CN113278857B - High-toughness magnesium alloy and preparation method thereof - Google Patents
High-toughness magnesium alloy and preparation method thereof Download PDFInfo
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- 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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- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
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Abstract
The invention discloses a high-toughness magnesium alloy which is characterized in that the magnesium alloy comprises the following components in percentage by mass: 1.7 wt% -2.5 wt%, Mn: 0.4 wt% -0.8 wt%, Ca: 0.2 wt% -0.6 wt%, Zn: 0.2 to 0.6 wt%, and the balance of Mg and inevitable impurities. According to the invention, by controlling the addition amounts of Sm, Mg, Zn, Ca and Mn, on one hand: rare earth Sm, Mg, Zn and Ca form a large amount of MgZnCaSm and MgZnSm nanophase, a large amount of alpha-Mn nanophase also exists in the alloy structure, the nanophase plays a role of strengthening a magnesium matrix, the strength of the alloy is improved, the nanophase is small in size, can be dispersed and distributed on the magnesium alloy matrix, has little influence on the elongation of the matrix, and can realize that the tensile strength of the magnesium alloy is 400-450 MPa, the yield strength is 390-420 MPa and the elongation is more than 15%.
Description
Technical Field
The invention belongs to the technical field of magnesium alloy, and particularly relates to a high-toughness magnesium alloy and a preparation method thereof.
Background
The magnesium alloy is used as the lightest metal structure material, has a series of advantages of small density, high specific strength, good thermal conductivity, excellent damping and shock absorption performance and the like, and has wide application prospect in the fields of aerospace, transportation, mobile communication and the like. However, the strength of the conventional magnesium alloy is not high, so that it still faces some challenges in practical application. At present, researchers mainly regulate and control the microstructure of the magnesium alloy by alloying, plastic deformation, heat treatment and other methods so as to obtain a novel magnesium alloy with excellent comprehensive mechanical properties and further meet the requirements of practical application.
Research has shown that the addition of rare earth elements to magnesium alloys can significantly improve the mechanical properties of the alloys, for example, the tensile strength of the magnesium alloys with Gd and Y added thereto after deformation and aging treatment reaches 500MPa, but the addition of high content of rare earth elements increases the density and cost of the alloys, so that the development of high-strength wrought magnesium alloy materials with low rare earth content is required to reduce the cost of the alloys. In recent years, magnesium alloy materials with high performance and deformability obtained by adding rare earth Sm have received much attention.
The patent (CN105088038A) proposes a high-heat-conductivity corrosion-resistant Mg-1.5-6% Sm-0.001-1.2% Ca-0.5-3.0% Zn-0.3-2.5% Mn alloy, and the extrusion deformation process comprises the following steps: carrying out homogenization treatment on the ingot at the temperature of 350-420 ℃ for 2-24h, wherein the extrusion speed is 0.1-6mm/s, the extrusion ratio is 14-30, and water quenching is carried out after extrusion, but the heat treatment process after extrusion deformation and the mechanical property after extrusion deformation are not explained; the Cui and the like extrude Mg-3.5Sm-0.6Zn-0.5Zr alloy to obtain fine dynamic recrystallization grains (0.47 m), and the yield strength of the alloy reaches 416MPa and the elongation rate reaches 5.1 percent after T5 aging treatment; the patent (CN111485453.A) provides a wrought magnesium alloy containing neodymium, samarium, light rare earth elements and high Mn content and a preparation method thereof, wherein the wrought magnesium alloy comprises the following components in percentage by mass: calcium: 0.3 to 1.9 percent; aluminum: 0.3 to 1.5 percent; zinc: 0.2 to 1.7 percent; manganese: 0.3 to 2.8 percent; light rare earth (neodymium or samarium): 0.3-3.0 percent, the material can obtain the mechanical property with the tensile strength of 368-.
At present, the high strength and low elongation at break are the problems commonly existing in high-strength wrought magnesium alloy materials, which greatly limit the application of the high-strength wrought magnesium alloy materials, so that the development of the high strength and high elongation at break is of great significance for promoting the application of the magnesium alloy materials.
Disclosure of Invention
The invention aims to solve the first technical problem of providing a high-strength high-toughness magnesium alloy with high strength and high elongation.
The technical scheme adopted by the invention for solving the first technical problem is as follows: the high-toughness magnesium alloy is characterized in that the magnesium alloy comprises Sm in percentage by mass: 1.7 wt% -2.5 wt%, Mn: 0.4 wt% -0.8 wt%, Ca: 0.2 wt% -0.6 wt%, Zn: 0.2 wt% -0.6 wt%, and the balance of Mg and inevitable impurities; the microstructure of the magnesium alloy contains MgZnCaSm phase, MgZnSm phase and alpha-Mn phase; wherein the MgZnCaSm phase and the MgZnSm phase with the size below 200nm account for more than 80 percent of the area content of the total MgZnCaSm phase and the MgZnSm phase, and the alpha-Mn phase with the size below 5-20 nm accounts for more than 80 percent of the area content of the total alpha-Mn phase.
Preferably, the microstructure of the magnesium alloy contains immobile dislocations and < c + a > dislocations, the proportion of the immobile dislocations is 30 to 60%, and the proportion of the < c + a > dislocations is 30 to 60%. By adjusting the proportional relationship between the immobile dislocation and the < c + a > dislocation, high strength can be maintained and high ductility and toughness can be obtained.
Preferably, the magnesium alloy has a tensile strength of 400 to 450MPa, a yield strength of 390 to 420MPa, and an elongation of 15% or more.
Preferably, the magnesium alloy has a yield ratio of 0.95 or more.
The second technical problem to be solved by the invention is to provide a preparation method of the high-toughness magnesium alloy.
The technical scheme adopted by the invention for solving the second technical problem is as follows: a preparation method of high-toughness magnesium alloy is characterized by comprising the following steps: the method comprises the following steps:
1) preparing a magnesium alloy cast rod: putting the Mg ingot, the Zn ingot, the Mg-Sm intermediate alloy, the Mg-Mn intermediate alloy and the Mg-Ca intermediate alloy into a smelting furnace for smelting, and casting a magnesium alloy cast rod;
2) forward extrusion: preheating a magnesium alloy cast rod and an extrusion die for 1.5-3.0 h at 270-320 ℃, preheating a ingot container of an extruder to 270-300 ℃, extruding at a ratio of 8: 1-25: 1 and an extrusion speed of 0.1-1.0 mm/s, and preparing a deformed magnesium alloy rod after extrusion deformation;
3) annealing treatment: and annealing the deformed magnesium alloy bar at 300-350 ℃ for 10-30 minutes to obtain the high-strength and high-toughness magnesium alloy.
Preferably, the step 1) comprises the following steps:
a) drying the Mg ingot, the Zn ingot, the Mg-Sm intermediate alloy, the Mg-Mn intermediate alloy and the Mg-Ca intermediate alloy at 200-300 ℃;
b) At SF6+CO2Melting the Mg ingot at 680-730 ℃ under the protection of gas;
c) adding a Zn ingot and an Mg-Mn intermediate alloy into the magnesium melt at 710-750 ℃, and fully stirring until the Zn ingot and the Mg-Mn intermediate alloy are melted;
d) adding the Mg-Sm intermediate alloy into the magnesium melt at 710-750 ℃, and fully stirring until the Mg-Sm intermediate alloy is molten;
e) adding the Mg-Ca intermediate alloy into the magnesium melt at 710-750 ℃, and fully stirring until the Mg-Ca intermediate alloy is molten;
f) heating the melt to 760-780 ℃, introducing Ar gas for refining for 10-15 minutes, cooling to 740-750 ℃, standing for 30-40 minutes, and scraping scum on the surface of the melt when the temperature is reduced to 700-720 ℃;
g) casting: semi-continuous casting is adopted, and the casting temperature is as follows: 700-720 ℃; casting speed: 100 mm/min-200 mm/min; cooling water flow rate: 50L/min to 100L/min to obtain the magnesium alloy cast rod.
Compared with the prior art, the invention has the advantages that:
1) according to the invention, by controlling the addition amounts of Sm, Mg, Zn, Ca and Mn, on one hand: rare earth Sm, Mg, Zn and Ca form a large amount of MgZnCaSm and MgZnSm nanophase, a large amount of alpha-Mn nanophase also exists in the alloy structure, the nanophase plays a role of strengthening a magnesium matrix, the strength of the alloy is improved, the nanophase is small in size, can be dispersed and distributed on the magnesium alloy matrix, has little influence on the elongation of the matrix, and can realize that the tensile strength of the magnesium alloy is 400-450 MPa, the yield strength is 390-420 MPa and the elongation is more than 15%.
2) The invention adopts a hot extrusion and annealing treatment mode to prepare the magnesium alloy bar, on one hand: high dislocation density appears in the alloy structure under the extrusion condition, but the material has poor toughness under the extrusion condition because of the main unmovable dislocation, and after annealing treatment, the high-density unmovable dislocation is converted into the < c + a > dislocation which is easy to slip, so that the toughness of the material is greatly improved.
Drawings
FIG. 1 is a photograph showing the annealed microstructure of a magnesium alloy in example 1 of the present invention. Wherein 1 in the figure (a) is MgZnCaSm phase or MgZnSm phase, and 2 is magnesium alloy matrix phase; in the figure (b), 1 is MgZnCaSm phase or MgZnSm phase, 2 is magnesium alloy matrix phase, and alpha-Mn nano phase is dispersed and distributed on the magnesium alloy matrix.
FIG. 2 is a photograph showing the annealed microstructure of the magnesium alloy in example 1 of the present invention. Wherein 1 in the diagram (a) is an alpha-Mn nanophase; FIG. (b) is an enlarged view of FIG. (a); FIG. C and FIG. D are electron diffraction patterns of the α -Mn nanophase.
Detailed Description
The invention is described in further detail below with reference to the accompanying examples.
Example 1:
the high-strength and high-toughness magnesium alloy comprises the following components in percentage by mass: sm: 2.0%, Mn: 0.8%, Ca: 0.6%, Zn: 0.5%, and the balance of Mg and inevitable impurities.
The preparation of the high-strength and high-toughness magnesium alloy in the embodiment comprises the following steps:
1) preparing a magnesium alloy cast rod:
a) calculating the respective weights of the required Mg ingot, Zn ingot, Mg-25Sm intermediate alloy, Mg-10Mn intermediate alloy and Mg-25Ca intermediate alloy according to the alloy components of the magnesium alloy, preparing materials, drying at 300 ℃, and drying for 1.5 h;
b) at SF6+CO2Under the protection of gas, putting the dried pure Mg ingot into a crucible preheated to 550 ℃, and raising the furnace temperature to 730 ℃ until Mg is completely melted;
c) adding the dried pure Zn ingot and Mg-10Mn intermediate alloy into the magnesium melt at 730 ℃, and fully stirring until the pure Zn ingot and the Mg-10Mn intermediate alloy are melted;
d) adding the dried Mg-25Sm intermediate alloy into the magnesium melt at 730 ℃, and fully stirring until the Mg-25Sm intermediate alloy is molten;
e) adding the dried Mg-25Ca master alloy into the magnesium melt at 730 ℃, and fully stirring until the Mg-25Ca master alloy is melted;
f) heating the melt to 770 ℃, introducing preheated Ar gas for refining for 15 minutes, cooling to 740 ℃, standing for 30 minutes, and scraping scum on the surface of the melt when the temperature is reduced to 710 ℃;
g) carrying out semi-continuous ingot casting, wherein the alloy casting temperature is as follows: 710 ℃; casting speed: 100 mm/min; cooling water flow rate: 70L/min to obtain the magnesium alloy cast rod.
2) Forward extrusion: peeling a magnesium alloy cast rod, preheating the peeled cast rod and an extrusion die in a 300 ℃ resistance furnace for 1.5h, preheating a large spindle barrel of an extruder to 290 ℃, extruding at a ratio of 20:1 and an extrusion speed of 0.1mm/s, and extruding and deforming to prepare a deformed magnesium alloy rod.
3) And (3) annealing treatment: and annealing the deformed magnesium alloy bar for 15 minutes at 320 ℃ to obtain the high-strength-toughness magnesium alloy.
Referring to the attached drawings 1 and 2, the microstructure of the magnesium alloy contains MgZnCaSm phase, MgZnSm phase and alpha-Mn phase; wherein the MgZnCaSm phase and the MgZnSm phase with the size below 200nm account for more than 80 percent of the area content of the total MgZnCaSm phase and the MgZnSm phase, and the alpha-Mn phase with the size below 5-20 nm accounts for more than 80 percent of the area content of the total alpha-Mn phase.
Example 2
The present embodiment 2 differs from embodiment 1 in that: casting speed of semi-continuous ingot casting is 150mm/min, cooling water flow is as follows: 90L/min, preheating the peeled cast rod and the extrusion die in a 270 ℃ resistance furnace for 1.5h, preheating a holding cylinder of an extruder to 270 ℃, extruding according to the ratio of 16:1, and annealing the extruded and deformed magnesium alloy bar material at 300 ℃ for 15 minutes.
Example 3
The difference between the embodiment and the embodiment 1 is that the magnesium alloy comprises the following components in percentage by mass: 1.7%, Mn: 0.8%, Ca: 0.5%, Zn: 0.5 percent, and the balance of Mg and inevitable impurities, preheating the peeled cast rod and an extrusion die in a 270 ℃ resistance furnace for 2 hours at an extrusion speed of 1mm/s, and annealing the extruded bar of the extrusion deformation magnesium alloy for 15 minutes at 350 ℃.
Example 4
The difference between the embodiment and the embodiment 1 is that the magnesium alloy comprises the following components in percentage by mass: 2.5%, Mn: 0.8%, Ca: 0.4%, Zn: 0.5 percent, and the balance of Mg and inevitable impurities, preheating the peeled cast rod and an extrusion die in a resistance furnace at 320 ℃ for 1.5 hours, wherein the extrusion ratio is 18: 1.
Example 5
The difference between the embodiment and the embodiment 1 is that the magnesium alloy comprises the following components in percentage by mass: 2.5%, Mn: 0.8%, Ca: 0.4%, Zn: 0.5 percent, and the balance of Mg and inevitable impurities, preheating the peeled cast rod and an extrusion die in a resistance furnace at 320 ℃ for 1.5 hours, wherein the extrusion ratio is 24:1, and the extrusion speed is 0.2 mm/s.
Comparative example: the comparative example is different from example 1 in that annealing treatment is not performed after extrusion.
The room temperature tensile properties of the wrought magnesium alloys obtained in examples 1 to 5 and comparative example were measured, and the results are shown in table 1.
TABLE 1 microstructure, mechanical properties of inventive and comparative examples
Claims (4)
1. The high-toughness magnesium alloy is characterized in that the magnesium alloy comprises the following components in percentage by mass: 1.7wt% -2.5 wt%, Mn: 0.4wt% -0.8 wt%, Ca: 0.2wt% -0.6 wt%, Zn: 0.2wt% -0.6 wt%, and the balance of Mg and inevitable impurities; the microstructure of the magnesium alloy contains MgZnCaSm phase, MgZnSm phase and alpha-Mn phase; wherein the MgZnCaSm phase and the MgZnSm phase with the size below 200nm account for more than 80 percent of the area content of the total MgZnCaSm phase and the MgZnSm phase, and the alpha-Mn phase with the size below 5-20 nm accounts for more than 80 percent of the area content of the total alpha-Mn phase; the microstructure of the magnesium alloy contains immovable dislocation and < c + a > dislocation, the occupation ratio of the immovable dislocation is 30-60%, and the occupation ratio of the < c + a > dislocation is 30-60%.
2. The high-toughness magnesium alloy according to claim 1, wherein: the tensile strength of the magnesium alloy is 400 MPa-450 MPa, the yield strength is 390 MPa-420 MPa, and the elongation is more than 15%.
3. A method for preparing a high-toughness magnesium alloy according to any one of claims 1 to 2, which is characterized in that: the method comprises the following steps:
1) preparing a magnesium alloy cast rod: putting the Mg ingot, the Zn ingot, the Mg-Sm intermediate alloy, the Mg-Mn intermediate alloy and the Mg-Ca intermediate alloy into a smelting furnace for smelting, and casting a magnesium alloy cast rod;
2) forward extrusion: preheating a magnesium alloy cast rod and an extrusion die for 1.5-3.0 h at 270-320 ℃, preheating a ingot container of an extruder to 270-300 ℃, extruding at a ratio of 8: 1-25: 1 and an extrusion speed of 0.1-1.0 mm/s, and preparing a deformed magnesium alloy rod after extrusion deformation;
3) annealing treatment: and annealing the deformed magnesium alloy bar at 300-350 ℃ for 10-30 minutes to obtain the high-strength and high-toughness magnesium alloy.
4. The method for preparing the high-strength tough magnesium alloy according to claim 3, which is characterized in that: the step 1) comprises the following steps:
a) drying the Mg ingot, the Zn ingot, the Mg-Sm intermediate alloy, the Mg-Mn intermediate alloy and the Mg-Ca intermediate alloy at 200-300 ℃;
b) At SF6+CO2Under the protection of gas, melting the Mg ingot at 680-730 ℃;
c) adding a Zn ingot and an Mg-Mn intermediate alloy into the magnesium melt at 710-750 ℃, and fully stirring until the Zn ingot and the Mg-Mn intermediate alloy are molten;
d) adding the Mg-Sm intermediate alloy into the magnesium melt at 710-750 ℃, and fully stirring until the Mg-Sm intermediate alloy is molten;
e) adding the Mg-Ca intermediate alloy into the magnesium melt at 710-750 ℃, and fully stirring until the Mg-Ca intermediate alloy is molten;
f) heating the melt to 760-780 ℃, introducing Ar gas for refining for 10-15 minutes, cooling to 740-750 ℃, standing for 30-40 minutes, and scraping scum on the surface of the melt when the temperature is reduced to 700-720 ℃;
g) casting: semi-continuous casting is adopted, and the casting temperature is as follows: 700-720 ℃; casting speed: 100 mm/min-200 mm/min; cooling water flow rate: and (5) 50L/min-100L/min to obtain the magnesium alloy cast rod.
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