CN114622117B - Low-alloying high-plasticity magnesium rare earth alloy and preparation method thereof - Google Patents
Low-alloying high-plasticity magnesium rare earth alloy and preparation method thereof Download PDFInfo
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- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
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Abstract
The invention discloses a low-alloying high-plasticity magnesium rare earth alloy and a preparation method thereof, and aims to solve the problem of poor room-temperature plasticity of magnesium alloy. The preparation method comprises the following steps: 1. adding pure Mg ingots and Mg-Er master alloy in raw materials into a resistance furnace for melting to obtain alloy liquid; 2. casting and molding the alloy liquid; 3. turning to remove the surface layer of the formed magnesium rare earth alloy; 4. preheating a blank and an extrusion die at an extrusion temperature, controlling the extrusion temperature to be 300-500 ℃, and controlling the extrusion ratio to be 20-60:1, obtaining an extruded alloy after water cooling; 5. annealing the extruded alloy at 300-400 ℃. According to the invention, the high-plasticity magnesium alloy is prepared by adding a single Er element. Since the solid solubility of an Er element in magnesium alloys is very high, it is easy to completely dissolve up to 3wt.% of the Er element in magnesium. So that the composition of the alloy is relatively stable and a large number of complex second phases do not exist.
Description
Technical Field
The invention belongs to the field of magnesium alloy, and particularly relates to a low-alloying magnesium rare earth binary (Mg-Er) alloy with high plasticity at room temperature and a preparation method thereof.
Background
Magnesium alloy has been widely used in the fields of aerospace, weaponry, 3C electronics, etc., as the lightest metal structural material. However, magnesium alloys have poor room temperature plasticity, which severely limits further applications of magnesium alloys. Insufficient independent deformation modes and strong texture are important reasons for the low plasticity of magnesium alloys. In one aspect. Although the deformation modes of the magnesium alloy are basal plane slippage, cylindrical surface slippage, pyramidal plane slippage and twin crystal, at room temperature, only basal plane slippage and tensile twin crystal are easy to activate, and the critical shear stress (CRSS) of other slippage systems and twin crystal is high and difficult to activate, so that the magnesium alloy lacks an independent plastic deformation mode at room temperature. On the other hand, extruded alloys tend to have stronger textures, for example, sheet ([ 0001]// ND) and bar ([ 10-10]// ED), which are typically formed during hot working.
The grain refinement is an important means for improving the plasticity of the magnesium alloy. Zeng et al (Z.R. Zeng et al, deformation modes reducing room temperature tension of fine-grained pure magnesium, acta mater.206 (2021) 116648.) prepared ultra-fine grain pure magnesium (grain size of about 1 μm) and obtained good room temperature plasticity. The reason is that the fine grains can easily activate non-basal plane slip, even grain boundary slip occurs, and the plasticity of the magnesium alloy is obviously improved. However, in large-scale industrial production, obtaining ultra-fine crystals is a great challenge and has low economic benefit. Therefore, there is an urgent need to develop a novel high-plasticity magnesium alloy that can be mass-produced.
Alloying is one of the important means for improving the plasticity of the alloy. On the one hand, alloying elements can effectively narrow the CRSS gap between different slip systems, making non-basal slip systems easier to activate. On the other hand, partially alloyed elements can weaken strong texture produced during hot working. However, in the patents disclosed so far, the reports of high plasticity alloys have focused on complex alloying elements or higher alloying elements. For example, patent No. CN201811375873.5, entitled "a high plasticity magnesium alloy and method for making same", discloses a high plasticity Mg-Bi-Nd-Mn alloy, which has an elongation at room temperature of more than 40%, but a total alloying content of the alloy of 3.5wt.% or more, and a complex second phase (BiNd phase, mg phase) 3 Bi 2 Phase).
The patent number is CN202010007746.0, and the patent name is "a high-plasticity low-rare earth magnesium alloy and a preparation method thereof", which discloses a high-plasticity low-cost Mg-Gd-Er-Zn-Zr alloy, wherein the elongation at room temperature can reach 35% at most, but the total alloying content of the alloy is more than 8.5 wt.%. The high alloying content and complex second phase composition tend to make it difficult to obtain stable properties of the alloy in practical mass production. Therefore, there is an urgent need to develop a high-plasticity low-alloying magnesium alloy with simple alloy components and stable performance.
Disclosure of Invention
The invention aims to solve the problem of poor room-temperature plasticity of magnesium alloy, provides a method for improving the plasticity of the magnesium alloy by combining simple rare earth alloying (Er element) regulation and grain refinement, and aims to develop a stable high-plasticity magnesium alloy at room temperature and widen the application of the magnesium alloy.
The low-alloying high-plasticity magnesium rare earth alloy is Mg-Er magnesium alloy and consists of 1-3 wt% of Er and 99-97 wt% of Mg, and the content of total alloying elements is less than 3 wt%.
The room temperature plasticity of the magnesium alloy is improved by adding a small amount of RE element (Er). On one hand, the Er element can reduce the CRSS of non-basal plane slippage and twin crystal of the magnesium alloy and activate more non-basal plane slippage and twin crystal; on the other hand, the Er element can help the magnesium alloy to generate a rare earth texture in the hot working process and weaken a strong base surface texture generated in the hot working process.
The preparation method of the low-alloying high-plasticity magnesium rare earth alloy is realized according to the following steps:
1. taking a pure Mg ingot and a Mg-Er intermediate alloy as raw materials, adding the pure Mg ingot in the raw materials into a resistance furnace, melting the pure Mg ingot into a liquid state at 750 ℃ under a protective atmosphere, cooling to 730 ℃, adding the Mg-Er intermediate alloy, and preserving heat until the pure Mg ingot and the Mg-Er intermediate alloy are completely melted to obtain an alloy liquid;
2. continuously cooling the alloy liquid obtained in the step one to 670-690 ℃, and casting to obtain a formed magnesium rare earth alloy;
3. turning to remove the surface layer of the formed magnesium rare earth alloy, and cutting to obtain a blank;
4. preheating a blank and an extrusion die at an extrusion temperature, controlling the extrusion temperature to be 300-500 ℃, and controlling the extrusion ratio to be 20-60:1, obtaining an extruded alloy after water cooling;
5. placing the extruded alloy in a resistance furnace for annealing treatment at 300-400 ℃ to obtain low-alloying high-plasticity magnesium rare earth alloy;
wherein the content of Er in the raw materials in the first step is 1-3 wt%, and the content of Mg in the raw materials in the first step is 99-97 wt%.
In the fourth step of the invention, the preheated extrusion die is used for extruding the preheated blank, so that the unevenness of the extrusion structure is reduced.
The low-alloying room-temperature high-plasticity Mg-Er magnesium alloy obtained by the method has extremely high plasticity, the fracture elongation at room temperature is more than 50%, and other grain refining elements such as Zr element and the like do not need to be added.
The low-alloying high-plasticity magnesium rare earth alloy and the preparation method thereof have the following beneficial effects:
1. according to the invention, the magnesium alloy with high plasticity (> 50%) is prepared by adding a single element (Er element). Since the solid solubility of an Er element in magnesium alloys is very high (maximum solid solubility >30 wt.%), it is easy to completely dissolve the Er element in magnesium at a concentration of 3wt.% or less. This makes the composition of the alloy relatively stable without the presence of large amounts of complex second phases, which means that the properties of the alloy are more easily stabilized in large-scale industrial production.
2. The extruded alloy of the invention has the obvious rare earth texture, and the basal plane texture generated in the processing process is greatly weakened. The strong basal plane texture can cause basal plane dislocation slip which is easy to start originally to be difficult to activate, the basal plane texture is greatly weakened by the addition of the Er element and the subsequent annealing process, and the plasticity of the alloy is obviously improved.
3. The grain size of the extruded alloy of the present invention is concentrated to 4-10 μm, at which both dislocation glide and twin of the magnesium alloy start. Due to the action of the Er element, the magnesium alloy shows the deformation mode activity of the ultra-pure magnesium under the grain size, and obtains good room temperature plasticity. Because the Er element has strong promoting effect on a sliding system, crystal grains are further refined without adding crystal grain refining elements such as Zr and the like. More importantly, the grain size is easy to obtain in large-scale industrial production, and the economic benefit is high.
4. The invention can obtain good plasticity even at a low extrusion ratio. Lower extrusion ratios tend to result in incomplete dynamic recrystallization of the alloy, the presence of non-dynamic recrystallization and higher dislocation densities. Annealing may cause the grains to be too large and thereby affect plasticity. The magnesium rare earth alloy of the invention has certain grain boundary segregation, which can inhibit abnormal growth of crystal grains in the annealing process, so that the alloy can still obtain uniform fine-grained structure after annealing, thereby obtaining good plasticity.
5. The alloy has the advantages of low element content (less than or equal to 3 wt.%), low cost and high economic value, and can be widely used for industrial production.
6. The invention has simple process flow, controllable extrusion speed and stable alloy performance, and can select proper extrusion speed and extrusion temperature in a large range according to different purposes.
Drawings
The mechanical property profile of the Mg-Er magnesium alloy obtained in the example of FIG. 1, wherein 1 represents comparative example 1,2 represents example 1,3 represents example 2, and 4 represents comparative example 2;
FIG. 2 is a grain distribution diagram of the low-alloying high-plasticity magnesium rare earth alloy obtained in example 1;
FIG. 3 is the (0001) pole figure of the low-alloying high-plasticity magnesium rare earth alloy obtained in example 1;
FIG. 4 is a reverse pole diagram of the low-alloying high-plasticity magnesium rare earth alloy obtained in example 1;
FIG. 5 is a high-angle annular dark field image at the grain boundary of the low-alloying high-plasticity magnesium rare earth alloy obtained in example 1.
Detailed description of the invention
The first embodiment is as follows: the low-alloying high-plasticity magnesium rare earth alloy is Mg-Er magnesium alloy and consists of 1-3 wt% of Er and 99-97 wt% of Mg, and the content of total alloying elements is less than 3 wt%.
The second embodiment is as follows: the difference between the embodiment and the first embodiment is that the Er-doped magnesium alloy consists of Er accounting for 1.5-2.5wt% and Mg accounting for 98.5% -97.5%.
The third concrete implementation mode: the preparation method of the low-alloying high-plasticity magnesium rare earth alloy is implemented according to the following steps:
1. taking a pure Mg ingot and a Mg-Er intermediate alloy as raw materials, adding the pure Mg ingot in the raw materials into a resistance furnace, melting the pure Mg ingot into a liquid state at 750 ℃ under a protective atmosphere, cooling to 730 ℃, adding the Mg-Er intermediate alloy, and preserving heat until the pure Mg ingot and the Mg-Er intermediate alloy are completely melted to obtain an alloy liquid;
2. continuously cooling the alloy liquid obtained in the step one to 670-690 ℃, and casting to obtain a formed magnesium rare earth alloy;
3. turning to remove the surface layer of the formed magnesium rare earth alloy, and cutting according to the size of the forming cylinder to obtain a blank;
4. preheating a blank and an extrusion die at an extrusion temperature, controlling the extrusion temperature to be 300-500 ℃, and controlling the extrusion ratio to be 20-60:1, obtaining an extruded alloy after water cooling;
5. placing the extruded alloy in a resistance furnace for annealing treatment at 300-400 ℃ to obtain low-alloying high-plasticity magnesium rare earth alloy;
wherein the content of Er in the raw materials in the first step is 1-3 wt%, and the content of Mg in the raw materials in the first step is 99-97 wt%.
The fourth concrete implementation mode: the difference between this embodiment and the third embodiment is that the protective atmosphere in the first step is SF 6 And CO 2 The mixed atmosphere of (3).
The fifth concrete implementation mode: the difference between the third embodiment and the fourth embodiment is that in the first step, the temperature is cooled to 730 ℃ at a speed of 5 ℃/min.
The sixth specific implementation mode: the difference between this embodiment and one of the third to fifth embodiments is that the cooling is continued to 670-690 ℃ at a rate of 5 ℃/min in the second step.
The seventh concrete implementation mode: the difference between the third embodiment and the sixth embodiment is that the diameter of the blank is 2mm smaller than the actual diameter of the forming cylinder in the third step.
The specific implementation mode is eight: the difference between this embodiment and one of the third to seventh embodiments is that the preheating time in step four is 2 hours.
The specific implementation method nine: the difference between the third embodiment and the eighth embodiment is that the extrusion temperature is controlled to be 300-350 ℃ in the fourth step, the extrusion ratio is 25-30:1.
the specific implementation mode is ten: the difference between this embodiment and one of the fourth to seventh embodiments is that the annealing time in the fifth step is 0.5 to 1 hour.
Example 1: the preparation method of the low-alloying high-plasticity magnesium rare earth alloy is implemented according to the following steps:
1. pure Mg ingot and Mg-Er intermediate alloy are used as raw materials, the pure Mg ingot in the raw materials is added into a resistance furnace and is treated in SF 6 And CO 2 Under the protection of the mixed atmosphere, melting the mixture into liquid at 750 ℃, cooling the mixture to 730 ℃ at the speed of 5 ℃/min, adding Mg-Er intermediate alloy, and preserving the heat until the mixture is completely melted to obtain alloy liquid;
2. continuously cooling the alloy liquid obtained in the first step to 680 ℃ at the speed of 5 ℃/min, and then casting to obtain a formed magnesium rare earth alloy;
3. turning to remove the surface layer of the formed magnesium rare earth alloy, and cutting according to the size of the forming cylinder to obtain a blank;
4. preheating a blank and an extrusion die for 2h at an extrusion temperature, controlling the extrusion temperature to be 320 ℃, and controlling the extrusion ratio to be 30:1, obtaining an extruded alloy after water cooling;
5. placing the extruded alloy in a resistance furnace, and annealing for 1h at 300 ℃ to obtain a low-alloying high-plasticity magnesium rare earth alloy;
wherein the content of Er in the raw material in the first step is 1.74wt percent, and the content of Mg in the raw material in the first step is 98.26 percent.
The surface of the extruded plate of this example was smooth and flat, and the inside of the extruded plate was dynamically recrystallized grains having an average size of about 5.4 μm and twinning was present (see FIG. 2). In addition, the basal texture of the alloy is significantly reduced from 28.9mrd in comparative example 1 to 15.97mrd (see fig. 3 and 4, table 1), and a significant "rare earth texture" is present. Segregation phenomena were also observed at the grain boundaries of the alloy, which is critical for maintaining the grain size during annealing (fig. 5). The elongation at break of the alloy was 51.6%. The combined action of the Er element and the fine grains can effectively improve the plasticity of the alloy.
Example 2: the preparation method of the low-alloying high-plasticity magnesium rare earth alloy is implemented according to the following steps:
1. pure Mg ingot and Mg-Er intermediate alloy are taken as raw materials, the pure Mg ingot in the raw materials is added into a resistance furnace in SF 6 And CO 2 Under the protection of the mixed atmosphere, the mixture is melted into liquid at 750 ℃, cooled to 730 ℃ at the speed of 5 ℃/min, added with Mg-Er intermediate alloy and kept warm until the mixture is completely melted to obtain the alloyLiquid;
2. continuously cooling the alloy liquid obtained in the first step to 680 ℃ at the speed of 5 ℃/min, and then casting to obtain a formed magnesium rare earth alloy;
3. turning to remove the surface layer of the formed magnesium rare earth alloy, and cutting according to the size of a forming cylinder to obtain a blank;
4. preheating a blank and an extrusion die for 2h at an extrusion temperature, controlling the extrusion temperature to be 320 ℃, and controlling the extrusion ratio to be 30:1, obtaining an extruded alloy after water cooling;
5. placing the extruded alloy in a resistance furnace, and annealing for 1h at 350 ℃ to obtain a low-alloying high-plasticity magnesium rare earth alloy;
wherein the content of Er in the raw material in the first step is 1.74wt%, and the content of Mg in the raw material in the first step is 98.26%.
The surface of the extrusion plate was smooth and flat, and the inside of the extrusion plate was dynamically recrystallized grains having an average size of about 8.55 μm and twinning was present. In addition, the basal plane texture of the alloy is significantly reduced from 28.9mrd in comparative example 1 to 10.4mrd (table 1), and a significant "rare earth texture" exists. The elongation at break of the alloy was 50.5%. The combined action of the Er element and the fine grains can effectively improve the plasticity of the alloy.
Comparative example 1
The difference from example 1 is that comparative example 1 is not subjected to the annealing treatment of step five.
The surface of the extruded plate was smooth and flat, and the inside of the extruded plate was dynamically recrystallized grains having an average size of about 4.4 μm (Table 1), and the elongation at break of the alloy was 12.5%. Although the crystal grain size of the alloy is small, the alloy is difficult to start basal plane slip and the like due to the strong basal plane texture of the alloy, and is difficult to adapt to deformation.
Comparative example 2
The difference from example 1 is that step five of comparative example 2 is annealing the as-extruded Mg-1.74wt.% Er alloy in a resistance furnace at 350 ℃ for 2h.
The surface of the extrusion plate is smooth and flat, dynamic recrystallization grains are formed inside the extrusion plate, the average size of the grains is about 12.4 mu m, and the fracture elongation of the alloy is 26 percent. Although the texture of this alloy is weak, the dislocation set-off is difficult due to the larger grain size, and therefore the plasticity of the alloy is significantly reduced compared to examples 1 and 2.
TABLE 1 basic Properties of the examples
Claims (5)
1. The preparation method of the low-alloying high-plasticity magnesium rare earth alloy is characterized by comprising the following steps of:
1. taking pure Mg ingots and Mg-Er intermediate alloy as raw materials, adding the pure Mg ingots in the raw materials into a resistance furnace, melting into a liquid state at 750 ℃ under a protective atmosphere, cooling to 730 ℃, adding the Mg-Er intermediate alloy, and preserving heat until the Mg-Er intermediate alloy is completely melted to obtain an alloy liquid;
2. continuously cooling the alloy liquid obtained in the first step to 670-690 ℃, and casting to obtain a formed magnesium rare earth alloy;
3. turning to remove the surface layer of the formed magnesium rare earth alloy, and cutting to obtain a blank;
4. preheating a blank and an extrusion die at an extrusion temperature, controlling the extrusion temperature to be 300-350 ℃, and controlling the extrusion ratio to be 25-30:1, obtaining an extruded alloy after water cooling, wherein the grain size of the extruded alloy is 4-10 mu m;
5. placing the extruded alloy in a resistance furnace, and annealing for 1h at 300-350 ℃ to obtain the low-alloying high-plasticity magnesium rare earth alloy, wherein the fracture elongation of the low-alloying high-plasticity magnesium rare earth alloy at room temperature is more than 50%;
wherein the content of Er in the raw materials in the first step is 1.5-2.5wt%, and the content of Mg in the raw materials in the first step is 98.5-97.5 wt%.
2. The method for preparing low-alloying high-plasticity magnesium rare earth alloy according to claim 1, wherein the protective atmosphere in the first step is SF 6 And CO 2 The mixed atmosphere of (3).
3. The method for preparing a low-alloyed high-plasticity magnesium rare earth alloy according to claim 1, wherein the cooling is performed at a rate of 5 ℃/min to 730 ℃ in the first step.
4. The method for preparing low-alloying high-plasticity magnesium rare earth alloy according to claim 1, wherein the cooling is continued to 670-690 ℃ at a speed of 5 ℃/min in the second step.
5. The method for preparing low-alloying high-plasticity magnesium rare earth alloy according to claim 1, wherein the preheating time in the fourth step is 2h.
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Citations (3)
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| CN102400071A (en) * | 2011-11-15 | 2012-04-04 | 中南大学 | Extrusion deformation technology for large-diameter high-strength heat resistant magnesium alloy pipes |
| CN109182864A (en) * | 2018-10-23 | 2019-01-11 | 重庆大学 | High-strength magnesium alloy profile and its preparation process and application |
| CN109680195A (en) * | 2019-02-19 | 2019-04-26 | 北京大学 | A kind of Mg-RE system magnesium alloy and the preparation method and application thereof |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102400071A (en) * | 2011-11-15 | 2012-04-04 | 中南大学 | Extrusion deformation technology for large-diameter high-strength heat resistant magnesium alloy pipes |
| CN109182864A (en) * | 2018-10-23 | 2019-01-11 | 重庆大学 | High-strength magnesium alloy profile and its preparation process and application |
| CN109680195A (en) * | 2019-02-19 | 2019-04-26 | 北京大学 | A kind of Mg-RE system magnesium alloy and the preparation method and application thereof |
Non-Patent Citations (2)
| Title |
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| B.L.Wu et al..The quasi-static mechanical properties of extruded binary Mg–Er alloys.《Materials Science & Engineering A》.2013,(第573期),第205-214页. * |
| The quasi-static mechanical properties of extruded binary Mg–Er alloys;B.L.Wu et al.;《Materials Science & Engineering A》;20130227(第573期);第206、209页 * |
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