CN112195382A - Self-foaming porous magnesium alloy and preparation method thereof - Google Patents
Self-foaming porous magnesium alloy and preparation method thereof Download PDFInfo
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- CN112195382A CN112195382A CN202011223069.2A CN202011223069A CN112195382A CN 112195382 A CN112195382 A CN 112195382A CN 202011223069 A CN202011223069 A CN 202011223069A CN 112195382 A CN112195382 A CN 112195382A
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C23/00—Alloys based on magnesium
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- B22—CASTING; POWDER METALLURGY
- B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
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- B22D25/005—Casting metal foams
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C1/00—Making non-ferrous alloys
- C22C1/08—Alloys with open or closed pores
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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
- C22C1/08—Alloys with open or closed pores
- C22C1/083—Foaming process in molten metal other than by powder metallurgy
- C22C1/086—Gas foaming process
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C23/02—Alloys based on magnesium with aluminium as the next major constituent
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- C22C23/04—Alloys based on magnesium with zinc or cadmium as the next major constituent
Abstract
The invention provides a self-foaming porous magnesium alloy which comprises the following components: 4-12 wt% of Zn, 4-12 wt% of Al, 2-10 wt% of Gd, 0-0.4 wt% of Mn, 0-2 wt% of La, 0-2 wt% of Ce, 0-2.0 wt% of Sr, 0-1 wt% of Ca, less than 0.3 wt% of total impurities and the balance of Mg. The porous magnesium alloy provided by the invention contains Gd, Zn and Al, a melt formed by the Gd, the Zn and the Al after melting can absorb a large amount of gas, and in the solidification process, along with the reduction of temperature, the gas is gradually separated out and is finally regulated and released by an eutectic phase, so that bubbles are formed, and the purpose of self-foaming is achieved. The porous magnesium alloy provided by the invention can be realized without any foaming agent, tackifier or any special casting process and condition. The invention provides a preparation method of a self-foaming porous magnesium alloy.
Description
Technical Field
The invention belongs to the technical field of magnesium alloy, and particularly relates to a self-foaming porous magnesium alloy and a preparation method thereof.
Background
The porous metal or foam metal material combining metal phase and gas has the characteristics of metal and gas holes due to the special structure, and has a plurality of special physical properties, such as small density, large specific surface area, impact energy absorption, sound insulation, noise reduction, shock absorption, good electromagnetic shielding performance and the like. Therefore, the porous metal material has wide application prospect in the fields of aerospace, automobiles, buildings and the like. The magnesium alloy is a metal structure material with the lowest density in engineering application at present, is an ideal matrix of a light porous metal material, is nontoxic to a human body, has the density and mechanical properties very close to those of human bones, has good biocompatibility and degradability, and can increase the cell adhesion due to the porous structure; therefore, the porous magnesium alloy also has great application prospect in the field of biomedical materials.
At present, the preparation method of the porous magnesium alloy mainly comprises a melt foaming method, a seepage casting method, an investment casting method, a solid-gas eutectic solidification method, a powder metallurgy method, a secondary foaming method and the like. The melt foaming method mainly utilizes foaming agents such as fly ash microspheres, magnesium carbonate, calcium carbonate and the like, and simultaneously needs to improve the viscosity of the magnesium alloy melt by adding other alloying elements. The seepage casting method mainly prepares the open-cell foam magnesium alloy by means of a porous gasket material, and the process has certain explosion risk. The investment casting method is mainly used for preparing the open-cell foam magnesium alloy in an investment mode. The solid-gas eutectic solidification method mainly uses MgH2The powder is used as a foaming agent, and the lotus-root-shaped porous magnesium alloy is prepared by directional solidification. The powder metallurgy method is mainly characterized in that hydride powder or urea and other foaming agents are added, and then the closed-cell foam magnesium alloy with uniform pores is prepared by the powder metallurgy method. The secondary foaming method is to prepare the porous magnesium alloy by a two-step method, and needs a foaming agent, a tackifier, aluminum powder and the like. In addition, there are some new methods for preparing the porous magnesium alloy, such as high-pressure casting method (only the center has a porous structure), titanium hydride foaming hot-rolled plate.
It can be seen that the preparation of the existing porous magnesium alloy needs various foaming agents, tackifiers or special processes, such as melting mold, high pressure, etc. At present, a porous magnesium alloy material which can be foamed by means of a traditional casting method does not exist. The traditional casting method for preparing the porous magnesium alloy has low cost, is simple and safe, and is bound to become a necessary trend for the development of the porous magnesium alloy.
Disclosure of Invention
In view of the above, the present invention provides a self-foaming porous magnesium alloy and a preparation method thereof, and the self-foaming porous magnesium alloy provided by the present invention has adjustable porosity, adjustable pore size and excellent mechanical properties.
The invention provides a self-foaming porous magnesium alloy which comprises the following components:
4 to 12 wt% of Zn, in which,
4 to 12 wt% of Al,
2 to 10 wt% of Gd,
0 to 0.4 wt% of Mn,
0 to 2 wt% of La,
0 to 2 wt% of Ce,
0 to 2.0 wt% of Sr,
0 to 1 wt% of Ca,
the total amount of impurity elements is less than 0.3wt percent,
the balance being Mg.
Preferably, the mass content of Zn in the self-foaming porous magnesium alloy is 6-9%.
Preferably, the mass content of the Al in the self-foaming porous magnesium alloy is 6-8%.
Preferably, the mass content of Gd in the self-foaming porous magnesium alloy is 4% to 6%.
The invention provides a preparation method of the self-foaming porous magnesium alloy, which comprises the following steps:
mixing an Mg source, a Zn source, an Al source, a Gd source, a Mn source, a La source, a Ce source, a Sr source and a Ca source, and smelting to obtain alloy liquid;
and casting the alloy liquid to obtain the self-foaming porous magnesium alloy.
Preferably, the smelting temperature is 680-780 ℃.
Preferably, the casting temperature in the casting process is 650-750 ℃.
Preferably, the preparation method of the alloy liquid comprises the following steps:
mixing an Mg source and a Gd source, and smelting to obtain a first mixed molten metal;
mixing the first mixed molten metal with a Mn source, a La source, a Ce source, a Sr source and a Ca source, and smelting to obtain a second mixed molten metal;
and mixing the second mixed molten metal with a Zn source and an Al source, and smelting to obtain alloy liquid.
Preferably, the mold adopted in the casting process is a metal mold or a sand mold.
Preferably, the cooling mode in the casting process is furnace cooling, air cooling or water cooling.
The self-foaming porous magnesium alloy contains Gd, Zn and Al, a melt formed by the Gd, the Zn and the Al after melting can absorb a large amount of gas, and the gas is gradually separated out along with the reduction of the temperature in the solidification process to form bubbles, so that the porous magnesium alloy provided by the invention can realize the porous magnesium alloy without any foaming agent, tackifier or any special casting process and condition, therefore, the porous magnesium alloy provided by the invention is the self-foaming porous magnesium alloy, the content, the size and the distribution of pores of the porous magnesium alloy are closely related to alloy components and the solidification rate, and the adjustment of alloy pores is very easy to realize.
Experimental results show that the porosity of the self-foaming porous magnesium alloy can reach 70% at room temperature, the compressive yield strength is 8-105 MPa, the elastic modulus is 2-34 GPa, and the self-foaming porous magnesium alloy provided by the invention has high porosity and good mechanical property.
Drawings
FIG. 1 is a picture of a porous magnesium alloy prepared in examples 1-4 of the present invention, wherein (a) is example 1, (b) is example 2, (c) is example 3, and (d) is example 4;
FIG. 2 shows scanning electron micrographs of a porous magnesium alloy prepared in examples 1-4 of the present invention under backscattered electron scattering (a) is example 1, (b) is example 2, (c) is example 3, and (d) is example 4.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other examples, which may be modified or appreciated by those of ordinary skill in the art based on the examples given herein, are intended to be within the scope of the present invention. It should be understood that the embodiments of the present invention are only for illustrating the technical effects of the present invention, and are not intended to limit the scope of the present invention. In the examples, the methods used were all conventional methods unless otherwise specified.
The invention provides a self-foaming porous magnesium alloy which comprises the following components:
4 to 12 wt% of Zn, in which,
4 to 12 wt% of Al,
2 to 10 wt% of Gd,
0 to 0.4 wt% of Mn,
0 to 2 wt% of La,
0 to 2 wt% of Ce,
0 to 2.0 wt% of Sr,
0 to 1 wt% of Ca,
the total amount of impurity elements is less than 0.3 wt%, and the impurity elements are preferably Fe, Ni, Cu, Be and the like;
the balance being Mg.
In the present invention, the mass content of Zn in the self-foaming porous magnesium alloy is preferably 6% to 9%. The content of Zn in the self-foaming porous magnesium alloy provided by the invention enables the self-foaming porous magnesium alloy to have very good flow property, and further the method provided by the invention can be used for producing large-size castings with complex structures.
In the present invention, the mass content of Al in the self-foaming porous magnesium alloy is preferably 6% to 8%. In the invention, the Al can act together with the Zn in the technical scheme to further improve the fluidity of the alloy liquid, and simultaneously inhibit the hot cracking behavior in the alloy casting process, so that the self-foaming porous magnesium alloy provided by the invention has better casting quality.
In the invention, the mass content of Gd in the self-foaming porous magnesium alloy is preferably 4-6%. In the invention, the Gd can enter the ternary phase formed by combining Mg, Al and Zn in the technical scheme, in particular to a ternary quasicrystal phase; the ternary quasicrystal phase has a regulating effect on the absorption and release of gas in the solidification process, so that the content and the size of the pores of the self-foaming porous magnesium alloy provided by the invention can be regulated.
In the invention, the mass content of Mn in the self-foaming porous magnesium alloy is preferably 0.1-0.3%, and more preferably 0.2%; the mass content of the La in the self-foaming porous magnesium alloy is preferably 0.5-1.5%, and more preferably 1%; the mass content of Ce in the self-foaming porous magnesium alloy is preferably 0.5-1.5%, and more preferably 1%; the mass content of the Sr in the self-foaming porous magnesium alloy is preferably 0.5-1.5%, and more preferably 1%; the mass content of Ca in the self-foaming porous magnesium alloy is preferably 0.2-0.8%, and more preferably 0.3-0.6%. In the invention, the Mn, La, Ce, Sr and Ca elements do not influence the self-foaming process of the alloy obviously, but the existence of the elements can reduce the content of impurity elements such as Fe, Ni and the like in the alloy or improve the mechanical property of the alloy, so that the self-foaming porous magnesium alloy provided by the invention has higher purity and excellent mechanical property.
The invention provides a preparation method of the self-foaming porous magnesium alloy, which comprises the following steps:
mixing an Mg source, a Zn source, an Al source, a Gd source, a Mn source, a La source, a Ce source, a Sr source and a Ca source, and smelting to obtain alloy liquid;
and casting the alloy liquid to obtain the self-foaming porous magnesium alloy.
In the invention, the smelting temperature is preferably 690-740 ℃, more preferably 700-730 ℃, and most preferably 720 ℃. The invention preferably performs the smelting under protective gas conditions; the protective gas preferably comprises SF6And CO2(ii) a The SF6And CO2Volume of (2)The ratio is preferably 1: (50-120), more preferably 1: (60-100), most preferably 1: 80; in the present invention, the melting is preferably carried out under stirring.
In the invention, before the Mg source, the Zn source, the Al source, the Gd source, the Mn source, the La source, the Ce source, the Sr source, and the Ca source are mixed and smelted, the Mg source, the Zn source, the Al source, the Gd source, the Mn source, the La source, the Ce source, the Sr source, and the Ca source are preferably preheated at a temperature of preferably 120 to 400 ℃, more preferably 200 to 360 ℃, and most preferably 300 ℃.
In the present invention, the method for preparing the alloy liquid preferably includes:
mixing an Mg source and a Gd source, and smelting to obtain a first mixed molten metal;
mixing the first mixed molten metal with a Mn source, a La source, a Ce source, a Sr source and a Ca source, and smelting to obtain a second mixed molten metal;
and mixing the second mixed molten metal with a Zn source and an Al source, and smelting to obtain alloy liquid.
In the invention, the temperature for mixing the first mixed molten metal and the Mn source, the La source, the Ce source, the Sr source and the Ca source for smelting is preferably 720-750 ℃, more preferably 725-740 ℃, and most preferably 730 ℃; the time is preferably 5 minutes to 10 minutes, more preferably 6 minutes to 8 minutes; if the Mn, La, Ce, Sr, and Ca contents are 0 in the present invention, omitting this step, no second mixed metal liquid is produced.
In the present invention, the time for mixing and melting the second mixed molten metal, the Zn source, and the Al source is preferably 10 minutes to 20 minutes, and more preferably 6 minutes to 12 minutes.
In the invention, the Zn source is preferably pure zinc, the Al source is preferably pure aluminum, the Mg source is preferably pure magnesium, the Gd source is preferably a magnesium-gadolinium intermediate alloy, the mass fraction of gadolinium in the magnesium-gadolinium intermediate alloy is preferably 15-40%, more preferably 20-30%, the Mn source is preferably a magnesium-manganese intermediate alloy, the mass fraction of manganese in the magnesium-manganese intermediate alloy is preferably 3-6%, more preferably 4%, the La source is preferably a magnesium-lanthanum intermediate alloy, the mass fraction of lanthanum in the magnesium-lanthanum intermediate alloy is preferably 15-25%, more preferably 20%, the Ce source is preferably a magnesium-cerium intermediate alloy, the mass fraction of cerium in the magnesium-cerium intermediate alloy is preferably 15-25%, more preferably 20%, and the Sr source is preferably a magnesium-strontium intermediate alloy, the mass fraction of strontium in the magnesium-strontium intermediate alloy is preferably 20-30%, more preferably 25%, the Ca source is preferably a magnesium-calcium intermediate alloy, and the mass fraction of calcium in the magnesium-calcium intermediate alloy is preferably 20-30%, more preferably 25%; the present invention is not particularly limited in the source of the above alloy raw materials and can be commercially available.
In the present invention, the casting temperature (temperature of molten metal at the time of casting) in the casting process is preferably 650 to 750 ℃, more preferably 670 to 730 ℃, and most preferably 700 to 720 ℃; the mould adopted in the casting process is preferably a metal mould or a sand mould; the cooling mode in the casting process is preferably furnace cooling, air cooling or water cooling.
In the invention, the alloy liquid is preferably not refined after being obtained, the alloy liquid is preferably kept still, and the standing time is preferably 3 to 80 minutes, more preferably 10 to 60 minutes, and most preferably 30 to 50 minutes; the temperature of the alloy liquid during standing is preferably 680-780 ℃, more preferably 700-750 ℃, and most preferably 720-730 ℃.
The self-foaming porous magnesium alloy contains Gd, Zn and Al, a melt formed by the Gd, the Zn and the Al after melting can absorb a large amount of gas, and the gas is gradually separated out along with the reduction of the temperature in the solidification process to form bubbles, so that the porous magnesium alloy provided by the invention can realize the porous magnesium alloy without any foaming agent, tackifier or any special casting process and condition, therefore, the porous magnesium alloy provided by the invention is the self-foaming porous magnesium alloy, the content, the size and the distribution of pores of the porous magnesium alloy are closely related to alloy components and the solidification rate, and the adjustment of alloy pores is very easy to realize.
The self-foaming porous magnesium alloy provided by the invention contains Zn and Al, the Zn and the Al can generate a ternary quasicrystal phase through reaction with Mg, and meanwhile, the alloy contains Gd which can change the structure of the quasicrystal phase, so that the adjustment of gas absorption and release is realized; therefore, the content, the size and the distribution of the pores of the porous magnesium alloy can be adjusted by controlling the alloy components and the solidification rate, and the method is reliable, simple and safe.
The alloy raw materials adopted in the following embodiments of the present invention are all commercially available products, the mass fraction of gadolinium in the magnesium-gadolinium intermediate alloy is 20%, the mass fraction of lanthanum in the magnesium-lanthanum intermediate alloy is 20%, the mass fraction of cerium in the magnesium-cerium intermediate alloy is 20%, the mass fraction of manganese in the magnesium-manganese intermediate alloy is 4%, the mass fraction of calcium in the magnesium-calcium intermediate alloy is 25%, and the mass fraction of strontium in the magnesium-strontium intermediate alloy is 25%, and the alloy raw materials are all provided by koximes magnesium industries, ltd.
Example 1
9000g of pure magnesium, 1800g of pure zinc, 1200g of pure aluminum and 3000g of magnesium-gadolinium intermediate alloy are preheated to 300 ℃; firstly, putting preheated pure magnesium and magnesium-gadolinium intermediate alloy into a crucible preheated to 300 ℃, and introducing SF into the crucible6And CO2Is 1:80, adding the pure zinc and the pure aluminum preheated to 300 ℃ into the crucible at 730 ℃ under the stirring condition, and carrying out mixed smelting for 8 minutes to obtain alloy liquid;
cooling the alloy liquid to 710 ℃, and standing for 15 minutes;
the alloy liquid after standing is directly cast into an open iron mold which is in a cuboid shape and is used for common ingot casting without a cooling device, the end face of the mold is in a trapezoid shape (80mm multiplied by 120mm), and the length of the mold is 400mm, so that the porous magnesium alloy is obtained.
The components of the porous magnesium alloy prepared in the embodiment 1 of the invention are detected by a spectrum analyzer, and the detection result shows that the components of the porous magnesium alloy prepared in the embodiment 1 of the invention are as follows: 11.74 wt% of Zn, 7.85 wt% of Al, 3.94 wt% of Gd, less than 0.03 wt% of the total amount of impurity elements Fe, Cu and Ni, and the balance of Mg.
The porous magnesium alloy prepared in example 1 of the present invention is observed by an optical photograph and a back-electron scattering scanning electron microscope, and the observation results are shown in fig. 1 (a)) and fig. 2 (a)), which shows that the porous magnesium alloy prepared in example 1 of the present invention has large pores and relatively uniform distribution.
The porous magnesium alloy prepared in example 1 of the present invention was measured for density and then calculated for porosity according to the standard of GB 4472-84 general rules for measuring Density and relative Density. The mechanical property at room temperature is tested according to the standard of GB/T7314-2017 metallic material room temperature compression test method, and then the yield strength is calculated according to the tested compression curve. The elastic modulus at room temperature is tested according to the standard of GB/T22315-. The detection result shows that the porosity of the porous magnesium alloy prepared in the embodiment 1 of the invention can reach 47% at room temperature, the compressive yield strength is 58MPa, and the elastic modulus is 17 GPa.
Example 2
8100g of pure magnesium, 1200g of pure zinc, 1200g of pure aluminum and 4500g of magnesium-gadolinium intermediate alloy are preheated to 300 ℃; firstly, putting preheated pure magnesium and magnesium-gadolinium intermediate alloy into a crucible preheated to 300 ℃, and introducing SF into the crucible6And CO2Is 1:80, adding the pure zinc and the pure aluminum preheated to 300 ℃ into the crucible at 730 ℃ under the stirring condition, and mixing for 8 minutes to obtain alloy liquid;
cooling the alloy liquid to 710 ℃, and standing for 15 minutes;
the alloy liquid after standing is directly cast into an open iron mold which is in a cuboid shape and is used for common ingot casting without a cooling device, the end face of the mold is in a trapezoid shape (80mm multiplied by 120mm), and the length of the mold is 400mm, so that the porous magnesium alloy is obtained.
The component detection of the porous magnesium alloy prepared in the embodiment 2 of the present invention is performed according to the method in the embodiment 1, and the detection result shows that the porous magnesium alloy prepared in the embodiment 2 of the present invention comprises the following components: 8.01 wt% of Zn, 7.92 wt% of Al, 5.71 wt% of Gd, less than 0.03% of the total amount of impurity elements of Fe, Cu and Ni, and the balance of Mg.
The porous magnesium alloy obtained in example 2 of the present invention was tested by the method of example 1, and the porous magnesium alloy obtained in example 2 of the present invention had small pores and relatively uniform distribution (fig. 1 (b) and fig. 2 (b)), and had a porosity of 66% at room temperature, a compressive yield strength of 18MPa, and an elastic modulus of 6 GPa.
Example 3
Preheating 9600g of pure magnesium, 1200g of pure zinc, 600g of pure aluminum and 3000g of magnesium-gadolinium intermediate alloy to 300 ℃; firstly, putting preheated pure magnesium and magnesium-gadolinium intermediate alloy into a crucible preheated to 300 ℃, and introducing SF into the crucible6And CO2Is 1:80, adding the pure zinc and the pure aluminum preheated to 300 ℃ into the crucible at 730 ℃ under the stirring condition, and mixing for 8 minutes to obtain alloy liquid;
cooling the alloy liquid to 710 ℃, and standing for 15 minutes;
the alloy liquid after standing is directly cast into an open iron mold which is in a cuboid shape and is used for common ingot casting without a cooling device, the end face of the mold is in a trapezoid shape (80mm multiplied by 120mm), and the length of the mold is 400mm, so that the porous magnesium alloy is obtained.
The component detection of the porous magnesium alloy obtained in the embodiment 3 of the invention is carried out by adopting a spectrum analyzer, and the detection result is that the porous magnesium alloy obtained in the embodiment 3 of the invention comprises the following components: 7.84 wt% of Zn, 3.89 wt% of Al, 3.81 wt% of Gd, less than 0.03 wt% of the total amount of impurity elements Fe, Cu and Ni, and the balance of Mg.
The porous magnesium alloy obtained in example 3 of the present invention was examined by the method of example 1, and the examination result showed that the porous magnesium alloy obtained in example 3 of the present invention has small pores and relatively uniform distribution (fig. 1 (c) and fig. 2 (c)), a porosity of 57% at room temperature, a compressive yield strength of 29MPa, and an elastic modulus of 10 GPa.
Example 4
6900g of pure magnesium, 1800g of pure zinc, 1800g of pure aluminum and 4500g of magnesium-gadolinium intermediate alloy are preheated to 300 ℃; firstly, putting preheated pure magnesium and magnesium-gadolinium intermediate alloy into a crucible preheated to 300 ℃, and introducing SF into the crucible6And CO2Is 1:80 at 73Adding the pure zinc and the pure aluminum preheated to 300 ℃ into the crucible at 0 ℃ under the stirring condition for mixing for 8 minutes to obtain alloy liquid;
cooling the alloy liquid to 710 ℃, and standing for 15 minutes;
the alloy liquid after standing is directly cast into an open iron mold which is in a cuboid shape and is used for common ingot casting without a cooling device, the end face of the mold is in a trapezoid shape (80mm multiplied by 120mm), and the length of the mold is 400mm, so that the porous magnesium alloy is obtained.
The component detection of the porous magnesium alloy prepared in the embodiment 4 of the present invention is performed according to the method of the embodiment 1, and the detection result shows that the porous magnesium alloy prepared in the embodiment 4 of the present invention has the following components: 11.73 wt% of Zn, 11.62 wt% of Al, 5.41 wt% of Gd, less than 0.03 wt% of the total amount of impurity elements Fe, Cu and Ni, and the balance of Mg.
The porous magnesium alloy obtained in example 4 of the present invention was tested by the method of example 1, and the test results showed that the porous magnesium alloy obtained in example 4 of the present invention has relatively small pores and relatively uniform distribution (fig. 1 (d) and fig. 2 (d)), and the porous magnesium alloy has a porosity of 58% at room temperature, a compressive yield strength of 21MPa, and an elastic modulus of 8 GPa.
Example 5
Preheating 6600g of pure magnesium, 1200g of pure zinc, 1200g of pure aluminum, 4500g of magnesium-gadolinium intermediate alloy and 1500g of magnesium-manganese intermediate alloy to 300 ℃; firstly, putting preheated pure magnesium and magnesium-gadolinium intermediate alloy into a crucible preheated to 300 ℃, and introducing SF into the crucible6And CO2Is 1:80, adding the magnesium-manganese intermediate alloy preheated to 300 ℃ into the crucible at 730 ℃ under the stirring condition, stirring for 5 minutes, and then adding pure zinc and pure aluminum preheated to 300 ℃ for mixing for 8 minutes to obtain alloy liquid;
cooling the alloy liquid to 710 ℃, and standing for 15 minutes;
the alloy liquid after standing is directly cast into an open iron mold which is in a cuboid shape and is used for common ingot casting without a cooling device, the end face of the mold is in a trapezoid shape (80mm multiplied by 120mm), and the length of the mold is 400mm, so that the porous magnesium alloy is obtained.
The component detection of the porous magnesium alloy prepared in the embodiment 5 of the present invention is performed according to the method of the embodiment 1, and the detection result shows that the porous magnesium alloy prepared in the embodiment 5 of the present invention has the following components: 7.90 wt% of Zn, 7.63 wt% of Al, 5.45 wt% of Gd, 0.37 wt% of Mn, less than 0.03 wt% of the total amount of impurity elements Fe, Cu and Ni, and the balance of Mg.
According to the method of the embodiment 1, the porous magnesium alloy prepared in the embodiment 5 of the present invention is detected, and the detection result shows that the porosity of the porous magnesium alloy prepared in the embodiment 5 of the present invention at room temperature can reach 47%, the compressive yield strength is 27MPa, and the elastic modulus is 13 GPa.
Example 6
Preheating 6600g of pure magnesium, 1200g of pure zinc, 1200g of pure aluminum, 4500g of magnesium-gadolinium intermediate alloy and 1500g of magnesium-lanthanum intermediate alloy to 300 ℃; firstly, putting preheated pure magnesium and magnesium-gadolinium intermediate alloy into a crucible preheated to 300 ℃, and introducing SF into the crucible6And CO2Is 1:80, adding the magnesium-lanthanum intermediate alloy preheated to 300 ℃ into the crucible under the conditions of stirring at 730 ℃, stirring for 5 minutes, and then adding pure zinc and pure aluminum preheated to 300 ℃ for mixing for 8 minutes to obtain alloy liquid;
cooling the alloy liquid to 710 ℃, and standing for 15 minutes;
the alloy liquid after standing is directly cast into an open iron mold which is in a cuboid shape and is used for common ingot casting without a cooling device, the end face of the mold is in a trapezoid shape (80mm multiplied by 120mm), and the length of the mold is 400mm, so that the porous magnesium alloy is obtained.
The components of the porous magnesium alloy prepared in example 6 of the present invention were detected by the method of example 1, and the detection result shows that the porous magnesium alloy prepared in example 6 of the present invention has the following components: 7.71 wt% of Zn, 7.92 wt% of Al, 5.42 wt% of Gd, 1.97 wt% of La, less than 0.03 wt% of the total amount of impurity elements Fe, Cu and Ni, and the balance of Mg.
According to the method of the embodiment 1, the porous magnesium alloy prepared in the embodiment 6 of the present invention is detected, and the detection result shows that the porosity of the porous magnesium alloy prepared in the embodiment 6 of the present invention at room temperature can reach 61%, the compressive yield strength is 19MPa, and the elastic modulus is 7 GPa.
Example 7
6900g of pure magnesium, 1200g of pure zinc, 1200g of pure aluminum, 4500g of magnesium-gadolinium intermediate alloy and 1200g of magnesium-calcium intermediate alloy are preheated to 300 ℃; firstly, putting preheated pure magnesium and magnesium-gadolinium intermediate alloy into a crucible preheated to 300 ℃, and introducing SF into the crucible6And CO2Is 1:80, adding the magnesium-calcium intermediate alloy preheated to 300 ℃ into the crucible at 730 ℃ under the stirring condition, stirring for 5 minutes, and then adding pure zinc and pure aluminum preheated to 300 ℃ for mixing for 8 minutes to obtain alloy liquid;
cooling the alloy liquid to 710 ℃, and standing for 15 minutes;
the alloy liquid after standing is directly cast into an open iron mold which is in a cuboid shape and is used for common ingot casting without a cooling device, the end face of the mold is in a trapezoid shape (80mm multiplied by 120mm), and the length of the mold is 400mm, so that the porous magnesium alloy is obtained.
The component detection of the porous magnesium alloy prepared in example 7 of the present invention was performed according to the method of example 1, and the detection result shows that the porous magnesium alloy prepared in example 7 of the present invention has the following components: 8.05 wt% of Zn, 7.88 wt% of Al, 5.51 wt% of Gd, 1.92 wt% of Ca, less than 0.03 wt% of the total amount of impurity elements Fe, Cu and Ni, and the balance of Mg.
According to the method of the embodiment 1, the porous magnesium alloy prepared in the embodiment 7 of the present invention is detected, and the detection result shows that the porosity of the porous magnesium alloy prepared in the embodiment 7 of the present invention at room temperature can reach 64%, the compressive yield strength is 19MPa, and the elastic modulus is 6 GPa.
Example 8
6900g of pure magnesium, 1200g of pure zinc, 1200g of pure aluminum, 4500g of magnesium-gadolinium intermediate alloy and 1200g of magnesium-strontium intermediate alloy are preheated to 300 ℃; firstly, putting preheated pure magnesium and magnesium-gadolinium intermediate alloy into a crucible preheated to 300 ℃, and introducing SF into the crucible6And CO2Is 1:80, adding the magnesium-strontium intermediate alloy preheated to 300 ℃ into the crucible under the conditions of stirring at 730 ℃, stirring for 5 minutes, and then adding pure zinc and pure aluminum preheated to 300 ℃ for mixing for 8 minutes to obtain alloy liquid;
cooling the alloy liquid to 710 ℃, and standing for 15 minutes;
the alloy liquid after standing is directly cast into an open iron mold which is in a cuboid shape and is used for common ingot casting without a cooling device, the end face of the mold is in a trapezoid shape (80mm multiplied by 120mm), and the length of the mold is 400mm, so that the porous magnesium alloy is obtained.
The component detection of the porous magnesium alloy prepared in the embodiment 8 of the present invention is performed according to the method of the embodiment 1, and the detection result shows that the porous magnesium alloy prepared in the embodiment 8 of the present invention has the following components: 7.93 wt% of Zn, 8.00 wt% of Al, 5.49 wt% of Gd, 1.83 wt% of Sr, the total amount of impurity elements Fe, Cu and Ni is less than 0.03 wt%, and the balance is Mg.
According to the method in the embodiment 1, the porous magnesium alloy prepared in the embodiment 8 of the present invention is detected, and the detection result shows that the porosity of the porous magnesium alloy obtained in the embodiment 8 of the present invention at room temperature can reach 67%, the compressive yield strength is 18MPa, and the elastic modulus is 6 GPa.
Example 9
7725g pure magnesium, 1200g pure zinc, 1200g pure aluminum, 4500g magnesium-gadolinium intermediate alloy and 1500g magnesium-cerium intermediate alloy are preheated to 300 ℃; firstly, putting preheated pure magnesium and magnesium-gadolinium intermediate alloy into a crucible preheated to 300 ℃, and introducing SF into the crucible6And CO2Is 1:80, adding the magnesium-cerium intermediate alloy preheated to 300 ℃ into the crucible at 730 ℃ under the stirring condition, stirring for 5 minutes, and then adding pure zinc and pure aluminum preheated to 300 ℃ for mixing for 8 minutes to obtain alloy liquid;
cooling the alloy liquid to 710 ℃, and standing for 15 minutes;
the alloy liquid after standing is directly cast into an open iron mold which is in a cuboid shape and is used for common ingot casting without a cooling device, the end face of the mold is in a trapezoid shape (80mm multiplied by 120mm), and the length of the mold is 400mm, so that the porous magnesium alloy is obtained.
The porous magnesium alloy prepared in example 9 of the present invention was subjected to component detection according to the method of example 1, and the detection result shows that the porous magnesium alloy prepared in example 9 of the present invention has the following components: 8.03 wt% of Zn, 7.95 wt% of Al, 5.62 wt% of Gd, 1.87 wt% of Ce, less than 0.03 wt% of the total amount of impurity elements Fe, Cu and Ni, and the balance of Mg.
According to the method of the embodiment 1, the porous magnesium alloy prepared in the embodiment 9 of the present invention is detected, and the detection result shows that the porosity of the porous magnesium alloy prepared in the embodiment 9 of the present invention at room temperature can reach 62%, the compressive yield strength is 27MPa, and the elastic modulus is 9 GPa.
Example 10
5850g of pure magnesium, 1200g of pure zinc, 1200g of pure aluminum, 4500g of magnesium-gadolinium intermediate alloy, 300g of magnesium-lanthanum intermediate alloy, 450g of magnesium-cerium intermediate alloy and 1500g of magnesium-manganese intermediate alloy are preheated to 300 ℃; firstly, putting preheated pure magnesium, magnesium-gadolinium intermediate alloy, magnesium-lanthanum intermediate alloy and magnesium-cerium intermediate alloy into a crucible preheated to 300 ℃, and introducing SF into the crucible6And CO2Is 1:80, adding the magnesium-manganese intermediate alloy preheated to 300 ℃ into the crucible for mixing for 5 minutes under the conditions of stirring at 730 ℃, and then adding pure zinc and pure aluminum preheated to 300 ℃ for mixing for 8 minutes to obtain alloy liquid;
cooling the alloy liquid to 710 ℃, and standing for 15 minutes;
the alloy liquid after standing is directly cast into an open iron mold which is in a cuboid shape and is used for common ingot casting without a cooling device, the end face of the mold is in a trapezoid shape (80mm multiplied by 120mm), and the length of the mold is 400mm, so that the porous magnesium alloy is obtained.
The component detection of the porous magnesium alloy prepared in example 10 of the present invention was performed according to the method of example 1, and the detection result shows that the porous magnesium alloy prepared in example 10 of the present invention has the following components: 7.91 wt% of Zn, 8.01 wt% of Al, 5.66 wt% of Gd, 0.37 wt% of La, 0.55 wt% of Ce, 0.28 wt% of Mn, less than 0.03 wt% of the total amount of impurity elements Fe, Cu and Ni, and the balance of Mg.
According to the method in the embodiment 1, the porous magnesium alloy prepared in the embodiment 10 of the present invention is detected, and the detection result shows that the porosity of the porous magnesium alloy obtained in the embodiment 10 of the present invention at room temperature can reach 65%, the compressive yield strength is 18MPa, and the elastic modulus is 6 GPa.
Example 11
Preheating 5250g of pure magnesium, 1200g of pure zinc, 1200g of pure aluminum, 4500g of magnesium-gadolinium intermediate alloy, 600g of magnesium-calcium intermediate alloy, 750g of magnesium-cerium intermediate alloy and 1500g of magnesium-manganese intermediate alloy to 300 ℃; firstly, putting preheated pure magnesium, magnesium-gadolinium intermediate alloy and magnesium-cerium intermediate alloy into a crucible preheated to 300 ℃, and introducing SF into the crucible6And CO2Is 1:80, adding the magnesium-manganese intermediate alloy and the magnesium-calcium intermediate alloy preheated to 300 ℃ into the crucible at 730 ℃ under the stirring condition for mixing for 5 minutes, and then adding pure zinc and pure aluminum preheated to 300 ℃ for mixing for 8 minutes to obtain alloy liquid;
cooling the alloy liquid to 710 ℃, and standing for 15 minutes;
the alloy liquid after standing is directly cast into an open iron mold which is in a cuboid shape and is used for common ingot casting without a cooling device, the end face of the mold is in a trapezoid shape (80mm multiplied by 120mm), and the length of the mold is 400mm, so that the porous magnesium alloy is obtained.
The porous magnesium alloy prepared in example 11 of the present invention was subjected to component detection by the method of example 1, and the detection result shows that the porous magnesium alloy prepared in example 11 of the present invention had the following components: 7.82 wt% of Zn, 7.87 wt% of Al, 5.41 wt% of Gd, 0.97 wt% of Ce, 0.92 wt% of Ca, 0.31 wt% of Mn, less than 0.03 wt% of the total amount of impurity elements Fe, Cu and Ni, and the balance of Mg.
When the porous magnesium alloy obtained in example 11 of the present invention was measured by the method of example 1, the porosity of the porous magnesium alloy obtained in example 11 of the present invention was 63% at room temperature.
Example 12
6450g of pure magnesium, 1200g of pure zinc, 900g of pure aluminum, 4500g of magnesium-gadolinium intermediate alloy, 750g of magnesium-lanthanum intermediate alloy, 600g of magnesium-strontium intermediate alloy and 600g of magnesium-calcium intermediate alloy are preheated to 300 ℃; firstly, putting preheated pure magnesium and magnesium-gadolinium intermediate alloy into a crucible preheated to 300 ℃, and introducing SF into the crucible6And CO2Is 1:80, adding the pure zinc and the pure aluminum preheated to 300 ℃ into the crucible at 730 ℃ under the stirring condition, and mixing for 8 minutes to obtain alloy liquid;
introducing argon into the alloy liquid for refining, wherein the introducing time is 30 minutes, then cooling to 710 ℃, and simultaneously standing for 15 minutes;
the alloy liquid after standing is directly cast into an open iron mold which is in a cuboid shape and is used for common ingot casting without a cooling device, the end face of the mold is in a trapezoid shape (80mm multiplied by 120mm), and the length of the mold is 400mm, so that the porous magnesium alloy is obtained.
The component detection of the porous magnesium alloy prepared in the embodiment 12 of the present invention is performed according to the method of the embodiment 1, and the detection result shows that the porous magnesium alloy prepared in the embodiment 12 of the present invention has the following components: 8.03 wt% of Zn, 5.82 wt% of Al, 5.53 wt% of Gd, 1.03 wt% of La, 0.91 wt% of Sr, 0.98 wt% of Ca, the total amount of impurity elements Fe, Cu and Ni is less than 0.03 wt%, and the balance of Mg.
When the porous magnesium alloy obtained in example 12 of the present invention was measured by the method of example 1, the porosity of the porous magnesium alloy obtained in example 12 of the present invention at room temperature was 61%.
Example 13
Preheating 12300g of pure magnesium, 600g of pure zinc, 600g of pure aluminum and 1500g of magnesium-gadolinium intermediate alloy to 300 ℃; firstly, putting preheated pure magnesium and magnesium-gadolinium intermediate alloy into a crucible preheated to 300 ℃, and introducing SF into the crucible6And CO2Is 1:80, adding the pure zinc and the pure aluminum preheated to 300 ℃ into the crucible at 730 ℃ under the stirring condition, and mixing for 8 minutes to obtain alloy liquid;
then cooling the alloy liquid to 710 ℃, and standing for 15 minutes;
the alloy liquid after standing is directly cast into an open iron mold which is in a cuboid shape and is used for common ingot casting without a cooling device, the end face of the mold is in a trapezoid shape (80mm multiplied by 120mm), and the length of the mold is 400mm, so that the porous magnesium alloy is obtained.
The porous magnesium alloy prepared in example 13 of the present invention was subjected to component detection by the method of example 1, and the detection result shows that the porous magnesium alloy prepared in example 13 of the present invention had the following components: 3.87 wt% of Zn, 3.98 wt% of Al, 1.66 wt% of Gd, less than 0.03 wt% of the total amount of impurity elements Fe, Cu and Ni, and the balance of Mg.
When the porous magnesium alloy obtained in example 13 of the present invention was measured by the method of example 1, the porosity of the porous magnesium alloy obtained in example 13 of the present invention was 21% at room temperature.
Example 14
Preheating 5100g of pure magnesium, 1200g of pure zinc, 1200g of pure aluminum and 7500g of magnesium-gadolinium intermediate alloy to 300 ℃; firstly, putting preheated pure magnesium and magnesium-gadolinium intermediate alloy into a crucible preheated to 300 ℃, and introducing SF into the crucible6And CO2Is 1:80, adding the pure zinc and the pure aluminum preheated to 300 ℃ into the crucible at 730 ℃ under the stirring condition, and mixing for 8 minutes to obtain alloy liquid;
introducing argon into the alloy liquid for refining, wherein the introducing time is 30 minutes, then cooling to 710 ℃, and simultaneously standing for 15 minutes;
the alloy liquid after standing is directly cast into an open iron mold which is in a cuboid shape and is used for common ingot casting without a cooling device, the end face of the mold is in a trapezoid shape (80mm multiplied by 120mm), and the length of the mold is 400mm, so that the porous magnesium alloy is obtained.
The components of the porous magnesium alloy prepared in example 14 of the present invention were measured by the method of example 1, and the measured results show that the porous magnesium alloy prepared in example 14 of the present invention has the following components: 7.72 wt% of Zn, 7.51 wt% of Al, 9.24 wt% of Gd, less than 0.03 wt% of the total amount of impurity elements Fe, Cu and Ni, and the balance of Mg.
When the porous magnesium alloy obtained in example 14 of the present invention was measured according to the method of example 1, the porosity of the porous magnesium alloy obtained in example 14 of the present invention at room temperature was 13%.
Example 15
Preheating 5100g of pure magnesium, 1800g of pure zinc, 600g of pure aluminum and 7500g of magnesium-gadolinium intermediate alloy to 300 ℃; firstly, putting preheated pure magnesium and magnesium-gadolinium intermediate alloy into a crucible preheated to 300 ℃, and introducing SF into the crucible6And CO2Is 1:80, adding the pure zinc and the pure aluminum preheated to 300 ℃ into the crucible at 730 ℃ under the stirring condition, and mixing for 8 minutes to obtain alloy liquid;
introducing argon into the alloy liquid for refining, wherein the introducing time is 30 minutes, then cooling to 680 ℃, and simultaneously standing for 15 minutes;
the alloy liquid after standing is directly cast into an open iron mold which is in a cuboid shape and is used for common ingot casting without a cooling device, the end face of the mold is in a trapezoid shape (80mm multiplied by 120mm), and the length of the mold is 400mm, so that the porous magnesium alloy is obtained.
The components of the porous magnesium alloy prepared in example 15 of the present invention were measured by the method of example 1, and the measured results show that the porous magnesium alloy prepared in example 15 of the present invention has the following components: 11.77 wt% of Zn, 3.76 wt% of Al, 9.27 wt% of Gd, less than 0.03 wt% of the total amount of impurity elements Fe, Cu and Ni, and the balance of Mg.
When the porous magnesium alloy obtained in example 15 of the present invention was measured according to the method of example 1, the porosity of the porous magnesium alloy obtained in example 15 of the present invention at room temperature was 17%.
The self-foaming porous magnesium alloy contains Gd, Zn and Al, a melt formed by the Gd, the Zn and the Al after melting can absorb a large amount of gas, and the gas is gradually separated out along with the reduction of the temperature in the solidification process to form bubbles, so that the porous magnesium alloy can be realized without any foaming agent, tackifier or any special casting process and condition, and the porous magnesium alloy provided by the invention is a self-foaming porous magnesium alloy. In addition, the porous magnesium alloy provided by the invention contains Zn and Al, the Zn and the Al can react with Mg to generate a ternary quasicrystal phase, and meanwhile, the alloy contains gadolinium, which can change the structure of the quasicrystal phase, thereby realizing the adjustment of gas absorption and release; therefore, the content, the size and the distribution of the pores of the porous magnesium alloy can be adjusted by controlling the alloy components and the solidification rate, and the method is reliable, simple and safe.
While only the preferred embodiments of the present invention have been shown and described, it will be understood by those skilled in the art that various changes in form and details may be made therein without departing from the spirit and scope of the invention.
Claims (10)
1. A self-foaming porous magnesium alloy comprises the following components:
4 to 12 wt% of Zn, in which,
4 to 12 wt% of Al,
2 to 10 wt% of Gd,
0 to 0.4 wt% of Mn,
0 to 2 wt% of La,
0 to 2 wt% of Ce,
0 to 2.0 wt% of Sr,
0 to 1 wt% of Ca,
the total amount of impurity elements is less than 0.3wt percent,
the balance being Mg.
2. The self-foaming porous magnesium alloy according to claim 1, wherein the Zn is contained in an amount of 6 to 9% by mass.
3. The self-foaming porous magnesium alloy according to claim 1, wherein the Al is contained in the self-foaming porous magnesium alloy in an amount of 6 to 8% by mass.
4. The self-foaming porous magnesium alloy according to claim 1, wherein the Gd is present in an amount of 4 to 6% by mass of the self-foaming porous magnesium alloy.
5. A method for preparing the self-foaming porous magnesium alloy of claim 1, comprising:
mixing an Mg source, a Zn source, an Al source, a Gd source, a Mn source, a La source, a Ce source, a Sr source and a Ca source, and smelting to obtain alloy liquid;
and casting the alloy liquid to obtain the self-foaming porous magnesium alloy.
6. The method of claim 5, wherein the temperature of the smelting is 680-780 ℃.
7. The method according to claim 5, wherein the casting temperature during casting is 650 to 750 ℃.
8. The method according to claim 5, wherein the preparation method of the alloy liquid comprises:
mixing an Mg source and a Gd source, and smelting to obtain a first mixed molten metal;
mixing the first mixed molten metal with a Mn source, a La source, a Ce source, a Sr source and a Ca source, and smelting to obtain a second mixed molten metal;
and mixing the second mixed molten metal with a Zn source and an Al source, and smelting to obtain alloy liquid.
9. The method according to claim 5, wherein the mold used in the casting process is a metal mold or a sand mold.
10. The method of claim 5, wherein the cooling during casting is furnace, air or water cooling.
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