys is to precipitate and form a large number of dispersed thermally stable precipitates in the alloy (it grows slowly and coarsens slowly under higher temperature conditions, and some structural transformations occur). In recent years, a large number of scholars at home and abroad have done a lot of research on the role of rare earth elements in the heat resistance of aluminum alloys. These studies mainly focus on the effects of La, Ce, Y, Sc, Zr and mixed rare earths on aluminum alloys, among which the rare earth element Sc is the most in-depth research, in Al-Si system, Al-Zn-Mg system and Al-Mg system, etc. The addition of Sc to aluminum alloys has achieved satisfactory research results. However, the addition of Sc greatly increases the production cost of aluminum alloys, which limits the industrial application of Sc-containing aluminum alloys. Adding Er to the aluminum alloy can generate the Al 3 Er phase with the same L1 2 structure as Al 3 Sc, which can increase the recrystallization temperature of the aluminum alloy, and can effectively play a positive role in fine grain strengthening and dispersion strengthening. , Improve the comprehensive performance of aluminum alloy. Moreover, the price of Er is relatively cheap. Adding a small amount of Er element in aluminum alloy will not greatly increase the production cost, and can be widely used in industrial production.

然而,在常规铸锭冶金的凝固过程中Er在铝合金中的固溶度有限,限制了其作用的进一步提高。通过复合添加其它能够生成L12结构析出相的合金元素有可能提高析出密度,从而进一步发挥合金化的作用。除了Sc以外,Zr是一种能够生成亚稳L12结构析出相的合金元素,Zr和Er复合微合金化后,在Al3Er相的诱导下有可能使得析出相保持稳定的L12结构,而且可以阻碍Al3Er相的长大和粗化,因此可以获得良好的强化效果和热稳定性,例如发明专利ZL201010515843.7所描述的一种Al-Er-Zr合金具有显著的时效强化效果。但是Zr本身的析出过程非常缓慢,尤其是成份较低的情况下需要几千个小时才能充分析出,Si的添加能够促进Zr的析出,因此Er,Zr和Si的复合有可能充分发挥各自的作用,起到更加良好的微合金化效果。本发明正是在基于以上考虑的情况下,设计了Al-Er-Zr-Si合金,寻找其合适的成份范围和相应的热处理工艺。However, the solid solubility of Er in aluminum alloys is limited during the solidification process of conventional ingot metallurgy, which limits the further improvement of its effect. It is possible to increase the precipitation density by adding other alloying elements capable of forming L1 2 structure precipitates, thereby further exerting the effect of alloying. In addition to Sc, Zr is an alloying element that can form metastable L1 2 structure precipitates. After Zr and Er composite microalloying, it is possible to make the precipitates maintain a stable L12 structure under the induction of Al 3 Er phase, and It can hinder the growth and coarsening of the Al 3 Er phase, so good strengthening effect and thermal stability can be obtained. For example, an Al-Er-Zr alloy described in the invention patent ZL201010515843.7 has a significant aging strengthening effect. However, the precipitation process of Zr itself is very slow, especially when the composition is low, it takes thousands of hours to fully separate out. The addition of Si can promote the precipitation of Zr, so the combination of Er, Zr and Si may give full play to their respective effects , Play a better microalloying effect. The present invention designs the Al-Er-Zr-Si alloy based on the above considerations, and seeks its suitable composition range and corresponding heat treatment process.

发明内容Contents of the invention

本发明的目的在于通过复合微合金化的方法,寻找Er,Zr,Si协同发挥强化作用的规律,从而提高铝合金的性能。The purpose of the present invention is to find out the law of Er, Zr and Si synergistically exerting strengthening effect through the method of composite microalloying, so as to improve the performance of aluminum alloy.

本发明所提供的Al‐Er‐Zr‐Si耐热铝合金,其特征在于,纯铝基体中加入了0.05~0.25%(重量百分比)的Er,0.2~0.3%(重量百分比)的Zr,0.01~0.2%(重量百分比)的Si,以及其它不可避免的杂质。The Al-Er-Zr-Si heat-resistant aluminum alloy provided by the present invention is characterized in that 0.05-0.25% (weight percentage) of Er, 0.2-0.3% (weight percentage) of Zr, 0.01 ~0.2% (weight percent) of Si, and other unavoidable impurities.

进一步优选纯铝基体中加入了0.15~0.25%(重量百分比)的Er,0.25~0.3%(重量百分比)的Zr,0.05~0.15%(重量百分比)的Si。It is further preferred that 0.15-0.25% (weight percent) of Er, 0.25-0.3 (weight percent) of Zr, and 0.05-0.15 (weight percent) of Si are added to the pure aluminum matrix.

该合金的制备方法是在熔炼铝的过程中加入AlEr和AlZr中间合金实现的,或进一步加入铝硅合金,调节合金的元素,熔炼温度为780±10℃,到达熔炼温度后保温30分钟,然后用铁模浇铸。The preparation method of the alloy is realized by adding AlEr and AlZr intermediate alloys in the process of smelting aluminum, or further adding aluminum-silicon alloys to adjust the elements of the alloys. The melting temperature is 780±10°C. Cast in iron molds.

铸锭随后进行固溶时效热处理,其工艺包括以下步骤:首先在630±10℃固溶20~30小时,随后水淬到室温,然后在350℃等温时效。优选350℃等温时效的保温时间10分钟-1000小时,更优选1-100小时。The cast ingot is then subjected to solid solution aging heat treatment, and the process includes the following steps: firstly solid solution at 630±10°C for 20 to 30 hours, then water quenched to room temperature, and then isothermally aged at 350°C. Preferably, the holding time for isothermal aging at 350° C. is 10 minutes to 1000 hours, more preferably 1 to 100 hours.

本发明由于采用了Er、Si和Zr复合微合金化,具有非常显著且较快速的时效强化效果,如附图1所示,Al-0.2Er-0.28Zr-0.1Si(S3号样)和Al-0.2Er-0.28Zr-0.2Si(S4号样)相对Al-Er-Zr(S1、S2)合金提高了时效强化效果的速度和峰值硬度,而且该合金具有良好的耐热性能。Because the present invention has adopted Er, Si and Zr composite micro-alloying, there is very remarkable and faster aging strengthening effect, as shown in accompanying drawing 1, Al-0.2Er-0.28Zr-0.1Si (S3 sample) and Al Compared with Al-Er-Zr (S1, S2) alloy, -0.2Er-0.28Zr-0.2Si (S4 sample) improves the speed of aging strengthening effect and peak hardness, and the alloy has good heat resistance.

附图说明Description of drawings

图1:350℃等温时效曲线;Figure 1: 350°C isothermal aging curve;

图2:S4合金的短时(1h)耐热性能曲线;Figure 2: Short-term (1h) heat resistance curve of S4 alloy;

图3:S4合金固溶态及时效态高温压缩强度。Figure 3: High-temperature compressive strength of S4 alloy in solid solution state and aging state.

具体实施方式Detailed ways

实例1:采用石墨坩埚熔炼和铁模铸造制备合金铸锭,所用原料为纯铝和Al-6Er,Al-4Zr,Al-20Si中间合金,熔炼温度为780±10℃。到达熔炼温度后保温30分钟,然后用铁模浇铸。制备了5种不同设计成份的合金,并通过XRF测试了其实际成分,如下表1所示。Example 1: The alloy ingot is prepared by melting in a graphite crucible and casting in an iron mold. The raw materials used are pure aluminum and Al-6Er, Al-4Zr, Al-20Si master alloy, and the melting temperature is 780±10°C. After reaching the melting temperature, keep it warm for 30 minutes, and then cast it with an iron mold. Five alloys with different design compositions were prepared, and their actual compositions were tested by XRF, as shown in Table 1 below.

表1实验合金成份Table 1 Experimental alloy composition

样品sample 设计成份(wt.%)Design composition (wt.%) Er实际成份Er actual composition Zr实际成份The actual composition of Zr Si实际成份Si actual composition

(wt.%)(wt.%) (wt.%)(wt.%) (wt.%)(wt.%) S1S1 Al-0.2Er-0.15ZrAl-0.2Er-0.15Zr 0.180.18 0.200.20 0.010.01 S2S2 Al-0.2Er-0.28ZrAl-0.2Er-0.28Zr 0.210.21 0.300.30 0.010.01 S3S3 Al-0.2Er-0.28Zr-0.1SiAl-0.2Er-0.28Zr-0.1Si 0.250.25 0.290.29 0.110.11 S4S4 Al-0.2Er-0.28Zr-0.2SiAl-0.2Er-0.28Zr-0.2Si 0.190.19 0.280.28 0.150.15 S5S5 Al-0.1Er-0.28Zr-0.2SiAl-0.1Er-0.28Zr-0.2Si 0.050.05 0.300.30 0.200.20

实例2:对实例1中的合金在640±10℃固溶20小时,水淬到室温,然后在350℃等温时效。图1给出了等温时效的硬度变化曲线,从图中可以看到S3和S4号样的最大硬度值要高于S2号试样,而且其达到硬度峰值的时间要快于S2号。虽然S2,S3,S4的Er、Zr成分比较接近,但S3和S4相对S2样品添加了Si,而S2中的0.01%的Si是纯铝中的杂质。这说明Er、Zr、Si复合添加能够加速析出相形成过程,而且能够提高析出相密度以至于提高合金的硬度。Example 2: The alloy in Example 1 was solid-dissolved at 640±10°C for 20 hours, water quenched to room temperature, and then aged at 350°C. Figure 1 shows the hardness change curve of isothermal aging. It can be seen from the figure that the maximum hardness values of samples S3 and S4 are higher than those of sample S2, and the time to reach the peak hardness is faster than that of sample S2. Although the Er and Zr components of S2, S3, and S4 are relatively close, Si is added to S3 and S4 relative to S2, and 0.01% of Si in S2 is an impurity in pure aluminum. This shows that the compound addition of Er, Zr and Si can accelerate the formation process of precipitates, and can increase the density of precipitates so as to improve the hardness of the alloy.

实例3:对实例1中S4号合金在635±10℃均匀化处理20小时,水淬到室温,然后在350℃等温时效100小时,之后采用冷轧方式轧制变形量为70%;轧制后在200~600℃退火1小时,其硬度变化如图2所示,可见在200~375℃温度范围内,合金的硬度几乎没有明显下降,375℃以上温度合金硬度才有显著的下降,这表明合金的再结晶温度在400℃左右,具有良好的耐热性能。Example 3: Homogenize alloy S4 in Example 1 at 635±10°C for 20 hours, water quench to room temperature, and then age at 350°C for 100 hours, and then use cold rolling to roll with a deformation of 70%; rolling After annealing at 200-600°C for 1 hour, the change in hardness is shown in Figure 2. It can be seen that within the temperature range of 200-375°C, the hardness of the alloy hardly decreases significantly, and the hardness of the alloy decreases significantly at temperatures above 375°C. It shows that the recrystallization temperature of the alloy is about 400℃, and it has good heat resistance.

实例4:对实例1中S4号合金在635±10℃均匀化处理20小时,水淬到室温,然后在350℃等温时效100小时,之后分别采用高温压缩变形试验(采用Gleeble3500进行等轴压缩试验),试验温度为300℃,应变速率应变速率范围为10-3-50s-1,试样以5℃/s的加热速度升至试验温度,保温3分钟,然后开始变形,压缩总应变为0.6。其固溶态及时效态高温压缩强度如图3所示,可见在300℃,相同应变速率下,S4时效态合金流变应力高于S4固溶态合金,即S4时效态合金高温强度高于S4固溶态合金。Example 4: Homogenize alloy S4 in Example 1 at 635±10°C for 20 hours, water quench to room temperature, and then age at 350°C for 100 hours. ), the test temperature is 300°C, the strain rate strain rate range is 10 -3 -50s -1 , the sample is heated up to the test temperature at a heating rate of 5°C/s, kept for 3 minutes, and then begins to deform, the total compression strain is 0.6 . Its high-temperature compressive strength in solid solution state and aging state is shown in Figure 3. It can be seen that at 300 °C and at the same strain rate, the flow stress of the S4 aging state alloy is higher than that of the S4 solid solution state alloy, that is, the high temperature strength of the S4 aging state alloy is higher than that of the S4 aging state alloy. S4 solid solution alloy.

Claims (6)

1. Al-Er-Zr-Si heat-resisting aluminium alloy, it is characterized in that, added the 0.05-0.25%(weight percent in the pure aluminum substrate) Er, the 0.2-0.3%(weight percent) Zr, the 0.01-0.2%(weight percent) Si, and other unavoidable impurities.
2. a kind of Al-Er-Zr-Si heat-resisting aluminium alloy of claim 1 is characterized in that, has added 0.15~0.25%(weight percent in the pure aluminum substrate) Er, 0.25~0.3%(weight percent) Zr, 0.05~0.15%(weight percent) Si.
3. the method for preparing the described aluminium alloy of claim 1, it is characterized in that, adding AlEr and AlZr master alloy are realized in the process of melting aluminium, or further add aluminum silicon alloy, regulate the element of alloy, smelting temperature is 780 ± 10 ℃, arrives behind the smelting temperature insulation 30 minutes, then with the swage casting and carry out solid-solution and aging heat treatment.
4. claim 1 Al-Er-Zr-Si heat-resisting aluminium alloy solid-solution and aging heat treatment method is characterized in that: at first at 630 ± 10 ℃ of solid solution 20-30 hours, shrend subsequently is to room temperature, then at 350 ℃ of isothermal agings.
5. according to the method for claim 4, it is characterized in that the soaking time of 350 ℃ of isothermal agings 10 minutes-1000 hours.
6. according to the method for claim 4, it is characterized in that the soaking time 1-100 of 350 ℃ of isothermal agings hour.
CN2013100849305A 2013-03-15 2013-03-15 Al-Er-Zr-Si heat-resistant aluminum alloy and its heat treatment technology Pending CN103225028A (en)

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104561669A (en) * 2014-12-27 2015-04-29 北京工业大学 Heat treatment process of Al-Er-Zr-Si alloy
CN105478746A (en) * 2015-12-08 2016-04-13 艾瑞福斯特(北京)技术开发有限公司 Heat-resisting aluminum alloy powder for engine
CN111500846A (en) * 2020-05-09 2020-08-07 贵州永红航空机械有限责任公司 Heat treatment method of welded closed impeller
CN112853162A (en) * 2021-01-07 2021-05-28 中铝材料应用研究院有限公司 High-conductivity heat-resistant aluminum alloy and preparation method thereof
CN113684403A (en) * 2021-08-17 2021-11-23 北京工业大学 A kind of high-strength aluminum alloy powder for 3D printing and preparation method thereof

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JPS57110645A (en) * 1980-12-26 1982-07-09 Sumitomo Electric Ind Ltd Electrically conductive and heat resistant aluminum alloy
CN102021443A (en) * 2010-10-15 2011-04-20 北京工业大学 Al-Er-Zr alloy and ageing strengthening process thereof

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Publication number Priority date Publication date Assignee Title
JPS57110645A (en) * 1980-12-26 1982-07-09 Sumitomo Electric Ind Ltd Electrically conductive and heat resistant aluminum alloy
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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104561669A (en) * 2014-12-27 2015-04-29 北京工业大学 Heat treatment process of Al-Er-Zr-Si alloy
CN105478746A (en) * 2015-12-08 2016-04-13 艾瑞福斯特(北京)技术开发有限公司 Heat-resisting aluminum alloy powder for engine
CN111500846A (en) * 2020-05-09 2020-08-07 贵州永红航空机械有限责任公司 Heat treatment method of welded closed impeller
CN112853162A (en) * 2021-01-07 2021-05-28 中铝材料应用研究院有限公司 High-conductivity heat-resistant aluminum alloy and preparation method thereof
CN113684403A (en) * 2021-08-17 2021-11-23 北京工业大学 A kind of high-strength aluminum alloy powder for 3D printing and preparation method thereof

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Application publication date: 20130731