CN114150195B - High-performance rare earth magnesium lithium alloy plate and preparation method thereof - Google Patents
High-performance rare earth magnesium lithium alloy plate and preparation method thereof Download PDFInfo
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Abstract
A high-performance rare earth magnesium lithium alloy plate and a preparation method thereof belong to the technical field of metal materials. The process comprises the following steps: preparing raw materials according to the components and the content of the alloy, smelting, solution treatment and cold rolling composite annealing treatment. The cold rolling rare earth magnesium lithium alloy technology can be used for preparing the rare earth magnesium lithium alloy sheet with the thickness of 0.6 mm. The Mg-Gd-Y-Zn-Li alloy plate prepared by the invention has excellent mechanical properties, the yield strength of the Mg-Gd-Y-Zn-Li alloy plate is more than 190MPa, and the elongation of the Mg-Gd-Y-Zn-Li alloy plate is more than 22%. The refinement of crystal grains and the generation of precipitated phases in the alloy after cold rolling have obvious effects on strengthening and toughening the alloy. Compared with the prior art, the rare earth magnesium lithium alloy plate has excellent performance, simple preparation method and high production efficiency, and has remarkable practical value.
Description
Technical Field
The invention belongs to the technical field of metal materials, and relates to a high-performance rare earth magnesium lithium alloy plate and a preparation method thereof.
Background
The magnesium-lithium alloy as a light metal material has the advantages of low density, high specific strength, high specific rigidity, vibration reduction, electromagnetic shielding performance, strong radiation resistance, easy cutting, easy recovery and the like, and has important application value and wide application prospect in the fields of aerospace and national defense and military industries.
The magnesium-lithium alloy matrix is gradually transformed from an alpha-Mg phase with a close-packed hexagonal structure to a beta-Li phase with a body-centered cubic structure with the increase of the lithium content. Since the hexagonal close-packed structure of magnesium results in poor plasticity and formability of magnesium alloys, conventional magnesium alloys are formed by cold working, but require hot working. However, the magnesium-lithium alloy with body-centered cubic has excellent plasticity and forming capability, and is the only magnesium alloy material with cold working forming capability. Although the addition of lithium can improve the plasticity and the forming performance of the magnesium-lithium alloy, the poor mechanical properties of the magnesium-lithium alloy limit the wide application of the magnesium-lithium alloy.
An effective method for improving the mechanical property of the magnesium-lithium alloy by alloying is widely applied at present. For magnesium-lithium alloys, common alloying elements include Al, Zn, Ca, and the like. However, the mechanical properties of the developed Mg-Li-Al, Mg-Li-Zn, Mg-Li-Al-Ca and Mg-Li-Zn-Ca magnesium-lithium alloys are still low. Rare earth elements, especially heavy rare earth elements Gd and Y are often used for preparing high-strength and high-toughness magnesium alloy, but the application of the rare earth elements in magnesium-lithium alloy is rarely reported. The heavy rare earth elements Gd and Y are added into the magnesium-lithium alloy, so that the generation of a Mg-RE precipitated phase can be promoted, the refinement of alloy grains can be promoted, and the development of the high-performance magnesium-lithium alloy is obviously facilitated. Therefore, the application of heavy rare earth elements in magnesium-lithium alloys is a potential method for continuously improving the mechanical properties of the magnesium-lithium alloys.
The traditional thermomechanical treatment method of the magnesium alloy mainly comprises extrusion, rolling, forging and the like. The method aims to refine the texture of the magnesium alloy, close casting defects, and increase the size of broken magnesium alloy, so as to improve the mechanical property. Compared with a hot working forming method, the cold working forming method has the characteristics of high yield, high efficiency, strong economy and the like, so that the development of the high-performance magnesium-lithium alloy which is reinforced by utilizing the rare earth elements and has excellent cold forming processing capacity has considerable economic value and scientific necessity.
Disclosure of Invention
In view of the above, the invention provides a high-performance rare earth magnesium-lithium alloy plate and a preparation method thereof, aiming at the problems that the existing magnesium-lithium alloy has poor strength and is difficult to realize large-scale application. The high-performance magnesium-lithium alloy plate is prepared by alloying heavy rare earth elements (Gd, Y and the like) and Zn elements, controlling the content of Li, and carrying out hot extrusion composite cold rolling and annealing process on the Mg-Gd-Y-Zn-Li alloy.
The technical scheme of the invention is as follows:
a high-performance magnesium-lithium alloy plate is characterized in that the magnesium-lithium alloy comprises the following components: 8 to 10 weight percent of Gd, 2 to 4 weight percent of Y, 0 to 2 weight percent of Zn which is not 0, 10 to 13 weight percent of Li, and the balance of Mg and inevitable impurities;
more preferably, 8 to 9 wt% of Gd, 2 to 3wt% of Y, and 0.5 to 1.5 wt% of Zn.
Further deforming the rare earth magnesium lithium alloy, wherein the alloy matrix is composed of beta-Li.
The preparation method of the rare earth magnesium-lithium alloy is characterized by comprising the following steps:
1) covering deformed rare earth magnesium-lithium alloy on lithium fluoride and lithium chloride molten salt and SF6：CO2Casting the mixture into a billet in a mixed protective atmosphere, wherein the casting temperature is 680-720 ℃; if the casting mold is a metal mold plate-shaped mold, then cutting the metal mold plate-shaped mold to form a cylindrical casting billet; for example, the dimensions of a cylindrical casting billet are as follows: 35mm in diameter and 34mm in height.
2) Solution treatment: putting the casting billet into argon protection for solution treatment at 400-500 ℃ for 1-12 h, then putting the casting billet into boiling water at 100 ℃ for quenching, and cooling to room temperature;
3) hot extrusion deformation treatment: placing the cast billet subjected to the solution treatment in an extruder ingot holding barrel for preheating treatment, namely, raising the temperature of the cast billet to a preset extrusion temperature to be subjected to extrusion deformation treatment, wherein the preheating temperature is 100-200 ℃, the preheating time is 0.1-1 h, and carrying out hot extrusion deformation treatment on the preheated cast billet, wherein the extrusion temperature is as follows: the extrusion speed is 1-3mm/s at 100-200 ℃, and the extrusion ratio is 10: 1-25: 1;
4) cold rolling composite annealing treatment (I): and (3) placing the extrusion rod on a double-roller mill to carry out multi-pass cold rolling treatment, wherein the rolling quantity of each pass is 5-10%, annealing treatment is carried out every four passes, the annealing temperature is 330 ℃, the time duration is 10min, and the cumulative total rolling quantity is 50% -95%, and finally the magnesium-lithium alloy rolled plate is obtained, for example, the magnesium-lithium alloy rolled plate with the thickness of 0.6mm is obtained.
Or cold rolling composite annealing treatment (II): placing the extrusion rod on a double-roller mill to carry out multi-pass cold rolling treatment, wherein the rolling reduction of each pass is 5-10%, and the accumulated total rolling reduction is 50% -70%; further, annealing treatment can be carried out on the obtained rare earth magnesium-lithium alloy rolled plate, wherein the annealing temperature is 330 ℃, the time duration is 10min, and finally the magnesium-lithium alloy rolled plate is obtained, for example, the magnesium-lithium alloy rolled plate with the thickness of 3.7mm is obtained.
The invention has the substantive characteristics that:
by adding Gd and Y heavy rare earth elements into the magnesium-lithium alloy and controlling the content of Li element by Zn element, the alloy matrix of beta-Li phase is obtained. The magnesium-lithium alloy is subjected to cogging treatment by a hot extrusion process to obtain a fine recrystallized structure so as to increase the cold forming capability of the alloy, and then the alloy is subjected to a multi-pass cold rolling composite annealing process with total rolling quantities of 70% and 95% respectively, so that crystal grains are further refined, and the purpose of improving the mechanical property of the magnesium-lithium alloy is achieved.
The invention has the beneficial effects that:
1. the high-performance magnesium-lithium alloy is obtained through a cold rolling process, and compared with the conventional rare earth magnesium alloy, the production efficiency and the productivity are greatly improved, and the economic cost is reduced.
2. The size of alloy crystal grains is effectively reduced by a multi-pass cold rolling composite annealing process with the total rolling quantity of 70% or 95%, so that the aim of improving the mechanical property of the magnesium-lithium alloy is fulfilled.
3. The yield strength of the Mg-Gd-Y-Zn-Li alloy treated by the method disclosed by the invention is more than 190MPa, and the elongation is more than 22%.
4. The argon used in the invention is inert protective gas commonly used in laboratories, and has the advantages of low price, easy storage and transportation, stable chemical performance, no toxicity, no pollution and low cost.
5. The device used in the invention is simple and convenient, has short experimental period, simple and safe operation, and is beneficial to large-scale industrial application.
Drawings
FIG. 1 is a diagram of a microstructure OM of a magnesium-lithium alloy rolled under 95% in accordance with example 4 of the present invention;
FIG. 2 is a diagram of a microstructure OM after 70% of magnesium-lithium alloy is rolled down according to example 6 of the present invention;
Detailed Description
The technical solution of the present invention is further explained by the following specific embodiments, and the following embodiments are all implemented on the premise of the technical solution of the present invention, and detailed embodiments and specific operation procedures are given, but the scope of the present invention is not limited to the following examples.
Example 1
Selecting an ingot with the component of Mg-8Gd-3Y-1Zn-12Li, cutting the ingot to prepare a cylindrical casting billet with the diameter of 35mm and the height of 34mm (the deformed rare earth magnesium-lithium alloy is covered by lithium fluoride and lithium chloride molten salt and SF6：CO2Casting into a billet in mixed protective atmosphere, wherein the casting temperature is 680-720 ℃, and the same applies below), and performing solution treatment, namely placing a sample in a tubular heat treatment furnace protected by argon, heating to 500 ℃ along with the furnace, preserving heat for 8 hours, then placing in boiling water at 100 ℃ for quenching, and cooling to room temperature. Then placing the cylindrical casting billet subjected to the solution treatment in a loading barrel of a pressurizing machine for preheating for 8min to the extrusion temperature of 120 ℃, and then carrying out hot extrusion deformation treatment at the extrusion speed of 1mm/s and the extrusion ratio of 10:1 to obtain the bar with the diameter of 12 mm. And (2) performing cold rolling composite annealing treatment (I) on the bar, accumulating the rolling amount to be 50%, obtaining a rare earth magnesium-lithium alloy plate with the thickness of 6mm, processing the rare earth magnesium-lithium alloy plate into a tensile test piece, and performing tensile test on the tensile test bar on a tension tester (by adopting a room temperature test method of part 1 of a GB/T228.1-2010 metal material tensile test) until the tensile test piece is broken to obtain the yield strength of 141MPa, the tensile strength of 151MPa and the elongation of 41.2%.
Example 2
The procedure is the same as example 1, except that the cumulative rolling reduction is 80%, and a rare earth magnesium lithium alloy plate with a thickness of 2.3mm is obtained. The yield strength is 164MPa, the tensile strength is 172MPa, and the elongation is 22.5%.
Example 3
The steps are the same as example 1, except that the lower rolling amount is 91%, and the rare earth magnesium-lithium alloy plate with the thickness of 1.1mm is obtained. The yield strength was 192MPa, the tensile strength was 200MPa, and the elongation was 22.4%.
Example 4
The procedure is the same as example 1 except that the amount of rolling is 95% to obtain a rare earth magnesium lithium alloy sheet having a thickness of 0.6 mm. The yield strength is 188MPa, the tensile strength is 192MPa, and the elongation is 22.6%.
Example 5
Selecting an ingot with the component of Mg-8Gd-3Y-1Zn-12Li, cutting the ingot to prepare a cylindrical casting billet with the diameter of 35mm and the height of 34mm (the deformed rare earth magnesium-lithium alloy is covered by lithium fluoride and lithium chloride molten salt and SF6：CO2Casting into a billet in mixed protective atmosphere, wherein the casting temperature is 680-720 ℃, and the same applies below), and performing solution treatment, namely placing a sample in a tubular heat treatment furnace protected by argon, heating to 500 ℃ along with the furnace, preserving heat for 8 hours, then placing in boiling water at 100 ℃ for quenching, and cooling to room temperature. Then placing the cylindrical casting billet subjected to the solution treatment in a loading barrel of a pressurizing machine for preheating for 8min to the extrusion temperature of 120 ℃, and then carrying out hot extrusion deformation treatment at the extrusion speed of 1mm/s and the extrusion ratio of 10:1 to obtain the bar with the diameter of 12 mm. And (2) performing cold rolling composite annealing treatment on the bar (II), when the accumulated rolling amount is 70%, annealing the bar at the annealing temperature of 330 ℃ for 10min to obtain a rare earth magnesium-lithium alloy plate with the thickness of 3.7mm, processing the rare earth magnesium-lithium alloy plate into a tensile test piece, and then performing tensile test on the tensile test bar on a tensil tester (by adopting the GB/T228.1-2010 metal material tensile test part 1 room temperature test method) until the tensile test bar is broken to obtain the yield strength of 101MPa, the tensile strength of 143MPa and the elongation of 29.5%.
Example 6
The procedure is the same as example 5, except that the cumulative rolling reduction is 70%, and the final annealing treatment is not performed, thereby obtaining a rare earth magnesium lithium alloy sheet with a thickness of 3.7 mm. The yield strength is 185MPa, the tensile strength is 200MPa, and the elongation is 23.5%.
Example 7
The procedure is the same as example 5 except that the cumulative rolling reduction is 50% and the final annealing treatment is not performed, thereby obtaining a rare earth magnesium lithium alloy sheet with a thickness of 6 mm. The yield strength was 193MPa, the tensile strength was 197MPa, and the elongation was 16%.
In conclusion: the invention relates to magnesium-lithium alloy and the processing technical field thereof, in particular to a rolling process of a deformed rare earth magnesium-lithium alloy plate, aiming at providing a cold rolling process of a high-performance magnesium alloy plate. The process comprises the following steps: preparing raw materials according to the components and the content of the alloy, smelting, solution treatment and cold rolling composite annealing treatment. The cold rolling rare earth magnesium lithium alloy technology can be used for preparing rare earth magnesium lithium alloy plates with the thickness of 0.6mm, and has important practical value due to simple and reliable preparation method and high production efficiency. The Mg-Gd-Y-Zn-Li alloy plate prepared by the invention has excellent mechanical properties, and particularly in example 3, the yield strength is over 190MPa and the elongation is over 22%. The grain size in the alloy after rolling is refined and a certain amount of precipitated phases appear. The grain refinement and the generation of precipitated phases have obvious effects on strengthening and toughening the alloy.
The above examples of the present invention are merely illustrative of the present invention and are not intended to limit the embodiments of the present invention. Variations and modifications in other variations will occur to those skilled in the art upon reading the foregoing description. Not all embodiments are exhaustive. All obvious changes and modifications of the present invention are within the scope of the present invention.
The invention is not the best known technology.
Claims (4)
1. A high-performance magnesium-lithium alloy plate is characterized in that the magnesium-lithium alloy comprises the following components: 8-10 wt% of Gd, 2-4 wt% of Y, 0-2 wt% of Zn which is not 0, 10-13 wt% of Li, and the balance of Mg and inevitable impurities;
the preparation method of the high-performance magnesium-lithium alloy plate comprises the following steps:
1) covering deformed rare earth magnesium-lithium alloy on lithium fluoride and lithium chloride molten salt and SF6：CO2Casting the blank ingot under mixed protective atmosphere, wherein the casting temperature is 680-720 ℃;
2) solution treatment: putting the casting billet into argon protection for solution treatment at the temperature of 400-500 ℃ for 1-12 h, then putting the casting billet into boiling water at the temperature of 100 ℃ for quenching, and then cooling to room temperature;
3) hot extrusion deformation treatment: placing the cast billet subjected to the solution treatment in an extruder ingot holding barrel for preheating treatment, namely, raising the temperature of the cast billet to a preset extrusion temperature to be subjected to extrusion deformation treatment, wherein the preheating temperature is 100-200 ℃, the preheating time is 0.1-1 h, and carrying out hot extrusion deformation treatment on the preheated cast billet, wherein the extrusion temperature is as follows: the extrusion speed is 1-3mm/s at 100-200 ℃, and the extrusion ratio is 10: 1-25: 1;
4) cold rolling composite annealing treatment (I): placing the extrusion rod on a double-roller mill to perform multi-pass cold rolling treatment, wherein the rolling reduction of each pass is 5-10%, annealing treatment is performed every four passes, the annealing temperature is 330 ℃, the time duration is 10min, and the accumulated total rolling reduction is 50% -95%, so that a magnesium-lithium alloy rolled plate is finally obtained;
or cold rolling composite annealing treatment (II): placing the extrusion rod on a double-roller mill for multi-pass cold rolling treatment, wherein the rolling reduction of each pass is 5-10%, and the accumulated total rolling reduction is 50-70%; and then annealing the rare earth magnesium-lithium alloy rolled plate with the accumulated total rolling amount of 50-70 percent at the annealing temperature of 330 ℃ for 10min to finally obtain the magnesium-lithium alloy rolled plate.
2. The high-performance magnesium-lithium alloy plate according to claim 1, wherein Gd is 8-9 wt%, Y is 2-3 wt%, and Zn is 0.5-1.5 wt%.
3. The method for preparing the high-performance magnesium-lithium alloy sheet material in claim 1 or 2, which is characterized by comprising the following steps of:
1) covering deformed rare earth magnesium-lithium alloy on lithium fluoride and lithium chloride molten salt and SF6：CO2Casting the blank ingot under mixed protective atmosphere, wherein the casting temperature is 680-720 ℃;
2) solution treatment: putting the casting billet into argon protection for solution treatment at the temperature of 400-500 ℃ for 1-12 h, then putting the casting billet into boiling water at the temperature of 100 ℃ for quenching, and then cooling to room temperature;
3) and (3) hot extrusion deformation treatment: placing the cast billet subjected to the solution treatment in an extruder ingot holding barrel for preheating treatment, namely, raising the temperature of the cast billet to a preset extrusion temperature to be subjected to extrusion deformation treatment, wherein the preheating temperature is 100-200 ℃, the preheating time is 0.1-1 h, and carrying out hot extrusion deformation treatment on the preheated cast billet, wherein the extrusion temperature is as follows: the extrusion speed is 1-3mm/s at 100-200 ℃, and the extrusion ratio is 10: 1-25: 1;
4) cold rolling composite annealing treatment (I): placing the extrusion rod on a double-roller mill to carry out multi-pass cold rolling treatment, wherein the rolling quantity in each pass is 5-10%, annealing treatment is carried out in each four passes, the annealing temperature is 330 ℃, the time duration is 10min, and the accumulated total rolling quantity is 50% -95%, so that the magnesium-lithium alloy rolled plate is finally obtained;
or cold rolling composite annealing treatment (II): placing the extrusion rod on a double-roller mill for multi-pass cold rolling treatment, wherein the rolling reduction of each pass is 5-10%, and the accumulated total rolling reduction is 50-70%; and then annealing the rare earth magnesium-lithium alloy rolled plate with the accumulated total rolling amount of 50-70 percent at the annealing temperature of 330 ℃ for 10min to finally obtain the magnesium-lithium alloy rolled plate.
4. A method according to claim 3, characterized in that the alloy matrix consists of the β -Li phase.
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