CN112746210B - A kind of multi-component microalloyed magnesium alloy and its preparation method and sheet extrusion forming process - Google Patents

A kind of multi-component microalloyed magnesium alloy and its preparation method and sheet extrusion forming process Download PDF

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CN112746210B
CN112746210B CN202110136691.8A CN202110136691A CN112746210B CN 112746210 B CN112746210 B CN 112746210B CN 202110136691 A CN202110136691 A CN 202110136691A CN 112746210 B CN112746210 B CN 112746210B
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CN112746210A (en
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邓坤坤
侯美丽
王翠菊
聂凯波
王晓军
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Taiyuan University of Technology
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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
    • C22C23/04Alloys based on magnesium with zinc or cadmium as the next major constituent
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B21MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
    • B21CMANUFACTURE OF METAL SHEETS, WIRE, RODS, TUBES OR PROFILES, OTHERWISE THAN BY ROLLING; AUXILIARY OPERATIONS USED IN CONNECTION WITH METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL
    • B21C37/00Manufacture of metal sheets, bars, wire, tubes or like semi-manufactured products, not otherwise provided for; Manufacture of tubes of special shape
    • B21C37/02Manufacture of metal sheets, bars, wire, tubes or like semi-manufactured products, not otherwise provided for; Manufacture of tubes of special shape of sheets
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B21MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
    • B21CMANUFACTURE OF METAL SHEETS, WIRE, RODS, TUBES OR PROFILES, OTHERWISE THAN BY ROLLING; AUXILIARY OPERATIONS USED IN CONNECTION WITH METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL
    • B21C37/00Manufacture of metal sheets, bars, wire, tubes or like semi-manufactured products, not otherwise provided for; Manufacture of tubes of special shape
    • B21C37/04Manufacture of metal sheets, bars, wire, tubes or like semi-manufactured products, not otherwise provided for; Manufacture of tubes of special shape of bars or wire
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    • C22C1/00Making non-ferrous alloys
    • C22C1/02Making non-ferrous alloys by melting
    • C22C1/03Making non-ferrous alloys by melting using master alloys
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    • 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
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    • 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

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Abstract

The invention discloses a multi-element microalloyed magnesium alloy, a preparation method thereof and a plate extrusion forming process, belonging to the technical field of magnesium alloy and comprising the following steps: firstly, a novel multi-element microalloyed magnesium alloy is provided; secondly, providing a preparation method of the novel multi-element microalloyed magnesium alloy; and thirdly, providing a new thermal deformation process. The invention optimizes the structure by adding the multi-element microalloy and improves the mechanical property of the magnesium alloy by utilizing mechanisms such as solid solution strengthening, aging strengthening, dispersion strengthening and the like; ultrasonic treatment is used, the nucleation rate is increased, the structure is refined, and the multi-element microalloy is uniformly dispersed; then, thermal deformation treatment is carried out on the basis, a multi-stage solid solution process is adopted, and then extrusion treatment is carried out, so that the mechanical property of the alloy is improved. By the invention, the tensile strength of the magnesium alloy is 350-370MPa, the yield strength is 340-350MPa, and the yield strength is improved by 210-230MPa compared with the cast magnesium alloy.

Description

Multi-element microalloyed magnesium alloy, preparation method thereof and plate extrusion forming process
Technical Field
The invention belongs to the technical field of magnesium alloy, and particularly relates to a multi-element microalloyed magnesium alloy, a preparation method thereof and a plate extrusion forming process.
Background
The magnesium alloy is the alloy with the minimum density in the structural materials, has the characteristics of high specific strength, high specific rigidity, good shock absorption performance, good electromagnetic shielding resistance, excellent cutting processing performance and the like, and is widely applied to the fields of automobiles, aerospace and electronic products. In particular, in the field of automobiles, magnesium alloy materials are adopted, so that the weight can be reduced, and the energy consumption can be saved.
Pure magnesium has a close-packed hexagonal structure, low symmetry and few slippage systems at room temperature, so that the plasticity is poor and the mechanical property is poor, and the pure magnesium is rarely directly used as a structural material. In addition, the cast Mg-Zn alloy is easy to generate defects such as shrinkage porosity and the like, so the mechanical property of the cast Mg-Zn alloy is poor.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a multi-element microalloyed magnesium alloy, a preparation method thereof and a plate extrusion forming process.
The design concept of the invention is as follows:
firstly, the invention provides an alloying method, alloy elements are added into the alloy, the composition design is carried out, the structure is optimized, and the mechanical property of the magnesium alloy is improved by utilizing mechanisms such as solid solution strengthening, aging strengthening, dispersion strengthening and the like, so that the wider application of the magnesium alloy is realized.
At present, in a plurality of alloying systems, Mg-Zn alloy is a more commonly applied alloying system. The addition of Zn element can not only bring double strengthening effects of solid solution strengthening and aging strengthening, but also remove impurities such as Fe, Ni and the like, and play a role in removing impurities and purifying melt. The rare earth element has the functions of purifying alloy solution, improving the casting performance of the alloy, refining and modifying the alloy structure, improving the mechanical property of the cast alloy and the like, the solid solubility of Gd in magnesium is 23.5 percent at 548 ℃, but the Gd exponentially decreases along with the temperature reduction, and the Gd is a very good alloying element for precipitation strengthening; the Y element has the function of refining grains; a small amount of Nd is added to refine grains and improve mechanical properties; a small amount of calcium element is added into the magnesium alloy, so that the casting structure of the magnesium alloy can be refined, and the mechanical property can be improved. Therefore, the invention improves the structure and the mechanical property of the magnesium alloy by adding the multielement microalloy elements into the Mg-Zn alloy.
Secondly, the mechanical property of the alloy is improved by an extrusion process, the extrusion is an effective mode for improving the structure and the property of the cast magnesium alloy, and because the material is subjected to strong three-dimensional compressive stress during extrusion deformation, the casting defect can be obviously eliminated, the structure is refined, and the plastic deformation of the blank is facilitated, so that the extrusion is very important for regulating and controlling the structure and the property of the magnesium alloy.
In order to solve the problems, the technical scheme of the invention is as follows:
a multi-component microalloyed magnesium alloy, wherein: the multi-element microalloyed magnesium alloy comprises the following elements in percentage by mass: zinc: 5.12-6.23wt.%, gadolinium: 0.89-1.21 wt.%, yttrium: 0.10-0.21wt.%, neodymium: 0.10-0.13 wt.%, calcium 0.020-0.03 wt.%, and magnesium in balance.
Further, the multi-element microalloyed magnesium alloy is Mg-6Zn-1Gd-0.12Y-0.11Nd-0.03 Ca.
A preparation method of a multi-element microalloyed magnesium alloy comprises the following steps:
s1, selecting raw materials: a magnesium block with the purity of 99.9 percent, a zinc block with the purity of 99.9 percent, a calcium block with the purity of 99.9 percent, a magnesium gadolinium intermediate alloy, a magnesium yttrium intermediate alloy and a magnesium neodymium intermediate alloy; cutting a magnesium block according to the size of the crucible, polishing the magnesium block on a grinding wheel, and removing oxide skin on the surface of the magnesium block to enable the surface of the magnesium block to be smooth and clean for later use;
s2, preparing Mg-10Gd-2Zn-2Y-Nd intermediate alloy:
s21, weighing a magnesium block, a zinc block, a magnesium gadolinium intermediate alloy, a magnesium yttrium intermediate alloy and a magnesium neodymium intermediate alloy according to the mass percentage of each element in the Mg-10Gd-2Zn-2Y-Nd intermediate alloy, so that the intermediate alloy to be prepared comprises the following elements in percentage by mass: zinc: 1.921-2.533wt.%, gadolinium: 9.132-10.672 wt.%, yttrium: 1.921-2.533wt.%, neodymium: 0.971-1.323 wt.%, the balance magnesium;
s22, preheating of the zinc block and the intermediate alloy:
wrapping the zinc block, the magnesium-gadolinium intermediate alloy, the magnesium-yttrium intermediate alloy and the magnesium-neodymium intermediate alloy weighed in the step S21 with aluminum foil, and then placing the zinc block, the magnesium-gadolinium intermediate alloy, the magnesium-yttrium intermediate alloy and the magnesium-neodymium intermediate alloy into a muffle furnace for preheating treatment at the preheating temperature of 100-130 ℃ for 60-90min for later use;
s23, casting Mg-10Gd-2Zn-2Y-Nd intermediate alloy:
firstly, cleaning a crucible used for smelting, placing the cleaned crucible in a resistance furnace, and setting the temperature of the resistance furnace to be 350-450 ℃; secondly, after the resistance furnace reaches the set temperature, uniformly coating a layer of talcum powder solution on the crucible, after the volatile components of the talcum powder solution are completely evaporated, uniformly coating a layer of zinc oxide solution on the outer surface of the talcum powder layer, and after the volatile components of the zinc oxide solution are completely evaporated, raising the temperature of the resistance heating furnace to 740-770 ℃; thirdly, putting the magnesium blocks weighed in the step S21, introducing protective gas when the magnesium blocks are completely melted, standing for 15-20min, and skimming the scum on the surface of the metal liquid by using a skimming spoon; finally, the zinc block, the magnesium-gadolinium intermediate alloy, the magnesium-yttrium intermediate alloy and the magnesium-neodymium intermediate alloy preheated in the step S22 are placed into magnesium liquid, stirred for 3-5 minutes by a mechanical stirring paddle at the temperature of 740-770 ℃, the stirring speed is 10-15r/S, the temperature is kept for 5-10 minutes, the alloy liquid is cast into a mold preheated to the temperature of 150-250 ℃ to prepare an Mg-10Gd-2Zn-2Y-Nd intermediate alloy cast ingot for later use;
s3, preparing Mg-6Zn-1Gd-0.12Y-0.11Nd-0.03Ca multi-element microalloyed magnesium alloy:
s31, weighing zinc blocks, calcium blocks, magnesium forging blocks and 120-150g of Mg-10Gd-2Zn-2Y-Nd intermediate alloy ingot prepared in the step S23 according to the mass percentage content of each element in the Mg-6Zn-1Gd-0.12Y-0.11Nd-0.03Ca magnesium alloy, and enabling the high-strength tough magnesium alloy to be prepared to have the following element compositions and mass percentage contents: zinc: 5.12-6.23wt.%, gadolinium: 0.89-1.21 wt.%, yttrium: 0.10-0.21wt.%, neodymium: 0.10-0.13 wt.%, calcium 0.020-0.03 wt.%, and magnesium in balance;
s32, wrapping the zinc block, the calcium block and the Mg-10Gd-2Zn-2Y-Nd intermediate alloy weighed in the step S31 by using aluminum foil, and putting the wrapped intermediate alloy into a heating furnace for preheating, wherein the preheating temperature is 100-130 ℃, and the preheating time is 90-110 min;
s33, Mg-6Zn-1Gd-0.12Y-0.11Nd-0.03Ca multi-element microalloyed magnesium alloy casting
Firstly, cleaning a crucible used for smelting, placing the cleaned crucible in a resistance furnace, setting the temperature of the resistance furnace to be 350-; secondly, putting the magnesium blocks weighed in the step S31, introducing protective gas after the solid metal is completely melted into a liquid phase, and standing for 15-20 min; thirdly, placing the calcium block, the zinc block and the Mg-10Gd-2Zn-2Y-Nd intermediate alloy preheated in the step S32 into the crucible; and finally, after the added raw materials are completely melted, carrying out ultrasonic treatment on the melt by using an ultrasonic treatment device, wherein the rated power is 2kW, the output power is 75-85%, the frequency is 19-19.6kHz, and the time is 15-20min, standing for 25-30min, and then casting to obtain the Mg-6Zn-1Gd-0.12Y-0.11Nd-0.03Ca multi-element microalloyed magnesium alloy ingot.
Further, the magnesium gadolinium intermediate alloy is Mg-30Gd, the magnesium yttrium intermediate alloy is Mg-30Y, and the magnesium neodymium intermediate alloy is Mg-30 Nd.
Further, in the steps S23 and S33, the ratio of the talc powder solution is: 80g of talcum powder, 250mL of water and 20mL of water glass.
Further, in the steps S23 and S33, the ratio of the zinc oxide solution is: 45g of zinc oxide, 250mL of water and 45mL of water glass.
Further, in the steps S23 and S33, the protective gas is continuously introduced, wherein the protective gas is SF6And CO2Mixed gas of SF6The volume fraction of (A) is 5-6%.
Furthermore, the surfaces of the slag removing spoon and the stirring paddle are coated with talcum powder and zinc oxide.
Further, in step S33, the preheated zinc block and calcium are added into the crucible, and then ultrasonic treatment is performed to assist melting. Wherein the preheating temperature of an ultrasonic device used for ultrasonic treatment auxiliary melting is 680 +/-10 ℃.
A multi-element microalloyed magnesium alloy plate extrusion forming process comprises the following steps:
A. solution treatment: firstly, placing a multi-element microalloyed magnesium alloy ingot in a heat treatment furnace for solution treatment, wherein the heating temperature is 360 ℃, and the heat preservation time is 2 hours; secondly, the temperature of the heat treatment furnace is raised to 430 ℃, and the heat preservation time is 2 hours; thirdly, raising the temperature to 510 ℃, and keeping the temperature for 9 hours; finally, taking out the magnesium alloy ingot after the solid solution is finished, and cooling by water for later use;
B. pretreatment: polishing the surface of the magnesium alloy ingot subjected to the solution treatment in the step A, preheating the magnesium alloy ingot at the preheating temperature of 260-280 ℃, and simultaneously preheating an extrusion die to the temperature of 260-280 ℃;
C. extrusion molding: and B, placing the magnesium alloy ingot preheated in the step B into an extrusion die, and extruding the magnesium alloy ingot into a bar, wherein the extrusion ratio is (15-17): 1, the extrusion temperature is 260 ℃ and 280 ℃, and the extrusion speed is 0.50-0.62 m/min; air cooling to room temperature after extrusion forming to prepare the high-strength and high-toughness magnesium alloy bar.
Compared with the prior art, the invention has the beneficial effects that:
the invention provides a high-strength and high-toughness magnesium alloy and a preparation method thereof by taking magnesium, zinc, calcium, magnesium gadolinium intermediate alloy, magnesium yttrium intermediate alloy and magnesium neodymium intermediate alloy as raw materials aiming at the conditions of low strength and poor plasticity of the magnesium alloy. By adding alloy elements and a hot extrusion deformation process, the tensile strength of the prepared multi-element microalloyed magnesium alloy is 350-370MPa, the yield strength is 340-350MPa, and the yield ratio is close to 1. The magnesium alloy has high yield strength which is improved by 210-230MPa compared with cast magnesium alloy, and the elongation can reach 8-11 percent, which is mainly due to the combined action of fine crystal strengthening, solid solution strengthening and second phase strengthening, and realizes the preparation of the high-strength high-toughness magnesium alloy.
Drawings
FIG. 1 is a stress-strain curve of an as-cast, solid solution, extruded Mg-6Zn-1Gd-0.12Y-0.11Nd-0.03Ca alloy;
FIG. 2 is a microstructure morphology diagram of an extruded Mg-6Zn-1Gd-0.12Y-0.11Nd-0.03Ca alloy;
FIG. 3 is a gold phase diagram of an extruded Mg-6Zn-1Gd-0.12Y-0.11Nd-0.03Ca alloy.
Detailed Description
The invention is described in further detail below with reference to the figures and examples.
A multi-component microalloyed magnesium alloy, wherein: the multi-element microalloyed magnesium alloy comprises the following elements in percentage by mass: zinc: 5.12-6.23wt.%, gadolinium: 0.89-1.21 wt.%, yttrium: 0.10-0.21wt.%, neodymium: 0.10-0.13 wt.%, calcium 0.020-0.03 wt.%, and magnesium in balance.
Further, the multi-element microalloyed magnesium alloy is Mg-6Zn-1Gd-0.12Y-0.11Nd-0.03 Ca.
A preparation method of a multi-element microalloyed magnesium alloy comprises the following steps:
s1, selecting raw materials: a magnesium block with the purity of 99.9 percent, a zinc block with the purity of 99.9 percent, a calcium block with the purity of 99.9 percent, a magnesium gadolinium intermediate alloy, a magnesium yttrium intermediate alloy and a magnesium neodymium intermediate alloy; cutting a magnesium block according to the size of the crucible, polishing the magnesium block on a grinding wheel, and removing oxide skin on the surface of the magnesium block to enable the surface of the magnesium block to be smooth and clean for later use;
s2, preparing Mg-10Gd-2Zn-2Y-Nd intermediate alloy:
s21, weighing a magnesium block, a zinc block, a magnesium gadolinium intermediate alloy, a magnesium yttrium intermediate alloy and a magnesium neodymium intermediate alloy according to the mass percentage of each element in the Mg-10Gd-2Zn-2Y-Nd intermediate alloy, so that the intermediate alloy to be prepared comprises the following elements in percentage by mass: zinc: 1.921-2.533wt.%, gadolinium: 9.132-10.672 wt.%, yttrium: 1.921-2.533wt.%, neodymium: 0.971-1.323 wt.%, the balance magnesium;
s22, preheating of the zinc block and the intermediate alloy:
wrapping the zinc block, the magnesium-gadolinium intermediate alloy, the magnesium-yttrium intermediate alloy and the magnesium-neodymium intermediate alloy weighed in the step S21 with aluminum foil, and then placing the zinc block, the magnesium-gadolinium intermediate alloy, the magnesium-yttrium intermediate alloy and the magnesium-neodymium intermediate alloy into a muffle furnace for preheating treatment at the preheating temperature of 100-130 ℃ for 60-90min for later use;
s23, casting Mg-10Gd-2Zn-2Y-Nd intermediate alloy:
firstly, cleaning a crucible used for smelting, placing the cleaned crucible in a resistance furnace, and setting the temperature of the resistance furnace to be 350-450 ℃; secondly, after the resistance furnace reaches the set temperature, uniformly coating a layer of talcum powder solution on the crucible, after the volatile components of the talcum powder solution are completely evaporated, uniformly coating a layer of zinc oxide solution on the outer surface of the talcum powder layer, and after the volatile components of the zinc oxide solution are completely evaporated, raising the temperature of the resistance heating furnace to 740-770 ℃; thirdly, putting the magnesium blocks weighed in the step S21, introducing protective gas when the magnesium blocks are completely melted, standing for 15-20min, and skimming the scum on the surface of the metal liquid by using a skimming spoon; finally, the zinc block, the magnesium-gadolinium intermediate alloy, the magnesium-yttrium intermediate alloy and the magnesium-neodymium intermediate alloy preheated in the step S22 are placed into magnesium liquid, stirred for 3-5 minutes by a mechanical stirring paddle at the temperature of 740-770 ℃, the stirring speed is 10-15r/S, the temperature is kept for 5-10 minutes, the alloy liquid is cast into a mold preheated to the temperature of 150-250 ℃ to prepare an Mg-10Gd-2Zn-2Y-Nd intermediate alloy cast ingot for later use;
s3, preparing Mg-6Zn-1Gd-0.12Y-0.11Nd-0.03Ca multi-element microalloyed magnesium alloy:
s31, weighing zinc blocks, calcium blocks, magnesium forging blocks and 120-150g of Mg-10Gd-2Zn-2Y-Nd intermediate alloy ingot prepared in the step S23 according to the mass percentage content of each element in the Mg-6Zn-1Gd-0.12Y-0.11Nd-0.03Ca magnesium alloy, and enabling the high-strength tough magnesium alloy to be prepared to have the following element compositions and mass percentage contents: zinc: 5.12-6.23wt.%, gadolinium: 0.89-1.21 wt.%, yttrium: 0.10-0.21wt.%, neodymium: 0.10-0.13 wt.%, calcium 0.020-0.03 wt.%, and magnesium in balance;
s32, wrapping the zinc block, the calcium block and the Mg-10Gd-2Zn-2Y-Nd intermediate alloy weighed in the step S31 by using aluminum foil, and putting the wrapped intermediate alloy into a heating furnace for preheating, wherein the preheating temperature is 100-130 ℃, and the preheating time is 90-110 min;
s33, Mg-6Zn-1Gd-0.12Y-0.11Nd-0.03Ca multi-element microalloyed magnesium alloy casting
Firstly, cleaning a crucible used for smelting, placing the cleaned crucible in a resistance furnace, setting the temperature of the resistance furnace to be 350-; secondly, putting the magnesium blocks weighed in the step S31, introducing protective gas after the solid metal is completely melted into a liquid phase, and standing for 15-20 min; thirdly, placing the calcium block, the zinc block and the Mg-10Gd-2Zn-2Y-Nd intermediate alloy preheated in the step S32 into the crucible; and finally, after the added raw materials are completely melted, carrying out ultrasonic treatment on the melt by using an ultrasonic treatment device, wherein the rated power is 2kW, the output power is 75-85%, the frequency is 19-19.6kHz, and the time is 15-20min, standing for 25-30min, and then casting to obtain the Mg-6Zn-1Gd-0.12Y-0.11Nd-0.03Ca multi-element microalloyed magnesium alloy ingot.
Compared with the prior art, the invention adds ultrasonic treatment to prepare the magnesium alloy, and the obtained as-cast magnesium alloy crystal grains are refined; due to the addition of the multiple trace elements, the mechanical property of the magnesium alloy is improved compared with that of the common magnesium alloy through the mechanisms of solid solution strengthening, fine grain strengthening and dispersion strengthening.
Further, the magnesium gadolinium intermediate alloy is Mg-30Gd, the magnesium yttrium intermediate alloy is Mg-30Y, and the magnesium neodymium intermediate alloy is Mg-30 Nd.
Further, in the steps S23 and S33, the ratio of the talc powder solution is: 80g of talcum powder, 250mL of water and 20mL of water glass.
Further, in the steps S23 and S33, the ratio of the zinc oxide solution is: 45g of zinc oxide, 250mL of water and 45mL of water glass.
Further, in the steps S23 and S33, the protective gas is continuously introduced, wherein the protective gas is SF6And CO2Mixed gas of SF6The volume fraction of (A) is 5-6%.
Furthermore, the surfaces of the slag removing spoon and the stirring paddle are coated with talcum powder and zinc oxide.
Further, in the step S33, the preheated zinc and calcium are added to the crucible and then the crucible is melted with the aid of ultrasonic treatment, wherein the preheating temperature of the ultrasonic aid is 680 ± 10 ℃
A multi-element microalloyed magnesium alloy plate extrusion forming process comprises the following steps:
A. solution treatment: firstly, placing a multi-element microalloyed magnesium alloy ingot in a heat treatment furnace for solution treatment, wherein the heating temperature is 360 ℃, and the heat preservation time is 2 hours; secondly, the temperature of the heat treatment furnace is raised to 430 ℃, and the heat preservation time is 2 hours; thirdly, raising the temperature to 510 ℃, and keeping the temperature for 9 hours; finally, taking out the magnesium alloy ingot after the solid solution is finished, and cooling by water for later use;
B. pretreatment: polishing the surface of the magnesium alloy ingot subjected to the solution treatment in the step A, preheating the magnesium alloy ingot at the preheating temperature of 260-280 ℃, and simultaneously preheating an extrusion die to the temperature of 260-280 ℃;
C. extrusion molding: and B, placing the magnesium alloy ingot preheated in the step B into an extrusion die, and extruding the magnesium alloy ingot into a bar, wherein the extrusion ratio is (15-17): 1, the extrusion temperature is 260 ℃ and 280 ℃, and the extrusion speed is 0.50-0.62 m/min; air cooling to room temperature after extrusion forming to prepare the high-strength and high-toughness magnesium alloy bar.
Comparing the magnesium alloy cast microstructure with the structure of the extruded magnesium alloy, the magnesium alloy has the advantages that the number of the grains of the extruded magnesium alloy is obviously increased, and the sizes of the grains are fine and uniform; the tensile strength of the extruded magnesium alloy is 350-370MPa, the yield strength is 340-350MPa, the yield strength is increased by 210-230MPa compared with the cast magnesium alloy, and the yield ratio is close to 1.
The above description is only for the specific embodiments of the present invention, but the scope of the present invention is not limited thereto, and any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope of the present invention are included in the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the appended claims.

Claims (8)

1. A preparation method of a multi-element microalloyed magnesium alloy is characterized by comprising the following steps:
s1, selecting raw materials: a magnesium block with the purity of 99.9 percent, a zinc block with the purity of 99.9 percent, a calcium block with the purity of 99.9 percent, a magnesium gadolinium intermediate alloy, a magnesium yttrium intermediate alloy and a magnesium neodymium intermediate alloy; cutting a magnesium block according to the size of the crucible, polishing the magnesium block on a grinding wheel, and removing oxide skin on the surface of the magnesium block to enable the surface of the magnesium block to be smooth and clean for later use;
s2, preparing Mg-10Gd-2Zn-2Y-Nd intermediate alloy:
s21, weighing a magnesium block, a zinc block, a magnesium gadolinium intermediate alloy, a magnesium yttrium intermediate alloy and a magnesium neodymium intermediate alloy according to the mass percentage of each element in the Mg-10Gd-2Zn-2Y-Nd intermediate alloy, so that the intermediate alloy to be prepared comprises the following elements in percentage by mass: zinc: 1.921-2.533wt.%, gadolinium: 9.132-10.672 wt.%, yttrium: 1.921-2.533wt.%, neodymium: 0.971-1.323 wt.%, the balance magnesium;
s22, preheating of the zinc block and the intermediate alloy:
wrapping the zinc block, the magnesium-gadolinium intermediate alloy, the magnesium-yttrium intermediate alloy and the magnesium-neodymium intermediate alloy weighed in the step S21 with aluminum foil, and then placing the zinc block, the magnesium-gadolinium intermediate alloy, the magnesium-yttrium intermediate alloy and the magnesium-neodymium intermediate alloy into a muffle furnace for preheating treatment at the preheating temperature of 100-130 ℃ for 60-90min for later use;
s23, casting Mg-10Gd-2Zn-2Y-Nd intermediate alloy:
firstly, cleaning a crucible used for smelting, placing the cleaned crucible in a resistance furnace, and setting the temperature of the resistance furnace to be 350-450 ℃; secondly, after the resistance furnace reaches the set temperature, uniformly coating a layer of talcum powder solution on the crucible, after the volatile components of the talcum powder solution are completely evaporated, uniformly coating a layer of zinc oxide solution on the outer surface of the talcum powder layer, and after the volatile components of the zinc oxide solution are completely evaporated, raising the temperature of the resistance heating furnace to 740-770 ℃; thirdly, putting the magnesium blocks weighed in the step S21, introducing protective gas when the magnesium blocks are completely melted, standing for 15-20min, and skimming the scum on the surface of the metal liquid by using a skimming spoon; finally, the zinc block, the magnesium-gadolinium intermediate alloy, the magnesium-yttrium intermediate alloy and the magnesium-neodymium intermediate alloy preheated in the step S22 are placed into magnesium liquid, stirred for 3-5 minutes by a mechanical stirring paddle at the temperature of 740-770 ℃, the stirring speed is 10-15r/S, the temperature is kept for 5-10 minutes, the alloy liquid is cast into a mold preheated to the temperature of 150-250 ℃ to prepare an Mg-10Gd-2Zn-2Y-Nd intermediate alloy cast ingot for later use;
s3, preparing Mg-6Zn-1Gd-0.12Y-0.11Nd-0.03Ca multi-element microalloyed magnesium alloy:
s31, weighing zinc blocks, calcium blocks, magnesium forging blocks and 120-150g of Mg-10Gd-2Zn-2Y-Nd intermediate alloy ingot prepared in the step S23 according to the mass percentage content of each element in the Mg-6Zn-1Gd-0.12Y-0.11Nd-0.03Ca magnesium alloy, and enabling the high-strength tough magnesium alloy to be prepared to have the following element compositions and mass percentage contents: zinc: 5.12-6.23wt.%, gadolinium: 0.89-1.21 wt.%, yttrium: 0.10-0.21wt.%, neodymium: 0.10-0.13 wt.%, calcium 0.020-0.03 wt.%, and magnesium in balance;
s32, wrapping the zinc block, the calcium block and the Mg-10Gd-2Zn-2Y-Nd intermediate alloy weighed in the step S31 by using aluminum foil, and putting the wrapped intermediate alloy into a heating furnace for preheating, wherein the preheating temperature is 100-130 ℃, and the preheating time is 90-110 min;
s33, Mg-6Zn-1Gd-0.12Y-0.11Nd-0.03Ca multi-element microalloyed magnesium alloy casting
Firstly, cleaning a crucible used for smelting, placing the cleaned crucible in a resistance furnace, setting the temperature of the resistance furnace to be 350-; secondly, putting the magnesium blocks weighed in the step S31, introducing protective gas after the solid metal is completely melted into a liquid phase, and standing for 15-20 min; thirdly, placing the calcium block, the zinc block and the Mg-10Gd-2Zn-2Y-Nd intermediate alloy preheated in the step S32 into the crucible; and finally, after the added raw materials are completely melted, carrying out ultrasonic treatment on the melt by using an ultrasonic treatment device, wherein the rated power is 2kW, the output power is 75-85%, the frequency is 19-19.6kHz, and the time is 15-20min, standing for 25-30min, and then casting to obtain the Mg-6Zn-1Gd-0.12Y-0.11Nd-0.03Ca multi-element microalloyed magnesium alloy ingot.
2. The method for preparing the multi-element microalloyed magnesium alloy as claimed in claim 1, wherein: the magnesium gadolinium intermediate alloy is Mg-30Gd, the magnesium yttrium intermediate alloy is Mg-30Y, and the magnesium neodymium intermediate alloy is Mg-30 Nd.
3. The method for preparing the multi-element microalloyed magnesium alloy as claimed in claim 1, wherein: in the steps S23 and S33, the proportion of the talcum powder solution is as follows: 80g of talcum powder, 250mL of water and 20mL of water glass.
4. The method for preparing the multi-element microalloyed magnesium alloy as claimed in claim 1, wherein: in the steps S23 and S33, the proportion of the zinc oxide solution is as follows: 45g of zinc oxide, 250mL of water and 45mL of water glass.
5. The multiplex micro-reactor of claim 1The preparation method of the alloyed magnesium alloy is characterized by comprising the following steps: in the steps S23 and S33, the protective gas is continuously introduced, wherein the protective gas is SF6And CO2Mixed gas of SF6The volume fraction of (A) is 5-6%.
6. The method for preparing the multi-element microalloyed magnesium alloy as claimed in claim 1, wherein: the surfaces of the slag removing spoon and the stirring paddle are coated with talcum powder and zinc oxide.
7. The method for preparing the multi-element microalloyed magnesium alloy as claimed in claim 1, wherein: in the step S33, the preheated zinc block and calcium are added into the crucible and then melted by ultrasonic treatment, wherein the preheating temperature of the ultrasonic device is 680 ± 10 ℃.
8. A process for extrusion forming a multi-component microalloyed magnesium alloy by the method of claim 1, which comprises the steps of:
A. solution treatment: firstly, placing a multi-element microalloyed magnesium alloy ingot in a heat treatment furnace for solution treatment, wherein the heating temperature is 360 ℃, and the heat preservation time is 2 hours; secondly, the temperature of the heat treatment furnace is raised to 430 ℃, and the heat preservation time is 2 hours; thirdly, raising the temperature to 510 ℃, and keeping the temperature for 9 hours; finally, taking out the magnesium alloy ingot after the solid solution is finished, and cooling by water for later use;
B. pretreatment: polishing the surface of the magnesium alloy ingot subjected to the solution treatment in the step A, preheating the magnesium alloy ingot at the preheating temperature of 260-280 ℃, and simultaneously preheating an extrusion die to the temperature of 260-280 ℃;
C. extrusion molding: and B, placing the magnesium alloy ingot preheated in the step B into an extrusion die, and extruding the magnesium alloy ingot into a bar, wherein the extrusion ratio is (15-17): 1, the extrusion temperature is 260 ℃ and 280 ℃, and the extrusion speed is 0.50-0.62 m/min; air cooling to room temperature after extrusion forming to prepare the high-strength and high-toughness magnesium alloy bar.
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