CN111485187A - A kind of non-isothermal overaging treatment method of large diameter AlZnMgCu alloy extruded rod - Google Patents
A kind of non-isothermal overaging treatment method of large diameter AlZnMgCu alloy extruded rod Download PDFInfo
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Abstract
Description
技术领域technical field
本发明涉及一种较大直径AlZnMgCu合金挤压棒的非等温过时效处理方法,属于铝合金的热处理强化技术领域。The invention relates to a non-isothermal overaging treatment method for a larger-diameter AlZnMgCu alloy extruded rod, and belongs to the technical field of heat treatment strengthening of aluminum alloys.
背景技术Background technique
采用高强AlZnMgCu合金挤压棒直接制造或配合机加工等制备承力结构件是实现快速轨道交通工具和航空器结构轻量化的重要途径之一。随着中国高速列车和“大飞机”计划的不断推进,交通工具载重量和性能的持续提升对结构减重、挤压棒材等的综合性能提出了更严格的要求。The use of high-strength AlZnMgCu alloy extruded rods to directly manufacture or cooperate with machining to prepare load-bearing structural parts is one of the important ways to realize the lightweight of fast rail vehicles and aircraft structures. With the continuous advancement of China's high-speed train and "large aircraft" plan, the continuous improvement of the carrying capacity and performance of vehicles has put forward more stringent requirements for the comprehensive performance of structural weight reduction and extruded bars.
作为典型的析出强化合金,高品质AlZnMgCu合金挤压棒的综合性能强烈依赖时效技术。但是,单级峰时效只能最大化AlZnMgCu合金的强度。等温双级过时效提高合金抗应力腐蚀性能的结果则是以牺牲合金力学性能为前提的。回归再时效仅仅从理论上解决了AlZnMgCu合金的强度和耐蚀性能可以协同提升的可能性,但是其工艺窗口狭窄,工业应用难度极大。因此,AlZnMgCu合金的力学性能和抗应力腐蚀的协同提升是该系合金时效热处理需要解决的关键技术难点。As a typical precipitation-strengthened alloy, the comprehensive properties of high-quality AlZnMgCu alloy extruded rods strongly depend on aging technology. However, single-stage aging can only maximize the strength of AlZnMgCu alloys. The result of isothermal double-stage overaging to improve the stress corrosion resistance of the alloy is based on the premise of sacrificing the mechanical properties of the alloy. Regression and reaging only theoretically solves the possibility that the strength and corrosion resistance of AlZnMgCu alloys can be synergistically improved, but its process window is narrow and industrial application is extremely difficult. Therefore, the synergistic improvement of the mechanical properties and stress corrosion resistance of AlZnMgCu alloys is the key technical difficulty to be solved in the aging heat treatment of this series of alloys.
此外,随着近净成型、整体制造理念的重视程度不断加深,大尺寸AlZnMgCu合金结构件的时效热处理还存在厚截面构件芯部和表面层的时效程度差异而导致的组织及性能不均匀性问题,如高速铁路和大型航空航天设备使用的高性能轻质挤压棒材,该类制品力学和腐蚀性能水平及其均匀性的突破对满足我国高速轨道交通和航空航天领域急需的超强轻质结构件起着关键作用。因此,较大直径AlZnMgCu合金挤压棒的热处理强化处理应达到以下两个目的:(1) 同时拥有较高的力学性能和抗应力腐蚀性能;(2) 性能的径向不均匀性低。In addition, with the increasing emphasis on near-net-shape and overall manufacturing concepts, the aging heat treatment of large-sized AlZnMgCu alloy structural parts also has the problem of microstructure and performance inhomogeneity caused by the difference in the aging degree of the core and surface layers of thick-section components. , such as high-performance light-weight extruded bars used in high-speed railways and large aerospace equipment, the breakthrough in the level of mechanical and corrosion properties of such products and their uniformity is very important to meet the urgent needs of my country's high-speed rail transit and aerospace fields. Structural parts play a key role. Therefore, the heat treatment strengthening treatment of AlZnMgCu alloy extruded rods with larger diameter should achieve the following two purposes: (1) have high mechanical properties and stress corrosion resistance at the same time; (2) have low radial inhomogeneity of properties.
发明内容SUMMARY OF THE INVENTION
针对现有的常规双级时效热处理的缺陷和不足,本发明提供了一种较大直径AlZnMgCu合金挤压棒的非等温过时效处理方法,已解决上述背景技术中的问题。Aiming at the defects and deficiencies of the existing conventional double-stage aging heat treatment, the present invention provides a non-isothermal over-aging treatment method of a larger diameter AlZnMgCu alloy extruded rod, which has solved the above-mentioned problems in the background technology.
本发明从第一阶段预时效、第二阶段升温时效的升温速率、最高时效温度点以及降温时效的冷却速率四个因素的优化匹配出发,首先通过第一阶段预时效使合金晶内析出具有一定比例的GP区、η′相以及晶界η相;再通过第二阶段升温时效的升温速率和最高时效温度点的匹配,在抑制晶内半共格相粗化的同时,促使晶界η相粗化和断续;接着再以一定的冷却速率降温至室温,利用过饱和固溶体的再次脱溶二次强化基体,同时利用较大直径挤压棒材表面层和芯部升温、降温速率的相互补偿效应,达到控制晶内、晶界析出相尺寸以及其在棒材径向的优化分布,有效提高较大直径AlZnMgCu合金挤压棒的径向性能均匀性。The present invention starts from the optimal matching of four factors: the first-stage pre-aging, the heating rate of the second-stage heating-up aging, the maximum aging temperature point, and the cooling rate of the cooling-aging aging. The proportion of GP region, η' phase and grain boundary η phase; through the matching of the heating rate of the second stage heating and aging and the maximum aging temperature point, while suppressing the coarsening of the intragranular semi-coherent phase, the grain boundary η phase is promoted. Coarse and intermittent; then cool down to room temperature at a certain cooling rate, use the supersaturated solid solution to re-desolubilize the matrix to strengthen the matrix, and use the larger diameter extruded bar surface layer and core heating and cooling rates. Compensation effect, to control the size of intragranular and grain boundary precipitation phase and its optimal distribution in the radial direction of the rod, and effectively improve the radial performance uniformity of the larger diameter AlZnMgCu alloy extruded rod.
本发明一种较大直径AlZnMgCu合金挤压棒的非等温过时效处理方法,包括如下步骤:A non-isothermal overaging treatment method for a larger diameter AlZnMgCu alloy extruded rod of the present invention comprises the following steps:
(1)在15~18的挤压比条件下,得到直径60~80mm的AlZnMgCu合金挤压棒材。对挤压棒材进行固溶处理。固溶温度为470~480℃,固溶时间为1~2h,淬火转移时间≤10s;(1) Under the condition of extrusion ratio of 15 to 18, an AlZnMgCu alloy extruded rod with a diameter of 60 to 80 mm is obtained. Solution treatment of extruded bars. The solution temperature is 470~480℃, the solution time is 1~2h, and the quenching transfer time is less than or equal to 10s;
(2)对固溶态的较大直径AlZnMgCu合金挤压棒按照低于最高时效温度点强化效果的欠时效进行第一阶段预时效处理。第一阶段预时效温度≤120℃,第一阶段预时效时间≤24h;(2) The first-stage pre-aging treatment is performed on the large-diameter AlZnMgCu alloy extruded rod in the solid solution state according to the under-aging that is lower than the strengthening effect at the maximum aging temperature point. The pre-aging temperature of the first stage is less than or equal to 120℃, and the pre-aging time of the first stage is less than or equal to 24h;
(3)第二阶段升温时效的升温速率为60℃~300℃/h,加热到预设的最高时效温度点为215~250℃,取消第二阶段时效的等温保温平台,升温至预设的最高时效温度点后立即以冷却速率为60℃~120℃/h进行降温时效。(3) The heating rate of the second-stage heating and aging is 60℃~300℃/h, and the temperature is heated to the preset maximum aging temperature of 215~250℃. The isothermal heat preservation platform of the second-stage aging is cancelled, and the temperature is increased to the preset temperature. Immediately after the maximum aging temperature point, the cooling and aging shall be carried out at a cooling rate of 60°C to 120°C/h.
本发明的有益效果是:The beneficial effects of the present invention are:
发明人在研究中发现,通过第一阶段预时效使合金晶内析出具有一定比例的GP区和η′相,同时在晶界析出η平衡相;在第二阶段升温时效中,晶内析出相由GP区和η′相演变为η′和η相,晶界相η完成粗化和断续过程。在冷却时效阶段,合金硬度随着晶内非平衡相的再次析出而升高,而晶界η相在降温的高温阶段继续粗化断续,使合金电导率持续增加。其中,第一阶段的时效组织状态将对升温时效行为产生重要影响。对固溶淬火态或严重欠时效样品态样品直接进行升温时效,不利于晶界析出相的断续和粗化,制约合金抗应力腐蚀性能的提升;而第一阶段如果采用峰时效或过时效处理,将导致非等温升温时效过程中晶内相的严重粗化,不利于合金强度的提升。非等温过时效的第二阶段升温时效的升温速率和最高时效温度点决定了合金的性能。升温速率越高,最高时效温度越高,合金的抗应力腐蚀性能越高。此外,取消等温保温阶段实现了热处理工艺的短流程操作。采用本发明的非等温过时效处理,较大直径AlZnMgCu合金挤压棒材的力学性能远远高于传统的双级热处理处理结果,但是电导率(%IACS)水平与传统的双级热处理处理结果相当。In the research, the inventor found that through the first stage of pre-aging, a certain proportion of GP region and η' phase was precipitated in the alloy, and η equilibrium phase was precipitated at the grain boundary; in the second stage of heating and aging, the intragranular precipitated phase. From GP region and η' phase to η' and η phase, the grain boundary phase η completes the coarsening and discontinuous process. During the cooling and aging stage, the hardness of the alloy increases with the re-precipitation of the intragranular non-equilibrium phase, while the grain boundary η phase continues to coarsen and discontinuously at the high temperature stage of cooling, resulting in a continuous increase in the electrical conductivity of the alloy. Among them, the aging organization state in the first stage will have an important influence on the aging behavior at temperature. The direct heating and aging of the solution quenched or severely underaged samples is not conducive to the discontinuity and coarsening of the grain boundary precipitates, and restricts the improvement of the alloy's stress corrosion resistance; and if peak aging or overaging is used in the first stage The treatment will lead to severe coarsening of the intragranular phase during the non-isothermal heating and aging process, which is not conducive to the improvement of the alloy strength. The heating rate and the maximum ageing temperature point of the second-stage heating-aging of non-isothermal overaging determine the properties of the alloy. The higher the heating rate and the higher the maximum aging temperature, the higher the stress corrosion resistance of the alloy. In addition, the elimination of the isothermal holding stage enables a short flow operation of the heat treatment process. By adopting the non-isothermal overaging treatment of the present invention, the mechanical properties of the larger diameter AlZnMgCu alloy extruded bars are much higher than the results of the traditional two-stage heat treatment treatment, but the electrical conductivity (%IACS) level is similar to the traditional two-stage heat treatment treatment results. quite.
附图说明Description of drawings
图1为本发明工艺流程示意图。Fig. 1 is the process flow schematic diagram of the present invention.
具体实施方式Detailed ways
下面对本发明的较佳实施例进行详细阐述,以使本发明的优点和特征能更容易被本领域技术人员理解,从而对本发明的保护范围做出更清楚明确的界点。The preferred embodiments of the present invention are described in detail below, so that the advantages and features of the present invention can be more easily understood by those skilled in the art, so as to make clearer and clearer boundaries of the protection scope of the present invention.
本发明对比例与实施例均采用挤压比为15的60mm直径的热挤压Al8Zn2Mg2Cu铝合金棒材,固溶热处理工艺为470℃,1h+480℃,1h,固溶后室温水淬火,淬火转移时间<10s。然后将对比例和实施例样品分别进行不同的时效处理,处理结束后对所有进行实施例和对比例样品进行电导率、硬度以及拉伸力学性能检测,性能测试结果见表1和表2。The comparative example and the embodiment of the present invention all use a hot extrusion Al8Zn2Mg2Cu aluminum alloy bar with an extrusion ratio of 15 and a diameter of 60mm. The solution heat treatment process is 470°C, 1h+480°C, 1h. Transfer time <10s. Then, the samples of the examples and the examples were subjected to different aging treatments respectively. After the treatment, all the samples of the examples and the comparative examples were tested for electrical conductivity, hardness and tensile mechanical properties. The performance test results are shown in Table 1 and Table 2.
对比例 1:Comparative Example 1:
挤压棒采用单级(120℃/24)峰时效方式进行时效。时效结束后进行硬度和电导率测试,实验结果见表1所示。随后对峰时效样品进行室温拉伸性能测试,测试结果见表2。The extruded rod was aged by a single-stage (120°C/24) peak aging method. After the aging, the hardness and electrical conductivity were tested, and the experimental results are shown in Table 1. The room temperature tensile properties were then tested on the peak aging samples, and the test results are shown in Table 2.
对比例 2:Comparative Example 2:
试样采用等温双级(120℃/12h+160℃/18h)过时效方式进行时效。时效结束后进行硬度和电导率测试,实验结果见表1所示。随后对双级时效样品进行室温拉伸性能测试,测试结果见表2。The samples were aged by isothermal two-stage (120℃/12h+160℃/18h) over-aging method. After the aging, the hardness and electrical conductivity were tested, and the experimental results are shown in Table 1. Subsequently, the room temperature tensile properties were tested on the double-aged samples, and the test results are shown in Table 2.
实施例 1:Example 1:
对经过自然时效(室温/24h)处理的预时效样品,以60℃/h的加热速率升温至215℃,到温后立即开始炉冷降温时效,降温速率为80℃/h。时效后进行硬度和电导率测试,实验结果见表1所示。对样品进行室温拉伸性能测试,测试结果见表2。For the pre-aged samples treated by natural aging (room temperature/24h), the temperature was raised to 215°C at a heating rate of 60°C/h, and the furnace cooling and cooling aging was started immediately after reaching the temperature, and the cooling rate was 80°C/h. After aging, the hardness and electrical conductivity were tested, and the experimental results are shown in Table 1. The samples were tested for tensile properties at room temperature, and the test results are shown in Table 2.
实施例 2:Example 2:
对经过自然时效(室温/24h)处理的预时效样品,在180下℃/h的加热速率升温至225℃,到温后立即开始炉冷降温时效,降温速率为80℃/h。时效后进行硬度和电导率测试,实验结果见表1所示。对样品进行室温拉伸性能测试,测试结果见表2。For the pre-aged samples treated by natural aging (room temperature/24h), the heating rate was raised to 225°C at a heating rate of 180°C/h, and the furnace cooling and cooling aging started immediately after reaching the temperature, and the cooling rate was 80°C/h. After aging, the hardness and electrical conductivity were tested, and the experimental results are shown in Table 1. The samples were tested for tensile properties at room temperature, and the test results are shown in Table 2.
实施例 3:Example 3:
对105℃/24h处理的预时效样品,以60℃/h的加热速率升温至215℃,到温后立即开始炉冷降温时效,降温速率为80℃/h。时效后进行硬度和电导率测试,实验结果见表1所示。对样品进行室温拉伸性能测试,测试结果见表2。For the pre-aged samples treated at 105°C/24h, the temperature was raised to 215°C at a heating rate of 60°C/h, and the furnace cooling and cooling aging was started immediately after reaching the temperature, and the cooling rate was 80°C/h. After aging, the hardness and electrical conductivity were tested, and the experimental results are shown in Table 1. The samples were tested for tensile properties at room temperature, and the test results are shown in Table 2.
实施例 4:Example 4:
对105℃/24h处理的预时效样品,,以180℃/h的加热速率升温至225℃,到温后立即开始炉冷降温时效,降温速率为80℃/h。时效后进行硬度和电导率测试,实验结果见表1所示。对样品进行室温拉伸性能测试,测试结果见表2。For the pre-aged samples treated at 105°C/24h, the temperature was raised to 225°C at a heating rate of 180°C/h, and the furnace cooling and cooling aging was started immediately after reaching the temperature, and the cooling rate was 80°C/h. After aging, the hardness and electrical conductivity were tested, and the experimental results are shown in Table 1. The samples were tested for tensile properties at room temperature, and the test results are shown in Table 2.
实施例 5:Example 5:
对120℃/24h处理的预时效样品,以60℃/h的加热速率升温至215℃,到温后立即开始炉冷降温时效,降温速率为80℃/h。时效后进行硬度和电导率测试,实验结果见表1所示。对样品进行室温拉伸性能测试,测试结果见表2。For the pre-aged samples treated at 120°C/24h, the temperature was raised to 215°C at a heating rate of 60°C/h, and the furnace cooling and cooling aging was started immediately after reaching the temperature, and the cooling rate was 80°C/h. After aging, the hardness and electrical conductivity were tested, and the experimental results are shown in Table 1. The samples were tested for tensile properties at room temperature, and the test results are shown in Table 2.
实施例 6:Example 6:
对120℃/24h处理的预时效样品,,以180℃/h的加热速率升温至225℃,到温后立即开始炉冷降温时效,降温速率为80℃/h。时效后进行硬度和电导率测试,实验结果见表1所示。对样品进行室温拉伸性能测试,测试结果见表2。For the pre-aged samples treated at 120°C/24h, the temperature was raised to 225°C at a heating rate of 180°C/h, and the furnace cooling and cooling aging started immediately after reaching the temperature, and the cooling rate was 80°C/h. After aging, the hardness and electrical conductivity were tested, and the experimental results are shown in Table 1. The samples were tested for tensile properties at room temperature, and the test results are shown in Table 2.
利用TecnaiG220型高分辨透射电子显微镜检测不同非等温过时效下的AlZnMgCu合金的微观组织。结果表明,晶内析出相以η′相为主,包含一定量GP区和少量η相,而晶界上存在粗大断续的η相,此种微观组织特征既能有效保证力学性能,又能有效切断应力腐蚀通道,提高挤压棒的耐蚀性能。实施例中的非等温过时效所获得的挤压棒材抗拉强度为650MPa左右,电导率高于38%IACS。The microstructures of AlZnMgCu alloys under different non-isothermal overaging conditions were detected by TecnaiG 2 20 high-resolution transmission electron microscope. The results show that the intragranular precipitation phase is dominated by η' phase, including a certain amount of GP region and a small amount of η phase, while there are coarse and intermittent η phase on the grain boundary. Effectively cut off the stress corrosion channel and improve the corrosion resistance of the extruded rod. The tensile strength of the extruded rod obtained by the non-isothermal overaging in the example is about 650MPa, and the electrical conductivity is higher than 38%IACS.
综上所述,经过本发明提供的非等温过时效处理,较大直径AlZnMgCu合金挤压棒材可获得优异的力学和抗应力腐蚀腐蚀性能,在高速轨道交通和航空航天领域具有广阔的应用前景。To sum up, after the non-isothermal overaging treatment provided by the present invention, the larger diameter AlZnMgCu alloy extruded bar can obtain excellent mechanical and stress corrosion resistance properties, and has broad application prospects in the fields of high-speed rail transit and aerospace. .
以上公开仅为本申请的具体实施例,任何落在本申请之内的工艺参数变化都应在本申请的保护范围内。The above disclosures are only specific embodiments of the present application, and any changes in process parameters that fall within the scope of the present application should fall within the protection scope of the present application.
表1不同热处理制度试样的电导率及硬度的比较Table 1 Comparison of electrical conductivity and hardness of samples with different heat treatment regimes
表2 不同热处理制度试样的常温力学性能比较Table 2 Comparison of mechanical properties at room temperature of samples with different heat treatment regimes
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