CN111705249A - High-strength heat-resistant rare earth magnesium alloy and preparation method thereof - Google Patents
High-strength heat-resistant rare earth magnesium alloy and preparation method thereof Download PDFInfo
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C23/00—Alloys based on magnesium
- C22C23/02—Alloys based on magnesium with aluminium as the next major constituent
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/02—Making non-ferrous alloys by melting
- C22C1/03—Making non-ferrous alloys by melting using master alloys
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/002—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working by rapid cooling or quenching; cooling agents used therefor
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/06—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of magnesium or alloys based thereon
Abstract
The invention relates to a high-strength heat-resistant rare earth magnesium alloy containing rare earth samarium and a preparation method thereof, belonging to the technical field of alloys, wherein the magnesium alloy comprises the following components in percentage by mass: 6.0-7.0% of Al, 0.5-1.5% of Zn, 1.0-2.0% of Sm, 0.2-0.5% of Sb, and the balance of Mg and inevitable impurities. The alloy has high strength and high plasticity due to the uniform distribution of multiple second phases in the alloy, uniform and fine microstructures and weak basal plane texture. The invention also discloses a preparation method of the high-strength heat-resistant rare earth magnesium alloy material, so that the prepared magnesium alloy structure is uniformly distributed with nano and micron-sized second phases and relatively fine grain sizes, and the mechanical property of the magnesium alloy is obviously improved.
Description
Technical Field
The invention belongs to the technical field of alloys, and particularly relates to a high-temperature high-strength magnesium rare earth alloy containing rare earth samarium and a preparation method thereof.
Background
Magnesium alloy is called '21 st century green metal material', is the third major metal structure material after steel and aluminum alloy, and has been widely used in aerospace, automobile industry, and 3C series products. Magnesium alloys are mainly classified into cast magnesium alloys and wrought magnesium alloys according to the difference of forming processes. Compared with cast magnesium alloy, the magnesium alloy subjected to extrusion deformation has finer grains and better mechanical property. Therefore, the extrusion deformation process of magnesium alloy is also the hot spot of the current research.
Magnesium alloy is the lightest metal structure material in the world, has important development potential in the field of automobiles, and particularly, the application of rare earth magnesium alloy in automobile crank cases and hubs is a recent research hotspot, such as WE43, WE54 and the like have certain research progress, but the magnesium alloy has serious microstructure segregation and poor casting performance when being solidified, and is greatly limited in practical applicationMg＝0.64nm，c＝cMg0.52nm, plate-like, coherent with the substrate, thin plate-like, {2110}αHabitual plane) → β' (CBCO, a ═ 2 × a)Mg＝0.64nm，b＝2.2nm，c＝cMg0.52nm, ellipsoid semi-coherent with the matrix, {2110 }sheetαHabitual plane) metastable phase → β1(FCC, a ═ 0.74nm, lath, 0110}αHabitual plane, isomorphic with MgRE) → β (FCC, a 2.22nm, lath, {0110}αHabitual plane, isomorphic with MgRE). Rare earth element Sm is added into magnesium alloy, Al separated out in ageing process2The Sm phase has high hardness and melting point and good thermal stability, and can effectively improve the strength and creep resistance of the alloy. Sb can improve the casting performance of the alloy, and simultaneously refine the as-cast alloy structure and the alloy precipitation phase to form Mg with a hexagonal structure3Sb2The phase particles can play a role in dispersion strengthening. Sb is usually added into the magnesium rare earth alloy, and is an effective grain refiner which is mainly distributed on a grain boundary to play a role in drawing and pinning the grain boundary and block dislocation movement and grain growth, so that the strength of the magnesium alloy is improved.
These methods suffer from several disadvantages:
1. although the alloying method can further improve the strength of the magnesium alloy through precipitation strengthening, the method for improving the strength is at the expense of the plasticity of the magnesium alloy;
2. although the alloying method of adding a proper amount of rare earth elements can obviously improve the strength of the magnesium alloy, the magnesium alloy produced by the method has extremely high cost and causes a large amount of consumption of rare earth resources because the rare earth is a more expensive resource;
3. although the method of large plastic deformation can obtain refined grain structure and simultaneously improve the plasticity and the strength of the magnesium alloy, the production equipment is complex and expensive, and the production period is long. Such a processing method is not suitable for practical engineering.
Further improvements in strength and ductility are needed if it is desired that magnesium alloys be able to be a substitute for steel materials.
Disclosure of Invention
One of the purposes of the invention is to provide a high-strength heat-resistant rare earth magnesium alloy containing rare earth samarium; the second purpose is to provide a preparation method of the high-strength heat-resistant rare earth magnesium alloy containing rare earth samarium. The magnesium alloy has few kinds of alloy elements, low cost and stable strength after the environmental temperature exceeds 200 ℃. The preparation method is simple and easy to operate.
In order to realize one of the purposes, the invention adopts the technical scheme that:
a heat-resistant magnesium alloy comprises the following components in percentage by mass: 6.0-7.0% of Al, 0.5-1.5% of Zn, 1.0-2.0% of Sm, 0.2-0.5% of Sb, and the balance of Mg and inevitable impurities.
Preferably, the heat-resistant magnesium alloy consists of the following components in percentage by mass: 6.5% of Al, 1.5% of Zn, 2.0% of Sm, 0.4% of Sb, and the balance of Mg and inevitable impurities.
The mass content of the impurities in the heat-resistant magnesium alloy is less than 0.1%.
The heat-resistant magnesium alloy is prepared by smelting and casting pure magnesium, pure aluminum, pure zinc, pure antimony and an intermediate alloy Mg-10Sm as raw materials and carrying out heat treatment.
In order to achieve the second purpose, the invention adopts the technical scheme that:
the preparation method of the heat-resistant magnesium alloy comprises the following steps:
(1) weighing pure magnesium, pure aluminum, pure zinc, pure antimony and master alloy Mg-10Sm according to the proportion and preheating;
(2) melting the preheated pure magnesium, pure aluminum, pure zinc and pure antimony, heating to 700-720 ℃, adding an intermediate alloy Mg-10Sm, and preserving heat until the alloy is completely melted; then heating to 710-740 ℃ for refining, removing surface scum, cooling to 700-720 ℃, standing and preserving heat to obtain alloy liquid;
(3) semi-continuously casting the alloy liquid obtained in the step (2) to obtain an as-cast alloy;
(4) and (4) carrying out homogenization heat treatment on the as-cast alloy obtained in the step (3), and carrying out solid solution and aging after hot extrusion to obtain the heat-resistant magnesium alloy.
In the preparation method of the heat-resistant magnesium alloy, in the step (1), the preheating temperature is 180-200 ℃, and the preheating time is 1-2 hours.
The preparation method of the heat-resistant magnesium alloy comprises the step (2) of preserving heat for 20-30 min at 700-720 ℃.
In the preparation method of the heat-resistant magnesium alloy, in the step (4), the heat treatment is homogenizing heat treatment on the as-cast alloy.
According to the preparation method of the heat-resistant magnesium alloy, the temperature of the homogenization heat treatment is 460-480 ℃, the treatment time is 18-24 hours, and then the water mist is cooled to the room temperature.
According to the preparation method of the heat-resistant magnesium alloy, the hot extrusion temperature is 320-350 ℃, and the extrusion speed is 1.5-2.5 m/min.
According to the preparation method of the heat-resistant magnesium alloy, the temperature of the solution heat treatment is 515-525 ℃, the temperature is kept for 1-3 hours, and the heat-resistant magnesium alloy is rapidly quenched to room temperature by water cooling.
According to the preparation method of the heat-resistant magnesium alloy, the aging treatment temperature is 205-225 ℃, the treatment time is 16-24 hours, and then the heat-resistant magnesium alloy is cooled to room temperature in air.
After the analysis and the detection, the utility model can analyze and detect,the alloy component of the heat-resistant rare earth magnesium alloy product is Mg-Al-Zn-Sm-Sb, and the metallographic structure of the heat-resistant rare earth magnesium alloy mainly comprises α -Mg matrix and eutectic (α -Mg + β -Mg)17Al12+β-Mg3Al2Zn3+β-Al2Sm + β -SmSb) and the average grain size of the alloy is 50-70 mu m.
The alloy of the invention has good and extremely stable tensile strength, the tensile strength at room temperature is more than 250MPa, the tensile strength at 200 ℃ is more than 190MPa, the tensile strength at 250 ℃ is more than 180MPa, and the tensile strength at 300 ℃ is more than 150 MPa.
The heat-resisting magnesium alloy of the invention, Al, Zn element are important constituents of this alloy, are important alloy element of magnesium alloy, have greater solid solubility in aluminium, its strengthening action surface is on two sides, one is through forming β -Mg17A1l2And β -Mg3Al2Zn3The second phase strengthening of intermetallic compounds, the solid solution strengthening by Al and Zn atoms forming solid solution in aluminum matrix β -Mg in Al-Zn-Mg alloys17A1l2And β -Mg3Al2Zn3The phase thermal stability is poor, and the alloy is easy to soften at high temperature, so that the high-temperature performance of the alloy is poor. In the heat-resistant magnesium alloy, Sm is an important rare earth additive element, the solid solubility of Sm in the magnesium alloy is high, the heat-resistant magnesium alloy has a good precipitation strengthening effect, intermetallic compounds with high melting points can be formed in the magnesium alloy, and the addition amount of Sm is not less than 0.5% in order to ensure that the alloy obtains good aging precipitation strengthening and solid solution strengthening effects, and meanwhile, in order to avoid too much increase of alloy density and excessive embrittlement of the alloy, the addition amount of Sm is not more than 2.5%, so that the addition amount of Sm in the alloy is 1.0-2.0%, and the optimal weight percentage is 2.0%. Sb is an important alloying element of the magnesium alloy, has a solid solubility of 23.21% at a eutectic temperature of 550 ℃ and a solid solubility of only 0.11% at 150 ℃, and therefore has good solid solution strengthening and precipitation strengthening effects in the magnesium alloy, and Sb can be formed in the magnesium alloyβ -Mg with high melting point3The Sb intermetallic compound has a dispersion strengthening effect, so that the addition amount of Sb in the alloy is 0.2-0.5%, and the optimal weight percentage is 0.4%.
Compared with the prior art, the invention has the advantages that;
1. the heat-resistant magnesium alloy has the advantages of few alloy element types, low cost, simple alloy components, easy control of the smelting and mixing process and reduction of the preparation difficulty; the obtained magnesium alloy has uniform microstructure, uniform and dispersed precipitated phase distribution, higher room temperature and high temperature tensile strength and yield strength, the tensile strength at 200 ℃ is more than 186MPa, the yield strength is more than 121MPa, the plasticity is greatly improved, and the cost performance is higher.
2. According to the preparation method of the heat-resistant magnesium alloy, a proper amount of Sm and Sb are added into the Mg-Al-Zn alloy by a smelting method, the alloy is modified, the obtained cast alloy is subjected to heat treatment, the microstructure of the obtained magnesium alloy is uniform, precipitated phases are uniformly distributed and dispersed, the high-temperature and room-temperature tensile strength is achieved, the plasticity is greatly improved, the preparation method is simple in process, convenient to operate, easy to control in process and suitable for large-scale industrial production.
Drawings
FIG. 1 is a photograph showing an aged sample of a heat-resistant magnesium alloy in example 1 of the present invention.
FIG. 2 is a photograph of an aged sample of a heat-resistant magnesium alloy in example 2 of the present invention.
FIG. 3 is a photograph showing an aged sample of a heat-resistant magnesium alloy in example 3 of the present invention.
Detailed Description
The present invention will be further described with reference to the following embodiments.
Example 1
The heat-resistant magnesium alloy comprises, by mass, 6.0% of Al, 0.5% of Zn, 1.0% of Sm, 0.2% of Sb, and the balance of Mg and inevitable impurities.
The preparation method of the heat-resistant magnesium alloy comprises the following steps:
(1) putting pure magnesium, pure aluminum, pure zinc, pure antimony and master alloy Mg-10Sm into a drying oven at 200 ℃ according to a certain proportion for drying and preheating for 1 h;
(2) melting preheated pure magnesium, pure aluminum, pure zinc and pure antimony, adding an intermediate alloy Mg-10Sm when heating to 700 ℃, then heating to 730 ℃ for refining, removing surface scum, cooling to 710 ℃, standing and preserving heat for 25min to obtain an alloy liquid;
(3) semi-continuously casting the alloy liquid obtained in the step (2) to obtain an as-cast alloy;
(4) and (4) carrying out homogenization heat treatment on the as-cast alloy obtained in the step (3), wherein the heat treatment temperature is 460 ℃, the treatment time is 18 hours, and then cooling to room temperature by water mist.
(5) And (4) carrying out hot extrusion deformation on the homogenized alloy obtained in the step (4), wherein the extrusion temperature is 350 ℃, the extrusion speed is 2.5m/min, and natural cooling is adopted.
(6) And (4) carrying out solution heat treatment on the extruded section obtained in the step (5), keeping the temperature at 520 ℃ for 3h, and rapidly carrying out water-cooling quenching to room temperature.
(7) And (4) carrying out aging heat treatment on the solid solution product obtained in the step (6), wherein the temperature is 215 ℃, and the temperature is kept for 16 h.
Through analysis and detection, the alloy component of the heat-resistant rare earth magnesium alloy product is Mg-Al-Zn-Sm-Sb, and the metallographic structure of the heat-resistant rare earth magnesium alloy mainly comprises α -Mg matrix and eutectic (α -Mg + β -Mg)17Al12+β-Mg3Al2Zn3+β-Al2Sm + β -SmSb) and the average grain size of the alloy is 60-70 mu m.
Example 2
The heat-resistant magnesium alloy consists of the following components in percentage by mass: 6.5% of Al, 1.0% of Zn, 1.5% of Sm, 0.4% of Sb, and the balance of Mg and inevitable impurities.
The preparation method of the heat-resistant magnesium alloy comprises the following steps:
(1) putting pure magnesium, pure aluminum, pure zinc, pure antimony and master alloy Mg-10Sm into a drying oven at 190 ℃ according to a certain proportion for drying and preheating for 1 h;
(2) melting preheated pure magnesium, pure aluminum, pure zinc and pure antimony, adding an intermediate alloy Mg-10Sm when heating to 710 ℃, then heating to 740 ℃ for refining, removing surface scum, cooling to 720 ℃, standing and preserving heat for 30min to obtain an alloy liquid;
(3) semi-continuously casting the alloy liquid obtained in the step (2) to obtain an as-cast alloy;
(4) and (4) carrying out homogenization heat treatment on the as-cast alloy obtained in the step (3), wherein the heat treatment temperature is 475 ℃, the treatment time is 21h, and then cooling the as-cast alloy to room temperature by water mist.
(5) And (4) carrying out hot extrusion deformation on the homogenized alloy obtained in the step (4), wherein the extrusion temperature is 350 ℃, the extrusion speed is 2.0m/min, and natural cooling is adopted.
(6) And (5) carrying out solid solution heat treatment on the extruded section obtained in the step (5), keeping the temperature at 525 ℃ for 2h, and rapidly carrying out water cooling quenching to room temperature.
(7) And (4) carrying out aging heat treatment on the solid solution product obtained in the step (6), wherein the temperature is 220 ℃, and the temperature is kept for 24 h.
Through analysis and detection, the alloy component of the heat-resistant rare earth magnesium alloy product is Mg-Al-Zn-Sm-Sb, and the metallographic structure of the heat-resistant rare earth magnesium alloy mainly comprises α -Mg matrix and eutectic (α -Mg + β -Mg)17Al12+β-Mg3Al2Zn3+β-Al2Sm + β -SmSb) and the average grain size of the alloy is 55-65 mu m.
Example 3
The heat-resistant magnesium alloy consists of the following components in percentage by mass: 6% of Zn, 3% of Mg, 2% of Cu, 0.2% of Sm, and the balance of Mg and inevitable impurities.
The preparation method of the heat-resistant magnesium alloy comprises the following steps:
(1) putting pure magnesium, pure aluminum, pure zinc, pure antimony and master alloy Mg-10Sm into a drying oven at 180 ℃ according to a certain proportion for drying and preheating for 2 hours;
(2) melting preheated pure magnesium, pure aluminum, pure zinc and pure antimony, adding an intermediate alloy Mg-10Sm when heating to 720 ℃, then heating to 710 ℃ for refining, removing surface scum, cooling to 700 ℃, standing and preserving heat for 20min to obtain an alloy liquid;
(3) semi-continuously casting the alloy liquid obtained in the step (2) to obtain an as-cast alloy;
(4) and (4) carrying out homogenization heat treatment on the as-cast alloy obtained in the step (3), wherein the heat treatment temperature is 480 ℃, the treatment time is 24 hours, and then cooling to room temperature by water mist.
(5) And (4) carrying out hot extrusion deformation on the homogenized alloy obtained in the step (4), wherein the extrusion temperature is 420 ℃, the extrusion speed is 1.5m/min, and natural cooling is adopted.
(6) And (4) carrying out solution heat treatment on the extruded section obtained in the step (5), keeping the temperature at 475 ℃ for 1h, and rapidly carrying out water-cooling quenching to room temperature.
(7) And (4) carrying out aging heat treatment on the solid solution product obtained in the step (6), wherein the temperature is 125 ℃, and keeping the temperature for 16 h.
Through analysis and detection, the alloy component of the heat-resistant rare earth magnesium alloy product is Al-Zn-Mg-Cu-Sm, and the metallographic structure of the heat-resistant rare earth magnesium alloy mainly comprises α -Mg matrix and eutectic (α -Mg + β -Mg)17Al12+β-Mg3Al2Zn3+β-Al2Sm + β -SmSb) and the average grain size of the alloy is 50-60 mu m.
The heat-resistant magnesium alloys obtained in examples 1 to 3 and conventional 7005, 7050 and 7075 magnesium alloys were evaluated for their properties, and the results are shown in Table 1.
TABLE 1 results of measuring properties of the heat-resistant magnesium alloys obtained in examples 1 to 3 and comparative magnesium alloys
As is apparent from Table 1, the room-temperature tensile strength of the aluminum-magnesium alloy obtained in example 1-3 is 238 to 262Mp, the tensile strength at 200 ℃ is 190 to 202MPa, the tensile strength at 250 ℃ is 181 to 199MPa, and the tensile strength at 300 ℃ is 152 to 165 MPa. Experimental results show that the heat-resistant magnesium alloy has high tensile strength within the range of 20-300 ℃, and excellent heat resistance and mechanical properties.
Claims (8)
1. The high-strength heat-resistant rare earth magnesium alloy material is characterized by comprising the following components in percentage by mass: 6.0-7.0% of Al, 0.5-1.5% of Zn, 1.0-2.0% of Sm, 0.2-0.5% of Sb, and the balance of Mg and inevitable impurities.
2. The high-strength heat-resistant rare earth magnesium alloy material as claimed in claim 1, wherein the mass fraction of the rare earth element samarium is 1.0-2.0%.
3. The preparation method of the high-strength heat-resistant rare earth magnesium alloy material as claimed in claim 1, wherein the alloy component of the heat-resistant rare earth magnesium alloy product is Mg-Al-Zn-Sm-Sb through analysis and detection, and the metallographic structure of the heat-resistant rare earth magnesium alloy mainly comprises α -Mg matrix and eutectic (α -Mg + β -Mg)17Al12+β-Mg3Al2Zn3+β-Al2Sm + β -SmSb) and the average grain size of the alloy is 50-70 mu m.
4. The preparation method of the high-strength heat-resistant rare earth magnesium alloy material is characterized by comprising the following steps of:
step (1): heating the preheated magnesium ingot to 720-750 ℃ to completely melt the magnesium ingot; adding preheated pure aluminum, pure zinc, pure antimony and magnesium samarium intermediate alloy to obtain magnesium alloy molten liquid; controlling the refining temperature to be 710-740 ℃, standing and preserving heat for 20-30 min, then casting, and cooling to obtain a magnesium alloy round ingot;
step (2): carrying out homogenization heat treatment on the magnesium alloy ingot at 460-480 ℃;
and (3): preheating the homogenized magnesium alloy ingot at 380-430 ℃ for 1-3 h, carrying out hot extrusion at 320-360 ℃ at an extrusion rate of 1.5-2.5 m/min, and air cooling or air cooling to room temperature after extrusion.
And (4): and heating the hot extruded section to 515-525 ℃ for solution heat treatment, preserving the heat for 1-3 h, and rapidly carrying out water cooling quenching to room temperature.
And (5): and (4) artificially aging the quenched section.
5. The preparation method of the high-strength heat-resistant rare earth magnesium alloy material according to claim 4, wherein in the step (1), the preheating temperature is 180-200 ℃ and the preheating time is 1-2 h.
6. The preparation method of the high-strength heat-resistant rare earth magnesium alloy material according to claim 4, wherein in the step (1), the temperature is maintained at 690-710 ℃ for 25-35 min.
7. The preparation method of the high-strength heat-resistant rare earth magnesium alloy material according to claim 4, wherein the homogenization heat treatment method comprises the following steps: the treatment temperature is 460-480 ℃, the treatment time is 18-24 h, and then the water mist is cooled to the room temperature.
8. The preparation method of the high-strength heat-resistant rare earth magnesium alloy material according to claim 4, wherein the aging treatment method comprises the following steps: the treatment temperature is 200-225 ℃, the treatment time is 16-24 h, and then the air cooling is carried out to the room temperature.
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Application publication date: 20200925 |