CN111304509A - VN particle-added refined magnesium alloy and preparation method thereof - Google Patents
VN particle-added refined magnesium alloy and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a VN particle-added refined magnesium alloy which comprises magnesium, zinc, aluminum, manganese and vanadium nitride, wherein the mass fractions of the components are as follows: 2.5-3.5% of aluminum, 0.6-1.4% of zinc, 0.2-1.0% of manganese, 0.5-2% of vanadium nitride and the balance of magnesium. The invention also provides a preparation method of the VN-added particle refined magnesium alloy, which comprises the following steps: magnesium alloy raw materials such as magnesium, zinc, aluminum, manganese and vanadium nitride are placed in a reaction vessel according to the raw material ratio, heating smelting and casting molding are carried out under the protective gas atmosphere, the refined magnesium alloy added with VN particles is obtained, and the mass fraction of the vanadium nitride in the magnesium alloy raw materials is 0.5-2%. The invention has the advantages of uniform grain refinement, good mechanical property and the like.
Description
Technical Field
The invention relates to the field of alloy materials, in particular to a VN-added particle refined magnesium alloy and a preparation method thereof.
Background
The magnesium alloy is light alloy with low density, high specific strength, high damping, high conductivity and good electromagnetic shielding propertyThe energy has the advantages of being widely applied to the fields of automobiles, aviation, communication and the like at present. However, the low strength and poor plastic deformation properties of magnesium alloys compared to aluminum alloys limit their further industrial and commercial applications. Therefore, in recent years, many researchers have conducted extensive studies on the improvement of strength and deformability of magnesium alloys according to the Hall-batch formula (σ = σ)0+Kd-1/2) It is known that refining the grains is an effective way to strengthen the magnesium alloy, and at the same time, refining the grains can also effectively improve the deformation performance of the magnesium alloy. The research and application of the magnesium alloy grain refinement mainly focus on two aspects, namely the refinement in the fusion casting process and the refinement in the hot working process. Currently, the refinement of magnesium alloy in the casting process is mainly realized by adding a refiner, which comprises carbon-containing substances, simple substance metals, rare earth, compound particles, intermediate alloy and the like. The magnesium alloy which is most widely applied at present is Mg-Al series alloy, and crystal grains can be effectively refined by adding compound particles.
At present, carbon-containing substances are more applied as the refiner, but how to accurately control the addition of the proper total amount of the refiner still needs to be researched, the refining effect is influenced when the amount of the refiner is less, and the corrosion resistance of the material is influenced by the residual carbon substances when the amount of the refiner is too much; the addition of the simple substance metal and the rare earth can also effectively refine the magnesium alloy, but in the smelting process, because the melting points of the simple substance metal and the rare earth are higher, the effective addition has higher requirements on the process, and secondly, partial metal and the rare earth melted into the matrix are easy to generate segregation, and in addition, the simple substance metal and the rare earth improve the production cost of the alloy; the compound particles and the intermediate alloy also have the problems of high melting point and uniform components after being added.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a VN-added grain refined magnesium alloy with uniform grain refinement and good mechanical property and a preparation method thereof.
In order to solve the technical problems, the invention adopts the following technical scheme:
the VN particle-added refined magnesium alloy comprises magnesium, zinc, aluminum, manganese and vanadium nitride, wherein the mass fractions of the components are as follows: 2.5-3.5% of aluminum, 0.6-1.4% of zinc, 0.2-1.0% of manganese, 0.5-2% of vanadium nitride and the balance of magnesium.
As a general inventive concept, the present invention also provides a method for preparing a VN particle-added refined magnesium alloy, comprising the steps of:
magnesium alloy raw materials such as magnesium, zinc, aluminum, manganese and vanadium nitride are placed in a reaction vessel according to the raw material ratio, heating smelting and casting molding are carried out under the protective gas atmosphere, the refined magnesium alloy added with VN particles is obtained, and the mass fraction of the vanadium nitride in the magnesium alloy raw materials is 0.5-2%.
As a further improvement to the above technical solution:
the heating smelting mode is electromagnetic induction smelting, and the specific steps are as follows:
s1, weighing magnesium alloy raw materials including magnesium, aluminum, manganese, zinc and vanadium nitride according to the raw material proportion, dividing the magnesium alloy raw materials into a magnesium alloy block I, magnesium alloy powder II and a foil III, placing the magnesium alloy block I into a reaction container, and carrying out electromagnetic induction melting in a protective gas atmosphere until the magnesium alloy block I is melted to obtain a molten magnesium alloy I;
and S2, uniformly mixing the magnesium alloy powder II and the vanadium nitride powder, pressing into blocks, coating the blocks with a foil III, adding the coated blocks into the molten magnesium alloy block I, continuously performing electromagnetic induction melting, and uniformly stirring to obtain the molten magnesium alloy.
In the step S2, the temperature of the electromagnetic induction melting is 720-760 ℃, and the time is 15-30 min.
In the step S2, the stirring step is carried out while the electromagnetic induction smelting is carried out, and the time is 10-20 min.
In the step S2, a standing step is further included after the electromagnetic induction smelting, and the standing time is 10-20 min.
The magnesium alloy powder II is magnesium powder, the mass ratio of the vanadium nitride powder to the magnesium powder is 1: 5, the magnesium alloy block I is an aluminum block, a manganese block, a zinc block and a magnesium block, and the foil III is an aluminum foil or a magnesium foil.
The foil III is an aluminum foil, and the mass fraction of the aluminum foil and the aluminum block in the alloy raw material is 3%.
The above-mentionedThe protective gas being CO2And SF6And (4) mixing the gases.
The particle size of the vanadium nitride is 1 mu m.
Compared with the prior art, the invention has the advantages that:
according to the preparation method, after the refiner vanadium nitride is added into the magnesium alloy raw material, a large number of Vanadium Nitride (VN) particles are uniformly distributed in the magnesium alloy crystal grains, and the particles are used as heterogeneous nucleation effect when the magnesium matrix is solidified, so that the magnesium alloy crystal grains are refined. Meanwhile, the mechanical property of the magnesium alloy prepared by the method is greatly improved, the process is simple, the refiner vanadium nitride is cheap, and the cost is low.
The VN particle refined magnesium alloy provided by the invention has the advantages that the component proportion of the magnesium alloy is changed, the mass fractions of Al, Zn and Mn are kept unchanged, 0.5-2% of VN is added as a grain refiner to refine magnesium alloy grains, VN is a face-centered cubic structure, the lattice constant of VN is a =4.1371 nm, α -Mg is a close-packed hexagonal structure, the lattice constant of VN is a =0.3209nm and c =0.5211 nm, and the lattice mismatching degree of VN and α -Mg is 6.85% and is far less than 15% by calculation of Bramfitt formula, so that VN can be used as an effective heterogeneous nucleation core of α -Mg during solidification, and the magnesium alloy grains are refined.
Drawings
Fig. 1 is a microstructure diagram of a magnesium alloy refined by adding VN particles in example 1 of the present invention.
FIG. 2 is a microstructure diagram of a magnesium alloy refined without the addition of VN particles of comparative example 1 of the present invention.
Fig. 3 is a microstructure diagram of a magnesium alloy refined by adding VN particles in example 2 of the present invention.
Fig. 4 is a microstructure diagram of a magnesium alloy refined by adding VN particles in example 3 of the present invention.
FIG. 5 is a graph comparing the tensile test results of the magnesium alloys of examples 1 to 3 of the present invention and comparative example 1.
Detailed Description
The invention will be described in further detail below with reference to the drawings and specific examples.
Example 1:
a VN particle-added refined magnesium alloy comprises Mg, Al, Mn and VN, wherein the mass fractions of the components are as follows: 3% of Al, 1% of Zn, 0.2% of Mn, 0.5% of VN and the balance of Mg.
The preparation method of the VN particle-added magnesium alloy provided by the embodiment comprises the following specific steps:
(1) preparing materials: weighing the following raw materials in parts by mass according to the design components of the alloy:
the magnesium, the aluminum, the manganese and the zinc in the magnesium alloy are divided into three groups, wherein the first group is a magnesium alloy block I, the embodiment is an aluminum block, a manganese block, a zinc block and a magnesium block, the second group is a magnesium alloy powder II, the embodiment is magnesium powder, the third group is a magnesium alloy foil III, the embodiment is an aluminum foil, the mass fraction of the sum of the mass of the magnesium block in the magnesium alloy block I and the mass of the magnesium powder in the magnesium alloy II in the raw materials is 95.3%, the mass fraction of the sum of the mass of the aluminum block in the magnesium alloy block I and the mass of the aluminum foil in the magnesium alloy foil III in the raw materials is 3%, the mass ratio of Vanadium Nitride (VN) powder to the mass of the magnesium powder in the magnesium alloy powder II is 1: 5, and the mass ratio of the aluminum block to the aluminum foil is 100.
(2) Putting the magnesium alloy block I prepared in the step (1) into a stainless steel crucible, and adding CO2And SF6And (3) smelting in an electromagnetic induction furnace under the protection of the mixed gas, and raising the temperature of the electromagnetic induction furnace to 750 ℃ until the magnesium alloy block I is completely melted to obtain a molten magnesium alloy block I.
(3) And uniformly mixing the magnesium alloy powder II and VN powder by using a ball mill, pressing into small blocks with the thickness of 5mm, coating by using a magnesium alloy foil III, adding the VN powder coated by the magnesium alloy foil III and the magnesium alloy powder II into the molten magnesium alloy block I, stirring, continuing performing electromagnetic induction smelting for 15 minutes, and standing for 10 minutes to obtain the smelted magnesium alloy.
(4) And taking out the stainless steel crucible by using an iron clamp, and casting and molding the smelted alloy to obtain the VN particle-added refined magnesium alloy.
In this embodiment, magnesium, aluminum, manganese, and zinc of the magnesium alloy are divided into three groups, and vanadium nitride powder and magnesium powder are mixed, pressed into a block, and coated with aluminum foil, so that vanadium nitride and other components in the magnesium alloy can be better fused and uniformly mixed. In other embodiments, vanadium nitride powder and magnesium powder (or one or more of magnesium, aluminum, manganese, zinc of a magnesium alloy) are mixed and pressed into a compact that is clad with magnesium foil.
The structure of the magnesium alloy with the added VN particles prepared in the example is shown in FIG. 1, and the grain size is 62.5 μm.
The magnesium alloy obtained in this example was subjected to tensile testing, and the yield strength, maximum tensile strength and elongation were 47.1. + -. 1.13MPa, 197.4. + -. 6.8MPa and 17.8. + -. 1.3%, respectively.
Comparative example 1
A magnesium alloy without VN particles comprises Mg, Al and Mn, wherein the mass fractions of the components are as follows: 3% of Al, 1% of Zn, 0.2% of Mn and the balance of Mg.
As a blank comparative example, this comparative example provides a method for preparing a magnesium alloy, comprising the specific steps of:
(1) preparing materials: the alloy comprises the following design components in percentage by mass: 3% of Al, 1% of Zn, 0.2% of Mn and the balance of Mg.
(2) Putting the alloy ingot proportioned in the step (1) into a stainless steel crucible, and adding into CO2And SF6Smelting in an electromagnetic induction furnace under the protection of mixed gas, raising the temperature of the induction furnace to 750 ℃, and standing for 10 minutes after the alloy ingot is completely melted.
(3) And taking out the stainless steel crucible by using an iron clamp, and casting and molding the molten alloy to obtain the magnesium alloy.
The structure of the magnesium alloy without VN particles added prepared in this comparative example is shown in fig. 2, and the grain size is 115.7 μm.
The magnesium alloy obtained in this comparative example was subjected to tensile tests and had a yield strength, a maximum tensile strength and an elongation of 39.5. + -. 0.85MPa, 140.7. + -. 9.9MPa and 10.6. + -. 1.4%, respectively.
Example 2
A VN particle-added refined magnesium alloy comprises Mg, Al, Mn and VN, wherein the mass fractions of the components are as follows: 3% of Al, 1% of Zn, 0.2% of Mn, 1% of VN and the balance of Mg.
(1) Preparing materials: weighing the following raw materials in parts by mass according to the design components of the alloy:
the magnesium, the aluminum, the manganese and the zinc in the magnesium alloy are divided into three groups, wherein the first group is a magnesium alloy block I, the embodiment is an aluminum block, a manganese block, a zinc block and a magnesium block, the second group is a magnesium alloy powder II, the embodiment is magnesium powder, the third group is a magnesium alloy foil III, the embodiment is an aluminum foil, the mass fraction of the sum of the mass of the magnesium block in the magnesium alloy block I and the mass of the magnesium powder in the magnesium alloy II in the raw materials is 94.8%, the mass fraction of the sum of the mass of the aluminum block in the magnesium alloy block I and the mass of the aluminum foil in the magnesium alloy foil III in the raw materials is 3%, the mass ratio of Vanadium Nitride (VN) powder to the mass of the magnesium powder II is 1: 5, and the mass ratio of the aluminum block to the aluminum foil is 100: 1.
(2) Putting the magnesium alloy block I prepared in the step (1) into a stainless steel crucible, and adding into CO2And SF6And (3) smelting in an electromagnetic induction furnace under the protection of the mixed gas, and raising the temperature of the electromagnetic induction furnace to 750 ℃ until the magnesium alloy block I is completely melted to obtain a molten magnesium alloy block I.
(3) And uniformly mixing the magnesium alloy powder II and VN powder by using a ball mill, pressing into small blocks with the thickness of 5mm, coating by using a magnesium alloy foil III, adding the VN powder coated by the magnesium alloy foil III and the magnesium alloy powder II into the molten magnesium alloy block I, stirring, continuing performing electromagnetic induction smelting for 15 minutes, and standing for 10 minutes to obtain the smelted magnesium alloy.
(4) And taking out the stainless steel crucible by using an iron clamp, and casting and molding the smelted alloy to obtain the VN particle-added refined magnesium alloy.
The structure of the VN-added particle magnesium alloy prepared in this example is shown in fig. 3, and its grain size is 67.5 μm.
The VN particle-added magnesium alloy prepared in this example was subjected to a tensile test, and the yield strength, maximum tensile strength and elongation were 50.3 ± 1.35MPa, 184.3 ± 10.2MPa and 12.4 ± 1.9%, respectively.
Example 3
A VN particle-added refined magnesium alloy comprises Mg, Al, Mn and VN, wherein the mass fractions of the components are as follows: 3% of Al, 1% of Zn, 0.2% of Mn, 2% of VN and the balance of Mg.
(1) Preparing materials: weighing the following raw materials in parts by mass according to the design components of the alloy:
the magnesium, the aluminum, the manganese and the zinc in the magnesium alloy are divided into three groups, wherein the first group is a magnesium alloy block I, the embodiment is an aluminum block, a manganese block, a zinc block and a magnesium block, the second group is a magnesium alloy powder II, the embodiment is magnesium powder, the third group is a magnesium alloy foil III, the embodiment is an aluminum foil, the mass fraction of the sum of the mass of the magnesium block in the magnesium alloy block I and the mass of the magnesium powder in the magnesium alloy II in the raw materials is 93.8%, the mass fraction of the sum of the mass of the aluminum block in the magnesium alloy block I and the mass of the aluminum foil in the magnesium alloy foil III in the raw materials is 3%, the mass ratio of Vanadium Nitride (VN) powder to the mass of the magnesium powder in the magnesium alloy powder II is 1: 5, and the mass ratio of the aluminum block to the aluminum foil is 100.
(2) Putting the magnesium alloy block I (prepared in the step (1)) into a stainless steel crucible and adding into CO2And SF6And (3) smelting in an electromagnetic induction furnace under the protection of the mixed gas, and raising the temperature of the electromagnetic induction furnace to 750 ℃ until the magnesium alloy block I is completely melted.
(3) And uniformly mixing the magnesium alloy powder II and VN powder by using a ball mill, pressing into small blocks with the thickness of 5mm, coating by using a magnesium alloy foil III, adding the VN powder coated by the magnesium alloy foil III and the magnesium alloy powder II into the molten magnesium alloy I, stirring, continuing to perform electromagnetic induction smelting for 15 minutes, and standing for 10 minutes to obtain the smelted magnesium alloy.
(4) And taking out the stainless steel crucible by using an iron clamp, and casting and molding the smelted alloy to obtain the VN particle-added refined magnesium alloy.
The structure of the VN-added particle magnesium alloy prepared in this example is shown in fig. 4, and its grain size is 69.8 μm.
The prepared VN particle added AZ31 magnesium alloy was subjected to tensile testing and had a yield strength, a maximum tensile strength and an elongation of 45.1 ± 0.95MPa, 145.2 ± 8.6MPa and 7.6 ± 0.8%, respectively.
Compared with the comparative example 1, the VN-added particle refined magnesium alloy prepared by the method has the advantages that the grain size is reduced from 115.7 mu m to 62.5 mu m at the minimum, and the grain refining effect is very obvious.
FIG. 5 is a comparison of the tensile test results of the magnesium alloys prepared in examples 1-3 and comparative example 1, and it can be seen that the mechanical properties of the magnesium alloy with the addition of VN are also significantly improved.
Although the present invention has been described with reference to the preferred embodiments, it is not intended to be limited thereto. Those skilled in the art can make numerous possible variations and modifications to the present invention, or modify equivalent embodiments to equivalent variations, without departing from the scope of the invention, using the teachings disclosed above. Therefore, any simple modification, equivalent change and modification made to the above embodiments according to the technical spirit of the present invention should fall within the protection scope of the technical scheme of the present invention, unless the technical spirit of the present invention departs from the content of the technical scheme of the present invention.
Claims (10)
1. A VN particle-added refined magnesium alloy is characterized in that: the alloy comprises magnesium, zinc, aluminum, manganese and vanadium nitride, wherein the mass fractions of the components are as follows: 2.5-3.5% of aluminum, 0.6-1.4% of zinc, 0.2-1.0% of manganese, 0.5-2% of vanadium nitride and the balance of magnesium.
2. A preparation method of VN particle-added refined magnesium alloy is characterized by comprising the following steps: the method comprises the following steps:
magnesium alloy raw materials such as magnesium, zinc, aluminum, manganese and vanadium nitride are placed in a reaction vessel according to the raw material ratio, heating smelting and casting molding are carried out under the protective gas atmosphere, the refined magnesium alloy added with VN particles is obtained, and the mass fraction of the vanadium nitride in the magnesium alloy raw materials is 0.5-2%.
3. The method of claim 2, wherein: the heating smelting mode is electromagnetic induction smelting, and the specific steps are as follows:
s1, weighing magnesium alloy raw materials including magnesium, aluminum, manganese, zinc and vanadium nitride according to the raw material proportion, dividing the magnesium alloy raw materials into a magnesium alloy block I, magnesium alloy powder II and a foil III, placing the magnesium alloy block I into a reaction container, and carrying out electromagnetic induction melting in a protective gas atmosphere until the magnesium alloy block I is melted to obtain a molten magnesium alloy I;
and S2, uniformly mixing the magnesium alloy powder II and the vanadium nitride powder, pressing into blocks, coating the blocks with a foil III, adding the coated blocks into the molten magnesium alloy block I, continuously performing electromagnetic induction melting, and uniformly stirring to obtain the molten magnesium alloy.
4. The production method according to claim 3, characterized in that: in the step S2, the temperature of the electromagnetic induction melting is 720-760 ℃, and the time is 15-30 min.
5. The method of claim 4, wherein: in the step S2, the stirring step is carried out while the electromagnetic induction smelting is carried out, and the time is 10-20 min.
6. The method of claim 5, wherein: in the step S2, a standing step is further included after the electromagnetic induction smelting, and the standing time is 10-20 min.
7. The production method according to any one of claims 3 to 6, characterized in that: the magnesium alloy powder II is magnesium powder, the mass ratio of the vanadium nitride powder to the magnesium powder is 1: 5, the magnesium alloy block I is an aluminum block, a manganese block, a zinc block and a magnesium block, and the foil III is an aluminum foil or a magnesium foil.
8. The method of claim 7, wherein: the foil III is an aluminum foil, and the mass fraction of the aluminum foil and the aluminum block in the alloy raw material is 3%.
9. The production method according to any one of claims 2 to 6, characterized in that: the protective gas is CO2And SF6And (4) mixing the gases.
10. The production method according to any one of claims 2 to 6, characterized in that: the particle size of the vanadium nitride is 1 mu m.
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| CN112831739A (en) * | 2020-12-31 | 2021-05-25 | 长沙理工大学 | Processing method for improving high-temperature creep property of magnesium alloy through rolling and hammering |
| CN112921226A (en) * | 2021-02-16 | 2021-06-08 | 河南工学院 | Mg-AlN master alloy grain refiner for magnesium-aluminum alloy and preparation method thereof |
| CN113174519A (en) * | 2021-03-23 | 2021-07-27 | 山东科技大学 | Superfine vanadium particle reinforced fine-grain magnesium-based composite material and preparation method thereof |
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| CN112921226B (en) * | 2021-02-16 | 2022-05-17 | 河南工学院 | Mg-AlN master alloy grain refiner for magnesium-aluminum alloy and preparation method thereof |
| CN113174519A (en) * | 2021-03-23 | 2021-07-27 | 山东科技大学 | Superfine vanadium particle reinforced fine-grain magnesium-based composite material and preparation method thereof |
| CN113174519B (en) * | 2021-03-23 | 2022-04-29 | 山东科技大学 | Superfine vanadium particle reinforced fine-grain magnesium-based composite material and preparation method thereof |
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Application publication date: 20200619 |