CN113073244A - High-strength and high-toughness rare earth heat-resistant magnesium alloy and preparation method thereof - Google Patents

High-strength and high-toughness rare earth heat-resistant magnesium alloy and preparation method thereof Download PDF

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CN113073244A
CN113073244A CN202110294891.6A CN202110294891A CN113073244A CN 113073244 A CN113073244 A CN 113073244A CN 202110294891 A CN202110294891 A CN 202110294891A CN 113073244 A CN113073244 A CN 113073244A
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magnesium alloy
heat
rare earth
strength
heating
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于建民
张治民
李兆灿
王强
李国俊
张紫薇
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North University of China
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North University of China
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    • 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
    • C22CALLOYS
    • C22C1/00Making non-ferrous alloys
    • C22C1/02Making non-ferrous alloys by melting
    • 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

Abstract

The invention discloses a high-strength and high-toughness rare earth heat-resistant magnesium alloy which comprises the following chemical components in percentage by mass: 8.0-10.8% of Gd, 3.1-4.0% of Y, 1.8-2.2% of Zn, 0.4-0.5% of Zr, and the balance of magnesium and inevitable impurity elements. Also discloses a preparation method thereof, which sequentially comprises the following steps: (1) preparing a magnesium alloy cast rod; (2) homogenizing the bar stock: heating and preserving heat of the magnesium alloy bar by adopting a grading homogenization system, then heating and preserving heat for homogenization treatment; (3) upsetting-extruding composite deformation: putting the bar stock into a heated upsetting-extruding composite die, and circularly upsetting and extruding for multiple times to obtain the high-strength-toughness deformation state rare earth heat-resistant magnesium alloy material; (4) solid solution and aging treatment: the heat treatment adopts solid solution aging treatment and heat preservation, and hot water quenching is adopted after discharging; and cooling to room temperature, aging and preserving heat. The magnesium alloy prepared by the scheme has good quality, and has more obvious high tensile strength and high elongation compared with the common magnesium alloy in the market.

Description

High-strength and high-toughness rare earth heat-resistant magnesium alloy and preparation method thereof
Technical Field
The invention relates to the technical field of deformation processing of non-ferrous metal materials, belongs to the technical field of metal materials, and particularly relates to a high-strength and high-toughness rare earth heat-resistant magnesium alloy and a preparation method thereof.
Background
Aerospace and national defense military equipment such as carrier rockets, space shuttles, strategic missiles and the like require key components to have the characteristics of high performance, light weight, high efficiency and the like. And more than 90% of conventional rocket/missile hoods, oil tanks and three cabin sections are made of aluminum materials, so that the phenomenon of overweight is serious, and various fighting and technical indexes are obviously influenced. Meanwhile, the aluminum alloy performance strengthening mechanism determines that the strength of the aluminum alloy rapidly decreases along with the rise of temperature, the aluminum alloy can not be used at the temperature of more than 250 ℃, and the requirement of the service environment of key bearing parts of major equipment can not be met.
The magnesium alloy is the lightest metal structure material in the current engineering application, has good heat dissipation and damping and anti-seismic performance, is an ideal material for light weight, energy conservation and emission reduction, and has wide application prospect. The common commercial magnesium alloy often generates strong basal plane texture in the machining process, which causes poor formability and asymmetric yield, and limits the application of the alloy. The trace addition of Rare Earth (RE) elements to magnesium alloys has proven to be an effective way to modify basal plane texture, both during thermomechanical processing and during subsequent annealing, leading to a significant increase in ductility. And the toughness of the steel plate can be greatly improved by combining large plastic deformation, and the service requirements of some special environments are met. The large plastic deformation can obviously improve the mechanical property of the magnesium alloy, thereby becoming the first choice for manufacturing a large-scale high-performance magnesium alloy main bearing component.
Chinese patent application No. 202010685440.0 discloses a high-strength rare earth heat-resistant magnesium alloy and a preparation method thereof, wherein the cast alloy is subjected to homogenization heat treatment, and after hot extrusion and solid solution aging, the room-temperature tensile strength is more than 250MPa, and the tensile strength at 200 ℃ is more than 190M Pa; chinese patent with application number 201911082720.6 discloses an LPSO phase reinforced high-damping rare earth magnesium alloy and a preparation method thereof, wherein a semi-continuous casting process is adopted, so that the tensile strength is more than 180MPa, and the elongation is more than 10%; the Chinese patent with the application number of 201910975737.8 discloses a rare earth magnesium alloy with ultrahigh heat conductivity coefficient and a preparation method thereof, and after the alloy is cast into a die, the tensile strength is more than 190MPa, the yield strength is more than 130MPa, and the elongation is more than 3%. The tensile strength of the rare earth magnesium alloy related to the above patents is less than 300MPa, and the whole bending strength is relatively low, so that the rare earth magnesium alloy is not suitable for bearing a large-load stressed member.
Chinese patent with application number 201910403252.1 discloses a high-strength high-plasticity rare earth magnesium alloy and a preparation method thereof, wherein the room-temperature tensile strength of the cast alloy in T6 state is more than 350MPa, and the elongation after fracture is more than 5.0 percent; the Chinese patent with the application number of 201910562454.0 discloses a low-density and medium-high-strength rare earth cast magnesium alloy and a preparation method thereof, wherein after the rare earth magnesium alloy is subjected to solid solution and aging, the density is less than 1.85g/cm3, the tensile strength is more than 320MPa, and the plastic elongation is more than 5 percent; the Chinese patent with the application number of 201910357927.3 discloses a high-strength magnesium alloy containing rare earth and a preparation method thereof, wherein the tensile strength of the rare earth magnesium alloy is 320-355 MPa, the yield strength is 150-170 MPa, and the elongation is 6.3-7.5% after solid solution aging. The rare earth magnesium alloy involved in the above patent has an elongation of less than 8%, relatively poor overall toughness and ductility, and weak resistance of the member to plastic deformation.
Therefore, rare earth magnesium alloys having both high strength and high plasticity are being developed.
Disclosure of Invention
The invention aims to provide a high-strength and high-toughness rare earth heat-resistant magnesium alloy and a preparation method thereof, and the prepared magnesium alloy has good quality and has more obvious high tensile strength and high elongation compared with the common magnesium alloy in the market.
In order to achieve the above purpose, the solution of the invention is: a high-strength and high-toughness rare earth heat-resistant magnesium alloy comprises the following chemical components in percentage by mass: 8.0-10.8% of Gd, 3.1-4.0% of Y, 1.8-2.2% of Zn, 0.4-0.5% of Zr, and the balance of magnesium and inevitable impurity elements.
Preferably, the high-strength and high-toughness rare earth heat-resistant magnesium alloy comprises the following chemical components in percentage by mass: 10.0% of Gd, 3.6% of Y, 2% of Zn, 0.5% of Zr, and the balance of magnesium and inevitable impurity elements.
Preferably, the high-strength and high-toughness rare earth heat-resistant magnesium alloy comprises the following chemical components in percentage by mass: 8.4% of Gd, 3.4% of Y, 2% of Zn, 0.4% of Zr, and the balance of magnesium and inevitable impurity elements.
Preferably, the high-strength and high-toughness rare earth heat-resistant magnesium alloy comprises the following chemical components in percentage by mass: 9.2% of Gd, 3.1% of Y, 1.8% of Zn, 0.5% of Zr, and the balance of magnesium and inevitable impurity elements.
Preferably, the impurity elements comprise Fe, Ni, Cu and Si, and the impurity elements account for the following alloy in percentage by mass: fe is less than or equal to 0.004%, Ni is less than or equal to 0.01%, Cu is less than or equal to 0.01%, and Si is less than or equal to 0.01%.
A preparation method of a high-strength and high-toughness rare earth heat-resistant magnesium alloy comprises the following steps:
(1) preparing a magnesium alloy cast rod: firstly, designing alloy element proportioning materials according to the mass percentage, preparing a magnesium alloy cast rod by adopting semi-continuous casting, and machining the magnesium alloy cast rod into a bar stock after cooling at room temperature;
(2) homogenizing the bar stock: heating the magnesium alloy bar to 300 ℃ by adopting a grading homogenization system, preserving heat for 4 hours, then heating to 525 ℃ and preserving heat for 8 hours for homogenization treatment;
(3) upsetting-extruding composite deformation: putting the bar stock into a heated upsetting-extruding composite die, wherein the heating temperature of the upsetting-extruding composite die is 420-450 ℃, the extrusion ratio is set to be 1.95, the extrusion speed is 2-4 mm/s, and the high-strength and high-toughness deformed rare earth heat-resistant magnesium alloy material is obtained after multi-pass circulating upsetting-extruding;
(4) solid solution and aging treatment: the heat treatment adopts solution aging treatment, the solution temperature is set to 400 ℃, the heat preservation is carried out for 8 hours, and hot water at 80 ℃ is adopted for quenching after discharging; and after cooling to room temperature, carrying out aging treatment at 225 ℃ for 16 h.
Preferably, the specific steps of step (1) include:
(1.1) melting of pure magnesium: smelting the alloy by using a resistance furnace, heating a crucible to 800 ℃, then uniformly paving a layer of covering agent on the bottom of the crucible, putting a pure magnesium block, and scattering the covering agent on the pure magnesium block for protection;
(1.2) addition of alloying elements: after pure magnesium is melted, directly heating the melt to 800 ℃, adding pure Y, preserving heat at 800 ℃, after Y is completely melted, sequentially adding Mg-Gd and Mg-Zr intermediate alloys at 760-780 ℃, and finally adding pure Zn at 750 ℃;
(1.3) stirring: after the alloy elements are completely melted, preserving the heat of the melt at 750 ℃, removing floating slag on the surface of the melt by using a preheated slag removing spoon, and stirring, wherein an up-and-down rolling mode is mainly adopted in the stirring process;
(1.4) refining: after stirring, standing the melt for 3-5min, and refining at 750 ℃ under the protection of argon after the temperature is stable, wherein the refining time is 3-5 min;
(1.5) semi-continuous casting: standing for 10min after refining is finished, introducing the magnesium alloy melt into a crystallizer through a drainage groove at 750 ℃, sealing the bottom of the crystallizer by a guide rod to form a single-opening space, and finishing initial solidification of the magnesium alloy melt in the single-opening space; after the liquid level of the magnesium alloy melt is stable and a solidified shell with a certain thickness is formed, starting a motor to drive a guide rod to move downwards, and simultaneously continuously injecting the magnesium alloy melt into the upper part of a crystallizer; and stopping the casting process after the cast rod reaches a certain length to obtain a magnesium alloy cast rod, and machining the magnesium alloy cast rod into a bar stock after the magnesium alloy cast rod is cooled at room temperature.
Preferably, in the step (3), before the bar is placed in the heated upsetting-extruding composite die, the bar is first placed in a heating furnace for heating, and the heating adopts a step heating system: the primary heating temperature is 300 ℃, and the heat preservation time is 2 hours; the secondary heating temperature is 480 ℃, and the heat preservation time is 6 h.
After the scheme is adopted, the invention has the beneficial effects that:
(1) the high-strength and high-toughness rare earth heat-resistant magnesium alloy has the advantages of high strength and high elongation, wherein the room-temperature tensile strength is more than or equal to 360MPa, and the elongation is more than or equal to 10 percent, so that the high-strength and high-toughness rare earth heat-resistant magnesium alloy is very suitable for aerospace high-end equipment bearing members with higher mechanical property requirements;
(2) the service use temperature of the high-strength and high-toughness rare earth heat-resistant magnesium alloy can reach 200 ℃, and the requirements of light weight, high use temperature, high specific strength and specific rigidity in a high-temperature use environment in model development are met;
(3) compared with alloy products with the same strength and elongation, the high-strength and high-toughness rare earth heat-resistant magnesium alloy has the advantages that the density is smaller, the structural weight of the product is reduced, various tactical and technical indexes can be improved, and the high-strength and high-toughness rare earth heat-resistant magnesium alloy can be widely applied to the fields of aerospace and the like.
The addition amount of Gd element in the magnesium alloy reaches more than 10 wt%, so that the magnesium alloy can obtain remarkable strengthening effect, the performance requirement is met, a large amount of Mg5Gd phase is generated, the phase has high melting point and good thermal stability, the Mg-Gd alloy system has the advantages of high strength and good heat resistance, and the addition of a large amount of heavy rare earth element Gd not only increases the density of the alloy, but also obviously increases the cost of the magnesium alloy. This makes the use of light alloy elements instead of Gd a direction of interest for researchers, which puts demands on light alloy elements: the crystal structures and chemical characteristics of the two are similar, the solid solubility is higher, and the price is cheaper. Y satisfies the above requirements and is an ideal element for substituting Gd. By adding Gd and Y elements, not only can a remarkable strengthening effect be obtained, but also the density of the alloy can be prevented from being increased.
Adding a certain amount of Zn element in Mg-RE alloy can form long-period ordered stacked structure (LPSO). The phase containing LPSO structure has good high-temperature stability and high hardness, and can improve the toughness and the comprehensive mechanical property of the alloy. The LPSO phase has special structure and performance and is an effective strengthening phase in the magnesium alloy, and the existence of the LPSO phase can obviously improve the room temperature and high temperature performance of the magnesium alloy. The LPSO phase has the elastic modulus of 66.7 +/-4.9 GPa, the hardness of 137 +/-35 Hv, the elastic modulus of 40.1 +/-5.2 GPa and the hardness of 31.3 +/-2.2 Hv which are much higher than those of pure magnesium, so that the movement of dislocation can be effectively hindered, and therefore, the LPSO phase can be used as a strengthening phase and can remarkably improve the mechanical properties of the material, such as hardness, strength and the like.
The addition of trace Zr can promote nucleation to form a fine crystal structure, and the fine crystal strengthening effect is achieved.
The homogenization treatment can realize the dissolution of eutectic phase, the proliferation or growth of cubic phase and the grain refinement in the alloy structure evolution process, and is used for making the internal components of the material uniform and eliminating residual stress. At present, a single-stage homogenization system is common, and the phenomena of coarse grains, serious alloy oxidation and the like are caused by overlong heat preservation time or overhigh temperature of the system, so that the mechanical property and the grain size of the alloy are seriously influenced. The grading homogenization system provided by the invention can improve the eutectic phase and the second phase structure form at the crystal boundary, obviously improve the mechanical property of the as-cast alloy, and the toughness of the alloy subjected to grading homogenization treatment is higher than that of a single-stage homogenization system.
The upsetting-extruding composite deformation method is a plastic deformation technology combining two traditional processes of upsetting and forward extrusion, in multi-pass upsetting-extruding composite deformation, the cross section area and the size of a blank are kept unchanged after each pass of upsetting-extruding deformation, the refining of alloy grains can be realized, the crushing of a blocky LPSO phase is promoted, and the dispersion strengthening effect is achieved, so that the upsetting-extruding composite deformation method is applied to practical engineering application as an important large plastic deformation means.
Drawings
FIG. 1 is a schematic view of an upsetting-extruding complex deformation process of the present invention;
FIG. 2 shows the as-cast metallographic structure of the high-toughness rare earth heat-resistant magnesium alloy Mg-10Gd-3.6Y-2Zn-0.5Zr in the first embodiment of the present invention;
FIG. 3 is a deformation structure diagram obtained after the high-toughness rare earth heat-resistant magnesium alloy Mg-10Gd-3.6Y-2Zn-0.5Zr is subjected to two-pass upsetting-extrusion composite deformation at 420 ℃;
FIG. 4 is a scanning electron microscope image of a microstructure obtained after the high-toughness rare earth heat-resistant magnesium alloy Mg-10Gd-3.6Y-2Zn-0.5Zr is subjected to two-pass upsetting-extruding composite deformation at 420 ℃;
FIG. 5 is a deformation structure diagram of the high-toughness rare earth heat-resistant magnesium alloy Mg-10Gd-3.6Y-2Zn-0.5Zr obtained after two-pass upsetting-extruding composite deformation heat treatment at 420 ℃.
Detailed Description
The invention provides a high-strength and high-toughness rare earth heat-resistant magnesium alloy which comprises the following chemical components in percentage by mass: 8.0-10.8% of Gd, 3.1-4.0% of Y, 1.8-2.2% of Zn, 0.4-0.5% of Zr, and the balance of magnesium and inevitable impurity elements.
The impurity elements comprise Fe, Ni, Cu and Si, and the impurity elements account for the following alloy in percentage by mass: fe is less than or equal to 0.004%, Ni is less than or equal to 0.01%, Cu is less than or equal to 0.01%, and Si is less than or equal to 0.01%.
The invention is described in detail below with reference to the accompanying drawings and specific embodiments.
Example one
The high-strength and high-toughness rare earth heat-resistant magnesium alloy comprises the following components in percentage by mass: 10.0 percent of Gd, 3.6 percent of Y, 2 percent of Zn and 0.5 percent of Zr, and the balance of magnesium and inevitable impurity elements, and is prepared into a magnesium alloy rod. The tensile strength and the elongation of the magnesium alloy bar are tested, and the specific test results are shown in table 1.
Table 1 mechanical property data obtained in magnesium alloy bar test prepared in example one
Tensile Strength (Rm)/MPa Yield strength (R)p0.2)/MPa Elongation (A)/%)
First heat 315 226 22
Second heat 323 231 20
Third heat 325 223 20
Fourth heat 313 219 22
The specific preparation method of the alloy comprises the following steps:
(1) preparing a magnesium alloy cast rod: firstly, designing alloy element proportioning materials according to the mass percent, preparing a magnesium alloy cast rod with the diameter of 400 mm multiplied by 4200mm by adopting semi-continuous casting, and machining the magnesium alloy cast rod into a bar with the diameter of 330mm after cooling at room temperature;
(2) homogenizing the cast rod: heating the magnesium alloy cast rod to 300 ℃ by adopting a grading homogenization system, preserving heat for 4 hours, then heating to 525 ℃ and preserving heat for 8 hours for homogenization treatment;
(3) upsetting-extruding composite deformation: putting the bar into a heating furnace for heating, wherein a step heating system is adopted for heating: the primary heating temperature is 300 ℃, and the heat preservation time is 2 hours; the secondary heating temperature is 480 ℃, the heat preservation time is 6h, the upsetting-extruding composite deformation process is shown in figure 1, the upsetting-extruding step is sequentially carried out according to the sequence of (a) → (b) → (c) → (d), two sets of different dies are adopted for upsetting-extruding, the cross section area and the size of the blank after each pass of upsetting-extruding deformation are the same as the initial size and are kept unchanged, the heating temperature of the dies is 420-450 ℃, the extrusion ratio is set to be 1.95, the extrusion speed is 2-4 mm/s, and the high-strength-toughness deformation state rare earth heat-resistant magnesium alloy material is obtained after twice circulating upsetting-extruding.
(4) Solid solution and aging treatment: the heat treatment adopts solid solution aging treatment, the solid solution temperature is set to 420 ℃, the temperature is kept for 8 hours, and hot water at 80 ℃ is adopted for quenching after discharging; and (3) cooling to room temperature, and then aging: the aging temperature is 225 ℃, and the heat preservation time is 16 h.
In the step (1), the step of preparing the magnesium alloy ingot comprises the following steps:
(1.1) melting of pure magnesium: the alloy is smelted by a resistance furnace, a crucible is heated to 800 ℃, then a layer of covering agent is uniformly laid at the bottom of the crucible, a pure Mg block is put on the covering agent, and the covering agent is also scattered on the covering agent for protection.
(1.2) addition of alloying elements: after pure Mg is melted, the melt is directly heated to 800 ℃, pure Y is put in the melt, the temperature is kept at 800 ℃, Mg-Gd and Mg-Zr intermediate alloys are sequentially added at about 760-780 ℃ after Y is completely melted, and finally pure Zn is put in the melt at about 750 ℃.
(1.3) stirring: after the alloy elements are completely melted, the melt is kept at about 750 ℃, the floating slag on the surface of the melt is removed by a preheated slag removing spoon and then is stirred, and the stirring process mainly adopts a mode of rolling up and down.
(1.4) refining: and after stirring, standing the melt for 3-5min, and refining at about 750 ℃ under the protection of argon after the temperature is stable, wherein the refining time is 3-5 min.
(1.5) semi-continuous casting: standing for 10min after refining is finished, introducing the magnesium alloy melt into a crystallizer through a drainage groove at 750 ℃, sealing the bottom of the crystallizer by a guide rod to form a single-opening space, and finishing initial solidification of the magnesium alloy melt in the single-opening space; after the liquid level of the magnesium alloy melt is stable and a solidified shell with a certain thickness is formed, starting a motor to drive a guide rod to move downwards, and simultaneously continuously injecting the magnesium alloy melt into the upper part of a crystallizer; and stopping the casting process after the cast rod reaches a certain length to obtain the magnesium alloy cast rod with the diameter of 400 mm multiplied by 4200 mm.
Through detection, the general room-temperature tensile strength of the magnesium alloy material prepared by the preparation method is more than or equal to 370MPa, the yield strength is more than or equal to 245MPa, the elongation is more than or equal to 11 percent, and the test results are shown in Table 2; the general tensile strength at high temperature (200 ℃) is more than or equal to 290MPa, and the elongation is more than or equal to 11 percent; fatigue strength sigma at room temperature-1125MPa or more, and the test results are shown in Table 3. It can be seen that the alloy exhibits excellent strength and plasticity properties.
TABLE 2 mechanical property data of magnesium alloy bars at room temperature after heat treatment in example I
Figure BDA0002983949970000061
Figure BDA0002983949970000071
TABLE 3 mechanical property data of magnesium alloy bars at 200 ℃ after heat treatment in example I
Tensile Strength (Rm)/MPa Elongation (A)/%)
First heat 330 12
Second heat 335 12
Third heat 338 12.5
Fourth heat 345 12.5
FIG. 2 is the as-cast metallographic structure of the high-toughness heat-resistant rare earth magnesium alloy Mg-10Gd-3.6Y-2Zn-0.5Zr in the first embodiment. FIG. 3 is a deformed structure of the high strength and toughness heat-resistant rare earth magnesium alloy Mg-10Gd-3.6Y-2Zn-0.5Zr in the first embodiment after two-pass upsetting-extruding composite deformation at 420 ℃. It can be seen that the structure after the press deformation is significantly thinned compared to the original cast structure, the average grain size is changed from 154 μm to 8.89 μm, and a bimodal microstructure in which dynamically recrystallized grains coexist with non-dynamically recrystallized grains is present. FIG. 4 is a scanning electron microscope image of a microstructure obtained after two-pass upsetting-extruding composite deformation of the high-toughness rare earth heat-resistant magnesium alloy Mg-10Gd-3.6Y-2Zn-0.5Zr at 420 ℃ in the first embodiment, and it can be seen that after the two-pass upsetting-extruding composite deformation, the discontinuous net-shaped blocky LPSO phase in the initial structure of the alloy is crushed into fine blocky materials and distributed at the grain boundary. Simultaneously, a great deal of fine Mg is precipitated near the grain boundary5(Gd, Y) particle phase. FIG. 5 is a photograph of a deformed structure of the high-toughness rare earth heat-resistant magnesium alloy Mg-10Gd-3.6Y-2Zn-0.5Zr after two-pass upsetting-extruding composite deformation heat treatment at 420 ℃. Compared with the structure of two-pass upsetting-extruding composite deformation, the structure has the advantages that the grains after heat treatment are finer and the sizes of the grains are uniform.
Example two
In the embodiment, the high-strength and high-toughness rare earth heat-resistant magnesium alloy is prepared from the following components in percentage by mass: 8.4% of Gd, 3.4% of Y, 2% of Zn, 0.4% of Zr, and the balance of magnesium and inevitable impurity elements, the alloy being prepared by the same preparation method as in example one, specifically, magnesium alloy cast rods having a diameter of 400X 4200mm were prepared by semi-continuous casting according to (1.1) to (1.5) of step (1) in example 1; then heating the magnesium alloy cast rod to 300 ℃, preserving heat for 4 hours, and then carrying out homogenization treatment for 8 hours at the temperature of 525 ℃; carrying out upsetting-extruding composite deformation on the cast rod after the homogenization treatment: firstly heating a cast rod to 300 ℃, preserving heat for 2h for primary heating, then heating the cast rod to 480 ℃, preserving heat for 6h for secondary heating, carrying out upsetting-extruding composite deformation on the heated rod, wherein the heating temperature of a die is 430 ℃, and the extrusion ratio is 1.95: 1, the extrusion speed is 2 mm/s; carrying out solution treatment on the alloy subjected to upsetting and extrusion at the temperature of 400 ℃ for 8h, and quenching in hot water at the temperature of 80 ℃; and after cooling to room temperature, carrying out aging treatment for 16h at 225 ℃ to obtain a target magnesium alloy rod, and testing the tensile strength and the elongation of the obtained magnesium alloy rod, wherein the specific test results are shown in tables 4, 5 and 6.
EXAMPLE III
In the embodiment, the high-strength and high-toughness rare earth heat-resistant magnesium alloy is prepared from the following components in percentage by mass: 9.2% of Gd, 3.1% of Y, 1.8% of Zn, 0.5% of Zr, and the balance of magnesium and inevitable impurity elements, the alloy being prepared by the same preparation method as in example one, specifically, magnesium alloy cast rods having a diameter of 400X 4200mm were prepared by semi-continuous casting according to (1.1) to (1.5) of step (1) in example 1; then heating the magnesium alloy cast rod to 300 ℃, preserving heat for 4 hours, and then carrying out homogenization treatment for 8 hours at the temperature of 525 ℃; carrying out upsetting-extruding composite deformation on the cast rod after the homogenization treatment: firstly heating a cast rod to 300 ℃, preserving heat for 2h for primary heating, then heating the cast rod to 480 ℃, preserving heat for 6h for secondary heating, carrying out upsetting-extruding composite deformation on the heated rod, wherein the heating temperature of a die is 440 ℃, and the extrusion ratio is 1.95: 1, the extrusion speed is 3 mm/s; carrying out solution treatment on the alloy subjected to upsetting and extrusion at the temperature of 400 ℃ for 8h, and quenching in hot water at the temperature of 80 ℃; and after cooling to room temperature, carrying out aging treatment for 16h at 225 ℃ to obtain a target magnesium alloy rod, and testing the tensile strength and the elongation of the obtained magnesium alloy rod, wherein the specific test results are shown in tables 4, 5 and 6.
Table 4 mechanical properties of edge and core obtained in the test of each magnesium alloy bar in examples one to three
Tensile strength (Rm)/MPa Yield strength (R)p0.2) Elongation (A)/%)
Mg-8Gd edge 313 219 22
Mg-8Gd core 315 226 22
Mg-9Gd edge 323 223 20
Mg-9Gd core 325 231 20
Mg-10Gd edge 331 227 19
Mg-10Gd core 332 235 19
TABLE 5 data of mechanical properties of edge and center obtained at room temperature after heat treatment of magnesium alloy bars in examples one to three
Figure BDA0002983949970000081
TABLE 6 data of mechanical properties of edge and core at 200 ℃ after heat treatment of magnesium alloy bars in examples one to three
Tensile Strength (Rm)/MPa Elongation (A)/%)
Mg-8Gd edge 330 13
Mg-8Gd core 335 12.5
Mg-9Gd edge 338 12.5
Mg-9Gd core 345 12
Mg-10Gd edge 348 12
Mg-10Gd core 352 11.5
The above description is only a preferred embodiment of the present invention, and is not intended to limit the design of the present invention, and all equivalent changes made in the design key point of the present invention fall within the protection scope of the present invention.

Claims (8)

1. The high-strength and high-toughness rare earth heat-resistant magnesium alloy is characterized by comprising the following chemical components in percentage by mass: 8.0-10.8% of Gd, 3.1-4.0% of Y, 1.8-2.2% of Zn, 0.4-0.5% of Zr, and the balance of magnesium and inevitable impurity elements.
2. The high-strength rare earth heat-resistant magnesium alloy as recited in claim 1, wherein the high-strength rare earth heat-resistant magnesium alloy comprises the following chemical components by mass percent: 10.0% of Gd, 3.6% of Y, 2% of Zn, 0.5% of Zr, and the balance of magnesium and inevitable impurity elements.
3. The high-strength rare earth heat-resistant magnesium alloy as recited in claim 1, wherein the high-strength rare earth heat-resistant magnesium alloy comprises the following chemical components by mass percent: 8.4% of Gd, 3.4% of Y, 2% of Zn, 0.4% of Zr, and the balance of magnesium and inevitable impurity elements.
4. The high-strength rare earth heat-resistant magnesium alloy as recited in claim 1, wherein the high-strength rare earth heat-resistant magnesium alloy comprises the following chemical components by mass percent: 9.2% of Gd, 3.1% of Y, 1.8% of Zn, 0.5% of Zr, and the balance of magnesium and inevitable impurity elements.
5. The high-strength rare earth heat-resistant magnesium alloy as claimed in any one of claims 1 to 4, wherein the impurity elements comprise Fe, Ni, Cu and Si, and the impurity elements respectively account for the following mass percentages of the alloy: fe is less than or equal to 0.004%, Ni is less than or equal to 0.01%, Cu is less than or equal to 0.01%, and Si is less than or equal to 0.01%.
6. The preparation method of the high-strength and high-toughness rare earth heat-resistant magnesium alloy is characterized by comprising the following steps of:
(1) preparing a magnesium alloy cast rod: firstly, designing alloy element proportioning materials according to the mass percentage, preparing a magnesium alloy cast rod by adopting semi-continuous casting, and machining the magnesium alloy cast rod into a bar stock after cooling at room temperature;
(2) homogenizing the bar stock: heating the magnesium alloy bar to 300 ℃ by adopting a grading homogenization system, preserving heat for 4 hours, then heating to 525 ℃ and preserving heat for 8 hours for homogenization treatment;
(3) upsetting-extruding composite deformation: putting the bar stock into a heated upsetting-extruding composite die, wherein the heating temperature of the upsetting-extruding composite die is 420-450 ℃, the extrusion ratio is set to be 1.95, the extrusion speed is 2-4 mm/s, and the high-strength and high-toughness deformed rare earth heat-resistant magnesium alloy material is obtained after multi-pass circulating upsetting-extruding;
(4) solid solution and aging treatment: the heat treatment adopts solution aging treatment, the solution temperature is set to 400 ℃, the heat preservation is carried out for 8 hours, and hot water at 80 ℃ is adopted for quenching after discharging; and after cooling to room temperature, carrying out aging treatment at 225 ℃ for 16 h.
7. The preparation method of the high-strength-and-toughness rare earth heat-resistant magnesium alloy as claimed in claim 6, wherein the specific steps of the step (1) comprise:
(1.1) melting of pure magnesium: smelting the alloy by using a resistance furnace, heating a crucible to 800 ℃, then uniformly paving a layer of covering agent on the bottom of the crucible, putting a pure magnesium block, and scattering the covering agent on the pure magnesium block for protection;
(1.2) addition of alloying elements: after pure magnesium is melted, directly heating the melt to 800 ℃, adding pure Y, preserving heat at 800 ℃, after Y is completely melted, sequentially adding Mg-Gd and Mg-Zr intermediate alloys at 760-780 ℃, and finally adding pure Zn at 750 ℃;
(1.3) stirring: after the alloy elements are completely melted, preserving the heat of the melt at 750 ℃, removing floating slag on the surface of the melt by using a preheated slag removing spoon, and stirring, wherein an up-and-down rolling mode is mainly adopted in the stirring process;
(1.4) refining: after stirring, standing the melt for 3-5min, and refining at 750 ℃ under the protection of argon after the temperature is stable, wherein the refining time is 3-5 min;
(1.5) semi-continuous casting: standing for 10min after refining is finished, introducing the magnesium alloy melt into a crystallizer through a drainage groove at 750 ℃, sealing the bottom of the crystallizer by a guide rod to form a single-opening space, and finishing initial solidification of the magnesium alloy melt in the single-opening space; after the liquid level of the magnesium alloy melt is stable and a solidified shell with a certain thickness is formed, starting a motor to drive a guide rod to move downwards, and simultaneously continuously injecting the magnesium alloy melt into the upper part of a crystallizer; and stopping the casting process after the cast rod reaches a certain length to obtain a magnesium alloy cast rod, and machining the magnesium alloy cast rod into a bar stock after the magnesium alloy cast rod is cooled at room temperature.
8. The preparation method of the high-strength-toughness rare earth heat-resistant magnesium alloy as claimed in claim 6, wherein in the step (3), before the bar is placed into the heated upsetting-extruding composite die, the bar is placed into a heating furnace for heating, and the step heating system is adopted for heating: the primary heating temperature is 300 ℃, and the heat preservation time is 2 hours; the secondary heating temperature is 480 ℃, and the heat preservation time is 6 h.
CN202110294891.6A 2021-03-19 2021-03-19 High-strength and high-toughness rare earth heat-resistant magnesium alloy and preparation method thereof Pending CN113073244A (en)

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CN113528916A (en) * 2021-07-21 2021-10-22 上海交通大学 Rare earth-containing heat-resistant high-strength magnesium alloy material and preparation method thereof
CN113802166A (en) * 2021-09-29 2021-12-17 上海交通大学 Micro-arc oxidation treatment method of Mg-Gd-Y-Zn-Zr magnesium alloy containing LPSO phase
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CN114717458A (en) * 2022-04-20 2022-07-08 上海交通大学 Rare earth magnesium alloy wire suitable for electric arc additive manufacturing and preparation method thereof
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CN115261694A (en) * 2022-04-20 2022-11-01 上海交通大学 Rare earth magnesium alloy suitable for electric arc additive manufacturing
CN115572927A (en) * 2022-11-09 2023-01-06 上海交通大学 Homogenization heat treatment method for large-size rare earth magnesium alloy ingot
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