CN110760728A - Long-period structure reinforced high-strength heat-resistant magnesium alloy and preparation method thereof - Google Patents
Long-period structure reinforced high-strength heat-resistant magnesium alloy and preparation method thereof Download PDFInfo
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- 229910000861 Mg alloy Inorganic materials 0.000 title claims abstract description 50
- 238000002360 preparation method Methods 0.000 title claims description 10
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 46
- 239000000956 alloy Substances 0.000 claims abstract description 46
- 239000011777 magnesium Substances 0.000 claims abstract description 37
- 238000001125 extrusion Methods 0.000 claims abstract description 15
- 239000012535 impurity Substances 0.000 claims abstract description 9
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 9
- 230000032683 aging Effects 0.000 claims abstract description 8
- 229910052742 iron Inorganic materials 0.000 claims abstract description 8
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 8
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims description 28
- 229910052749 magnesium Inorganic materials 0.000 claims description 28
- 238000010438 heat treatment Methods 0.000 claims description 16
- 239000000155 melt Substances 0.000 claims description 10
- 238000007670 refining Methods 0.000 claims description 10
- 238000003756 stirring Methods 0.000 claims description 10
- 229910052751 metal Inorganic materials 0.000 claims description 7
- 239000002184 metal Substances 0.000 claims description 7
- 238000012545 processing Methods 0.000 claims description 7
- 238000002844 melting Methods 0.000 claims description 6
- 230000008018 melting Effects 0.000 claims description 6
- 229910052725 zinc Inorganic materials 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 5
- 238000000465 moulding Methods 0.000 claims description 5
- 239000002893 slag Substances 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 4
- 238000003723 Smelting Methods 0.000 claims description 3
- 230000000694 effects Effects 0.000 abstract description 4
- 238000000034 method Methods 0.000 abstract description 4
- 230000002787 reinforcement Effects 0.000 abstract description 4
- 229910052761 rare earth metal Inorganic materials 0.000 description 9
- 239000007789 gas Substances 0.000 description 8
- 150000002910 rare earth metals Chemical class 0.000 description 6
- 239000000463 material Substances 0.000 description 5
- 229910052688 Gadolinium Inorganic materials 0.000 description 3
- 229910052692 Dysprosium Inorganic materials 0.000 description 2
- 229910052691 Erbium Inorganic materials 0.000 description 2
- 229910052771 Terbium Inorganic materials 0.000 description 2
- 229910052802 copper Inorganic materials 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 229910052727 yttrium Inorganic materials 0.000 description 2
- 229910052726 zirconium Inorganic materials 0.000 description 2
- 229910000838 Al alloy Inorganic materials 0.000 description 1
- 229910052689 Holmium Inorganic materials 0.000 description 1
- 229910052772 Samarium Inorganic materials 0.000 description 1
- 229910052775 Thulium Inorganic materials 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 239000002872 contrast media Substances 0.000 description 1
- 238000013016 damping Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- -1 rare earth compound Chemical class 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C23/00—Alloys based on magnesium
- C22C23/06—Alloys based on magnesium with a rare earth metal as the next major constituent
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/02—Making non-ferrous alloys by melting
- C22C1/03—Making non-ferrous alloys by melting using master alloys
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/06—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of magnesium or alloys based thereon
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Crystallography & Structural Chemistry (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
The invention discloses a magnesium alloy which comprises the following elements in percentage by mass: gd: 6.5 wt% -8.0 wt%; y: 1.0 wt% -2.2 wt%; zn: 0.2 wt% -0.6 wt%; cu: 0.3 wt% -0.6 wt%; zr: 0.1 wt% -0.5 wt%; impurity elements Si, Fe and Ni are not more than 0.02 wt.%, and the balance is Mg; the mass percentage ratio of (Gd + Y)/(Zn + Cu) is 10-20: 1. The high-strength heat-resistant magnesium alloy reinforced by the long-period structure obtains the long-period phase with excellent medium-high temperature reinforcement effect by designing and improving the alloy components, further refines the grain size by a large-deformation extrusion process, and fully exerts the second-phase reinforcement effect of the alloy by combining aging treatment.
Description
Technical Field
The invention relates to the technical field of metal smelting, in particular to a long-period structure-reinforced high-strength heat-resistant magnesium alloy and a preparation method thereof.
Background
The magnesium alloy is taken as the lightest commercial metal engineering structural material, has the advantages of higher specific strength and specific stiffness, superior damping and shock absorption performance, easy recycling and the like, and is known as a green structural material in the 21 st century. However, the lack of strength and poor heat resistance of magnesium alloy seriously hinders the pace of magnesium alloy in replacing aluminum alloy and other materials in aerospace, military and other industries.
The purpose of improving the heat strength of the magnesium alloy is realized by the following means: (1) introducing a second phase with high thermal stability; (2) reducing the diffusion rate of elements in the magnesium matrix; (3) improve the structure state and the structure form of the grain boundary. Among the alloy elements added into the magnesium alloy, rare earth is the most effective alloy element for improving the heat resistance of the magnesium alloy, and the main reason is that the rare earth element has larger solid solubility limit in magnesium, and the solid solubility is sharply reduced along with the reduction of the temperature, so that larger supersaturation can be obtained, and dispersed and high-melting-point rare earth compound phase is separated out in the subsequent aging process. The high-melting-point precipitated phases can effectively pin the intragranular dislocation and the grain boundary slippage at high temperature, so that the material can still keep relatively stable mechanical properties at medium and high temperature. The most commonly used commercial heat resistant magnesium alloy at present is the WE54 alloy (Mg-5% Y-2% Nd-2.0% HRE-0.5% Zr, wt.%), where HRE is a mixed heavy rare earth element such as Tb, Er, Dy and Gd. The WE54 alloy is a magnesium alloy with the best high-temperature mechanical property in the current commerce, the heat-resistant temperature can reach 250 ℃, however, the strength of the alloy is still insufficient when the alloy is used at medium and high temperatures, and the performance requirement of a light-weight structural member in service in a high-temperature environment is difficult to meet. Some rare earth-containing heat-resistant magnesium alloys have been developed in China, for example, Chinese patent application (publication number: CN1962914A) discloses a rare earth-containing magnesium alloy, the rare earth-containing cast magnesium alloy comprises 6-15 wt% of Gd; 2 to 6 weight percent of Sm; 0.35 wt% -0.8 wt% of Zr; the balance of magnesium and impurities, and the total content of impurities of Si, Fe, Cu and Ni is less than 0.02 percent. The heat resistance of the alloy is remarkably lowered with the increase of temperature, and further the alloy is insufficient in high-temperature strength. For example, Chinese patent application (publication No. CN102676895B) discloses a rare earth-containing cast magnesium alloy, which is composed of 0.1-5% of Sr, 1-20% of Si, 0.1-2% of Ca and the balance of Mg, but the alloy has obviously insufficient high-temperature strength.
Disclosure of Invention
Aiming at the problems of insufficient strength and poor heat resistance of the magnesium alloy in the prior art, the invention provides a long-period structure-reinforced high-strength heat-resistant magnesium alloy and a preparation method thereof. An important finding of research on high-strength rare earth magnesium alloys in recent years is that addition of a certain amount of Zn, Cu or Ni element to Mg — RE (RE ═ Y, Gd, Tb, Dy, Ho, Er or Tm) magnesium alloy results in formation of long-period phase (LPSO), and magnesium alloys containing such long-period phase have good room-temperature strength and high-temperature strength. Therefore, the microstructure of the long-period phase is regulated and controlled through alloy composition design, a heat treatment process and a hot working process, and the heat-resistant magnesium alloy is expected to replace the traditional WE54 heat-resistant magnesium alloy, so that the light weight of the structural part in the fields of automobiles, traffic, aerospace and the like is promoted.
The technical scheme adopted for further solving the technical problems is as follows:
a magnesium alloy comprises the following elements in percentage by mass:
gd: 6.5 wt% to 8.0 wt%, preferably 7.0 wt% to 7.5 wt%;
y: 1.0 wt% to 2.2 wt%, preferably 1.5 wt% to 2.0 wt%;
zn: 0.2 wt% to 0.6 wt%, preferably 0.3 wt% to 0.5 wt%;
cu: 0.3 wt% to 0.6 wt%, preferably 0.3 wt% to 0.5 wt%;
zr: 0.1 wt% to 0.5 wt%, preferably 0.1 wt% to 0.3 wt%;
the impurity elements Si, Fe and Ni are not more than 0.02 wt.%, preferably not more than 0.015 wt.%, and the balance is Mg;
the mass percentage ratio of (Gd + Y)/(Zn + Cu) is 10-20: 1, preferably 10-18.3: 1.
The invention also provides a preparation method of the magnesium alloy, which comprises the following steps:
step one, alloy smelting:
(1) respectively preheating high-purity magnesium, pure Cu, pure Zn, Mg-25 wt.% of Gd intermediate alloy, Mg-25 wt.% of Y intermediate alloy and Mg-30 wt.% of Zr intermediate alloy;
(2) heating to 710-750 ℃, heating and melting the magnesium ingot in a crucible, and introducing CO when the magnesium ingot begins to melt2+0.5vol％SF6Mixing the gases until the pure magnesium ingot is completely melted, adding pure Zn and pure Cu into the magnesium liquid at the temperature of 720-760 ℃, fully dissolving, and stirring for 3-5 minutes;
(3) heating to 760-800 ℃, adding Mg-25 wt.% of Gd intermediate alloy, Mg-25 wt.% of Y intermediate alloy and Mg-30 wt.% of Zr intermediate alloy, stirring for 5-10 minutes, and standing for 10-15 minutes;
(4) refining the melt, removing slag after refining, and reducing the temperature to 700-720 ℃; in CO2+0.5vol％SF6Under the mixed gas, pouring the melt into a metal mold preheated to 450-500 ℃ for molding to obtain a magnesium alloy ingot;
step two, extrusion processing:
homogenizing magnesium alloy ingots at 490-510 ℃ for 15-40 hours, then processing by a cutting machine, extruding into a profile at 350-400 ℃, wherein the extrusion ratio is 25:1, and the extrusion speed is 0.5-2 m/min; the obtained magnesium alloy extruded section is subjected to aging treatment for 24-40 h at the temperature of 150-210 ℃.
In summary, compared with the prior art, the invention has the following advantages:
the high-strength heat-resistant magnesium alloy reinforced by the long-period structure obtains the long-period phase with excellent medium-high temperature reinforcement effect by designing and improving the alloy components, further refines the grain size by a large-deformation extrusion process, and fully exerts the second-phase reinforcement effect of the alloy by combining aging treatment.
Drawings
Fig. 1 is a scanning electron micrograph of the high strength heat resistant magnesium alloy having a Long Period Structure (LPSO) prepared in example 1.
Detailed Description
The technical solution of the present invention is further specifically described below by way of specific examples, but the present invention is not limited to these examples.
Embodiment 1, a long period structure reinforced high strength heat resistant magnesium alloy, comprising the following elements by mass percent: gd: 7.4 wt%; y: 1.6 wt%; zn: 0.3 wt%; cu: 0.4 wt%; zr: 0.13 wt% of impurity elements Si, Fe and Ni are not more than 0.015 wt%, and the balance is Mg.
The preparation method comprises the following steps:
(1) preheating high-purity magnesium, pure Cu, pure Zn, Mg-25 wt.% Gd intermediate alloy, Mg-25 wt.% Y intermediate alloy and Mg-30 wt.% Zr intermediate alloy at 182 ℃ respectively;
(2) heating to 720 ℃, heating and melting the magnesium ingot in a crucible, and introducing CO when the magnesium ingot begins to melt2+0.5vol％SF6Mixing the gases until the pure magnesium ingot is completely melted, adding pure Zn and pure Cu into the magnesium liquid at 760 ℃, fully dissolving, and stirring for 5 minutes;
(3) heating to 784 ℃, adding Mg-25 wt.% of Gd intermediate alloy, Mg-25 wt.% of Y intermediate alloy and Mg-30 wt.% of Zr intermediate alloy, stirring for 5 minutes, and standing for 15 minutes;
(4) refining the melt, removing slag after refining and reducing the temperature to 700 ℃; in CO2+0.5vol％SF6Under the mixed gas, pouring the melt into a metal mold preheated to 450 ℃ for molding;
(5) homogenizing magnesium alloy ingots at about 500 ℃ for 20 hours, then processing by a cutting machine, extruding into a profile at 370 ℃, wherein the extrusion ratio is 25:1, and the extrusion speed is 0.5 m/min;
(6) the magnesium alloy extruded section is subjected to aging treatment for 40 hours at the temperature of 150 ℃.
The scanning electron microscope image of the long period structure strengthened high strength heat resistant magnesium alloy obtained in this example is shown in fig. 1. The points indicated by the white arrow points in the figure are all LPSO phase structures.
Embodiment 2, a long period structure reinforced high strength heat resistant magnesium alloy, comprising the following elements by mass percent: gd: 7.3 wt%; y: 1.8 wt%; zn: 0.41 wt%; cu: 0.45 wt%; zr: 0.15 wt%; the impurity elements Si, Fe and Ni are not more than 0.015 wt.%, and the balance is Mg. The preparation method comprises the following steps:
(1) preheating high-purity magnesium, pure Cu, pure Zn, Mg-25 wt.% of Gd intermediate alloy, Mg-25 wt.% of Y intermediate alloy and Mg-30 wt.% of Zr intermediate alloy at 180 ℃ respectively;
(2) heating to 725 ℃, heating and melting the magnesium ingot in the crucible, and introducing CO when the magnesium ingot begins to melt2+0.5vol％SF6Mixing the gases until the pure magnesium ingot is completely melted, adding pure Zn and pure Cu into a magnesium liquid at 745 ℃, fully dissolving, and stirring for 5 minutes;
(3) heating to 794 ℃, adding Mg-25 wt.% of Gd intermediate alloy, Mg-25 wt.% of Y intermediate alloy and Mg-30 wt.% of Zr intermediate alloy, stirring for 10 minutes, and standing for 15 minutes;
(4) refining the melt, removing slag after refining and reducing the temperature to 712 ℃; in CO2+0.5vol％SF6Under the mixed gas, pouring the melt into a metal mold preheated to 450 ℃ for molding;
(5) homogenizing magnesium alloy ingot at about 505 ℃ for 30 hours, then processing by a cutting machine, extruding into a profile at 355 ℃ with an extrusion ratio of 25:1 and an extrusion speed of 0.7 m/min;
(6) the magnesium alloy extruded section is subjected to aging treatment for 30 hours at the temperature of 175 ℃.
Embodiment 3, a long period structure reinforced high strength heat resistant magnesium alloy, the magnesium alloy comprising the following elements by mass percent: gd: 7.0 wt.%; y: 1.9 wt%; zn: 0.33 wt%; cu: 0.41 wt%; zr: 0.23 wt%; the impurity elements Si, Fe and Ni are not more than 0.015 wt.%, and the balance is Mg. The preparation method comprises the following steps:
(1) preheating high-purity magnesium, pure Cu, pure Zn, Mg-25 wt.% of Gd intermediate alloy, Mg-25 wt.% of Y intermediate alloy and Mg-30 wt.% of Zr intermediate alloy at 181 ℃;
(2) heating to 722 ℃, heating and melting the magnesium ingot in a crucible, introducing CO2+0.5 vol% SF6 mixed gas when the magnesium ingot starts to melt, adding pure Zn and pure Cu into 744 ℃ magnesium liquid after the pure magnesium ingot is completely melted, fully dissolving, and stirring for 5 minutes;
(3) heating to 783 ℃, adding Mg-25 wt.% of Gd intermediate alloy, Mg-25 wt.% of Y intermediate alloy and Mg-30 wt.% of Zr intermediate alloy, stirring for 8 minutes, and standing for 15 minutes;
(4) refining the melt, removing slag after refining and reducing the temperature to 715 ℃; in CO2+0.5vol％SF6Under the mixed gas, pouring the melt into a metal mold preheated to 450 ℃ for molding;
(5) homogenizing magnesium alloy ingots at 510 ℃ for 25 hours, then processing by a cutting machine, extruding into a profile at 400 ℃, wherein the extrusion ratio is 25:1, and the extrusion speed is 1.5 m/min;
(6) the magnesium alloy extruded section is subjected to aging treatment for 30 hours at 190 ℃.
The tensile properties in the extrusion direction of the long-period structure-reinforced high-strength heat-resistant magnesium alloy obtained in each of the above examples are compared with those of a comparative material (WE54) shown in table 1.
TABLE 1 comparison of tensile Properties
| Room temperature yield strength (MPa) | Yield strength (MPa) at 200 ℃ | |
| Example 1 | 385 | 301 |
| Example 2 | 393 | 318 |
| Example 3 | 343 | 273 |
| Contrast material | 310 | 255 |
The preferred embodiments of the present invention have been described in detail, but the present invention is not limited to the details of the above embodiments, and various simple modifications can be made to the technical solution of the present invention within the technical idea of the present invention, which fall within the protective scope of the present invention.
Claims (4)
1. The magnesium alloy is characterized by comprising the following elements in percentage by mass:
gd: 6.5 wt% -8.0 wt%; y: 1.0 wt% -2.2 wt%; zn: 0.2 wt% -0.6 wt%; cu: 0.3 wt% -0.6 wt%; zr: 0.1 wt% -0.5 wt%; impurity elements Si, Fe and Ni are not more than 0.02 wt.%, and the balance is Mg; the mass percentage ratio of (Gd + Y)/(Zn + Cu) is 10-20.
2. The magnesium alloy of claim 1, comprising the following elements in mass percent:
gd: 7.0 wt% -7.5 wt%; y: 1.5 wt% -2.0 wt%; zn: 0.3 wt% -0.5 wt%; cu: 0.3 wt% -0.5 wt%; zr: 0.1 wt% -0.3 wt%; impurity elements Si, Fe and Ni are not more than 0.015 wt.%, and the balance is Mg; the mass percentage ratio of (Gd + Y)/(Zn + Cu) is 10-18.3.
3. A preparation method of magnesium alloy is characterized by comprising the following steps:
step one, alloy smelting:
(1) respectively preheating high-purity magnesium, pure Cu, pure Zn, Mg-25 wt.% of Gd intermediate alloy, Mg-25 wt.% of Y intermediate alloy and Mg-30 wt.% of Zr intermediate alloy;
(2) heating to 710-750 ℃, heating and melting the magnesium ingot in a crucible, and introducing CO when the magnesium ingot begins to melt2+0.5vol％SF6Mixing the gas until the pure magnesium ingot is completelyAfter melting, adding pure Zn and pure Cu into the magnesium liquid at the temperature of 720-760 ℃, fully dissolving, and stirring for 3-5 minutes;
(3) heating to 760-800 ℃, adding Mg-25 wt.% of Gd intermediate alloy, Mg-25 wt.% of Y intermediate alloy and Mg-30 wt.% of Zr intermediate alloy, stirring for 5-10 minutes, and standing for 10-15 minutes;
(4) refining the melt, removing slag after refining, and reducing the temperature to 700-720 ℃; in CO2+0.5vol％SF6Under the mixed gas, pouring the melt into a metal mold preheated to 450-500 ℃ for molding to obtain a magnesium alloy ingot;
step two, extrusion processing:
homogenizing magnesium alloy ingots at 490-510 ℃ for 15-40 hours, then processing by a cutting machine, and extruding into a profile at 350-400 ℃, wherein the extrusion ratio is 25:1, and the extrusion speed is 0.5-2 m/min.
4. The preparation method of the magnesium alloy according to claim 3, wherein the magnesium alloy extruded section prepared in the second step is subjected to aging treatment at 150-210 ℃ for 24-40 h.
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| CN113755734A (en) * | 2021-08-30 | 2021-12-07 | 西安交通大学 | High-strength high-plasticity heat-resistant magnesium alloy with LPSO phase and SFs structure and preparation method thereof |
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| CN113755734A (en) * | 2021-08-30 | 2021-12-07 | 西安交通大学 | High-strength high-plasticity heat-resistant magnesium alloy with LPSO phase and SFs structure and preparation method thereof |
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