CN112680643B - Rare earth Y-containing self-foaming porous magnesium alloy and preparation method thereof - Google Patents
Rare earth Y-containing self-foaming porous magnesium alloy and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a porous magnesium alloy containing rare earth Y and a preparation method thereof, belonging to the technical field of magnesium alloy. Solves the problem that the preparation of the existing porous magnesium alloy needs various foaming agents and tackifiers or needs special processes. The self-foaming porous magnesium alloy comprises the following components: 3-9 wt% of Zn, 3-9 wt% of Al, 1-7 wt% of Y, 0-0.4 wt% of Mn, 0-2 wt% of La, 0-2 wt% of Ce, 0-2 wt% of Ca, 0-2 wt% of Sr, and the balance of Mg and inevitable impurity elements. The porosity of the porous magnesium alloy is adjustable, the pore size is adjustable, the mechanical property is excellent, and the preparation method of the porous magnesium alloy is reliable, low in cost, simple and safe based on the traditional casting method.
Description
Technical Field
The invention belongs to the technical field of magnesium alloy, and particularly relates to a porous magnesium alloy containing rare earth Y and a preparation method thereof.
Background
The porous metal material or the foam metal material formed by combining the metal phase and the gas phase has the characteristics of metal and pores due to the special structure, and has multiple special performances 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.
In the prior art, 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 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 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. There are other methods for preparing the porous magnesium alloy, such as high-pressure casting (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. In the prior art, 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
The invention aims to provide a rare earth Y-containing self-foaming porous magnesium alloy which is adjustable in porosity, pore size and mechanical property, and the preparation method of the porous magnesium alloy is reliable, low in cost, simple and safe based on a traditional casting method.
The technical scheme adopted by the invention for realizing the aim is as follows.
The invention provides a self-foaming porous magnesium alloy containing rare earth Y, which comprises the following components: 3-9 wt% of zinc (Zn), 3-9 wt% of aluminum (Al), 1-7 wt% of yttrium (Y), 0-0.4 wt% of manganese (Mn), 0-2 wt% of lanthanum (La), 0-2 wt% of cerium (Ce), 0-2 wt% of calcium (Ca), 0-2 wt% of strontium (Sr), and the balance of magnesium (Mg) and inevitable impurity elements.
Preferably, the mass content of Zn in the porous magnesium alloy is 6% to 8%.
Preferably, the mass content of Al in the porous magnesium alloy is 6% to 8%.
Preferably, the mass content of Y in the porous magnesium alloy is 4% to 5%.
The invention provides a preparation method of a self-foaming porous magnesium alloy containing rare earth Y, which comprises the following steps:
1) smelting a magnesium source, a zinc source, an aluminum source, an yttrium source, a manganese source, a lanthanum source, a cerium source, a calcium source and a strontium source according to the components to obtain an alloy liquid;
2) carrying out gravity casting on the alloy liquid obtained in the step 1) to obtain the self-foaming porous magnesium alloy containing the rare earth Y.
Preferably, in the step 1), the melting temperature is 680-780 ℃.
Preferably, in the step 1), smelting is carried out under the condition of protective gas, and the volume ratio of the protective gas to SF is 1 (50-120)6And CO2。
Preferably, in the step 1), the magnesium source, the zinc source, the aluminum source, the yttrium source, the manganese source, the lanthanum source, the cerium source, the calcium source and the strontium source are preheated before being smelted, and the preheating temperature is 120-400 ℃.
Preferably, in the step 1), the yttrium source is a magnesium-yttrium intermediate alloy with yttrium mass fraction of 15-40%.
Preferably, the process of step 1) is:
1a) taking a magnesium source, a zinc source, an aluminum source, an yttrium source, a manganese source, a lanthanum source, a cerium source, a calcium source and a strontium source according to the composition;
1b) smelting a magnesium source and an yttrium source to obtain a first mixed molten metal;
1c) mixing a manganese source, a lanthanum source, a cerium source, a calcium source and a strontium source with the first mixed molten metal obtained in the step 1b) to obtain a second mixed molten metal;
1d) and mixing the second mixed metal liquid, a zinc source and an aluminum source to obtain an alloy liquid.
More preferably, in the step 1c), the mixing time of the manganese source, the zirconium source, the silicon source, the calcium source, the strontium source, the silver source, the lanthanum source, the cerium source and the first mixed molten metal is 5min to 10min, the mixing temperature is 720 ℃ to 750 ℃, and in the step 1d), the mixing time of the second mixed molten metal, the zinc source and the aluminum source is 10min to 20 min.
Preferably, in the step 2), the alloy liquid is allowed to stand for 3 to 80min before gravity casting, and the temperature of the alloy liquid is 680 to 780 ℃ during standing.
Preferably, in the step 2), the mold adopted for gravity casting is a metal mold or a sand mold.
Preferably, in the step 2), the gravity casting is carried out in a cooling mode of furnace cooling, air cooling or water cooling.
Compared with the prior art, the invention has the beneficial effects that:
the self-foaming porous magnesium alloy provided by the invention contains Y, Zn and Al, a melt formed by the melted Y, Zn and Al 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, namely, the self-foaming is realized. In addition, Zn, Al and Mg react to generate a ternary quasicrystal phase, and Y can change the structure of the quasicrystal phase, so that the gas absorption and release can be adjusted, and therefore, the content, the size and the distribution of pores of the self-foaming porous magnesium alloy provided by the invention can be adjusted by controlling the alloy components and the solidification rate.
The self-foaming porous magnesium alloy provided by the invention has high porosity and good mechanical property, and experiments show that the porosity of the self-foaming porous magnesium alloy provided by the invention can reach 65% at room temperature, the compressive yield strength is 15-97 MPa, and the elastic modulus is 5-31 GPa.
The preparation method of the self-foaming porous magnesium alloy is based on the traditional casting method, and is reliable, low in cost, simple and safe.
Drawings
In order to more clearly illustrate the technical solutions in the embodiments of the present invention, the drawings needed to be used in the embodiments will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art that other drawings can be obtained according to the drawings without creative efforts.
In FIG. 1, (a) to (d) are optical photographs of the self-foaming porous magnesium alloy obtained in examples 1 to 4 of the present invention, respectively;
in FIG. 2, (a) to (d) are back electron scattering scanning electron micrographs of the self-foaming porous magnesium alloys obtained in examples 1 to 4 of the present invention, respectively.
Detailed Description
For a further understanding of the invention, preferred embodiments of the invention are described below in conjunction with the detailed description, but it is to be understood that the description is intended to further illustrate the features and advantages of the invention and not to limit the claims to the invention.
The invention relates to a self-foaming porous magnesium alloy containing rare earth Y, which comprises the following components: 3-9 wt% of Zn, 3-9 wt% of Al, 1-7 wt% of Y, 0-0.4 wt% of Mn, 0-2 wt% of La, 0-2 wt% of Ce, 0-2 wt% of Ca, 0-2 wt% of Sr, and the balance of Mg and inevitable impurity elements (if the impurity elements can be avoided, the impurity elements do not exist).
The porous magnesium alloy provided by the invention comprises 3-9 wt% of Zn. In the present invention, the mass content of Zn in the porous magnesium alloy is preferably 6% to 8%. The Zn content in the porous magnesium alloy provided by the invention ensures that the self-foaming porous magnesium alloy has very good flow property, and further the porous magnesium alloy provided by the invention can be used for producing large-size castings with complex structures.
The porous magnesium alloy provided by the invention comprises 3-9 wt% of Al. In the present invention, the mass content of Al in the porous magnesium alloy is preferably 6% to 8%. In the invention, Al can act together with 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 porous magnesium alloy provided by the invention has better casting quality.
The porous magnesium alloy provided by the invention comprises 1-7 wt% of Y. In the present invention, the mass content of Y in the porous magnesium alloy is preferably 4% to 5%. In the invention, Y 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 porous magnesium alloy provided by the invention can be regulated.
The porous magnesium alloy provided by the invention can also comprise other alloy elements, such as 0-0.4 wt% of Mn, 0-2 wt% of La, 0-2 wt% of Ce, 0-2 wt% of Ca and 0-2 wt% of Sr. In the present invention, other alloying elements do not significantly affect the self-foaming process of the alloy, but their presence may either reduce the content of impurity elements such as Fe, Ni, etc. in the alloy or may improve the mechanical properties of the alloy. Therefore, the porous magnesium alloy provided by the invention has higher purity and excellent mechanical property.
In the present invention, the inevitable impurity elements are one or more of Fe, Ni, Cu, Be, etc., and the total amount of the impurity elements is less than 0.3 wt%.
The preparation method of the rare earth Y-containing self-foaming porous magnesium alloy comprises the following steps:
1) smelting a magnesium source, a zinc source, an aluminum source, an yttrium source, a manganese source, a lanthanum source, a cerium source, a calcium source and a strontium source according to the components to obtain an alloy liquid;
2) carrying out gravity casting on the alloy liquid obtained in the step 1) to obtain the self-foaming porous magnesium alloy containing the rare earth Y.
In step 1) of the present invention, the melting method of the magnesium source, the zinc source, the aluminum source, the yttrium source, and the other alloying element sources is not particularly limited, and the technical scheme of metal melting known to those skilled in the art can be adopted.
The smelting temperature of the invention is 680-780 ℃, preferably 690-740 ℃, and most preferably 720 ℃.
The invention preferably carries out smelting under the condition of protective gas; the invention has no special limitation on the type and source of the protective gas, and the protective gas used in the preparation of the magnesium alloy, which is well known to those skilled in the art, can be obtained by market purchase; preferably the protective gas is SF6And CO2Mixed gas of (2), SF6And CO2The volume ratio of (A) to (B) is preferably 1 (50-120), more preferably 1: 80.
In the present invention, the melting is preferably carried out under stirring.
When the porous magnesium alloy does not contain other alloy elements, the magnesium source and the yttrium source are preferably smelted to obtain a first mixed molten metal; and then mixing the first mixed metal liquid, a zinc source and an aluminum source to obtain an alloy liquid. The mixing time of the first mixed metal liquid, the zinc source and the aluminum source is preferably 10 to 20min, and more preferably 6 to 12 min.
When the porous magnesium alloy contains other alloy elements, the magnesium source and the yttrium source are preferably smelted to obtain a first mixed molten metal; then mixing the first mixed molten metal with other alloy elements (one or more of a manganese source, a lanthanum source, a cerium source, a calcium source and a strontium source) to obtain a second mixed molten metal; and finally, mixing the second mixed metal liquid, a zinc source and an aluminum source to obtain the alloy liquid. In the present invention, the mixing temperature of the first mixed molten metal and the source of the other alloying element is preferably 720 ℃ to 750 ℃, more preferably 725 ℃ to 740 ℃, and most preferably 730 ℃. In the present invention, the mixing time of the first mixed molten metal and the other alloying elements is preferably 5 to 10min, and more preferably 6 to 8 min. The mixing time of the second mixed metal liquid, the zinc source and the aluminum source is preferably 10min to 20min, and more preferably 6min to 12 min.
In the present invention, before the magnesium source, the zinc source, the aluminum source, the yttrium source, and the other alloying element sources are melted, the magnesium source, the zinc source, the aluminum source, the yttrium source, and the other alloying element sources are preferably preheated. In the present invention, the temperature for preheating the magnesium source, the zinc source, the aluminum source, the yttrium source, and the other alloying element source is preferably 120 to 400 ℃, more preferably 200 to 360 ℃, and most preferably 300 ℃.
In the present invention, the zinc source is preferably pure zinc. In the present invention, the aluminum source is preferably pure aluminum. In the present invention, the magnesium source is preferably pure magnesium. The sources of the zinc source, the aluminum source and the magnesium source are not particularly limited and commercially available. In the present invention, the yttrium source is preferably a magnesium yttrium master alloy. In the present invention, the mass fraction of yttrium in the magnesium-yttrium master alloy is preferably 15% to 40%, more preferably 20% to 30%. In the present invention, the other alloying element source is preferably a magnesium-other alloying element master alloy, such as a magnesium-manganese master alloy, a magnesium-lanthanum master alloy, a magnesium-cerium master alloy, a magnesium-calcium master alloy, and a magnesium-strontium master alloy. In the invention, the mass fractions of other alloy elements in the magnesium-other alloy element intermediate alloy are not particularly limited, and the alloy preparation conditions can be met. The sources of yttrium source and other alloying element sources are not particularly limited in the present invention, and any source of the above kind known to those skilled in the art may be used, and may be commercially available.
In the present invention, after the alloy liquid is obtained, argon gas may be introduced into the alloy liquid to refine the alloy liquid. In the present invention, it is preferable not to refine. In the present invention, the alloy liquid is preferably left to stand. In the present invention, the time for the standing is preferably 3 to 80min, and the melt temperature at the time of the standing is preferably 680 to 780 ℃.
In the present invention, the temperature for gravity casting is preferably 650 to 750 ℃, more preferably 670 to 730 ℃, and most preferably 700 to 720 ℃. In the present invention, the gravity casting rate is not particularly limited, and a magnesium alloy casting method known to those skilled in the art may be used. The gravity casting mold of the present invention is not particularly limited, and a metal mold or a sand mold known to those skilled in the art may be used.
The porous magnesium alloy provided by the invention contains Y, Zn and Al, a melt formed by the melted Y, Zn and Al can absorb a large amount of gas, and the gas is gradually separated out along with the reduction of 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, and the porous magnesium alloy provided by the invention is a self-foaming porous magnesium alloy. In addition, Zn, Al and Mg react to generate a ternary quasicrystal phase, and Y can change the structure of the quasicrystal phase, so that the gas absorption and release can be adjusted.
The density of the porous magnesium alloy provided by the invention is tested according to the standard of GB 4472-84 general rule for measuring density and relative density, and then the porosity of the porous magnesium alloy is calculated. The mechanical property at room temperature is tested according to the standard of GB/T7314-2017 metallic material room temperature compression test method. Then calculating the yield strength and the absorption energy according to the tested compression curve; the elastic modulus at room temperature is tested according to the standard of GB/T22315-. The experimental result shows that the porosity of the self-foaming porous magnesium alloy can reach 65% at room temperature, the compressive yield strength is 15-97 MPa, and the elastic modulus is 5-31 GPa.
For further understanding of the present invention, the self-foaming porous magnesium alloy and the preparation method thereof provided by the present invention will be described in detail with reference to the following examples, which should not be construed as limiting the scope of the present invention.
The raw materials used in the following examples of the present invention are all commercially available products (llc of siemei, kohami, changchun), and the mass fraction of yttrium in all of the magnesium-yttrium master alloys used is 20%, the mass fraction of manganese in the magnesium-manganese master alloy used is 4%, the mass fraction of zirconium in the magnesium-lanthanum master alloy used is 20%, the mass fraction of silicon in the magnesium-cerium master alloy used is 20%, the mass fraction of calcium in the magnesium-calcium master alloy used is 25%, and the mass fraction of strontium in the magnesium-strontium master alloy used is 25%.
Example 1
9900g of pure magnesium, 1050g of pure zinc, 1050g of pure aluminum, 3000g of magnesium yttrium master alloy were preheated to 300 ℃. Firstly, putting preheated pure magnesium and magnesium-yttrium 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 8min to obtain alloy liquid; and cooling the alloy liquid to 710 ℃, and standing for 15 min.
The alloy liquid after standing was directly cast into an open rectangular parallelepiped mold for ordinary ingot casting without a cooling device, the end face of the mold was trapezoidal (80 mm. times.120 mm) and the length was 400 mm.
The component detection of the porous magnesium alloy obtained in the embodiment 1 of the present invention is performed by using a spectrum analyzer, and the detection result is that the porous magnesium alloy obtained in the embodiment 1 of the present invention includes: 6.94 wt% of Zn, 6.69 wt% of Al, 3.67 wt% of Y, less than 0.03 wt% of the total amount of impurity elements Fe, Cu and Ni, and the balance of magnesium. The porous magnesium alloy obtained in example 1 of the present invention was observed by an optical photograph and a scanning photograph, and the observation results are shown in fig. 1 (a) and fig. 2 (a). It can be seen that the porous magnesium alloy obtained in example 1 of the present invention has a relatively uniform pore distribution.
The porosity, the compressive yield strength, the absorption work and the elastic modulus are tested according to the standards of GB 4472-84 general rules for measuring density and relative density, GB/T7314 + 2017 + test method for metal material room temperature compression, GB/T22315 + 2008 + test method for elastic modulus and Poisson ratio of metal material. The experimental result shows that the porosity at room temperature can reach 65%, the compressive yield strength is 15MPa, and the elastic modulus is 5 GPa.
Example 2
11100g of pure magnesium, 1200g of pure zinc, 450g of pure aluminum and 3000g of magnesium-yttrium master alloy were preheated to 300 ℃. Firstly, putting preheated pure magnesium and magnesium-yttrium intermediate alloy into a crucible preheated to 300 ℃, and introducing SF into the crucible6And CO2Is 1:80, adding the above-mentioned mixed gas preheated to 730 deg.C into the crucible under the condition of stirringMixing pure zinc and pure aluminum at 300 ℃ for 8min to obtain alloy liquid; and cooling the alloy liquid to 710 ℃, and standing for 15 min.
The alloy liquid after standing was directly cast into an open rectangular parallelepiped mold for ordinary ingot casting without a cooling device, the end face of the mold was trapezoidal (80 mm. times.120 mm) and the length was 400 mm.
The component detection of the porous magnesium alloy obtained in the embodiment 2 of the present invention is performed by using a spectrum analyzer, and the detection result is that the porous magnesium alloy obtained in the embodiment 2 of the present invention includes: 7.79 wt% of Zn, 2.87 wt% of Al, 3.71 wt% of Y, less than 0.03 wt% of the total amount of impurity elements Fe, Cu and Ni, and the balance of magnesium. The porous magnesium alloy obtained in example 2 of the present invention was observed by an optical photograph and a scanning photograph, and the observation results are shown in fig. 1 (b) and fig. 2 (b). It can be seen that the porous magnesium alloy obtained in example 2 of the present invention has fewer pores.
The porosity, the compressive yield strength, the absorption work and the elastic modulus are tested according to the standards of GB 4472-84 general rules for measuring density and relative density, GB/T7314 + 2017 + test method for metal material room temperature compression, GB/T22315 + 2008 + test method for elastic modulus and Poisson ratio of metal material. The experimental result shows that the porosity at room temperature can reach 12%, the compressive yield strength is 97MPa, and the elastic modulus is 31 GPa.
Example 3
8550g of pure magnesium, 1350g of pure zinc, 1350g of pure aluminum, 3750g of magnesium-yttrium master alloy were preheated to 300 ℃. Firstly, putting preheated pure magnesium, magnesium yttrium and 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 8min to obtain alloy liquid; and cooling the alloy liquid to 710 ℃, and standing for 15 min.
The alloy liquid after standing was directly cast into an open rectangular parallelepiped mold for ordinary ingot casting without a cooling device, the end face of the mold was trapezoidal (80 mm. times.120 mm) and the length was 400 mm.
The component detection of the porous magnesium alloy obtained in the embodiment 3 of the present invention is performed by using a spectrum analyzer, and the detection result is that the porous magnesium alloy obtained in the embodiment 3 of the present invention includes: 8.77 wt% Zn, 8.56 wt% Al, 4.51 wt% Y, less than 0.03 wt% of impurity elements Fe, Cu and Ni, and the balance magnesium. The porous magnesium alloy obtained in example 3 of the present invention was observed by optical photograph and scanning photograph, and the observation results are shown in fig. 1 (c) and fig. 2 (c). .
The porosity, the compressive yield strength, the absorption work and the elastic modulus are tested according to the standards of GB 4472-84 general rules for measuring density and relative density, GB/T7314 + 2017 + test method for metal material room temperature compression, GB/T22315 + 2008 + test method for elastic modulus and Poisson ratio of metal material. The experimental result shows that the porosity at room temperature can reach 39%, the compressive yield strength is 42MPa, and the elastic modulus is 21 GPa.
Example 4
10050g of pure magnesium, 1050g of pure zinc, 900g of pure aluminum, 3000g of magnesium yttrium master alloy were preheated to 300 ℃. Firstly, putting preheated pure magnesium and magnesium-yttrium 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 8min to obtain alloy liquid; and cooling the alloy liquid to 710 ℃, and standing for 15 min.
The alloy liquid after standing was directly cast into an open rectangular parallelepiped mold for ordinary ingot casting without a cooling device, the end face of the mold was trapezoidal (80 mm. times.120 mm) and the length was 400 mm.
The component detection of the porous magnesium alloy obtained in the embodiment 4 of the present invention is performed by using a spectrum analyzer, and the detection result is that the porous magnesium alloy obtained in the embodiment 4 of the present invention includes: 6.87 wt% of Zn, 5.78 wt% of Al, 3.72 wt% of Y, less than 0.03 wt% of the total amount of impurity elements Fe, Cu and Ni, and the balance of magnesium. The porous magnesium alloy obtained in example 4 of the present invention was observed by optical photograph and scanning photograph, and the observation results are shown in fig. 1 (d) and fig. 2 (d).
The porosity, the compressive yield strength, the absorption work and the elastic modulus are tested according to the standards of GB 4472-84 general rules for measuring density and relative density, GB/T7314 + 2017 + test method for metal material room temperature compression, GB/T22315 + 2008 + test method for elastic modulus and Poisson ratio of metal material. The experimental result shows that the porosity at room temperature can reach 59%, the compressive yield strength is 22MPa, and the elastic modulus is 13 GPa.
Example 5
8400g of pure magnesium, 1050g of pure zinc, 1050g of pure aluminum, 3000g of magnesium-yttrium master alloy and 1500g of magnesium-manganese master alloy are preheated to 300 ℃. Firstly, putting preheated pure magnesium and magnesium-yttrium 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 a crucible at 730 ℃ under the stirring condition, stirring for 5min, and then adding pure zinc and pure aluminum preheated to 300 ℃ for mixing for 8min to obtain alloy liquid; and (3) cooling the alloy liquid to 710 ℃, and standing for 15 min.
The alloy liquid after standing was directly cast into an open rectangular parallelepiped mold for ordinary ingot casting without a cooling device, the end face of the mold was trapezoidal (80 mm. times.120 mm) and the length was 400 mm.
The component detection of the porous magnesium alloy obtained in the embodiment 5 of the present invention is performed by using a spectrum analyzer, and the detection result is that the porous magnesium alloy obtained in the embodiment 5 of the present invention includes: 6.71 wt% Zn, 6.52 wt% Al, 3.45 wt% Y, 0.33 wt% Mn, less than 0.03 wt% of the total amount of impurity elements Fe, Cu and Ni, and the balance magnesium. The porous magnesium alloy obtained in example 5 of the present invention was observed, and the observation results are shown in fig. 1.
The porosity, the compressive yield strength, the absorption work and the elastic modulus are tested according to the standards of GB 4472-84 general rules for measuring density and relative density, GB/T7314 + 2017 + test method for metal material room temperature compression, GB/T22315 + 2008 + test method for elastic modulus and Poisson ratio of metal material. The experimental result shows that the porosity at room temperature can reach 61%, the compressive yield strength is 16MPa, and the elastic modulus is 5 GPa.
Example 6
8400g of pure magnesium, 1050g of pure zinc, 1050g of pure aluminum, 3000g of magnesium-yttrium master alloy and 1500g of magnesium-lanthanum master alloy are preheated to 300 ℃. Firstly, putting preheated pure magnesium, magnesium lanthanum intermediate alloy and magnesium yttrium 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 for mixing for 8min to obtain alloy liquid; and cooling the alloy liquid to 710 ℃, and standing for 15 min.
The alloy liquid after standing was directly cast into an open rectangular parallelepiped mold for ordinary ingot casting without a cooling device, the end face of the mold was trapezoidal (80 mm. times.120 mm) and the length was 400 mm.
The component detection of the porous magnesium alloy obtained in the embodiment 6 of the present invention is performed by using a spectrum analyzer, and the detection result is that the porous magnesium alloy obtained in the embodiment 6 of the present invention includes: 7.01 wt% of Zn, 6.45 wt% of Al, 3.69 wt% of Y, 1.81 wt% of La, the total amount of impurity elements Fe, Cu and Ni is less than 0.03 wt%, and the balance is magnesium
The porosity, the compressive yield strength, the absorption work and the elastic modulus are tested according to the standards of GB 4472-84 general rules for measuring density and relative density, GB/T7314 + 2017 + test method for metal material room temperature compression, GB/T22315 + 2008 + test method for elastic modulus and Poisson ratio of metal material. The experimental result shows that the porosity at room temperature can reach 59%, the compressive yield strength is 17MPa, and the elastic modulus is 6 GPa.
Example 7
8700g of pure magnesium, 1050g of pure zinc, 1050g of pure aluminum, 3000g of magnesium-yttrium master alloy and 1200g of magnesium-calcium master alloy are preheated to 300 ℃. Firstly, putting preheated pure magnesium and magnesium-yttrium 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 the temperature of 730 ℃ under the stirring condition, stirring for 5min, and then adding the preheated magnesium-calcium intermediate alloyMixing pure zinc and pure aluminum at 300 ℃ for 8min to obtain alloy liquid; and cooling the alloy liquid to 710 ℃, and standing for 15 min.
The alloy liquid after standing was directly cast into an open rectangular parallelepiped mold for ordinary ingot casting without a cooling device, the end face of the mold was trapezoidal (80 mm. times.120 mm) and the length was 400 mm.
The component detection of the porous magnesium alloy obtained in the embodiment 7 of the present invention is performed by using a spectrum analyzer, and the detection result is that the porous magnesium alloy obtained in the embodiment 7 of the present invention includes: 6.91 wt% Zn, 6.55 wt% Al, 3.73 wt% Y, 1.91 wt% Ca, less than 0.03 wt% of the total amount of impurity elements Fe, Cu and Ni, and the balance magnesium.
The porosity, the compressive yield strength, the absorption work and the elastic modulus are tested according to the standards of GB 4472-84 general rules for measuring density and relative density, GB/T7314 + 2017 + test method for metal material room temperature compression, GB/T22315 + 2008 + test method for elastic modulus and Poisson ratio of metal material. The experimental result shows that the porosity at room temperature can reach 60%, the compressive yield strength is 20MPa, and the elastic modulus is 6 GPa.
Example 8
8700g of pure magnesium, 1050g of pure zinc, 10500g of pure aluminum, 3000g of magnesium yttrium master alloy, 1200g of magnesium strontium master alloy were preheated to 300 ℃. Firstly, putting preheated pure magnesium and magnesium-yttrium 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 a crucible at 730 ℃ under the stirring condition, stirring for 5min, and then adding pure zinc and pure aluminum preheated to 300 ℃ for mixing for 8min to obtain alloy liquid; and cooling the alloy liquid to 710 ℃, and standing for 15 min.
The alloy liquid after standing was directly cast into an open rectangular parallelepiped mold for ordinary ingot casting without a cooling device, the end face of the mold was trapezoidal (80 mm. times.120 mm) and the length was 400 mm.
The component detection of the porous magnesium alloy obtained in the embodiment 8 of the present invention is performed by using a spectrum analyzer, and the detection result is that the porous magnesium alloy obtained in the embodiment 8 of the present invention includes: 6.98 wt% of Zn, 6.63 wt% of Al, 3.53 wt% of Y, 1.80 wt% of Sr, the total amount of impurity elements Fe, Cu and Ni is less than 0.03 wt%, and the balance is magnesium.
The porosity, the compressive yield strength, the absorption work and the elastic modulus are tested according to the standards of GB 4472-84 general rules for measuring density and relative density, GB/T7314 + 2017 + test method for metal material room temperature compression, GB/T22315 + 2008 + test method for elastic modulus and Poisson ratio of metal material. The experimental result shows that the porosity at room temperature can reach 64%, the compressive yield strength is 17MPa, and the elastic modulus is 9 GPa.
Example 9
9525g of pure magnesium, 1050g of pure zinc, 1050g of pure aluminum, 3000g of magnesium-yttrium master alloy, 375g of magnesium-cerium master alloy were preheated to 300 ℃. Firstly, putting preheated pure magnesium, magnesium-cerium intermediate alloy and magnesium-yttrium 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 8min to obtain alloy liquid; and cooling the alloy liquid to 710 ℃, and standing for 15 min.
The alloy liquid after standing was directly cast into an open rectangular parallelepiped mold for ordinary ingot casting without a cooling device, the end face of the mold was trapezoidal (80 mm. times.120 mm) and the length was 400 mm.
The composition of the porous magnesium alloy obtained in the embodiment 9 of the present invention is detected by a spectrum analyzer, and the detection result is that the porous magnesium alloy obtained in the embodiment 9 of the present invention includes: 6.90 wt% of Zn, 6.62 wt% of Al, 3.51 wt% of Y, 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 magnesium.
The porosity, the compressive yield strength, the absorption work and the elastic modulus are tested according to the standards of GB 4472-84 general rules for measuring density and relative density, GB/T7314 + 2017 + test method for metal material room temperature compression, GB/T22315 + 2008 + test method for elastic modulus and Poisson ratio of metal material. The experimental result shows that the porosity at room temperature can reach 62%, the compressive yield strength is 17MPa, and the elastic modulus is 8 GPa.
Example 10
6450g of pure magnesium, 1050g of pure zinc, 1050g of pure aluminum, 3000g of magnesium yttrium master alloy, 750g of magnesium cerium master alloy, 1200g of magnesium calcium master alloy, 1500g of magnesium manganese master alloy were preheated to 300 ℃. Firstly, putting preheated pure magnesium, magnesium intermediate alloy and magnesium yttrium intermediate alloy into a crucible preheated to 300 ℃, and introducing SF into the crucible6And CO2Is 1:80, adding the magnesium-calcium intermediate alloy and the magnesium-manganese intermediate alloy preheated to 300 ℃ into a crucible at 730 ℃ under the stirring condition, stirring for 5min, and then adding pure zinc and pure aluminum preheated to 300 ℃ for mixing for 8min to obtain alloy liquid; and cooling the alloy liquid to 710 ℃, and standing for 15 min.
The alloy liquid after standing was directly cast into an open rectangular parallelepiped mold for ordinary ingot casting without a cooling device, the end face of the mold was trapezoidal (80 mm. times.120 mm) and the length was 400 mm.
The component detection of the porous magnesium alloy obtained in the embodiment 10 of the present invention is performed by using a spectrum analyzer, and the detection result is that the porous magnesium alloy obtained in the embodiment 10 of the present invention includes: 7.01 wt% of Zn, 6.73 wt% of Al, 3.64 wt% of Y, 0.91 wt% of Ce, 1.88 wt% of Ca, 0.32 wt% of Mn, less than 0.03 wt% of the total amount of impurity elements Fe, Cu and Ni, and the balance of magnesium.
The porosity, the compressive yield strength, the absorption work and the elastic modulus are tested according to the standards of GB 4472-84 general rules for measuring density and relative density, GB/T7314 + 2017 + test method for metal material room temperature compression, GB/T22315 + 2008 + test method for elastic modulus and Poisson ratio of metal material. The experimental result shows that the porosity at room temperature can reach 58%, the compressive yield strength is 15MPa, and the elastic modulus is 6 GPa.
Example 11
9600g of pure magnesium, 1050g of pure zinc, 1050g of pure aluminum, 3000g of magnesium-yttrium intermediate alloy, 600g of magnesium-strontium intermediate alloy, 1500g of magnesium-manganese intermediate alloy, 450g of magnesium-cerium intermediate alloy and 300g of magnesium-lanthanum intermediate alloyAnd (3) alloying. Firstly, putting preheated pure magnesium, magnesium-yttrium 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 and the magnesium-strontium intermediate alloy preheated to 300 ℃ into a crucible at 730 ℃ under the stirring condition for mixing for 5min, and then adding the pure zinc and the pure aluminum preheated to 300 ℃ for mixing for 8min to obtain alloy liquid; and cooling the alloy liquid to 710 ℃, and standing for 15 min.
The alloy liquid after standing was directly cast into an open rectangular parallelepiped mold for ordinary ingot casting without a cooling device, the end face of the mold was trapezoidal (80 mm. times.120 mm) and the length was 400 mm.
The composition of the porous magnesium alloy obtained in the embodiment 11 of the present invention was detected by a spectrum analyzer, and the detection result shows that the porous magnesium alloy obtained in the embodiment 11 of the present invention includes: 6.74 wt% of Zn, 6.56 wt% of Al, 3.73 wt% of Y, 0.58 wt% of Ce, 0.36 wt% of La, 0.26 wt% of Mn, 0.88 wt% of Sr, the total amount of impurity elements Fe, Cu and Ni is less than 0.03 wt%, and the balance of magnesium.
The porosity was measured according to the standard of GB 4472-84 general rules for measuring Density and relative Density. The experimental result was that the porosity at room temperature was 60%.
Example 12
10500g of pure magnesium, 450g of pure zinc, 1050g of pure aluminum, 3000g of magnesium yttrium master alloy were preheated to 300 ℃. Firstly, putting preheated pure magnesium and magnesium-yttrium 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 8min to obtain alloy liquid; introducing argon gas into the alloy liquid for refining, wherein the introducing time is 30min, then cooling to 710 ℃, and simultaneously standing for 15 min.
The alloy liquid after standing was directly cast into an open rectangular parallelepiped mold for ordinary ingot casting without a cooling device, the end face of the mold was trapezoidal (80 mm. times.120 mm) and the length was 400 mm.
The composition of the porous magnesium alloy obtained in the embodiment 12 of the present invention is detected by a spectrum analyzer, and the detection result is that the porous magnesium alloy obtained in the embodiment 12 of the present invention includes: 2.93 wt% Zn, 6.52 wt% Al, 3.54 wt% Y, less than 0.03 wt% of impurity elements Fe, Cu and Ni, and the balance magnesium.
The porosity was measured according to the standard of GB 4472-84 general rules for measuring Density and relative Density. The experimental result was that the porosity at room temperature was 28%.
Example 13
12150g of pure magnesium, 1050g of pure zinc, 1050g of pure aluminum, 750g of magnesium-yttrium master alloy were preheated to 300 ℃. Firstly, putting preheated pure magnesium and magnesium-yttrium 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 8min to obtain alloy liquid; then, the temperature is reduced to 710 ℃, and the mixture is kept still for 3 min.
The alloy liquid after standing was directly cast into an open rectangular parallelepiped mold for ordinary ingot casting without a cooling device, the end face of the mold was trapezoidal (80 mm. times.120 mm) and the length was 400 mm.
The composition of the porous magnesium alloy obtained in the embodiment 13 of the present invention was detected by a spectrum analyzer, and the detection result shows that the porous magnesium alloy obtained in the embodiment 13 of the present invention includes: 6.88 wt% of Zn, 6.51 wt% of Al, 0.91 wt% of Y, less than 0.03 wt% of the total amount of impurity elements Fe, Cu and Ni, and the balance of magnesium.
The porosity was measured according to the standard of GB 4472-84 general rules for measuring Density and relative Density. As a result of the experiment, the porosity at room temperature was 13%.
Example 14
7650g pure magnesium, 1050g pure zinc, 1050g pure aluminum, 5250g magnesium yttrium master alloy was preheated to 300 ℃. Firstly, putting preheated pure magnesium and magnesium-yttrium intermediate alloy into a crucible preheated to 300 ℃, and introducing SF into the crucible6And CO2In a volume ratio of1:80, adding the pure zinc and the pure aluminum preheated to 300 ℃ into the crucible at 730 ℃ under the stirring condition, and mixing for 8min to obtain alloy liquid; then, the temperature is reduced to 710 ℃, and the mixture is kept still for 15 min.
The alloy liquid after standing was directly cast into an open rectangular parallelepiped mold for ordinary ingot casting without a cooling device, the end face of the mold was trapezoidal (80 mm. times.120 mm) and the length was 400 mm.
The composition of the porous magnesium alloy obtained in the embodiment 14 of the present invention is detected by a spectrum analyzer, and the detection result shows that the porous magnesium alloy obtained in the embodiment 14 of the present invention includes: 6.88 wt% of Zn, 6.50 wt% of Al, 6.36 wt% of Y, less than 0.03 wt% of the total amount of impurity elements Fe, Cu and Ni, and the balance of magnesium.
The porosity was measured according to the standard of GB 4472-84 general rules for measuring Density and relative Density. As a result of the experiment, the porosity at room temperature was 31%.
From the above embodiments, the present invention provides a self-foaming porous magnesium alloy, including: 3-9 wt% of Zn, 3-9 wt% of Al, 1-7 wt% of Y, 0-0.4 wt% of Mn, 0-2 wt% of La, 0-2 wt% of Ce, 0-2 wt% of Ca, 0-2 wt% of Sr, less than 0.3 wt% of impurity elements Fe, Ni, Cu, Be and the like, and the balance of magnesium. The self-foaming porous magnesium alloy provided by the invention contains Y, Zn and Al, a melt formed by the three components after melting can absorb a large amount of gas, and the gas is gradually separated out along with the reduction of 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, namely, the self-foaming is realized. In addition, Zn, Al and Mg react to generate a ternary quasicrystal phase, and Y 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 above description of the embodiments is only intended to facilitate the understanding of the method of the invention and its core idea. It should be noted that, for those skilled in the art, it is possible to make several improvements and modifications to the present invention without departing from the principle of the present invention, and those improvements and modifications also fall within the protection scope of the claims of the present invention. The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention, and many modifications of these embodiments will be apparent to those skilled in the art. The general principles defined herein may be implemented in other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (8)
1. A self-foaming porous magnesium alloy containing rare earth Y, characterized by comprising: 3-9 wt% of Zn, 3-9 wt% of Al, 1-7 wt% of Y, 0-0.4 wt% of Mn, 0-2 wt% of La, 0-2 wt% of Ce, 0-2 wt% of Ca, 0-2 wt% of Sr, and the balance of Mg and inevitable impurity elements;
the preparation method of the self-foaming porous magnesium alloy containing the rare earth Y comprises the following steps:
1)
1a) taking a magnesium source, a zinc source, an aluminum source, an yttrium source, a manganese source, a lanthanum source, a cerium source, a calcium source and a strontium source according to the composition, wherein the yttrium source is a magnesium-yttrium intermediate alloy with the mass fraction of yttrium of 15-40%;
1b) smelting a magnesium source and an yttrium source to obtain a first mixed molten metal;
1c) mixing a manganese source, a lanthanum source, a cerium source, a calcium source and a strontium source with the first mixed molten metal obtained in the step 1b) to obtain a second mixed molten metal;
1d) mixing the second mixed metal liquid, a zinc source and an aluminum source to obtain an alloy liquid;
2) carrying out gravity casting on the alloy liquid obtained in the step 1) to obtain the self-foaming porous magnesium alloy containing the rare earth Y.
2. The rare earth Y-containing self-foaming porous magnesium alloy according to claim 1, wherein the mass content of Zn in the porous magnesium alloy is 6% to 8%; the mass content of Al in the porous magnesium alloy is 6-8 percent; the mass content of Y in the porous magnesium alloy is 4-5%.
3. The method for preparing a rare earth Y-containing self-foaming porous magnesium alloy according to claim 1 or 2, comprising the steps of:
1)
1a) taking a magnesium source, a zinc source, an aluminum source, an yttrium source, a manganese source, a lanthanum source, a cerium source, a calcium source and a strontium source according to the composition, wherein the yttrium source is a magnesium-yttrium intermediate alloy with the mass fraction of yttrium of 15-40%;
1b) smelting a magnesium source and an yttrium source to obtain a first mixed molten metal;
1c) mixing a manganese source, a lanthanum source, a cerium source, a calcium source and a strontium source with the first mixed molten metal obtained in the step 1b) to obtain a second mixed molten metal;
1d) mixing the second mixed metal liquid, a zinc source and an aluminum source to obtain an alloy liquid;
2) carrying out gravity casting on the alloy liquid obtained in the step 1) to obtain the self-foaming porous magnesium alloy containing the rare earth Y.
4. The preparation method of the self-foaming porous magnesium alloy containing the rare earth Y as claimed in claim 3, wherein in the step 1), smelting is carried out under the condition of protective gas, and the volume ratio of the protective gas to SF is 1 (50-120)6And CO2(ii) a The smelting temperature is 680-780 ℃.
5. The method for preparing a self-foaming porous magnesium alloy containing rare earth Y as claimed in claim 3, wherein the preheating is performed at a temperature of 120-400 ℃ before the magnesium source, the zinc source, the aluminum source, the yttrium source, the manganese source, the lanthanum source, the cerium source, the calcium source and the strontium source are melted in the step 1).
6. The method for preparing a self-foaming porous magnesium alloy containing rare earth Y as claimed in claim 3, wherein the mixing time of the manganese source, the zirconium source, the silicon source, the calcium source, the strontium source, the silver source, the lanthanum source, the cerium source and the first mixed molten metal in step 1c) is 5min to 10min, the mixing temperature is 720 ℃ to 750 ℃, and the mixing time of the second mixed molten metal, the zinc source and the aluminum source in step 1d) is 10min to 20 min.
7. The method for preparing a rare earth Y-containing self-foaming porous magnesium alloy according to claim 3, wherein in the step 2), the alloy liquid is allowed to stand for 3 to 80 minutes before gravity casting, and the temperature of the alloy liquid during standing is 680 to 780 ℃.
8. The method for preparing the self-foaming porous magnesium alloy containing the rare earth Y according to the claim 3, wherein in the step 2), the mold adopted for gravity casting is a metal mold or a sand mold; the cooling mode adopted by gravity casting is furnace cooling, air cooling or water cooling.
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