CN105039817B - The preparation method and multicomponent heat-resistant magnesium alloy of a kind of multicomponent heat-resistant magnesium alloy - Google Patents
The preparation method and multicomponent heat-resistant magnesium alloy of a kind of multicomponent heat-resistant magnesium alloy Download PDFInfo
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- 238000002360 preparation method Methods 0.000 title claims abstract description 36
- 238000010438 heat treatment Methods 0.000 claims abstract description 107
- 238000001816 cooling Methods 0.000 claims abstract description 43
- 238000000034 method Methods 0.000 claims abstract description 24
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 21
- 239000011777 magnesium Substances 0.000 claims abstract description 18
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- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical group [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims abstract description 3
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Abstract
本发明公开了一种多元耐热镁合金的制备方法及多元耐热镁合金。该方法包括以下步骤:1)所述铸态镁合金由以下质量百分比的组分组成:Al 7.5~8.5%,Zn 0.8~1.2%,RE 1.2~2.4%,Ca 0.5~1.4%,余量为镁和杂质;将铸态镁合金进行一级热处理,一级热处理温度为420~440℃,时间为4~6h,随炉冷却;2)进行二级热处理,二级热处理温度为390~410℃,时间为8~10小时,水冷;3)进行三级热处理,三级热处理温度为200~220℃,时间为12~15小时,空冷,即得。本发明提供的热处理方法,通过两级固溶处理,使镁合金的显微组织得到优化,从而提高了镁合金的最终力学性能。
The invention discloses a preparation method of a multi-element heat-resistant magnesium alloy and the multi-element heat-resistant magnesium alloy. The method comprises the following steps: 1) the cast magnesium alloy is composed of the following components in mass percentage: Al 7.5-8.5%, Zn 0.8-1.2%, RE 1.2-2.4%, Ca 0.5-1.4%, and the balance is Magnesium and impurities; the as-cast magnesium alloy is subjected to primary heat treatment at a temperature of 420-440°C for 4-6 hours and cooled with the furnace; 2) secondary heat treatment is performed at a temperature of 390-410°C , the time is 8-10 hours, water cooling; 3) carry out three-stage heat treatment, the temperature of the three-stage heat treatment is 200-220 ℃, the time is 12-15 hours, air-cooling, to obtain. The heat treatment method provided by the invention optimizes the microstructure of the magnesium alloy through two-stage solid solution treatment, thereby improving the final mechanical properties of the magnesium alloy.
Description
技术领域technical field
本发明属于金属材料冶金及热处理技术领域,具体涉及一种多元耐热镁合金的制备方法及多元耐热镁合金。The invention belongs to the technical field of metallurgy and heat treatment, and in particular relates to a preparation method of a multi-element heat-resistant magnesium alloy and the multi-element heat-resistant magnesium alloy.
背景技术Background technique
镁合金作为最轻的金属结构材料,具有高的比强度和比刚度、优异的铸造性能、机械加工性能,有着非常广泛的应用前景。近年来镁合金在汽车上应用日益增多,汽车采用镁合金可以减重,同时减少了尾气排放,因此镁合金的研究开发对于节约能源、抑制环境污染有着重要意义。As the lightest metal structural material, magnesium alloy has high specific strength and specific stiffness, excellent casting performance and machining performance, and has a very wide application prospect. In recent years, magnesium alloys have been increasingly used in automobiles. The use of magnesium alloys in automobiles can reduce weight and reduce exhaust emissions. Therefore, the research and development of magnesium alloys is of great significance for saving energy and suppressing environmental pollution.
Mg-Al-Zn系镁合金(如AZ31、AZ61、AZ91等)是目前工业上应用最为广泛的镁合金系列。此系列镁合金兼有良好的强度、塑性、耐腐蚀性以及低廉的成本等优点。但它本身存在着难以克服的缺点:首先,铸态Mg-Al-Zn系镁合金中Mg17Al12相以离异共晶的形式呈网状沿晶界析出,这些粗大的Mg17Al12相的存在不利于合金的力学性能。此外,当工作温度高于120℃以后,此系列合金中的主要强化相Mg17Al12会发生粗化或软化,使得其对基体的强化作用大幅度降低,从而降低了此系列镁合金在高温下的力学性能,限制了Mg-Al-Zn系镁合金的应用范围。Mg-Al-Zn series magnesium alloys (such as AZ31, AZ61, AZ91, etc.) are currently the most widely used magnesium alloy series in industry. This series of magnesium alloys has the advantages of good strength, plasticity, corrosion resistance and low cost. But it has its own insurmountable shortcomings: First, the Mg 17 Al 12 phase in the as-cast Mg-Al-Zn series magnesium alloy precipitates in the form of a dissociated eutectic network along the grain boundaries, and these coarse Mg 17 Al 12 phases The presence of is detrimental to the mechanical properties of the alloy. In addition, when the working temperature is higher than 120 °C, the main strengthening phase Mg 17 Al 12 in this series of alloys will be coarsened or softened, so that its strengthening effect on the matrix is greatly reduced, thereby reducing the high temperature performance of this series of magnesium alloys. The lower mechanical properties limit the application range of Mg-Al-Zn series magnesium alloys.
添加合金元素是提高镁合金性能的有效途径之一。向Mg-Al-Zn系镁合金中主要添加的合金元素主要有三类:①Ca、Sr等碱土元素;②稀土元素RE;③第Ⅳ、Ⅴ族元素,如Si、Sn、Sb、Bi等。这些合金元素在为镁合金提供新的性能的同时,也对镁合金的热处理方法提出了更高的要求。由于Mg-Al-Zn系镁合金的特殊性,常规的热处理工艺难以有效改善镁合金的偏析及析出相的均匀性,且合金组织中容易出现缩松和气孔等组织缺陷,进而影响了镁合金的力学性能。Adding alloying elements is one of the effective ways to improve the properties of magnesium alloys. There are three main types of alloying elements added to Mg-Al-Zn series magnesium alloys: ① Alkaline earth elements such as Ca and Sr; ② Rare earth elements RE; ③ Group IV and V elements, such as Si, Sn, Sb, Bi, etc. While these alloying elements provide new properties for magnesium alloys, they also put forward higher requirements for the heat treatment methods of magnesium alloys. Due to the particularity of Mg-Al-Zn series magnesium alloys, conventional heat treatment processes are difficult to effectively improve the segregation of magnesium alloys and the uniformity of precipitated phases, and structural defects such as shrinkage porosity and pores are prone to appear in the alloy structure, which in turn affects the quality of magnesium alloys. mechanical properties.
专利CN103469039A公开了一种含钙和稀土钐的镁-铝-锌变形镁合金,其质量百分含量为Al 5.3~6.0%,Zn 0.7~1.0%,Ca 0.4~0.5%,Sm 0.2~1.5%,余量为Mg;通过原料熔化,盐浴快冷,得到的合金锭子在400℃下均匀化退火空冷至室温,360℃挤压比为25:1进行热挤压,得到含钙、稀土钐的镁-铝-锌变形镁合金。该镁合金通过热挤压变形后,合金相细化,材料的抗拉强度、屈服强度和延伸率均得到提高。但热挤压工艺需要特定的挤压设备,且对材料的尺寸、形状都有限制;同时,热挤压过程常伴有较严重的氧化和脱碳等加热缺陷,影响了挤压件的尺寸精度和表面粗糙度;上述特点影响了该工艺在工业生产中的大规模应用。Patent CN103469039A discloses a magnesium-aluminum-zinc deformed magnesium alloy containing calcium and rare earth samarium, its mass percentage content is Al 5.3-6.0%, Zn 0.7-1.0%, Ca 0.4-0.5%, Sm 0.2-1.5% , the balance is Mg; through the melting of raw materials and quick cooling in salt bath, the obtained alloy ingot is homogenized and annealed at 400°C and air-cooled to room temperature, and hot-extruded at 360°C with an extrusion ratio of 25:1 to obtain calcium and rare earth samarium magnesium-aluminum-zinc wrought magnesium alloy. After the magnesium alloy is deformed by hot extrusion, the alloy phase is refined, and the tensile strength, yield strength and elongation of the material are all improved. However, the hot extrusion process requires specific extrusion equipment, and has limitations on the size and shape of the material; at the same time, the hot extrusion process is often accompanied by heating defects such as serious oxidation and decarburization, which affects the size of the extrusion Precision and surface roughness; the above characteristics affect the large-scale application of this process in industrial production.
开发一种设备简单,成本较低,安全可靠,操作方便的热处理方法对于Mg-Al-Zn系镁合金具有重要作用。热处理可以有效减少铸件内应力,消除合金组织中的偏析,使非平衡相溶解于基体中,使合金成分均匀化,当合金元素的固溶度随温度变化而变化时,通过固溶处理可显著提高镁合金性能。Mg-Al-Zn系铸造镁合金的热处理一般包括固溶处理和时效处理两个步骤,其中固溶处理是合金后续时效处理的基础和关键,如何通过工艺控制获得良好的固溶效果对于Mg-Al-Zn系合金的热处理强化显得尤为关键。固溶处理需较好地控制处理温度和处理上时间,若温度过高或加热时间过长,会使得组织长大粗化,浪费热量;若温度过低或加热时间过短,合金元素溶解不足,影响其力学性能。因此,如何优化镁合金的热处理工艺,研究开发新型镁合金热处理方法对于最大限度地发挥铸造Mg-Al-Zn系合金的强化作用显得尤为重要。The development of a heat treatment method with simple equipment, low cost, safety, reliability, and convenient operation plays an important role for Mg-Al-Zn series magnesium alloys. Heat treatment can effectively reduce the internal stress of the casting, eliminate segregation in the alloy structure, dissolve the non-equilibrium phase in the matrix, and homogenize the alloy composition. When the solid solubility of alloy elements changes with temperature, the solid solution treatment can significantly Improve the performance of magnesium alloy. The heat treatment of Mg-Al-Zn cast magnesium alloys generally includes two steps of solution treatment and aging treatment, among which solution treatment is the basis and key of subsequent aging treatment of the alloy. How to obtain a good solution effect through process control is very important for Mg- The heat treatment strengthening of Al-Zn alloys is particularly critical. Solution treatment needs to control the treatment temperature and treatment time well. If the temperature is too high or the heating time is too long, the structure will grow and coarsen, wasting heat; if the temperature is too low or the heating time is too short, the alloying elements will not dissolve enough , affecting its mechanical properties. Therefore, how to optimize the heat treatment process of magnesium alloys and research and development of new heat treatment methods for magnesium alloys is particularly important for maximizing the strengthening effect of cast Mg-Al-Zn alloys.
发明内容Contents of the invention
本发明的目的是提供一种多元耐热镁合金的制备方法,解决现有技术中Mg-Al-Zn系镁合金因偏析和析出相分布均匀性差导致镁合金力学性能差的技术问题。The purpose of the present invention is to provide a method for preparing a multi-component heat-resistant magnesium alloy, which solves the technical problem of poor mechanical properties of the magnesium alloy due to segregation and poor uniformity of precipitated phase distribution in the prior art.
本发明的第二个目的是提供一种由上述制备方法得到的多元耐热镁合金。The second object of the present invention is to provide a multi-component heat-resistant magnesium alloy obtained by the above preparation method.
为了实现以上目的,本发明所采用的技术方案是:In order to achieve the above object, the technical solution adopted in the present invention is:
一种多元耐热镁合金的制备方法,包括以下步骤:A method for preparing a multi-component heat-resistant magnesium alloy, comprising the following steps:
1)将铸态镁合金进行一级热处理,所述一级热处理温度为420~440℃,热处理时间为4~6h,冷却;所述铸态镁合金由以下质量百分比的组分组成:Al 7.5~8.5%,Zn 0.8~1.2%,RE 1.2~2.4%,Ca 0.5~1.4%,余量为镁和杂质;1) The as-cast magnesium alloy is subjected to primary heat treatment, the temperature of the primary heat treatment is 420-440°C, the heat treatment time is 4-6h, and cooled; the as-cast magnesium alloy is composed of the following components in mass percentage: Al 7.5 ~8.5%, Zn 0.8~1.2%, RE 1.2~2.4%, Ca 0.5~1.4%, the balance is magnesium and impurities;
2)将步骤1)冷却后的镁合金进行二级热处理,所述二级热处理温度为390~410℃,热处理时间为8~10小时,冷却;2) performing secondary heat treatment on the magnesium alloy cooled in step 1), the temperature of the secondary heat treatment is 390-410°C, the heat treatment time is 8-10 hours, and then cooled;
3)将步骤2)冷却后的镁合金进行三级热处理,所述三级热处理温度为200~220℃,热处理时间为12~15小时,冷却,即得。3) The magnesium alloy cooled in step 2) is subjected to tertiary heat treatment, the temperature of the tertiary heat treatment is 200-220° C., the heat treatment time is 12-15 hours, and cooling is obtained.
步骤1)中,RE为Gd、Y、Nd、Sm中任意一种。In step 1), RE is any one of Gd, Y, Nd, and Sm.
杂质为Fe、Cu和Ni,总量小于0.2wt%。The impurities are Fe, Cu and Ni, and the total amount is less than 0.2wt%.
上述多元耐热镁合金的制备方法中,一级热处理和二级热处理为固溶处理步骤,三级热处理为时效处理步骤。固溶处理通过将合金加热至高温单相区并恒温保持,使过剩相充分溶于固溶体中,再通过冷却得到过饱和固溶体;本发明提供的热处理方法,通过两级固溶处理,避免了合金元素溶解不足或合金组织长大粗化的弊病,使合金析出相分布均匀,合金组织得到优化,从而提高了镁合金的最终力学性能。合金组分中,Ca在镁合金中具有良好的晶粒细化和抗氧化作用,能够细化镁合金基体组织从而提高镁合金强度和塑性;在Mg-Al系镁合金中少量的Ca会固溶进Mg17Al12相中提高其热稳定性,且Ca易与Al形成高温稳定的Al-Ca相从而提高合金高温性能。稀土元素RE加入镁合金中具有固溶强化和第二相强化效果,从而改善合金机械性能。此外,本发明提供的热处理方法具有所用设备简单,成本较低,安全可靠,操作方便的优点,适合大规模工业化生产应用。In the preparation method of the above multi-component heat-resistant magnesium alloy, the primary heat treatment and the secondary heat treatment are solid solution treatment steps, and the tertiary heat treatment is an aging treatment step. Solution treatment heats the alloy to a high-temperature single-phase region and maintains it at a constant temperature, so that the excess phase is fully dissolved in the solid solution, and then a supersaturated solid solution is obtained by cooling; the heat treatment method provided by the invention avoids the alloy Insufficient dissolution of elements or the growth and coarsening of the alloy structure make the alloy precipitates evenly distributed and the alloy structure is optimized, thereby improving the final mechanical properties of the magnesium alloy. Among the alloy components, Ca has good grain refinement and anti-oxidation effects in magnesium alloys, and can refine the matrix structure of magnesium alloys to improve the strength and plasticity of magnesium alloys; a small amount of Ca in Mg-Al series magnesium alloys will solidify Dissolving into the Mg 17 Al 12 phase improves its thermal stability, and Ca easily forms a high-temperature stable Al-Ca phase with Al to improve the high-temperature performance of the alloy. The addition of rare earth element RE to magnesium alloy has solid solution strengthening and second phase strengthening effects, thereby improving the mechanical properties of the alloy. In addition, the heat treatment method provided by the invention has the advantages of simple equipment, low cost, safety and reliability, and convenient operation, and is suitable for large-scale industrial production applications.
步骤1)一级热处理可在各种热处理炉(如箱式电阻炉等)中进行,一级热处理优选冷却方式为随炉冷却,该处理能够使合金中的元素发生固态扩散,减轻晶内偏析以及枝晶偏析,使得成分均匀化,随炉缓慢冷却能够加大合金元素的扩散,减轻铸造缺陷,优化合金的显微组织。Step 1) The primary heat treatment can be carried out in various heat treatment furnaces (such as box-type resistance furnaces, etc.). The preferred cooling method for the primary heat treatment is cooling with the furnace. This treatment can cause solid-state diffusion of elements in the alloy and reduce intragranular segregation And dendrite segregation, which makes the composition uniform, and slow cooling with the furnace can increase the diffusion of alloying elements, reduce casting defects, and optimize the microstructure of the alloy.
步骤2)二级热处理的冷却方式优选为热水冷却;所用热水温度为70~90℃,能够得到镁合金的过饱和固溶体,并且热水淬火能减少合金的热裂倾向,提高组织的完整性。Step 2) The cooling method of the secondary heat treatment is preferably hot water cooling; the temperature of the hot water used is 70-90°C, which can obtain a supersaturated solid solution of the magnesium alloy, and hot water quenching can reduce the hot cracking tendency of the alloy and improve the integrity of the structure sex.
步骤3)三级热处理的冷却方式优选为空冷,该过程为人工时效处理,从过饱和固溶体中析出弥散相能够起到弥散强化的作用。Step 3) The cooling method of the tertiary heat treatment is preferably air cooling, and this process is artificial aging treatment, and the precipitation of the dispersed phase from the supersaturated solid solution can play a role of dispersion strengthening.
步骤1)由原料得到铸态镁合金可采用多种现有技术。步骤1)所述铸态镁合金优选由以下方法制备得到:在保护气氛下,将原料按配比进行熔炼,浇铸,即得铸态镁合金。所述保护气氛为CO2和SF6的混合气体。所述浇铸的温度为710~730℃。Step 1) A variety of existing technologies can be used to obtain the cast magnesium alloy from raw materials. Step 1) The as-cast magnesium alloy is preferably prepared by the following method: under a protective atmosphere, the raw materials are melted according to the ratio, and then cast to obtain the as-cast magnesium alloy. The protective atmosphere is a mixed gas of CO 2 and SF 6 . The casting temperature is 710-730°C.
本发明同时提供一种由上述多元耐热镁合金的制备方法得到的多元耐热镁合金。本发明提供的多元耐热镁合金,合金中各相分布均匀,合金的强度、耐热性得到显著提高,室温抗拉强度达到273Mpa,屈服强度达到204MPa;200℃工作温度下,抗拉强度和屈服强度分别达到196Mpa和141Mpa;力学性能优异,具有广阔的应用空间。The present invention also provides a multi-element heat-resistant magnesium alloy obtained by the above-mentioned preparation method of the multi-element heat-resistant magnesium alloy. In the multi-component heat-resistant magnesium alloy provided by the invention, each phase in the alloy is evenly distributed, the strength and heat resistance of the alloy are significantly improved, the tensile strength at room temperature reaches 273Mpa, and the yield strength reaches 204MPa; at a working temperature of 200°C, the tensile strength and The yield strength reaches 196Mpa and 141Mpa respectively; the mechanical properties are excellent and have broad application space.
附图说明Description of drawings
图1为传统镁合金热处理方法温度-时间示意图;Fig. 1 is the temperature-time schematic diagram of traditional magnesium alloy heat treatment method;
图2为本发明多元耐热镁合金的制备方法温度-时间关系示意图;Fig. 2 is the temperature-time relation schematic diagram of the preparation method of multi-element heat-resistant magnesium alloy of the present invention;
图3为本发明对比例1和实施例1的金相组织图,其中(a)为对比例1的金相组织图,(b)为实施例1的金相组织图。3 is the metallographic structure diagram of Comparative Example 1 and Example 1 of the present invention, wherein (a) is the metallographic structure diagram of Comparative Example 1, and (b) is the metallographic structure diagram of Example 1.
具体实施方式detailed description
下面结合具体实施例对本发明作进一步的说明。The present invention will be further described below in conjunction with specific examples.
实施例1Example 1
本实施例多元耐热镁合金的制备方法,包括以下步骤:The preparation method of the multi-element heat-resistant magnesium alloy of the present embodiment comprises the following steps:
1)将装有原料的刚玉坩埚放入中频感应炉中,在CO2+SF6混合气体保护下进行熔炼,原料熔化后,将镁合金熔液升温至720℃时,浇铸至钢制模具中,得到铸态镁合金;铸态镁合金的质量百分比组成为:Al 8.0%,Zn 1%,Y 1.7%,Ca 0.8%,余量为Mg和杂质;1) Put the corundum crucible with raw materials into an intermediate frequency induction furnace, and melt under the protection of CO 2 +SF 6 mixed gas. After the raw materials are melted, when the temperature of the magnesium alloy melt is raised to 720°C, it is cast into a steel mold , to obtain the cast magnesium alloy; the mass percent of the cast magnesium alloy consists of: Al 8.0%, Zn 1%, Y 1.7%, Ca 0.8%, and the balance is Mg and impurities;
2)将步骤1)所得铸态镁合金在箱式电阻炉中进行一级热处理,一级热处理温度为430℃,一级热处理时间为4小时,随炉冷却;2) The as-cast magnesium alloy obtained in step 1) is subjected to primary heat treatment in a box-type resistance furnace, the primary heat treatment temperature is 430° C., the primary heat treatment time is 4 hours, and the furnace is cooled;
3)将步骤2)冷却后的镁合金放入热处理炉中进行二级热处理,二级热处理温度为400℃,二级热处理时间为8小时,用80℃的热水冷却;3) putting the cooled magnesium alloy in step 2) into a heat treatment furnace for secondary heat treatment, the secondary heat treatment temperature is 400°C, the secondary heat treatment time is 8 hours, and cooled with 80°C hot water;
4)将步骤3)冷却后的镁合金放入热处理炉中进行三级热处理,三级热处理温度为210℃,三级热处理时间为14小时,空冷,即得。4) Put the cooled magnesium alloy in step 3) into a heat treatment furnace for three-stage heat treatment, the temperature of the three-stage heat treatment is 210° C., the time of the three-stage heat treatment is 14 hours, and air cooling is obtained.
本实施例的制备方法所得多元耐热镁合金的质量百分比组成为Al 8%,Zn 1%,Y1.7%,Ca 0.8%,余量为Mg和杂质。The mass percentage composition of the multi-component heat-resistant magnesium alloy obtained by the preparation method of this embodiment is 8% Al, 1% Zn, 1.7% Y, 0.8% Ca, and the balance is Mg and impurities.
对比例1Comparative example 1
对比例1多元耐热镁合金原料的组成与实施例1相同;铸态镁合金的制备工艺与实施例1相同。对比例1多元耐热镁合金的制备方法,包括以下步骤:The composition of the raw material of the multi-element heat-resistant magnesium alloy of comparative example 1 is the same as that of Example 1; the preparation process of the as-cast magnesium alloy is the same as that of Example 1. The preparation method of comparative example 1 multi-element heat-resistant magnesium alloy comprises the following steps:
1)将铸态镁合金在箱式电阻炉中进行固溶处理,固溶处理温度为420℃,固溶处理时间为12小时,用80℃的热水冷却;1) The as-cast magnesium alloy is subjected to solution treatment in a box-type resistance furnace, the solution treatment temperature is 420°C, the solution treatment time is 12 hours, and cooled with 80°C hot water;
2)将步骤1)冷却后的镁合金放入热处理炉中进行时效处理,时效处理温度为210℃,时效处理时间为14小时,空冷,即得。2) Put the cooled magnesium alloy in step 1) into a heat treatment furnace for aging treatment, the aging treatment temperature is 210° C., the aging treatment time is 14 hours, air-cooled, and the product is obtained.
实施例2Example 2
本实施例多元耐热镁合金的制备方法,包括以下步骤:The preparation method of the multi-element heat-resistant magnesium alloy of the present embodiment comprises the following steps:
1)将装有原料的刚玉坩埚放入中频感应炉中,在CO2+SF6混合气体保护下进行熔炼,原料熔化后,将镁合金熔液升温至710℃时,浇铸至钢制模具中,得到铸态镁合金;铸态镁合金的质量百分比组成为:Al 7.6%,Zn 1.2%,Gd 2.0%,Ca 0.6%,余量为Mg和杂质;1) Put the corundum crucible with raw materials into an intermediate frequency induction furnace, and melt under the protection of CO 2 +SF 6 mixed gas. After the raw materials are melted, when the temperature of the magnesium alloy melt is raised to 710°C, it is cast into a steel mold , to obtain the cast magnesium alloy; the mass percent of the cast magnesium alloy consists of: Al 7.6%, Zn 1.2%, Gd 2.0%, Ca 0.6%, and the balance is Mg and impurities;
2)将步骤1)所得铸态镁合金在箱式电阻炉中进行一级热处理,一级热处理温度为420℃,一级热处理时间为5小时,随炉冷却;2) The as-cast magnesium alloy obtained in step 1) is subjected to primary heat treatment in a box-type resistance furnace, the primary heat treatment temperature is 420° C., the primary heat treatment time is 5 hours, and the furnace is cooled;
3)将步骤2)冷却后的镁合金放入热处理炉中进行二级热处理,二级热处理温度为410℃,二级热处理时间为9小时,80℃热水冷却;3) Put the cooled magnesium alloy in step 2) into a heat treatment furnace for secondary heat treatment, the secondary heat treatment temperature is 410°C, the secondary heat treatment time is 9 hours, and 80°C hot water cooling;
4)将步骤3)冷却后的镁合金放入热处理炉中进行三级热处理,三级热处理温度为200℃,三级热处理时间为13小时,空冷,即得。4) Put the cooled magnesium alloy in step 3) into a heat treatment furnace for three-stage heat treatment, the temperature of the three-stage heat treatment is 200° C., the time of the three-stage heat treatment is 13 hours, and air cooling is obtained.
本实施例的制备方法所得多元耐热镁合金的质量百分比组成为Al 8%,Zn 1%,Gd 2.0%,Ca 0.6%,余量为Mg和杂质。The mass percentage composition of the multi-component heat-resistant magnesium alloy obtained by the preparation method of this embodiment is 8% Al, 1% Zn, 2.0% Gd, 0.6% Ca, and the balance is Mg and impurities.
对比例2Comparative example 2
对比例2多元耐热镁合金原料的组成与实施例2相同;铸态镁合金的制备工艺与实施例2相同。对比例2多元耐热镁合金的制备方法,包括以下步骤:Comparative Example 2 The composition of the multi-component heat-resistant magnesium alloy raw material is the same as that of Example 2; the preparation process of the as-cast magnesium alloy is the same as that of Example 2. The preparation method of comparative example 2 multi-element heat-resistant magnesium alloy comprises the following steps:
1)将铸态镁合金在箱式电阻炉中进行固溶处理,固溶处理温度为415℃,固溶处理时间为14小时,80℃热水冷却;1) The as-cast magnesium alloy is subjected to solution treatment in a box-type resistance furnace, the solution treatment temperature is 415°C, the solution treatment time is 14 hours, and cooled with 80°C hot water;
2)将步骤1)冷却后的镁合金放入热处理炉中进行时效处理,时效处理温度为200℃,时效处理时间为13小时,空冷,得到多元耐热镁合金。2) Put the cooled magnesium alloy in step 1) into a heat treatment furnace for aging treatment, the aging treatment temperature is 200° C., the aging treatment time is 13 hours, and air-cooled to obtain a multi-element heat-resistant magnesium alloy.
实施例3Example 3
本实施例多元耐热镁合金的制备方法,包括以下步骤:The preparation method of the multi-element heat-resistant magnesium alloy of the present embodiment comprises the following steps:
1)将装有原料的刚玉坩埚放入中频感应炉中,在CO2+SF6混合气体保护下进行熔炼,原料熔化后,将镁合金熔液升温至730℃时,浇铸至钢制模具中,得到铸态镁合金;铸态镁合金的质量百分比组成为:Al 7.8%,Zn 0.9%,Nd 1.9%,Ca 1.0%,余量为Mg和杂质;1) Put the corundum crucible with raw materials into an intermediate frequency induction furnace, and melt under the protection of CO 2 +SF 6 mixed gas. After the raw materials are melted, when the temperature of the magnesium alloy melt is raised to 730°C, it is cast into a steel mold , to obtain the cast magnesium alloy; the mass percent of the cast magnesium alloy consists of: Al 7.8%, Zn 0.9%, Nd 1.9%, Ca 1.0%, and the balance is Mg and impurities;
2)将步骤1)所得铸态镁合金在箱式电阻炉中进行一级热处理,一级热处理温度为430℃,一级热处理时间为4小时,随炉冷却;2) The as-cast magnesium alloy obtained in step 1) is subjected to primary heat treatment in a box-type resistance furnace, the primary heat treatment temperature is 430° C., the primary heat treatment time is 4 hours, and the furnace is cooled;
3)将步骤2)冷却后的镁合金放入热处理炉中进行二级热处理,二级热处理温度为390℃,二级热处理时间为10小时,90℃热水冷却;3) Put the cooled magnesium alloy in step 2) into a heat treatment furnace for secondary heat treatment, the secondary heat treatment temperature is 390°C, the secondary heat treatment time is 10 hours, and 90°C hot water cooling;
4)将步骤3)冷却后的镁合金放入热处理炉中进行三级热处理,三级热处理温度为200℃,三级热处理时间为15小时,空冷,即得。4) Put the cooled magnesium alloy in step 3) into a heat treatment furnace for three-stage heat treatment, the temperature of the three-stage heat treatment is 200° C., the time of the three-stage heat treatment is 15 hours, and air cooling is obtained.
本实施例的制备方法所得多元耐热镁合金的质量百分比组成为Al 8%,Zn 1%,Nd 1.9%,Ca 1.0%,余量为Mg和杂质。The mass percentage composition of the multi-component heat-resistant magnesium alloy obtained by the preparation method of this embodiment is 8% Al, 1% Zn, 1.9% Nd, 1.0% Ca, and the balance is Mg and impurities.
对比例3Comparative example 3
对比例3多元耐热镁合金原料的组成与实施例3相同;铸态镁合金的制备工艺与实施例3相同。对比例3多元耐热镁合金的制备方法,包括以下步骤:The composition of the raw material of the multi-element heat-resistant magnesium alloy in comparative example 3 is the same as that of Example 3; the preparation process of the as-cast magnesium alloy is the same as that of Example 3. The preparation method of comparative example 3 multi-element heat-resistant magnesium alloy comprises the following steps:
1)将铸态镁合金在箱式电阻炉中进行固溶处理,固溶处理温度为425℃,固溶处理时间为11小时,90℃热水冷却;1) The as-cast magnesium alloy is subjected to solution treatment in a box-type resistance furnace, the solution treatment temperature is 425 ° C, the solution treatment time is 11 hours, and 90 ° C hot water cooling;
2)将步骤1)所得镁合金放入热处理炉中进行时效处理,时效处理温度为200℃,时效处理时间为15小时,空冷,得到多元耐热镁合金。2) Put the magnesium alloy obtained in step 1) into a heat treatment furnace for aging treatment, the aging treatment temperature is 200° C., the aging treatment time is 15 hours, and air-cooled to obtain a multi-element heat-resistant magnesium alloy.
实施例4Example 4
本实施例多元耐热镁合金的制备方法,包括以下步骤:The preparation method of the multi-element heat-resistant magnesium alloy of the present embodiment comprises the following steps:
1)将装有原料的刚玉坩埚放入中频感应炉中,在CO2+SF6混合气体保护下进行熔炼,原料熔化后,将镁合金熔液升温至710℃时,浇铸至钢制模具中,得到铸态镁合金;铸态镁合金的质量百分比组成为:Al 8.3%,Zn 0.8%,Sm 1.3%,Ca 1.2%,余量为Mg和杂质;1) Put the corundum crucible with raw materials into an intermediate frequency induction furnace, and melt under the protection of CO 2 +SF 6 mixed gas. After the raw materials are melted, when the temperature of the magnesium alloy melt is raised to 710°C, it is cast into a steel mold , to obtain the as-cast magnesium alloy; the mass percentage of the as-cast magnesium alloy consists of: Al 8.3%, Zn 0.8%, Sm 1.3%, Ca 1.2%, and the balance is Mg and impurities;
2)将步骤1)所得铸态镁合金在箱式电阻炉中进行一级热处理,一级热处理温度为430℃,一级热处理时间为6小时,随炉冷却;2) The as-cast magnesium alloy obtained in step 1) is subjected to primary heat treatment in a box-type resistance furnace, the primary heat treatment temperature is 430° C., the primary heat treatment time is 6 hours, and the furnace is cooled;
3)将步骤2)冷却后的镁合金放入热处理炉中进行二级热处理,二级热处理温度为410℃,二级热处理时间为8小时,80℃热水冷却;3) Put the cooled magnesium alloy in step 2) into a heat treatment furnace for secondary heat treatment, the secondary heat treatment temperature is 410°C, the secondary heat treatment time is 8 hours, and 80°C hot water cooling;
4)将步骤3)冷却后的镁合金放入热处理炉中进行三级热处理,三级热处理温度为200℃,三级热处理时间为15小时,空冷,即得。4) Put the cooled magnesium alloy in step 3) into a heat treatment furnace for three-stage heat treatment, the temperature of the three-stage heat treatment is 200° C., the time of the three-stage heat treatment is 15 hours, and air cooling is obtained.
本实施例的制备方法所得多元耐热镁合金的质量百分比组成为Al 8%,Zn 1%,Sm 1.3%,Ca 1.2%,余量为Mg和杂质。The mass percent composition of the multi-component heat-resistant magnesium alloy obtained by the preparation method of this embodiment is 8% Al, 1% Zn, 1.3% Sm, 1.2% Ca, and the balance is Mg and impurities.
对比例4Comparative example 4
对比例4多元耐热镁合金原料的组成与实施例4相同;铸态镁合金的制备工艺与实施例4相同。对比例4多元耐热镁合金的制备方法,包括以下步骤:The composition of the raw material of the multi-element heat-resistant magnesium alloy in Comparative Example 4 is the same as that of Example 4; the preparation process of the as-cast magnesium alloy is the same as that of Example 4. The preparation method of comparative example 4 multi-element heat-resistant magnesium alloy comprises the following steps:
1)将铸态镁合金在箱式电阻炉中进行固溶处理,固溶处理温度为430℃,固溶处理时间为10小时,80℃热水冷却;1) The as-cast magnesium alloy is subjected to solution treatment in a box-type resistance furnace, the solution treatment temperature is 430 ° C, the solution treatment time is 10 hours, and 80 ° C hot water cooling;
2)将步骤1)冷却后的镁合金放入热处理炉中进行时效处理,时效处理温度为200℃,时效处理时间为15小时,空冷,得到多元耐热镁合金。2) Put the cooled magnesium alloy in step 1) into a heat treatment furnace for aging treatment, the aging treatment temperature is 200° C., the aging treatment time is 15 hours, air cooling to obtain a multi-element heat-resistant magnesium alloy.
实施例5Example 5
本实施例多元耐热镁合金的制备方法,包括以下步骤:The preparation method of the multi-element heat-resistant magnesium alloy of the present embodiment comprises the following steps:
1)将装有原料的刚玉坩埚放入中频感应炉中,在CO2+SF6混合气体保护下进行熔炼,原料熔化后,将镁合金熔液升温至730℃时,浇铸至钢制模具中,得到铸态镁合金;铸态镁合金的质量百分比组成为:Al 8.4%,Zn 1.1%,Gd 2.3%,Ca 1.4%,余量为Mg和杂质;1) Put the corundum crucible with raw materials into an intermediate frequency induction furnace, and melt under the protection of CO 2 +SF 6 mixed gas. After the raw materials are melted, when the temperature of the magnesium alloy melt is raised to 730°C, it is cast into a steel mold , to obtain the cast magnesium alloy; the mass percent of the cast magnesium alloy consists of: Al 8.4%, Zn 1.1%, Gd 2.3%, Ca 1.4%, and the balance is Mg and impurities;
2)将步骤1)所得铸态镁合金在箱式电阻炉中进行一级热处理,一级热处理温度为440℃,一级热处理时间为5小时,随炉冷却;2) Carrying out the primary heat treatment of the as-cast magnesium alloy obtained in step 1) in a box-type resistance furnace, the primary heat treatment temperature is 440° C., the primary heat treatment time is 5 hours, and is cooled with the furnace;
3)将步骤2)冷却后的镁合金放入热处理炉中进行二级热处理,二级热处理温度为390℃,二级热处理时间为10小时,70℃热水冷却;3) Put the cooled magnesium alloy in step 2) into a heat treatment furnace for secondary heat treatment, the secondary heat treatment temperature is 390°C, the secondary heat treatment time is 10 hours, and 70°C hot water cooling;
4)将步骤3)冷却后的镁合金放入热处理炉中进行三级热处理,三级热处理温度为220℃,三级热处理时间为14小时,空冷,即得。4) Put the magnesium alloy cooled in step 3) into a heat treatment furnace for three-stage heat treatment, the temperature of the three-stage heat treatment is 220° C., the time of the three-stage heat treatment is 14 hours, and air cooling is obtained.
本实施例制备方法所得多元耐热镁合金的质量百分比组成为Al 8%,Zn 1%,Gd2.3%,Ca 1.4%,余量为Mg和杂质。The mass percentage composition of the multi-element heat-resistant magnesium alloy obtained by the preparation method of this embodiment is 8% Al, 1% Zn, 2.3% Gd, 1.4% Ca, and the balance is Mg and impurities.
对比例5Comparative example 5
对比例5多元耐热镁合金原料的组成与实施例5相同;铸态镁合金的制备工艺与实施例5相同。对比例5多元耐热镁合金的制备方法,包括以下步骤:Comparative Example 5 The composition of the multi-component heat-resistant magnesium alloy raw material is the same as that of Example 5; the preparation process of the as-cast magnesium alloy is the same as that of Example 5. The preparation method of comparative example 5 multi-element heat-resistant magnesium alloy comprises the following steps:
1)将铸态镁合金在箱式电阻炉中进行固溶处理,固溶处理温度为410℃,固溶处理时间为15小时,70℃热水冷却;1) The as-cast magnesium alloy is subjected to solution treatment in a box-type resistance furnace, the solution treatment temperature is 410 ° C, the solution treatment time is 15 hours, and 70 ° C hot water cooling;
2)将步骤1)冷却后的镁合金放入热处理炉中进行时效处理,时效处理温度为220℃,时效处理时间为14小时,空冷,得到多元耐热镁合金。2) Put the cooled magnesium alloy in step 1) into a heat treatment furnace for aging treatment, the aging treatment temperature is 220° C., the aging treatment time is 14 hours, and air-cooled to obtain a multi-element heat-resistant magnesium alloy.
试验例Test case
检测各实施例和对比例的多元耐热镁合金在常温和工作温度下(200℃)的抗拉强度和屈服强度,检测结果如表1所示。由表1可以看出,以本发明热处理方法得到的多元耐热镁合金在常温和200℃下均具有较高的抗拉强度和屈服强度,力学性能优异。The tensile strength and yield strength of the multi-element heat-resistant magnesium alloys of various examples and comparative examples were tested at room temperature and working temperature (200° C.), and the test results are shown in Table 1. It can be seen from Table 1 that the multi-component heat-resistant magnesium alloy obtained by the heat treatment method of the present invention has high tensile strength and yield strength at room temperature and 200° C., and has excellent mechanical properties.
表1各实施例和对比例的多元耐热镁合金的力学性能检测结果The mechanical property detection result of the multi-element heat-resistant magnesium alloy of table 1 each embodiment and comparative example
(注:(炉)表示冷却方式为炉冷;(水)表示冷却方式为热水冷却,水温为70~90℃;(空)表示冷却方式为空冷。)(Note: (furnace) means that the cooling method is furnace cooling; (water) means that the cooling method is hot water cooling, and the water temperature is 70-90°C; (empty) means that the cooling method is air cooling.)
传统镁合金热处理方法温度-时间示意图如图1所示,经过一次固溶处理后,水冷冷却;然后进行时效处理,空冷,得到镁合金;本发明的多元耐热镁合金的制备方法的温度-时间关系示意图如图2所示,经过二次固溶处理,二次固溶处理的冷却方式分别为炉冷和水冷;然后进行时效处理,空冷,得到多元耐热镁合金。通过对热处理工艺的优化,可以使镁合金的金相组织得到优化,从而使合金的强度、耐热性得到显著提高。Traditional magnesium alloy heat treatment method temperature-time schematic diagram as shown in Figure 1, after a solid solution treatment, water cooling; Then aging treatment, air cooling, obtain magnesium alloy; the temperature of the preparation method of multi-element heat-resistant magnesium alloy of the present invention- The schematic diagram of the time relationship is shown in Figure 2. After the second solution treatment, the cooling methods of the second solution treatment are furnace cooling and water cooling respectively; then aging treatment and air cooling are performed to obtain a multi-component heat-resistant magnesium alloy. By optimizing the heat treatment process, the metallographic structure of the magnesium alloy can be optimized, so that the strength and heat resistance of the alloy can be significantly improved.
图3为本发明对比例1和实施例1的金相组织图,其中(a)为对比例1的金相组织图,(b)为实施例1的金相组织图。与对比例的金相组织相比,实施例1得到的多元耐热镁合金,晶内偏析以及枝晶偏析少,合金成分均匀化程度高,且弥散相晶粒细化,分布均匀,有利于减少缺陷的产生,保持组织的完整性,提高宏观力学性能。3 is the metallographic structure diagram of Comparative Example 1 and Example 1 of the present invention, wherein (a) is the metallographic structure diagram of Comparative Example 1, and (b) is the metallographic structure diagram of Example 1. Compared with the metallographic structure of the comparative example, the multi-element heat-resistant magnesium alloy obtained in Example 1 has less intragranular segregation and dendrite segregation, a high degree of homogeneity of alloy components, and the dispersed phase grains are refined and evenly distributed, which is beneficial to Reduce the generation of defects, maintain the integrity of the organization, and improve the macroscopic mechanical properties.
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