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CN116516269A - Forming process of Mg-Gd-Zn alloy - Google Patents

Forming process of Mg-Gd-Zn alloy Download PDF

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Publication number
CN116516269A
CN116516269A CN202310496870.1A CN202310496870A CN116516269A CN 116516269 A CN116516269 A CN 116516269A CN 202310496870 A CN202310496870 A CN 202310496870A CN 116516269 A CN116516269 A CN 116516269A
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extrusion
ingot
alloy
forming process
ingot blank
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CN116516269B (en
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周小杰
夏海友
卢先正
张健
陈小敏
曾钢
肖宏超
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Changsha University of Science and Technology
Aerospace Science and Industry Changsha New Materials Research Institute Co Ltd
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Changsha University of Science and Technology
Aerospace Science and Industry Changsha New Materials Research Institute Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22FCHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
    • C22F1/00Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
    • C22F1/06Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of magnesium or alloys based thereon
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B21MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
    • B21CMANUFACTURE OF METAL SHEETS, WIRE, RODS, TUBES OR PROFILES, OTHERWISE THAN BY ROLLING; AUXILIARY OPERATIONS USED IN CONNECTION WITH METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL
    • B21C23/00Extruding metal; Impact extrusion
    • B21C23/001Extruding metal; Impact extrusion to improve the material properties, e.g. lateral extrusion
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B21MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
    • B21CMANUFACTURE OF METAL SHEETS, WIRE, RODS, TUBES OR PROFILES, OTHERWISE THAN BY ROLLING; AUXILIARY OPERATIONS USED IN CONNECTION WITH METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL
    • B21C25/00Profiling tools for metal extruding
    • B21C25/02Dies
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B21MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
    • B21CMANUFACTURE OF METAL SHEETS, WIRE, RODS, TUBES OR PROFILES, OTHERWISE THAN BY ROLLING; AUXILIARY OPERATIONS USED IN CONNECTION WITH METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL
    • B21C29/00Cooling or heating work or parts of the extrusion press; Gas treatment of work
    • B21C29/003Cooling or heating of work
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B21MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
    • B21CMANUFACTURE OF METAL SHEETS, WIRE, RODS, TUBES OR PROFILES, OTHERWISE THAN BY ROLLING; AUXILIARY OPERATIONS USED IN CONNECTION WITH METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL
    • B21C31/00Control devices, e.g. for regulating the pressing speed or temperature of metal; Measuring devices, e.g. for temperature of metal, combined with or specially adapted for use in connection with extrusion presses
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C23/00Alloys based on magnesium
    • C22C23/06Alloys based on magnesium with a rare earth metal as the next major constituent
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22FCHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
    • C22F1/00Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
    • C22F1/002Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working by rapid cooling or quenching; cooling agents used therefor

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Extrusion Of Metal (AREA)

Abstract

The invention discloses a forming process of Mg-Gd-Zn alloy, which mainly comprises the following steps: A. casting and machining to obtain a cuboid Mg-Gd-Zn alloy ingot blank with the cross section side length of 40-60mm and the length of 60-120 mm; B. homogenizing annealing treatment is carried out on the ingot blank, and the annealing process is as follows: after 15-40h of heat preservation at 495-525 ℃, placing the mixture at 450-480 ℃ for 3-10h of heat preservation, and then cooling the mixture to room temperature at a speed of 1-10 ℃/min; C. performing equal-diameter angular extrusion on the ingot blank subjected to the homogenizing annealing in a die with an angle of 90 degrees; before extrusion, heating the ingot blank and the mould to 300-400 ℃ respectively, and preserving heat for 1-3 hours; extruding the ingot blank along the length direction by using a hydraulic press, and co-extruding for 4-8 times, wherein the extrusion rate is 4-8mm/min; the surface temperature of the ingot blank is reduced by 20-50 ℃ in each pass of extrusion relative to the previous pass, and the surface temperature of the ingot blank is 140-200 ℃ when the extrusion is finished; D. quenching treatment is carried out immediately after extrusion is completed. By adopting the process, a large number of LPSO phase kink bands are formed in the prepared Mg-Gd-Zn alloy, so that the strength and the plasticity of the alloy are obviously improved synchronously, and the application range of the Mg-Gd-Zn component is widened.

Description

一种Mg-Gd-Zn合金的成形工艺A Forming Process of Mg-Gd-Zn Alloy

技术领域technical field

本发明涉及镁合金变形加工领域,特别涉及一种Mg-Gd-Zn合金的塑性成形工艺。The invention relates to the field of deformation processing of magnesium alloys, in particular to a plastic forming process of Mg-Gd-Zn alloys.

背景技术Background technique

作为目前最轻的实用金属结构材料,镁合金具有密度低、阻尼减震、易于回收等优点,受到航空航天、交通运输等领域的日益青睐。其中,含长周期有序结构(LPSO)的Mg-Gd-Zn合金的室温和高温强度表现优异,相对于常规AZ系、ZK系镁合金具有更广阔的应用潜力。然而,与铝合金及钢铁结构材料相比,Mg-Gd-Zn合金的强度与塑性还存在很大差距,特别是常规塑性成形工艺在提升其力学性能过程中通常存在强塑性矛盾,即合金的强度和塑性难以同时提高,这严重限制了合金的应用范围。As the lightest practical metal structural material at present, magnesium alloy has the advantages of low density, shock absorption and easy recycling, and is increasingly favored by aerospace, transportation and other fields. Among them, Mg-Gd-Zn alloys containing long-period ordered structure (LPSO) have excellent room temperature and high temperature strength, and have wider application potential than conventional AZ and ZK series magnesium alloys. However, compared with aluminum alloys and steel structural materials, there is still a big gap between the strength and plasticity of Mg-Gd-Zn alloys, especially in the process of improving the mechanical properties of conventional plastic forming processes. It is difficult to improve the strength and plasticity at the same time, which severely limits the application range of the alloy.

作为一种严重塑性变形工艺,等径角挤压具有不改变锭坯初始形状即可累积塑性应变的优点,近年来被广泛应用于加工镁合金以细化晶粒、累积位错进而提高强度。然而,常规的等径角挤压工艺在提升合金强度的同时往往降低了延伸率。因此,亟需一种能同时增强增塑Mg-Gd-Zn合金的成形工艺以提升其综合力学性能并扩大其应用范围。本发明充分利用Mg-Gd-Zn合金的特性,通过合金成分、均匀化退火制度与等径角挤压工艺之间的紧密配合,实现了合金强度和塑性的同步显著提升,对含LPSO相镁合金的塑性成形及性能优化具有重要的指导意义。As a severe plastic deformation process, equal-diameter angular extrusion has the advantage of accumulating plastic strain without changing the initial shape of the billet. In recent years, it has been widely used in processing magnesium alloys to refine grains, accumulate dislocations, and improve strength. However, the conventional equal angular extrusion process often reduces the elongation while increasing the strength of the alloy. Therefore, there is an urgent need for a forming process that can simultaneously strengthen the plasticized Mg-Gd-Zn alloy to improve its comprehensive mechanical properties and expand its application range. The invention makes full use of the characteristics of the Mg-Gd-Zn alloy, through the close cooperation between the alloy composition, the uniform annealing system and the equal-diameter angular extrusion process, the synchronous and significant improvement of the alloy strength and plasticity is realized, and the magnesium containing LPSO phase The plastic forming and performance optimization of alloys have important guiding significance.

发明内容Contents of the invention

为了同时提升Mg-Gd-Zn合金的强度与塑性,使其综合力学性能满足更高的服役要求,本发明提供一种Mg-Gd-Zn合金的成形工艺,具体技术方案如下。In order to simultaneously improve the strength and plasticity of the Mg-Gd-Zn alloy so that its comprehensive mechanical properties meet higher service requirements, the invention provides a forming process for the Mg-Gd-Zn alloy, and the specific technical scheme is as follows.

一种Mg-Gd-Zn合金的成形工艺,主要包括以下步骤:A forming process of Mg-Gd-Zn alloy mainly comprises the following steps:

A.铸造并机械加工出横截面边长为40-60mm、长度为60-120mm的Mg-Gd-Zn合金长方体锭坯;合金的质量百分比成分为Gd:4.0-7.0%、Zn:0.5-1.5%,其余为Mg和不可去除的杂质元素;A. Casting and machining a Mg-Gd-Zn alloy cuboid ingot with a side length of 40-60mm and a length of 60-120mm; the mass percentage of the alloy is Gd: 4.0-7.0%, Zn: 0.5-1.5 %, the rest are Mg and non-removable impurity elements;

B.对锭坯进行均匀化退火处理;B. Carry out homogenization annealing treatment to ingot;

C.在角度为90°的模具中对均匀化退火后的锭坯进行等径角挤压;挤压前,分别将锭坯和模具加热至300-400℃保温1-3h;保温结束后取出锭坯装入模具,立即用液压机将锭坯沿长度方向开始挤压,共挤压4-8道次;模具和样品中途不加热,通过自然冷却控制每道次挤压时锭坯表面温度相对于前一道次降低20-50℃;C. Extrude the homogenized annealed ingot in a mold with an angle of 90°; before extrusion, heat the ingot and the mold to 300-400°C for 1-3 hours; take it out after the heat preservation The ingot is loaded into the mold, and the ingot is immediately extruded along the length direction with a hydraulic press, co-extruded for 4-8 passes; the mold and the sample are not heated in the middle, and the surface temperature of the ingot is controlled by natural cooling during each pass. 20-50°C lower than the previous pass;

D.挤压完成后立即淬火处理,水温为20-40℃。D. Quenching immediately after extrusion, the water temperature is 20-40°C.

优选地,所述步骤B中,均匀化退火工艺为:495-525℃保温15-40h后,置于450-480℃保温3-10h,再以1-10℃/min的速度降至室温。Preferably, in the step B, the homogenization annealing process is as follows: heat at 495-525°C for 15-40h, heat at 450-480°C for 3-10h, and then cool down to room temperature at a rate of 1-10°C/min.

优选地,所述步骤C中,挤压速率为4-8mm/min。Preferably, in the step C, the extrusion rate is 4-8 mm/min.

优选地,所述步骤C中,挤压终了时锭坯表面温度为140-200℃。Preferably, in the step C, the surface temperature of the billet at the end of extrusion is 140-200°C.

其中,所述步骤C中每道次等径角挤压时锭坯长度方向首尾依次对调,且样品不沿长度方向转动。Wherein, in the step C, during each pass of equal radial angle extrusion, the length direction of the ingot is reversed sequentially from the beginning to the end, and the sample does not rotate along the length direction.

其中,所述步骤D中淬火后构件沿挤压方向的室温屈服强度≥200MPa、抗拉强度≥250MPa、断后延伸率≥10%。Wherein, the room temperature yield strength of the member after quenching in the step D along the extrusion direction is ≥ 200 MPa, the tensile strength is ≥ 250 MPa, and the elongation after fracture is ≥ 10%.

上述方案中,对长方体铸锭进行均匀化处理的目的主要包括以下几个方面:在495-525℃保温15-40h是为了促进铸态合金中的共晶组织溶解,使Gd、Zn原子向Mg基体内充分扩散,为后续在α-Mg晶粒内析出大量LPSO相提供充足的固溶原子;此外可使铸锭显微组织更均匀,消除铸造残余应力,提升其可加工性。在450-480℃保温3-10h可促使α-Mg晶粒内部均匀地形成层错,使Gd、Zn元素充分在层错附近聚集,为后续针状LPSO相的大量形核及生长提供有利场所。随后以1-10℃/min的速度降至室温,一方面Gd、Zn元素固溶度随温度下降而降低,从而能以LPSO相的形式在层错位置析出;另一方面,防止温度下降过快而显著降低固溶原子的扩散速率,导致LPSO相的析出被严重抑制。通过该工艺的均匀化处理,在Mg-Gd-Zn合金α-Mg晶粒内部调控出密集的针状LPSO相,为后续广泛的LPSO相扭折变形奠定组织基础。In the above scheme, the purpose of homogenizing the rectangular parallelepiped ingot mainly includes the following aspects: holding at 495-525°C for 15-40h is to promote the dissolution of the eutectic structure in the as-cast alloy, so that the Gd and Zn atoms are transferred to the Mg Sufficient diffusion in the matrix provides sufficient solid-solution atoms for the subsequent precipitation of a large amount of LPSO phase in the α-Mg grains; in addition, it can make the microstructure of the ingot more uniform, eliminate casting residual stress, and improve its machinability. Insulation at 450-480°C for 3-10h can promote the uniform formation of stacking faults inside the α-Mg grains, so that Gd and Zn elements can fully gather near the stacking faults, providing a favorable place for the subsequent massive nucleation and growth of needle-like LPSO phases . Then it drops to room temperature at a rate of 1-10°C/min. On the one hand, the solid solubility of Gd and Zn elements decreases with the decrease of temperature, so that they can be precipitated at the stacking fault position in the form of LPSO phase; on the other hand, it prevents the temperature from falling too much Rapidly and significantly reduce the diffusion rate of solid-solution atoms, resulting in the severe inhibition of the precipitation of the LPSO phase. Through the homogenization treatment of this process, a dense needle-like LPSO phase is regulated inside the α-Mg grains of the Mg-Gd-Zn alloy, which lays the foundation for the subsequent extensive LPSO phase kink deformation.

以300-400℃为初始温度进行每道次降温幅度为20-50℃的等径角挤压,既可以防止合金在变形过程中因温度过低而开裂,又抑制了合金的非基面滑移。当合金经过首尾依次对调、不沿长度方向转动的1-3次挤压后,密集的针状LPSO相倾向于沿特定方向平行排列,该取向也导致LPSO相基面滑移受抑制。后续4-8道次的挤压促使这些针状LPSO相在基面、非基面滑移同时受抑制的情况下发生广泛的扭折变形并形成大量扭折带,这些扭折带既可以阻碍位错运动又阻碍了微裂纹的扩张,可同时显著提升合金的强度与延伸率。然而,继续增加挤压道次将导致LPSO相被破碎、细化,扭折带也随之减少或消失,合金强度可略微提升,但延伸率明显下降。淬火处理可保持挤压结束后的组织,防止在空冷过程中发生再结晶从而破坏扭折带。通过上述成形工艺,获得大量LPSO相扭折带,实现Mg-Gd-Zn合金强度和塑性的同步显著提升。With the initial temperature of 300-400°C, the equal-diameter angular extrusion with a cooling range of 20-50°C per pass can not only prevent the alloy from cracking due to too low temperature during the deformation process, but also inhibit the non-base surface slip of the alloy. shift. When the alloy undergoes 1-3 extrusions with head-to-tail rotation and no rotation along the length direction, the dense needle-like LPSO phase tends to be arranged in parallel in a specific direction, and this orientation also leads to the inhibition of LPSO phase basal slip. Subsequent extrusion of 4-8 passes prompts these acicular LPSO phases to undergo extensive kink deformation and form a large number of kink bands under the condition that the basal plane and non-basal plane slip are simultaneously suppressed, and these kink bands can hinder The dislocation movement hinders the expansion of microcracks, which can significantly improve the strength and elongation of the alloy at the same time. However, continuing to increase the number of extrusion passes will cause the LPSO phase to be broken and refined, and the kink band will also decrease or disappear. The strength of the alloy can be slightly increased, but the elongation is significantly reduced. Quenching treatment can maintain the structure after extrusion and prevent recrystallization during air cooling to destroy the kink band. Through the above forming process, a large number of LPSO phase kink bands are obtained, and the strength and plasticity of the Mg-Gd-Zn alloy are significantly improved simultaneously.

附图说明Description of drawings

图1是实施例1中等径角挤压成品的宏观照片;Fig. 1 is the macrophotograph of equal-diameter angular extrusion finished product in embodiment 1;

图2是实施例1中均匀化退火态合金的扫描电镜显微组织;Fig. 2 is the scanning electron microscope microstructure of uniform annealed state alloy in embodiment 1;

图3是实施例1中等径角挤压成品的扫描电镜显微组织;Fig. 3 is the scanning electron microscope microstructure of the equal diameter angular extrusion finished product in embodiment 1;

图4是实施例2中等径角挤压成品的扫描电镜显微组织;Fig. 4 is the scanning electron microscope microstructure of the equal diameter angular extrusion finished product in embodiment 2;

图5是对比例1中等径角挤压成品的扫描电镜显微组织;Fig. 5 is the scanning electron microscope microstructure of the equal-diameter angular extrusion finished product in Comparative Example 1;

图6是对比例2中等径角挤压成品的扫描电镜显微组织;Fig. 6 is the scanning electron microscope microstructure of the equal-diameter angular extrusion finished product in Comparative Example 2;

图7是对比例3中等径角挤压成品的扫描电镜显微组织;Fig. 7 is the scanning electron microscope microstructure of the equal-diameter angular extrusion finished product in Comparative Example 3;

图8是实施例与对比例中样品的室温拉伸应力应变曲线。Fig. 8 is the tensile stress-strain curve at room temperature of samples in Examples and Comparative Examples.

具体实施方式Detailed ways

本发明通过调节成形工艺参数,做了大量对比实验。下面例举部分实施例对本发明作进一步说明。这些实施例是用于说明本发明,而不是对本发明的限制,在本发明构思前提下对本发明工艺进行改进,都属于本发明保护的范围。In the present invention, a large number of comparative experiments have been done by adjusting the forming process parameters. Some examples are given below to further illustrate the present invention. These examples are used to illustrate the present invention, but not to limit the present invention. Improvements to the process of the present invention under the premise of the concept of the present invention all belong to the protection scope of the present invention.

实施例1Example 1

铸造并机加工出尺寸为60×60×120mm的长方体锭坯,铸锭质量百分比含量为Mg-7.0Gd-0.5Zn。均匀化退火工艺为525℃保温15h后置于480℃保温3h,再以10℃/min的速度降温至室温。在角度为90°的模具中对均匀化态锭坯进行等径角挤压。挤压前,将锭坯和模具加热至400℃保温1h。保温结束后取出锭坯装入模具,立即用液压机将锭坯沿长度方向开始挤压,共挤压4道次,每道次锭坯长度方向首尾依次对调且样品不沿长度方向转动,挤压速率为8mm/min。模具和样品中途不加热,通过自然冷却控制每道次挤压时锭坯表面温度相对于前一道次降低50℃,挤压终了时锭坯表面温度为200℃,立即在25℃的水中进行淬火处理,最终得到成品实物如图1所示。均匀化退火态合金的扫描照片见附图2,沿长度方向的室温拉伸力学性能列于表1,应力应变曲线见附图8。挤压成品的扫描照片见附图3,沿长度方向的室温拉伸力学性能列于表1,应变应变曲线见附图8。A cuboid ingot with a size of 60×60×120 mm is cast and machined, and the mass percentage content of the ingot is Mg-7.0Gd-0.5Zn. The homogenization annealing process is to hold at 525°C for 15 hours, then place at 480°C for 3 hours, and then cool down to room temperature at a rate of 10°C/min. The homogenized ingot is subjected to equal-diameter angular extrusion in a die with an angle of 90°. Before extrusion, heat the billet and mold to 400°C for 1 hour. After the heat preservation is over, take out the ingot and put it into the mold, and immediately use a hydraulic press to extrude the ingot along the length direction, and extrude 4 times in total. The rate is 8mm/min. The mold and the sample are not heated in the middle, and the surface temperature of the ingot is lowered by 50°C during each pass of extrusion by natural cooling, and the surface temperature of the billet is 200°C at the end of extrusion, and it is quenched in water at 25°C immediately After processing, the finished product is finally obtained as shown in Figure 1. The scanning photo of the homogenized annealed alloy is shown in Figure 2, the tensile mechanical properties at room temperature along the length direction are listed in Table 1, and the stress-strain curve is shown in Figure 8. The scanned photo of the extruded product is shown in Figure 3, the tensile mechanical properties at room temperature along the length direction are listed in Table 1, and the strain-strain curve is shown in Figure 8.

实施例2Example 2

铸造并机加工出尺寸为40×40×60mm的长方体锭坯,铸锭质量百分比含量为Mg-4.0Gd-1.5Zn。均匀化退火工艺为495℃保温40h后置于450℃保温10h,再以1℃/min的速度降温至室温。在角度为90°的模具中对均匀化态锭坯进行等径角挤压。挤压前,将锭坯和模具加热至300℃保温3h。保温结束后取出锭坯装入模具,立即用液压机将锭坯沿长度方向开始挤压,共挤压8道次,每道次锭坯长度方向首尾依次对调且样品不沿长度方向转动,挤压速率为4mm/min。模具和样品中途不加热,通过自然冷却控制每道次挤压时锭坯表面温度相对于前一道次降低20℃,挤压终了时锭坯表面温度为140℃,立即在30℃的水中进行淬火处理。挤压成品的扫描照片见附图4,沿长度方向的室温拉伸力学性能列于表1,应力应变曲线见附图8。A cuboid ingot with a size of 40×40×60 mm is cast and machined, and the mass percentage content of the ingot is Mg-4.0Gd-1.5Zn. The homogenization annealing process is to hold at 495°C for 40 hours, then place at 450°C for 10 hours, and then cool down to room temperature at a rate of 1°C/min. The homogenized ingot is subjected to equal-diameter angular extrusion in a die with an angle of 90°. Before extrusion, heat the billet and mold to 300°C for 3 hours. After the heat preservation is over, take out the ingot and put it into the mold, and immediately use a hydraulic press to extrude the ingot along the length direction, and extrude 8 times in total. The rate is 4 mm/min. The mold and sample are not heated in the middle, and the surface temperature of the ingot is lowered by 20°C during each pass of extrusion by natural cooling, and the surface temperature of the billet is 140°C at the end of extrusion, and it is quenched in water at 30°C immediately deal with. The scanned photo of the extruded product is shown in Figure 4, the tensile mechanical properties at room temperature along the length direction are listed in Table 1, and the stress-strain curve is shown in Figure 8.

实施例3Example 3

铸造并机加工出尺寸为50×50×100mm的长方体锭坯,铸锭质量百分比含量为Mg-5.7Gd-1.1Zn。均匀化退火工艺为515℃保温25h后置于465℃保温7h,再以5℃/min的速度降温至室温。在角度为90°的模具中对均匀化态锭坯进行等径角挤压。挤压前,将锭坯和模具加热至350℃保温2h。保温结束后取出锭坯装入模具,立即用液压机将锭坯沿长度方向开始挤压,共挤压6道次,每道次锭坯长度方向首尾依次对调且样品不沿长度方向转动,挤压速率为6mm/min。模具和样品中途不加热,通过自然冷却控制每道次挤压时锭坯表面温度相对于前一道次降低30℃,挤压终了时锭坯表面温度为170℃,立即在30℃的水中进行淬火处理。沿长度方向的室温拉伸力学性能列于表1,应力应变曲线见附图8。A cuboid ingot with a size of 50×50×100 mm is cast and machined, and the mass percentage content of the ingot is Mg-5.7Gd-1.1Zn. The homogenization annealing process is to hold at 515°C for 25h, then place at 465°C for 7h, and then cool down to room temperature at a rate of 5°C/min. The homogenized ingot is subjected to equal-diameter angular extrusion in a die with an angle of 90°. Before extrusion, heat the billet and mold to 350°C for 2 hours. After the heat preservation is over, take out the ingot and put it into the mold, and immediately use a hydraulic press to extrude the ingot along the length direction, and extrude 6 times in total. The rate is 6 mm/min. The mold and sample are not heated in the middle, and the surface temperature of the ingot is lowered by 30°C during each pass of extrusion by natural cooling, and the surface temperature of the billet is 170°C at the end of extrusion, and it is quenched in water at 30°C immediately deal with. The tensile mechanical properties at room temperature along the length direction are listed in Table 1, and the stress-strain curve is shown in Figure 8.

对比例1Comparative example 1

铸造并机加工出尺寸为60×60×120mm的长方体锭坯,铸锭质量百分比含量为Mg-7.0Gd-0.5Zn。均匀化退火工艺为525℃保温15h后空冷至室温。在角度为90°的模具中对均匀化态锭坯进行等径角挤压。挤压前,将锭坯和模具加热至400℃保温1h。保温结束后取出锭坯装入模具,立即用液压机将锭坯沿长度方向开始挤压,共挤压4道次,每道次锭坯长度方向首尾依次对调且样品不沿长度方向转动,挤压速率为8mm/min。模具和样品中途不加热,通过自然冷却控制每道次挤压时锭坯表面温度相对于前一道次降低50℃,挤压终了时锭坯表面温度为200℃,立即在25℃的水中进行淬火处理。挤压成品的扫描照片见附图5,沿长度方向的室温拉伸力学性能列于表1,应力应变曲线见附图8。A cuboid ingot with a size of 60×60×120 mm is cast and machined, and the mass percentage content of the ingot is Mg-7.0Gd-0.5Zn. The homogenization annealing process is to hold at 525°C for 15 hours and then air cool to room temperature. The homogenized ingot is subjected to equal-diameter angular extrusion in a die with an angle of 90°. Before extrusion, heat the billet and mold to 400°C for 1 hour. After the heat preservation is over, take out the ingot and put it into the mold, and immediately use a hydraulic press to extrude the ingot along the length direction, and extrude 4 times in total. The rate is 8mm/min. The mold and the sample are not heated in the middle, and the surface temperature of the ingot is lowered by 50°C during each pass of extrusion by natural cooling, and the surface temperature of the billet is 200°C at the end of extrusion, and it is quenched in water at 25°C immediately deal with. The scanned photo of the extruded product is shown in Figure 5, the tensile mechanical properties at room temperature along the length direction are listed in Table 1, and the stress-strain curve is shown in Figure 8.

对比例2Comparative example 2

铸造并机加工出尺寸为60×60×120mm的长方体锭坯,铸锭质量百分比含量为Mg-7.0Gd-0.5Zn。均匀化退火工艺为525℃保温15h后置于480℃保温3h,再以10℃/min的速度降温至室温。在角度为90°的模具中对均匀化态锭坯进行等径角挤压。挤压前,将锭坯和模具加热至450℃保温1h。保温结束后取出锭坯装入模具,立即用液压机将锭坯沿长度方向开始挤压,共挤压4道次,每道次锭坯长度方向首尾依次对调且样品不沿长度方向转动,挤压速率为8mm/min。模具和样品中途不加热,通过自然冷却控制每道次挤压时锭坯表面温度相对于前一道次降低50℃,挤压终了时锭坯表面温度为250℃,立即在25℃的水中进行淬火处理。挤压成品的扫描照片见附图6,沿长度方向的室温拉伸力学性能列于表1,应力应变曲线见附图8。A cuboid ingot with a size of 60×60×120 mm is cast and machined, and the mass percentage content of the ingot is Mg-7.0Gd-0.5Zn. The homogenization annealing process is to hold at 525°C for 15 hours, then place at 480°C for 3 hours, and then cool down to room temperature at a rate of 10°C/min. The homogenized ingot is subjected to equal-diameter angular extrusion in a die with an angle of 90°. Before extrusion, heat the billet and mold to 450°C for 1 hour. After the heat preservation is over, take out the ingot and put it into the mold, and immediately use a hydraulic press to extrude the ingot along the length direction, and extrude 4 times in total. The rate is 8mm/min. The mold and sample are not heated in the middle, and the surface temperature of the ingot is lowered by 50°C during each pass of extrusion by natural cooling, and the surface temperature of the billet is 250°C at the end of extrusion, and quenched in water at 25°C immediately deal with. The scanned photo of the extruded product is shown in Figure 6, the tensile mechanical properties at room temperature along the length direction are listed in Table 1, and the stress-strain curve is shown in Figure 8.

对比例3Comparative example 3

铸造并机加工出尺寸为40×40×60mm的长方体锭坯,铸锭质量百分比含量为Mg-4.0Gd-1.5Zn。均匀化退火工艺为495℃保温40h后置于450℃保温10h,再以1℃/min的速度降温至室温。在角度为90°的模具中对均匀化态锭坯进行等径角挤压。挤压前,将锭坯和模具加热至300℃保温3h。保温结束后取出锭坯装入模具,立即用液压机将锭坯沿长度方向开始挤压,共挤压10道次,每道次锭坯长度方向首尾依次对调且样品不沿长度方向转动,挤压速率为4mm/min。模具和样品中途不加热,通过自然冷却控制每道次挤压时锭坯表面温度相对于前一道次降低20℃,挤压终了时锭坯表面温度为100℃,立即在30℃的水中进行淬火处理。挤压成品的扫描照片见附图7,沿长度方向的室温拉伸力学性能列于表1,应力应变曲线见附图8。A cuboid ingot with a size of 40×40×60 mm is cast and machined, and the mass percentage content of the ingot is Mg-4.0Gd-1.5Zn. The homogenization annealing process is to hold at 495°C for 40 hours, then place at 450°C for 10 hours, and then cool down to room temperature at a rate of 1°C/min. The homogenized ingot is subjected to equal-diameter angular extrusion in a die with an angle of 90°. Before extrusion, heat the billet and mold to 300°C for 3 hours. After the heat preservation is over, take out the ingot and put it into the mold, and immediately use a hydraulic press to extrude the ingot along the length direction, and extrude 10 times in total. The rate is 4 mm/min. The mold and sample are not heated in the middle, and the surface temperature of the ingot is lowered by 20°C during each pass of extrusion by natural cooling, and the surface temperature of the billet is 100°C at the end of extrusion, and it is quenched in water at 30°C immediately deal with. The scanned photo of the extruded product is shown in Figure 7, the tensile mechanical properties at room temperature along the length direction are listed in Table 1, and the stress-strain curve is shown in Figure 8.

表1实施例与对比例中镁合金构件力学性能Mechanical properties of magnesium alloy members in the embodiment and comparative examples in table 1

从图2可以看出Mg-Gd-Zn合金经过本发明所述工艺的均匀化退火后出现了密集的针状LPSO相。从图3、4可以看出,实施例1、2中的等径角挤压成品形成了大量扭折带。同时,从表1、图8可以看出,实施例1、2的Mg-Gd-Zn合金等径角挤压构件的增强增塑效果明显优于对比例1-3。It can be seen from Fig. 2 that dense acicular LPSO phases appear in the Mg-Gd-Zn alloy after homogenization annealing in the process of the present invention. It can be seen from Figures 3 and 4 that a large number of twisted bands are formed in the equal diameter angular extrusion products in Examples 1 and 2. At the same time, it can be seen from Table 1 and Figure 8 that the enhanced plasticizing effect of the Mg-Gd-Zn alloy ESA components of Examples 1 and 2 is significantly better than that of Comparative Examples 1-3.

结合图3和图5,通过对比实施例1和对比例1,发现若不采用本发明所述均匀化退火工艺,即便后续等径角挤压工艺相同仍不能获得大量扭折带,导致合金强度和塑性的提升效果差。结合图3和图6,通过对比实施例1和对比例2,发现锭坯和模具的保温温度过高,促进了合金的动态再结晶及LPSO相的溶解,使得扭折带的数量急剧下降,导致合金的强度显著降低,而延伸率相对于均匀化态略微提升。结合图4和图7,通过对比实施例2和对比例3,发现挤压道次的增加和终了温度的降低导致试样中LPSO相的破碎和溶解程度增加、晶粒细化、扭折带数量减少,虽然强度的提升效果更好,但延伸率急剧下降,不能起到同步增强增塑的作用,合金的综合力学性能不如实施例。Combining Figure 3 and Figure 5, by comparing Example 1 and Comparative Example 1, it is found that if the homogenization annealing process described in the present invention is not adopted, even if the subsequent equal-diameter angular extrusion process is the same, a large number of kink bands cannot be obtained, resulting in an increase in the strength of the alloy. And the effect of improving plasticity is poor. Combining Figure 3 and Figure 6, by comparing Example 1 and Comparative Example 2, it is found that the holding temperature of the ingot and the mold is too high, which promotes the dynamic recrystallization of the alloy and the dissolution of the LPSO phase, resulting in a sharp decrease in the number of kink bands. As a result, the strength of the alloy is significantly reduced, while the elongation is slightly increased relative to the homogenized state. Combining Figure 4 and Figure 7, by comparing Example 2 and Comparative Example 3, it is found that the increase in the number of extrusion passes and the decrease in the final temperature lead to an increase in the degree of fragmentation and dissolution of the LPSO phase in the sample, grain refinement, and kink bands. If the number is reduced, although the effect of improving the strength is better, the elongation drops sharply, which cannot play the role of synchronous reinforcement and plasticization, and the comprehensive mechanical properties of the alloy are not as good as those of the examples.

上面结合附图对本发明的实施例进行了描述,在不冲突的情况下,本发明中的实施例及实施例中的特征可以相互组合。本发明并不局限于上述的具体实施方式,上述的具体实施方式仅仅是示意性的,而不是局限性的,本领域的普通技术人员在本发明的启示下,在不脱离本发明宗旨和权利要求所保护的范围情况下,还可做出很多形式,这些均属于本发明的保护范围之内。The embodiments of the present invention have been described above with reference to the accompanying drawings, and the embodiments and features in the embodiments of the present invention can be combined with each other if there is no conflict. The present invention is not limited to the above specific implementation, the above specific implementation is only illustrative, rather than limiting, those skilled in the art under the enlightenment of the present invention, without departing from the purpose and rights of the present invention In the case of requiring the scope of protection, many forms can also be made, and these all belong to the scope of protection of the present invention.

Claims (7)

1.一种Mg-Gd-Zn合金的成形工艺,其特征在于,主要包括以下步骤:1. a forming process of Mg-Gd-Zn alloy, is characterized in that, mainly comprises the following steps: A.铸造并机械加工出横截面边长为40-60mm、长度为60-120mm的Mg-Gd-Zn合金长方体锭坯;合金的质量百分比成分为Gd:4.0-7.0%、Zn:0.5-1.5%,其余为Mg和不可去除的杂质元素;A. Casting and machining a Mg-Gd-Zn alloy cuboid ingot with a side length of 40-60mm and a length of 60-120mm; the mass percentage of the alloy is Gd: 4.0-7.0%, Zn: 0.5-1.5 %, the rest are Mg and non-removable impurity elements; B.对锭坯进行均匀化退火处理;B. Carry out homogenization annealing treatment to ingot; C.在角度为90°的模具中对均匀化退火后的锭坯进行等径角挤压;挤压前,分别将锭坯和模具加热至300-400℃保温1-3h;保温结束后取出锭坯装入模具,立即用液压机将锭坯沿长度方向开始挤压,共挤压4-8道次;通过自然冷却控制每道次挤压时锭坯表面温度相对于前一道次降低20-50℃;C. Extrude the homogenized annealed ingot in a mold with an angle of 90°; before extrusion, heat the ingot and the mold to 300-400°C for 1-3 hours; take it out after the heat preservation The ingot is loaded into the mold, and the ingot is immediately extruded along the length direction with a hydraulic press, co-extruded for 4-8 passes; the surface temperature of the billet is reduced by 20-20% compared with the previous pass through natural cooling control. 50°C; D.挤压完成后立即淬火处理。D. Quenching treatment immediately after extrusion. 2.根据权利要求1所述的一种Mg-Gd-Zn合金的成形工艺,其特征在于:所述步骤B中,均匀化退火工艺为:495-525℃保温15-40h后,置于450-480℃保温3-10h,再以1-10℃/min的速度降至室温。2. The forming process of a Mg-Gd-Zn alloy according to claim 1, characterized in that: in the step B, the homogenization annealing process is: after holding at 495-525°C for 15-40h, place it at 450 Incubate at -480°C for 3-10h, then cool down to room temperature at a rate of 1-10°C/min. 3.根据权利要求1所述的一种Mg-Gd-Zn合金的成形工艺,其特征在于:所述步骤C中,挤压速率为4-8mm/min。3. The forming process of a Mg-Gd-Zn alloy according to claim 1, characterized in that: in the step C, the extrusion rate is 4-8 mm/min. 4.根据权利要求1所述的一种Mg-Gd-Zn合金的成形工艺,其特征在于:所述步骤C中,挤压终了时锭坯表面温度为140-200℃。4. The forming process of a Mg-Gd-Zn alloy according to claim 1, characterized in that: in the step C, the surface temperature of the billet at the end of extrusion is 140-200°C. 5.根据权利要求1所述的一种Mg-Gd-Zn合金的成形工艺,其特征在于:所述步骤C中,每道次等径角挤压时锭坯长度方向首尾依次对调,且样品不沿长度方向转动。5. The forming process of a Mg-Gd-Zn alloy according to claim 1, characterized in that: in the step C, the length direction of the ingot is reversed sequentially from the beginning to the end during each pass of equal diameter angular extrusion, and the sample Does not rotate along length. 6.根据权利要求1所述的一种Mg-Gd-Zn合金的成形工艺,其特征在于:所述步骤D中,淬火处理的水温为20-40℃。6. The forming process of a Mg-Gd-Zn alloy according to claim 1, characterized in that: in the step D, the water temperature for the quenching treatment is 20-40°C. 7.根据权利要求1所述的一种Mg-Gd-Zn合金的成形工艺,其特征在于:所述步骤D中淬火后构件沿挤压方向的室温屈服强度≥200MPa、抗拉强度≥250MPa、断后延伸率≥10%。7. The forming process of a Mg-Gd-Zn alloy according to claim 1, characterized in that: in the step D, the room temperature yield strength of the member after quenching along the extrusion direction is ≥200MPa, the tensile strength is ≥250MPa, Elongation after breaking ≥ 10%.
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CN112981204A (en) * 2021-03-19 2021-06-18 中北大学 High-strength Mg-Gd-Y-Zn-Zr rare earth magnesium alloy and preparation method thereof

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CN106756370A (en) * 2016-12-10 2017-05-31 哈尔滨工业大学 A kind of anti-flaming Mg Gd Y Zn Zr alloys of high-strength anticorrosion and preparation method thereof
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