CN115449684A - Magnesium alloy, preparation method thereof, magnesium alloy ingot and application - Google Patents
Magnesium alloy, preparation method thereof, magnesium alloy ingot and application Download PDFInfo
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- CN115449684A CN115449684A CN202210982492.3A CN202210982492A CN115449684A CN 115449684 A CN115449684 A CN 115449684A CN 202210982492 A CN202210982492 A CN 202210982492A CN 115449684 A CN115449684 A CN 115449684A
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- C—CHEMISTRY; METALLURGY
- 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
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/06—Making non-ferrous alloys with the use of special agents for refining or deoxidising
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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
- C22F1/04—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of aluminium or alloys based thereon
Abstract
The invention discloses a magnesium alloy and a preparation method thereof, a magnesium alloy ingot and application thereof, wherein the magnesium alloy comprises, by weight, 5% -12% of gadolinium, 1% -5% of yttrium, 1% -5% of samarium, 0.1% -0.8% of zirconium, 0.01% -0.5% of metal A and 80% -90% of magnesium, wherein the metal A is selected from one or more of lanthanum and strontium. The magnesium alloy material strengthens matrix metal magnesium by regulating and controlling raw material components and separating out dispersed nano-scale rare earth phase from rare earth metal samarium, gadolinium and yttrium in a grain boundary, and inhibits coarsening and growth of crystal grains in a heat treatment process by utilizing a high-temperature stable phase separated out by lanthanum or strontium. The metal raw material can fully exert the solid solution strengthening, the aging strengthening, the fine grain strengthening and the synergistic strengthening of the elements, thereby improving the heat resistance, the strength and the ductility of the magnesium alloy.
Description
Technical Field
The invention relates to the field of metallurgical materials, in particular to a magnesium alloy, a preparation method thereof, a magnesium alloy ingot and application.
Background
The magnesium alloy has the advantages of high specific strength, high specific rigidity, good castability, thermal conductivity, shock absorption, electromagnetic shielding property, easiness in recovery and the like, shows huge application potential in the fields of aerospace, rail transit, automobile industry, 3C products and the like, and is considered as an ideal material with the advantages of effective light weight, energy conservation and sustainable development. However, magnesium alloys have disadvantages such as low strength, poor plasticity and heat resistance, and the like, and have become one of the main factors that restrict their large-scale application.
The magnesium-gadolinium alloy (MgGd) cast magnesium alloy with Gd as a main precipitation strengthening element has mechanical properties far higher than that of the traditional commercial cast magnesium alloys such as WE43, WE54 and the like, and although the magnesium-gadolinium alloy is applied in the field of material light weight, the magnesium-gadolinium alloy can not meet the increasingly strict requirements of equipment such as aerospace, rail transit and the like on the high temperature resistance of the materials.
The traditional common means for improving the material performance comprise multi-element alloying and regulation and control of precipitated phase form, size and distribution through a heat treatment process, so that the material performance is improved, and the problems of difficult control of alloy components, complex interaction among elements, difficult regulation and control of reinforced phase composition and the like are caused by excessive types (nine or more) of alloying elements added in the multi-element alloying, so that the multi-element alloying is difficult to realize in actual production. And the other method realizes that fine and dispersed high-temperature stable phases are precipitated in the crystal interior and the crystal boundary by optimizing the heat treatment process, and plays a role in strengthening the plasticity and the heat resistance of the material by the cooperative pinning dislocation of the crystal interior and the crystal boundary. But the problems of coarsening of crystal grains, embrittlement of grain boundary precipitated phases and cooperative strengthening among elements in the heat treatment process cannot be well solved.
Disclosure of Invention
Accordingly, in order to improve the heat resistance, strength and ductility of magnesium alloys, it is necessary to provide a magnesium alloy, a method for producing the same, a magnesium alloy ingot, and applications thereof.
The invention provides a magnesium alloy which comprises, by weight, 5% -12% of gadolinium, 1% -5% of yttrium, 1% -5% of samarium, 0.1% -0.8% of zirconium, 0.01% -0.5% of metal A and 80% -90% of magnesium, wherein the metal A is selected from one or more of lanthanum and strontium.
In one embodiment, the alloy comprises, by weight, 7% to 10% of gadolinium, 1% to 4% of yttrium, 1% to 4% of samarium, 0.2% to 0.6% of zirconium, 0.01% to 0.4% of lanthanum, and 83% to 88% of magnesium, or
Comprises, by weight, 7-10% of gadolinium, 1-4% of yttrium, 1-4% of samarium, 0.2-0.6% of zirconium, 0.01-0.05% of strontium and 83-88% of magnesium.
Further, the invention also provides a preparation method of the magnesium alloy, which comprises the following steps:
s10: preparing metal magnesium, magnesium gadolinium intermediate alloy, magnesium yttrium intermediate alloy, magnesium zirconium intermediate alloy and intermediate alloy B according to the composition of the magnesium alloy, wherein the intermediate alloy B is selected from one or more of magnesium lanthanum intermediate alloy and magnesium strontium intermediate alloy;
s20: mixing magnesium, magnesium gadolinium intermediate alloy, magnesium samarium intermediate alloy, magnesium yttrium intermediate alloy and intermediate alloy B, heating to melt, stirring for the first time, and preparing premixed magnesium alloy;
s30: adding a magnesium-zirconium intermediate alloy into the premixed magnesium alloy, heating to melt, stirring for the second time, preserving heat, adding a refining agent, stirring for the third time, and refining for one or more times to prepare a precast alloy;
s40: casting the pre-cast alloy.
In one embodiment, step S20 includes SF 6 The temperature of the mixture is heated to 730-750 ℃ in the gas environment, and the first stirring time is 2-5 min.
In one embodiment, in step S30, the second stirring time is 2min to 5min, the holding time is 10min to 20min, and the third stirring time is 2min to 5min.
In one embodiment, after step S30 and before step S40, the method further comprises the step of degassing the pre-cast alloy: and carrying out one or more times of degassing treatment on the pre-cast alloy in an argon atmosphere, wherein the time of each degassing treatment is 4-8 min.
In one embodiment, the refining agent is selected from one or more of JDMJ refining agent, RJ2 refining agent, and RJ6 refining agent.
In one embodiment, the mass of the refining agent is 0.8-1.5% of the mass of the magnesium alloy.
Still further, the present invention also provides a magnesium alloy ingot, comprising a heat treatment of the magnesium alloy as described above, the heat treatment comprising:
and sequentially carrying out solid solution treatment, room-temperature water quenching, aging treatment and room-temperature water cooling on the magnesium alloy.
The invention also provides application of the magnesium alloy or the magnesium alloy ingot in preparation of aerospace materials, rail transit parts or automobile parts.
The magnesium alloy material strengthens matrix metal magnesium by regulating and controlling raw material components and separating out dispersed nano-scale rare earth phase at grain boundary by using rare earth samarium, gadolinium and yttrium, and inhibits coarsening and growth of crystal grains in the heat treatment process by using high-temperature stable phase separated out by lanthanum or strontium. The metal raw material can fully exert the solid solution strengthening, the aging strengthening, the fine grain strengthening and the synergistic strengthening of the elements, thereby improving the heat resistance, the strength and the ductility of the magnesium alloy.
Drawings
FIG. 1 is a microstructure of an example and a comparative example in an aged state (a) comparative example 1; (b) comparative example 2; (c) example 1; (d) example 2.
Detailed Description
The present invention may be embodied in many different forms and is not limited to the embodiments described herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete. Of course, they are merely examples and are not intended to limit the present invention. Moreover, the present disclosure may repeat reference numerals and/or letters in the various examples. This repetition is for the purpose of simplicity and clarity and does not in itself dictate a relationship between the various embodiments and/or configurations discussed.
Furthermore, the terms "first", "second" and "first" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include at least one of the feature. In the description of the invention, "a plurality" means at least two, e.g., two, three, etc., unless explicitly specified otherwise. In the description of the present invention, "a plurality" means at least one, e.g., one, two, etc., unless specifically limited otherwise.
The words "preferably," "more preferably," and the like, in the context of the present invention, refer to embodiments of the invention that may, in some instances, provide certain benefits. However, other embodiments may be preferred, under the same or other circumstances. Furthermore, the recitation of one or more preferred embodiments does not imply that other embodiments are not useful, nor is it intended to exclude other embodiments from the scope of the invention.
When a range of values is disclosed herein, the range is considered to be continuous and includes both the minimum and maximum values of the range, as well as each value between such minimum and maximum values. Further, when a range refers to an integer, each integer between the minimum and maximum values of the range is included. Further, when multiple range describing features or characteristics are provided, the ranges may be combined. In other words, unless otherwise indicated, all ranges disclosed herein are to be understood to encompass any and all subranges subsumed therein.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used in the description of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. As used herein, the term "and/or" includes any and all combinations of one or more of the associated listed items.
The invention provides a magnesium alloy which comprises, by weight, 5% -12% of gadolinium, 1% -5% of yttrium, 1% -5% of samarium, 0.1% -0.8% of zirconium, 0.01% -0.5% of metal A and 80% -90% of magnesium, wherein the metal A is selected from one or more of lanthanum and strontium.
In a specific example, the magnesium alloy further comprises an impurity element with a mass percentage of more than 0 and less than or equal to 0.03%, and the impurity element is selected from one or more of iron, nickel, copper and silicon.
Still further, the impurity element contains, in mass percent, more than 0 and less than or equal to 0.005% of iron, more than 0 and less than or equal to 0.005% of nickel, more than 0 and less than or equal to 0.005% of copper, and more than 0 and less than or equal to 0.005% of silicon.
In a specific example, the magnesium alloy comprises, in weight percent, 7% to 10% gadolinium, 1% to 4% yttrium, 1% to 4% samarium, 0.2% to 0.6% zirconium, 0.01% to 0.4% lanthanum, and 83% to 88% magnesium, or
The magnesium alloy comprises 7-10% of gadolinium, 1-4% of yttrium, 1-4% of samarium, 0.2-0.6% of zirconium, 0.01-0.05% of strontium and 83-88% of magnesium.
The magnesium alloy material strengthens matrix metal magnesium by regulating and controlling raw material components and separating out dispersed nano-scale rare earth phase from rare earth metal samarium, gadolinium and yttrium in a grain boundary, and inhibits coarsening and growth of crystal grains in a heat treatment process by utilizing a high-temperature stable phase separated out by lanthanum or strontium. The metal raw materials can fully play the roles of solid solution strengthening, aging strengthening, fine grain strengthening and synergistic strengthening of elements, thereby improving the heat resistance, strength and ductility of the magnesium alloy.
Further, the invention also provides a preparation method of the magnesium alloy, which comprises the following steps:
s10: preparing metal magnesium, magnesium-gadolinium alloy, magnesium-yttrium alloy, magnesium-samarium alloy, magnesium-zirconium alloy and alloy B according to the composition of the magnesium alloy, wherein the alloy B is selected from one or more of magnesium-lanthanum alloy and magnesium-strontium alloy;
s20: mixing and adding metal magnesium, magnesium-gadolinium alloy, magnesium-samarium alloy, magnesium-yttrium alloy and alloy B, heating to melt, stirring for the first time, and preparing premixed magnesium alloy;
s30: adding a magnesium-zirconium intermediate alloy into the premixed magnesium alloy, heating to melt, stirring for the second time, preserving heat, adding a refining agent, stirring for the third time, and refining for one or more times to prepare a precast alloy;
s40: the pre-cast alloy is cast.
In one specific example, step S20 includes SF 6 The temperature of the mixture is heated to 730-750 ℃ in the gas environment, and the first stirring time is 2-5 min.
It can be understood that the magnesium gadolinium intermediate alloy is Mg-Gd, the magnesium yttrium intermediate alloy is Mg-Y, the magnesium samarium intermediate alloy is Mg-Sm, the magnesium lanthanum intermediate alloy is Mg-La, the magnesium strontium intermediate alloy is Mg-Sr and the magnesium zirconium intermediate alloy is Mg-Zr.
Further, in step S20, the melting crucible and the intermediate alloy raw material are preheated to 180-220 ℃, then the magnesium, magnesium-gadolinium alloy, magnesium-yttrium alloy, magnesium-samarium alloy and alloy B are sequentially placed into the melting crucible according to the melting point, specifically from low to high, and when the temperature of the melting furnace is raised to 650-700 ℃, the melting furnace containing SF is heated 6 The smelting crucible is placed in a smelting furnace in the gas environment, the temperature is raised to 730-750 ℃, then the heat preservation is carried out, after the raw materials are completely melted, the surface scum is skimmed off, and the mechanical stirring is carried out for 2 min-5 mnin.
In a particular example, the melting crucible is selected from a graphite crucible, a magnesia crucible or a corundum crucible, preferably a graphite crucible.
Further, the above contains SF 6 Also comprises carbon dioxide, preferably from SF 6 And carbon dioxide, and SF 6 The volume content of (A) is 0.5-1.5%.
In a specific example, in step S30, the second stirring time is 2min to 5min, the holding time is 10min to 20min, and the third stirring time is 2min to 5min.
When the refining frequency is more than one time, the interval of each refining is 10 min-20 min.
In one particular example, the refining agent is selected from one or more of JDMJ, RJ2, and RJ 6.
In a specific example, the mass of the refining agent is 0.8% to 1.5% of the mass of the magnesium alloy.
Preferably, the number of refining is two.
Further, in step S30, adding a magnesium-zirconium intermediate alloy into the pre-mixed magnesium alloy, heating to melt, skimming the surface scum after melting, stirring for the second time, mechanically stirring for 2min to 5min, keeping the temperature for 10min to 20min, adding a refining agent, stirring for the third time, mechanically stirring for 2min to 5min, refining for 2 times with an interval of 10min to 20min each time, and preparing the pre-cast alloy.
In a specific example, after step S30 and before step S40, the method further includes a step of degassing the pre-cast alloy: and carrying out one or more times of degassing treatment on the pre-cast alloy in the argon atmosphere, wherein the time of each degassing treatment is 4-8 min.
When the degassing treatment times are more than one time, the degassing treatment interval is 10 min-20 min.
Further, the degassing treatment is performed 10min to 20min after the refining treatment, the surface scum is skimmed after the degassing is completed, and the step S50 is performed after the surface scum is skimmed after the refining treatment is performed for 20min to 40 min.
Still further, the purity of the argon is greater than or equal to 99.999%.
In step S50, a steel mold is adopted for casting, and the steel mold is heated to 200-250 ℃ for casting to obtain the magnesium alloy.
Still further, the present invention provides a magnesium alloy ingot comprising a magnesium alloy as described above subjected to a heat treatment, the heat treatment comprising the steps of:
the magnesium alloy is sequentially subjected to solid solution treatment, room temperature water quenching, aging treatment and room temperature water cooling.
Further, the solid solution treatment is to keep the temperature of the magnesium alloy at 470-500 ℃ for 3-8 hours.
Furthermore, the aging treatment is carried out for 10 to 30 hours at 190 to 225 ℃ after water quenching at room temperature.
The invention also provides application of the magnesium alloy or the magnesium alloy ingot in preparation of aerospace materials, rail transit parts or automobile parts.
The following specific examples are provided to further illustrate the magnesium alloy and the method of manufacturing the same in detail.
The metal materials involved in the following embodiments are commercially available and include: magnesium ingots (99.99% magnesium, 0.0017% iron, 0.0003% nickel, 0.0003% copper, 0.0015% silicon), metallic gadolinium (99.5% gadolinium, 0.0095% iron, 0.0143% silicon, relative purity), metallic yttrium (99.9% yttrium, 0.026% iron, 0.0027% nickel, 0.01% silicon), metallic samarium (99.9% samarium, 0.0069% silicon, relative purity), metallic lanthanum (99.5% yttrium, 0.36% iron, relative purity), metallic strontium (99.0% strontium, 0.0025% iron, 0.002% silicon), metallic zirconium (99.4% zirconium, 0.038% iron, 0.035% nickel, 0.0019% copper, 0.0029% silicon). The intermediate alloy comprises a magnesium-gadolinium alloy with gadolinium content of 20-30% by mass, a magnesium-yttrium alloy with yttrium content of 20-30%, a magnesium-samarium alloy with samarium content of 20-30%, a magnesium-lanthanum alloy with lanthanum content of 20-30%, a magnesium-strontium alloy with strontium content of 20-30% and a magnesium-zirconium alloy with zirconium content of 15-25%.
Example 1
The embodiment provides a magnesium alloy, which comprises the following components: 8.0wt% Gd, 3.0wt% Y, 2.0wt% Sm, 0.15wt% La, 0.5wt% Zr, impurity elements 0.001wt% Fe, 0.003wt% Ni, 0.003wt% Cu, 0.002wt% Si, the balance Mg.
The preparation steps of the magnesium alloy are as follows: preparing alloy according to the above components, and mixing pure Mg and intermediate alloy Mg-Gd (the intermediate alloy)30% of medium gadolinium, 30% of Mg-Y (30% of yttrium in the intermediate alloy), mg-Sm (30% of samarium in the intermediate alloy), mg-La (30% of lanthanum in the intermediate alloy), mg-Zr (20% of zirconium in the intermediate alloy) and a crucible are preheated to 200 ℃, and then Mg-Sm, mg-Y, mg-Gd, mg-La and pure Mg are sequentially placed into the crucible according to the melting point; when the temperature of the smelting furnace rises to 670 ℃, putting the smelting furnace into a crucible containing raw materials and using SF 6 +CO 2 Protecting the mixed gas; heating to 740 ℃, preserving heat, skimming surface scum after the raw materials are completely melted, and mechanically stirring for 3 minutes; adding Mg-Zr intermediate alloy, skimming the surface scum after the Mg-Zr intermediate alloy is melted, and mechanically stirring for 3 minutes; keeping the temperature for 15 minutes, adding a refining agent JDMJ, mechanically stirring for 3 minutes, refining for 2 times and spacing for 15 minutes; keeping the temperature for 15 minutes after refining, degassing for 5 minutes, degassing for 2 times by adopting high-purity argon, wherein the degassing interval is 15 minutes each time, and then skimming the scum on the surface; after standing for 30 minutes, skimming the scum on the surface for casting, and preheating the surface to 200 ℃ by adopting a steel mould for casting to obtain the Mg-8Gd-3Y-2Sm-0.15La-0.5Zr alloy of the embodiment.
The heat treatment process of the magnesium alloy comprises the following steps: solution treatment is carried out for 4 hours at 480 ℃, and isothermal aging is carried out for 12 hours at 210 ℃.
Example 2
The embodiment provides a magnesium alloy, which comprises the following components: 9.0wt% Gd, 2.0wt% Y, 3.0wt% Sm, 0.15wt% La, 0.5wt% Zr, impurity elements 0.001wt% Fe, 0.003wt% Ni, 0.003wt% Cu, 0.002wt% Si, the balance Mg.
The preparation steps of the magnesium alloy are as follows: preparing an alloy according to the components, preheating pure Mg, an intermediate alloy Mg-Gd (30 percent of gadolinium in the intermediate alloy), mg-Y (30 percent of yttrium in the intermediate alloy), mg-Sm (30 percent of samarium in the intermediate alloy), mg-La (30 percent of lanthanum in the intermediate alloy), mg-Zr (20 percent of zirconium in the intermediate alloy) and a crucible to 200 ℃, and then sequentially putting the Mg-Sm, the Mg-Y, the Mg-Gd, the Mg-La and the pure Mg into the crucible according to the melting point; when the temperature of the smelting furnace rises to 670 ℃, putting the crucible containing the raw materials into the smelting furnace and using SF 6 +CO 2 Protecting the mixed gas; heating to 740 ℃, preserving heat, and waiting for the raw materialsSkimming the surface scum after the materials are completely melted and mechanically stirring for 3 minutes; adding Mg-Zr intermediate alloy, skimming the surface scum after the Mg-Zr intermediate alloy is melted, and mechanically stirring for 3 minutes; keeping the temperature for 15 minutes, adding a refining agent JDMJ, mechanically stirring for 3 minutes, refining for 2 times and keeping the interval between the two times of 15 minutes; after refining, keeping the temperature for 15 minutes, degassing for 5 minutes, degassing for 2 times by adopting high-purity argon gas, wherein the degassing interval is 15 minutes each time, and then skimming the surface scum; after standing for 30 minutes, skimming the dross on the surface for casting, and preheating the casting to 200 ℃ by adopting a steel mould to obtain the Mg-9.0Gd-2.0Y-3.0Sm-0.15La-0.5Zr alloy of the embodiment.
The heat treatment process of the magnesium alloy comprises the following steps: solution treatment is carried out for 5 hours at 480 ℃, and isothermal aging is carried out for 14 hours at 210 ℃.
Example 3
The embodiment provides a magnesium alloy, which comprises the following components: 8.0wt% Gd, 3.0wt% Y, 2.0wt% Sm, 0.02wt% Sr, 0.5wt% Zr, impurity elements 0.001wt% Fe, 0.003wt% Ni, 0.003wt% Cu, 0.002wt% Si, the balance Mg.
The preparation steps of the magnesium alloy are as follows: preparing an alloy according to the components, preheating pure Mg, an intermediate alloy Mg-Gd (the gadolinium content in the intermediate alloy is 30%), mg-Y (the yttrium content in the intermediate alloy is 30%), mg-Sm (the samarium content in the intermediate alloy is 30%), mg-Sr (the strontium content in the intermediate alloy is 20%), mg-Zr (the zirconium content in the intermediate alloy is 20%) and a crucible to 200 ℃, and then sequentially putting Mg-Sm, mg-Y, mg-Gd, mg-Sr and pure Mg into the crucible according to the melting point; when the temperature of the smelting furnace rises to 670 ℃, putting the smelting furnace into a crucible containing raw materials and using SF 6 +CO 2 Protecting the mixed gas; heating to 740 ℃, preserving heat, skimming surface scum after the raw materials are completely melted, and mechanically stirring for 3 minutes; adding Mg-Zr intermediate alloy, skimming the surface scum after the Mg-Zr intermediate alloy is melted, and mechanically stirring for 3 minutes; keeping the temperature for 15 minutes, adding a refining agent JDMJ, mechanically stirring for 3 minutes, refining for 2 times and keeping the interval between the two times of 15 minutes; after refining, keeping the temperature for 15 minutes, degassing for 5 minutes, degassing for 2 times by adopting high-purity argon gas, wherein the degassing interval is 15 minutes each time, and then skimming the surface scum; standing for 30 min, skimming off the surface scum, casting, and pouringThe casting was carried out by preheating a steel mold to 200 ℃ to obtain the Mg-8Gd-3Y-2Sm-0.02Sr-0.5Zr alloy of this example.
The heat treatment process of the magnesium alloy comprises the following steps: solution treatment is carried out for 5 hours at 480 ℃, and isothermal aging is carried out for 16 hours at 210 ℃.
Example 4
The embodiment provides a magnesium alloy, which comprises the following components: 8.0wt% Gd, 3.0wt% Y, 2.0wt% Sm, 0.04wt% Sr, 0.5wt% Zr, impurity elements 0.001wt% Fe, 0.003wt% Ni, 0.003wt% Cu, 0.002wt% Si, the balance Mg.
The preparation steps of the magnesium alloy are as follows: preparing an alloy according to the components, preheating pure Mg, an intermediate alloy Mg-Gd (the gadolinium content in the intermediate alloy is 30%), mg-Y (the yttrium content in the intermediate alloy is 30%), mg-Sm (the samarium content in the intermediate alloy is 30%), mg-Sr (the strontium content in the intermediate alloy is 20%), mg-Zr (the zirconium content in the intermediate alloy is 20%) and a crucible to 200 ℃, and then sequentially putting Mg-Sm, mg-Y, mg-Gd, mg-Sr and pure Mg into the crucible according to the melting point; when the temperature of the smelting furnace rises to 670 ℃, putting the crucible containing the raw materials into the smelting furnace and using SF 6 +CO 2 Protecting the mixed gas; heating to 740 ℃, preserving heat, skimming surface scum after the raw materials are completely melted, and mechanically stirring for 3 minutes; adding Mg-Zr intermediate alloy, skimming the surface scum after the Mg-Zr intermediate alloy is melted, and mechanically stirring for 3 minutes; keeping the temperature for 15 minutes, adding a refining agent JDMJ, mechanically stirring for 3 minutes, refining for 2 times and spacing for 15 minutes; keeping the temperature for 15 minutes after refining, degassing for 5 minutes, degassing for 2 times by adopting high-purity argon, wherein the degassing interval is 15 minutes each time, and then skimming the scum on the surface; after standing for 30 minutes, skimming the surface scum for casting, and preheating to 200 ℃ by adopting a steel mould for casting to obtain the Mg-8Gd-3Y-2Sm-0.04Sr-0.5Zr alloy of the embodiment.
The heat treatment process of the magnesium alloy comprises the following steps: solution treatment is carried out for 5 hours at 480 ℃, and isothermal aging is carried out for 16 hours at 210 ℃.
Comparative example 1
The comparative example provides a magnesium alloy comprising the following components: 8.0wt% Gd, 3.0wt% Y, 2.0wt% Sm, 0.5wt% Zr, 0.001wt% Fe, 0.003wt% impurity elements 0.003wt% Ni, 0.003wt% Cu, 0.002wt% Si, the balance Mg.
The preparation steps of the magnesium alloy are as follows: preparing an alloy according to the components, preheating pure Mg, an intermediate alloy Mg-Gd (the gadolinium content in the intermediate alloy is 30%), mg-Y (the yttrium content in the intermediate alloy is 30%), mg-Sm (the samarium content in the intermediate alloy is 30%), mg-Zr (the zirconium content in the intermediate alloy is 20%) and a crucible to 200 ℃, and then sequentially putting Mg-Sm, mg-Y, mg-Gd and pure Mg into the crucible according to the melting point; when the temperature of the smelting furnace rises to 670 ℃, putting the smelting furnace into a crucible containing raw materials and using SF 6 +CO 2 Protecting the mixed gas; heating to 740 ℃, preserving heat, skimming surface scum after the raw materials are completely melted, and mechanically stirring for 3 minutes; adding Mg-Zr intermediate alloy, skimming the surface scum after the Mg-Zr intermediate alloy is melted, and mechanically stirring for 3 minutes; keeping the temperature for 15 minutes, adding a refining agent JDMJ, mechanically stirring for 3 minutes, refining for 2 times and keeping the interval between the two times of 15 minutes; after refining, keeping the temperature for 15 minutes, degassing for 5 minutes, degassing for 2 times by adopting high-purity argon gas, wherein the degassing interval is 15 minutes each time, and then skimming the surface scum; and after standing for 30 minutes, skimming the scum on the surface for casting, and preheating the casting to 200 ℃ by adopting a steel mould to obtain the Mg-8Gd-3Y-2Sm-0.5Zr alloy of the comparative example.
The heat treatment process of the magnesium alloy comprises the following steps: solution treatment is carried out for 6 hours at 480 ℃, and isothermal aging is carried out for 16 hours at 210 ℃.
Comparative example 2
The comparative example provides a magnesium alloy comprising the following components: 10.0wt% Gd, 3.0wt% Y, 0.5wt% Zr, 0.001wt% Fe, 0.003wt% Ni, 0.003wt% Cu, 0.002wt% Si, the balance being Mg.
The preparation steps of the magnesium alloy are as follows: preparing an alloy according to the components, preheating pure Mg, an intermediate alloy Mg-Gd (the content of gadolinium in the intermediate alloy is 30%), mg-Y (the content of yttrium in the intermediate alloy is 30%), mg-Zr (the content of zirconium in the intermediate alloy is 20%) and a crucible to 200 ℃, and then sequentially putting Mg-Y, mg-Gd and pure Mg into the crucible according to the melting point; when the temperature of the smelting furnace rises to 670 ℃, putting the crucible containing the raw materials into the smelting furnace and using SF 6 +CO 2 Protecting the mixed gas; heating to 740 deg.C, and maintaining the temperature until the raw materials are completely meltedSkimming the surface scum and mechanically stirring for 3 minutes; adding Mg-Zr intermediate alloy, skimming surface scum after the Mg-Zr intermediate alloy is melted, and mechanically stirring for 3 minutes; keeping the temperature for 15 minutes, adding a refining agent JDMJ, mechanically stirring for 3 minutes, refining for 2 times and spacing for 15 minutes; after refining, keeping the temperature for 15 minutes, degassing for 5 minutes, degassing for 2 times by adopting high-purity argon gas, wherein the degassing interval is 15 minutes each time, and then skimming the surface scum; and after standing for 30 minutes, skimming the scum on the surface for casting, and preheating the casting to 200 ℃ by adopting a steel mould to obtain the Mg-10Gd-3Y-0.4Zr alloy of the comparative example.
The heat treatment process of the magnesium alloy comprises the following steps: solution treatment is carried out for 8 hours at 500 ℃ and isothermal aging is carried out for 16 hours at 215 ℃.
Comparative example 3
Comparative example 3 the magnesium alloy is gravity cast magnesium alloy with Mg-9Gd-2Y-0.5Zr metal type prepared by national magnesium alloy engineering technology research center of Chongqing university (Jiang bin high performance cast magnesium alloy and high quality member preparation and processing [ R ]. Wuhan special casting and non-ferrous alloy 2022.5).
Comparative example 4
Comparative example 4 Mg-4Y-3.3RE (Y, nd) -0.5Zr (WE 43) metal type gravity cast magnesium alloy prepared by national magnesium alloy engineering and technology research center of Chongqing university (Jiangsan. High performance cast magnesium alloy and high quality member preparation and processing [ R ]. Wuhan: special casting and non-ferrous alloy.2022.5) was referred.
Comparative example 5
Comparative example 5A permanent type magnesium alloy of Mg-10Gd-3Y-0.5Zr in a cast magnesium alloy ingot as promulgated by the national Standard of the people's republic of China (GB/T19078-2016) was referred to.
Comparative example 6
Comparative example 6A permanent type Mg-4Y-3RE-0.5Zr (WE 43) cast magnesium alloy in a cast magnesium alloy ingot as promulgated by the national Standard of the people's republic of China (GB/T19078-2016) was referred to.
For the magnesium alloys of the above examples and comparative examples, the sample preparation and mechanical property test were carried out according to the GB/T228.1-2010 Metal Material tensile test-Room temperature test and GB/T228.1-2015 Metal Material tensile test-high temperature test standards, the electronic tensile test was carried out on a Shimadzu precision Universal test machine in Japan, the tensile rate was 0.96mm/min, the samples were kept at the corresponding temperature for 25min, the temperature fluctuation was + -1 ℃, the specific properties are shown in the following Table 1, and the microstructure diagrams of examples 1-2 and comparative examples 1-2 are shown in FIG. 1, wherein (a) is comparative example 1; (b) is comparative example 2; (c) is example 1; example 2 is (d).
TABLE 1 mechanical Properties of magnesium alloy specimens in aging State
Therefore, the magnesium alloy provided by the invention not only has higher Vickers hardness, but also has good tensile strength at room temperature and 300 ℃, namely has heat resistance, strength and ductility.
All possible combinations of the technical features of the above embodiments may not be described for the sake of brevity, but should be considered as within the scope of the present disclosure as long as there is no contradiction between the combinations of the technical features.
The above-mentioned embodiments only express several embodiments of the present invention, so as to understand the technical solutions of the present invention specifically and in detail, but not to be understood as the limitation of the protection scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. It should be understood that the technical solutions provided by the present invention and obtained by logical analysis, reasoning or limited experiments by those skilled in the art are all within the scope of the appended claims. Therefore, the protection scope of the patent of the invention is subject to the content of the appended claims, and the description can be used for explaining the content of the claims.
Claims (10)
1. The magnesium alloy is characterized by comprising, by weight, 5% -12% of gadolinium, 1% -5% of yttrium, 1% -5% of samarium, 0.1% -0.8% of zirconium, 0.01% -0.5% of metal A and 80% -90% of magnesium, wherein the metal A is selected from one or more of lanthanum and strontium.
2. A magnesium alloy according to claim 1, comprising, in weight percent, 7% to 10% gadolinium, 1% to 4% yttrium, 1% to 4% samarium, 0.2% to 0.6% zirconium, 0.01% to 0.4% lanthanum and 83% to 88% magnesium, or
Comprises, by weight, 7-10% of gadolinium, 1-4% of yttrium, 1-4% of samarium, 0.2-0.6% of zirconium, 0.01-0.05% of strontium and 83-88% of magnesium.
3. The preparation method of the magnesium alloy is characterized by comprising the following steps of:
s10: preparing magnesium metal, a magnesium gadolinium master alloy, a magnesium yttrium master alloy, a magnesium zirconium master alloy and a master alloy B according to the composition of the magnesium alloy in claim 1 or 2, wherein the master alloy B is one or more selected from a magnesium lanthanum master alloy and a magnesium strontium master alloy;
s20: mixing magnesium, magnesium gadolinium intermediate alloy, magnesium samarium intermediate alloy, magnesium yttrium intermediate alloy and intermediate alloy B, heating to melt, stirring for the first time, and preparing premixed magnesium alloy;
s30: adding a magnesium-zirconium intermediate alloy into the premixed magnesium alloy, heating to be molten, stirring for the second time, preserving heat, adding a refining agent, stirring for the third time, and refining for one or more times to prepare a precast alloy;
s40: casting the pre-cast alloy.
4. The method for producing a magnesium alloy according to claim 3, wherein the step S20 includes SF 6 Is heated to 730 ℃ in a gas environmentThe first stirring time is 2min to 5min at the temperature of 750 ℃.
5. The method for preparing magnesium alloy according to claim 3, wherein in step S30, the time for the second stirring is 2min to 5min, the holding time is 10min to 20min, and the time for the third stirring is 2min to 5min.
6. The method for producing a magnesium alloy according to claim 3, further comprising, after step S30 and before step S40, a step of degassing the pre-cast alloy: and carrying out one or more times of degassing treatment on the pre-cast alloy in an argon atmosphere, wherein the time of each degassing treatment is 4-8 min.
7. The method for producing a magnesium alloy according to any one of claims 3 to 6, wherein the refining agent is one or more selected from the group consisting of JDMJ refining agent, RJ2 refining agent and RJ6 refining agent.
8. The method of producing a magnesium alloy according to any one of claims 3 to 6, wherein the mass of the refining agent is 0.8 to 1.5% of the mass of the magnesium alloy.
9. A magnesium alloy ingot comprising the magnesium alloy according to claim 1 or 2 subjected to heat treatment, the heat treatment comprising:
and sequentially carrying out solid solution treatment, room-temperature water quenching, aging treatment and room-temperature water cooling on the magnesium alloy.
10. Use of a magnesium alloy according to claim 1 or 2 or a magnesium alloy ingot according to claim 9 for the manufacture of an aerospace material, a rail transit component or an automotive part.
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