CN115161528A - Mg-RE-based high-temperature-resistant high-performance magnesium alloy and preparation method thereof - Google Patents
Mg-RE-based high-temperature-resistant high-performance magnesium alloy and preparation method thereof Download PDFInfo
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- CN115161528A CN115161528A CN202210671276.7A CN202210671276A CN115161528A CN 115161528 A CN115161528 A CN 115161528A CN 202210671276 A CN202210671276 A CN 202210671276A CN 115161528 A CN115161528 A CN 115161528A
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C23/00—Alloys based on magnesium
- C22C23/06—Alloys based on magnesium with a rare earth metal as the next major constituent
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
- B21C—MANUFACTURE OF METAL SHEETS, WIRE, RODS, TUBES OR PROFILES, OTHERWISE THAN BY ROLLING; AUXILIARY OPERATIONS USED IN CONNECTION WITH METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL
- B21C23/00—Extruding metal; Impact extrusion
- B21C23/02—Making uncoated products
- B21C23/04—Making uncoated products by direct extrusion
- B21C23/08—Making wire, bars, tubes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
- B21C—MANUFACTURE OF METAL SHEETS, WIRE, RODS, TUBES OR PROFILES, OTHERWISE THAN BY ROLLING; AUXILIARY OPERATIONS USED IN CONNECTION WITH METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL
- B21C25/00—Profiling tools for metal extruding
- B21C25/02—Dies
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/02—Making non-ferrous alloys by melting
- C22C1/03—Making non-ferrous alloys by melting using master alloys
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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 discloses a Mg-RE base high temperature resistant high performance magnesium alloy and a preparation method thereof, and the Mg-RE base high temperature resistant high performance magnesium alloy comprises the following components by mass percent: 5.0 to 9.0 weight percent of yttrium, 0.6 to 3.0 weight percent of tin and the balance of magnesium. The alloy obtained by the invention has very small recrystallization size, the structure is a multi-scale structure with coexisting substructure lamellar crystal grains and small crystal grains, the deformation can be coordinated, and a large number of micron-scale and nanometer-scale Sn3Y5 phases are dispersed and distributed, the tensile mechanical property at room temperature is obviously improved, and the industrial application field of the heat-resistant magnesium alloy is expanded on the basis of low cost.
Description
Technical Field
The invention relates to the technical field of magnesium alloy, in particular to a Mg-RE base high-temperature-resistant high-performance magnesium alloy and a preparation method thereof.
Background
The magnesium alloy has the outstanding advantages of low density, high specific strength, excellent damping and shock absorbing performance, good machinability and the like, and can be widely applied to the fields of automobiles, electronic equipment, aerospace parts and biomedical equipment. Among them, the Mg-RE based alloy is one of the most important heat resistant magnesium alloys. For example, the Mg-Y based alloy and the rare earth element yttrium are added, so that the texture and the refined grains in the magnesium alloy can be weakened, and the effects of solid solution strengthening and second phase strengthening are generated to improve the mechanical properties of the magnesium alloy at room temperature and high temperature. In order to save cost and further improve the mechanical property of magnesium alloy, early literature research shows that the plasticity and the formability of the magnesium alloy can be improved after a proper amount of tin element is added, and fine and dispersed high-melting-point phase Sn generated by the action of Sn and Y acts 3 Y 5 MgSnY can block dislocation to improve the high-temperature mechanical property of the magnesium alloy. But the popularization and application of the magnesium alloy in the fields of automobiles and aviation are limited by the poor heat resistance of the magnesium alloy. At present, the demand for light parts which can work in a high temperature environment of more than 200 ℃ is increasing, and the existing heat-resistant magnesium alloy is difficult to meet all the requirements.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides the Mg-RE based high-temperature-resistant high-performance magnesium alloy and the preparation method thereof, wherein the Mg-RE based high-temperature-resistant high-performance magnesium alloy can improve the mechanical properties of the magnesium alloy at room temperature and high temperature and expand the application of the magnesium alloy in a high-temperature environment.
The technical scheme adopted by the invention is as follows:
an Mg-RE base high temperature resistant high performance magnesium alloy comprises the following components by mass percent: 5.0 to 9.0 weight percent of yttrium, 0.6 to 3.0 weight percent of tin and the balance of magnesium.
Further, the components comprise the following components in percentage by mass: yttrium 6.0wt.%, tin 0.6-3.0 wt. -%)
A preparation method of Mg-RE base high temperature resistant high performance magnesium alloy comprises the following steps:
step 1: preparing materials according to the mass percentage;
and 2, step: smelting the raw materials and then casting to obtain a sample;
and step 3: carrying out heat treatment on the sample;
and 4, step 4: rapidly and unevenly extruding the sample subjected to heat treatment at 400 ℃ to obtain a rod-shaped alloy with the required diameter of 10 mm;
the extrusion speed is 2-5 mm/s; the extrusion was carried out in three stages, with a first stage extrusion ratio of 2.25, a second stage extrusion ratio of 1.7, and a third stage extrusion ratio of 2.25.
Further, extruding by adopting an uneven transition extrusion die in the extruding process in the step 4; the extrusion die is divided into three sections from an inlet to an outlet, the three sections are all frustum structures, the length of the first section is 10mm, the length of the second section is 20mm, and the length of the third section is 7mm; the diameter of the inlet end face of the first section is 30mm, the diameter of the inlet end face of the second section is 20mm, and the diameter of the inlet end face of the third section is 15mm.
Further, the raw material in step 1 includes Mg with a purity of 99.99wt.%, sn with a purity of 99.9wt.% and a Y master alloy of Mg-30 wt.%.
Further, before smelting in the step 2, the raw materials are firstly polished to remove surface oxide skin; at SF 6 And CO 2 Heating to 720-730 ℃ under the protective atmosphere, completely melting the magnesium ingot, sequentially adding pure Sn and Mg-30Y intermediate alloy, preserving the temperature for 10-15 min, and stirring and fishing slag after melting;
then casting is carried out at 710-720 ℃.
Further, the heat treatment temperature in the step 3 is 500 ℃, and the heat treatment time is 8-10 h.
Further, the SF 6 And CO 2 Is 1.99.
The invention has the beneficial effects that:
(1) The alloy obtained by the invention has very small recrystallization size, the structure is a multi-scale structure with coexisting substructure lamellar crystal grains and small crystal grains, the alloy can be coordinately deformed, and a large amount of micron-scale and nano-scale Sn which is dispersedly distributed is arranged 3 Y 5 Meanwhile, the tensile mechanical property at room temperature is remarkably improved, and the industrial application field of the heat-resistant magnesium alloy is expanded on the basis of low cost;
(2) The invention can ensure that the obtained alloy has a specific alloy structure and good surface quality by rapid and uneven extrusion.
Drawings
FIG. 1 is a secondary electron image and a back-scattered electron image of an as-extruded microstructure of an alloy obtained in an example of the present invention. a is a secondary electron diagram of the alloy obtained in example 1, c is a secondary electron diagram of the alloy obtained in example 2, b is an XRD image of the alloy obtained in example 1, f is a scanning spot diagram corresponding to b, d is an XRD image of the alloy obtained in example 2, and h is a scanning spot diagram corresponding to d.
FIG. 2 shows SEM and EBSD images of the alloy obtained in example 1 of the present invention before and after 300 ℃ high temperature quasi in-situ tensile experiment.
FIG. 3 is a drawing illustrating the tensile properties of the alloy obtained in example 1 of the present invention.
FIG. 4 is a graph showing the tensile property curve of the alloy obtained in example 2 of the present invention.
FIG. 5 is a schematic cross-sectional view of a non-uniform over-extrusion die of the present invention.
Detailed Description
The invention is further described below with reference to the figures and the specific embodiments.
An Mg-RE base high temperature resistant high performance magnesium alloy comprises the following components by mass percent: 5.0 to 9.0 weight percent of yttrium, 0.6 to 3.0 weight percent of tin and the balance of magnesium. Preferably 6.0wt.% of yttrium, 0.6 to 3.0wt.% of tin and the balance of magnesium.
A preparation method of Mg-RE base high temperature resistant high performance magnesium alloy comprises the following steps:
step 1: preparing materials according to the mass percentage; the feedstock comprised Mg of 99.99wt.% purity, sn of 99.9wt.% purity and a Y master alloy of Mg-30 wt.%.
And 2, step: smelting the raw materials and then casting to obtain a sample;
before smelting, the raw materials are firstly polished by a steel brush to remove surface scale, and tools such as the raw materials, a crucible, a metal die and the like are dried in a preheating furnace at the temperature of 150-200 ℃; then placing the pure magnesium ingot into a crucible in a well-type resistance furnace, and introducing 90vol.% CO 2 And 10 mol.% SF 6 Mixing protective gas; heating the resistance furnace to 720-730 ℃ to completely melt the magnesium ingot, sequentially adding pure Sn and Mg-30Y intermediate alloy according to the alloy proportion, stirring after the alloy is completely melted to uniformly distribute alloy elements, standing for 10-15 min, powering off the resistance furnace, and fishing slag;
and (4) casting when the temperature is reduced to about 710-720 ℃ to obtain a round cast ingot with the diameter of 90 mm.
And step 3: carrying out heat treatment on the sample; and carrying out homogenization heat treatment on the cast ingot at 500 ℃ for 8-10 h, and then cooling the cast ingot to room temperature in air.
And 4, step 4: rapidly and unevenly extruding the sample subjected to heat treatment at 400 ℃ to obtain a rod-shaped alloy with the required diameter of 10 mm;
the extrusion speed is 2-5 mm/s; the extrusion was carried out in three stages, with a first stage extrusion ratio of 2.25, a second stage extrusion ratio of 1.7, and a third stage extrusion ratio of 2.25.
Extruding by adopting an uneven transition extrusion die in the extrusion process; the extrusion die is divided into three sections from the inlet to the outlet, the three sections are all of frustum structures, the length of the first section is 10mm, the length of the second section is 20mm, and the length of the third section is 7mm; the diameter of the inlet end face of the first section is 30mm, the diameter of the inlet end face of the second section is 20mm, and the diameter of the inlet end face of the third section is 15mm.
In the extrusion process, a round ingot with the diameter of 90mm is firstly processed into a small ingot suitable for extrusion, the diameter of the small ingot is 30mm, and the length of the small ingot is 30mm. The non-uniform transition extrusion die is designed according to needs, the stress on the alloy is non-uniform in the whole extrusion process, and the forming belt area is in a non-uniform transition mode. The extrusion ratio of the first stage is small extrusion ratio of 2.25, the deformation stress is small, the driving force of dynamic recrystallization is small, and the layered substructure grains are favorably formed. The second stage extrusion ratio is gradually reduced to 1.7, and the stage is longer and is not beneficial to dynamic recrystallization, so that the laminated substructure grains in the first stage do not continue to be recrystallized, and the alloy is further subjected to thermal deformation. The third stage was shorter and an extrusion ratio of 2.25 was consistent with the first stage goal, minimizing more dynamic recrystallization behavior.
FIG. 5 is a sectional view of a non-uniform transition mode extrusion die designed according to the present invention, wherein the ingot is extruded from left to right for forming the die. The included angles between the tangent line of the side surface and the inlet end surface of the first stage and the third stage are both about 60 degrees, and the included angle of the first stage is 63 degrees. The angle can ensure that the thermal stress is not too large in the alloy extrusion process, so that the casting is cracked, and the surface quality can also be ensured. The longest dimension of the second stage can ensure the maintenance of the layered sub-crystalline grain structure. The shortest third stage can ensure that the sample is not adhered to the mould after being demoulded and has good surface quality.
The following description will be given with reference to specific examples.
Example 1
A preparation method of Mg-RE based high-temperature-resistant high-performance magnesium alloy comprises the following steps:
step 1: preparing the materials according to the mass percentage; yttrium 6wt.%, tin 1.5wt.%, and the balance magnesium.
The feedstock comprised Mg of 99.99wt.% purity, sn of 99.9wt.% purity and a Y master alloy of Mg-30 wt.%.
And 2, step: smelting the raw materials and then casting to obtain a sample;
before smelting, the raw materials are firstly polished by a steel brush to remove surface scale, and tools such as the raw materials, a crucible, a metal die and the like are dried in a preheating furnace at the temperature of 150-200 ℃; then placing the pure magnesium ingot into a crucible in a well-type resistance furnace, and introducing 90vol.% CO 2 And 10 mol.% SF 6 Mixing protective gas; heating the resistance furnace to 720-730 ℃ to completely melt the magnesium ingot, sequentially adding pure Sn and Mg-30Y intermediate alloy according to the alloy proportion, and stirring to ensure that the alloy elements are molten completelyUniformly distributing elements, standing for 10-15 min, powering off the resistance furnace, and fishing slag;
and (4) casting when the temperature is reduced to about 710-720 ℃ to obtain a round cast ingot with the diameter of 90 mm.
And step 3: carrying out heat treatment on the sample; and carrying out homogenization heat treatment on the cast ingot at 500 ℃ for 8-10 h, and then cooling the cast ingot to room temperature in air.
And 4, step 4: rapidly and unevenly extruding the heat-treated sample at 400 ℃ to obtain a rod-shaped alloy with the required diameter of 10 mm;
the extrusion speed is 2mm/s; the extrusion was carried out in three stages, the first stage extrusion ratio being 2.25, the second stage extrusion ratio being 1.7 and the third stage extrusion ratio being 2.25.
Example 2
The other steps are the same as the example 1, except that the components in percentage by weight comprise: yttrium 6wt.%, tin 0.6wt.%, and the balance magnesium.
Example 3
The other steps are the same as the example 1, except that the components in percentage by weight comprise: yttrium 5wt.%, tin 3wt.%, and the balance magnesium.
Example 4
The other steps are the same as the example 1, except that the components in percentage by weight comprise: 9wt.% yttrium, 3wt.% tin, and the balance magnesium.
Example 5
The other steps were the same as in example 1 except that the extrusion speed in step 4 was 5mm/s.
Comparative example 1
The other steps are the same as the embodiment, except that the components in percentage by weight comprise: yttrium 6wt.%, balance magnesium.
Comparative example 2
The other steps are the same as the embodiment, except that the step 4 adopts a common speed uniform extrusion mode for extrusion, and the extrusion speed is 1mm/s.
The extrusion alloys obtained in examples 1 to 4 and the respective proportions were subjected to room temperature and high temperature tensile mechanical property tests, and the tensile yield strength and ultimate tensile yield strength thereof were counted, and the results are shown in table 1.
TABLE 1
In the table, RT represents room temperature, UTS represents ultimate tensile yield strength, and TYS represents tensile yield strength.
As can be seen from the statistical results in Table 1, the ternary alloy of yttrium, tin and magnesium has a significant grain refinement and an improvement in tensile properties at room temperature over the binary magnesium alloy with 6% yttrium. The room temperature tensile properties of the non-uniform rapid extrusion of example 1 are significantly better than those of comparative example 2 of uniform extrusion with the same composition.
On the one hand, the uneven rapid extrusion can contribute to the formation of a substructure lamellar grain structure; on the other hand, sn 3 Y 5 The phase is used as the core of heterogeneous nucleation, so that the nucleation rate is increased to promote discontinuous dynamic recrystallization to realize grain refinement, the multi-scale structure can be coordinately deformed under the action of external force, and the high-temperature performance of the alloy is improved. Wherein the nano-scale Sn is dynamically precipitated in the extrusion process 3 Y 5 The phase is dispersed in the magnesium alloy matrix and can block the movement of dislocation in high-temperature deformation, thereby improving the high-temperature mechanical property of the alloy.
FIG. 1 is a secondary electron image and a back-scattered electron image of the as-extruded microstructures of the alloys of examples 1 and 2. a is a secondary electron diagram of the alloy obtained in example 1, c is a secondary electron diagram of the alloy obtained in example 2, b is an XRD image of the alloy obtained in example 1, f is a scanning spot diagram corresponding to b, d is an XRD image of the alloy obtained in example 2, and h is a scanning spot diagram corresponding to d. From fig. 1a and fig. 1c, it can be seen that the extruded alloy structure after non-uniform rapid extrusion is a multi-scale structure with non-recrystallized grains and recrystallized grains coexisting, and the structure can be coordinately deformed under the action of external force to improve the strength of the alloy. Fig. 1e and 1g show the backscattered electron images and enlarged partial areas of examples 1 and 2. It can be seen from the figure that the precipitated phase has two dimensions, namely a large number of micron-sized precipitated phases and a large number of nano-sized precipitated phases which are dispersed and distributed. Wherein, in FIG. 1b, FIG. 1d, FIG. 1f and FIG. 1h, it can be seen that the atomic ratio of Sn to Y at points 1 and 2 in the figure is 3. Because the precipitated phase has an inhibiting effect on the slippage of dislocation in the crystal, the precipitated phase strengthening effect is generated, and the strength and the plasticity of the alloy can be greatly improved. In addition, the microstructure observed face corresponds to the ED-TD face (the face found perpendicular to the extrusion direction ED).
FIG. 2a is an SEM image of a 13% high temperature quasi-in-situ tensile test at 300 ℃ and FIG. 2b is an SEM image of the tensile test. Fig. 2c is an EBSD image before the tensile test, and fig. 2d is an EBSD image after the tensile test. As can be seen from the figure, the morphology and the size of the precipitated phase are not obviously changed, and the multi-scale grain structure is not obviously recovered and recrystallized. The dislocation number is not dissipated at high temperature, but increased by more than 2 times. From the above figures, it can be seen that the developed novel alloy has good thermal stability at high temperature, and ensures the strengthening effect at high temperature.
FIG. 3 is a true stress-strain curve corresponding to the alloy after extrusion in example 1 being stretched at room temperature, 200 deg.C, 300 deg.C. FIG. 4 is a true stress-strain curve corresponding to the extrusion of example 2 at room temperature, 200 deg.C, and 300 deg.C under tension.
The proper extrusion process can give play to the maximum shaping of the magnesium alloy, effectively refine the grain structure of the magnesium alloy and improve the strength and the shaping of the magnesium alloy. Through rapid uneven extrusion, the structure can be changed into a multi-scale structure with overlapped substructure lamellar grains and dynamic recrystallization grains, simultaneously, a precipitated phase with a nanometer scale is dynamically precipitated, and a coarse precipitated phase generated in the crushing casting process is a precipitated phase with a micrometer scale. On one hand, the substructure layer-shaped crystal grains and the dynamic recrystallization crystal grains can be coordinately deformed in the deformation process, and the high-temperature strength of the alloy is improved. On the other hand, the multi-scale precipitated phase with strong thermal stability pins the grain boundary, so that the multi-scale structure is kept stable in the thermal deformation process.
Claims (8)
1. The Mg-RE-based high-temperature-resistant high-performance magnesium alloy is characterized by comprising the following components in percentage by mass: 5.0 to 9.0 weight percent of yttrium, 0.6 to 3.0 weight percent of tin and the balance of magnesium.
2. The Mg-RE based high-temperature-resistant high-performance magnesium alloy as claimed in claim 1, which is characterized by comprising the following components in percentage by mass: 6.0wt.% of yttrium, 0.6-3.0 wt.% of tin and the balance of magnesium.
3. The method for preparing the Mg-RE based high-temperature-resistant high-performance magnesium alloy as claimed in any one of claims 1 to 2, which is characterized by comprising the following steps:
step 1: preparing the materials according to the mass percentage;
step 2: smelting the raw materials and then casting to obtain a sample;
and step 3: carrying out heat treatment on the sample;
and 4, step 4: rapidly and unevenly extruding the heat-treated sample at 400 ℃ to obtain a rod-shaped alloy with the required diameter of 10 mm;
the extrusion speed is 2-5 mm/s; the extrusion was carried out in three stages, with a first stage extrusion ratio of 2.25, a second stage extrusion ratio of 1.7, and a third stage extrusion ratio of 2.25.
4. The method for preparing the Mg-RE based high-temperature-resistant high-performance magnesium alloy according to the claim 3, wherein the step 4 is carried out by adopting a non-uniform transition extrusion die in the extrusion process; the extrusion die is divided into three sections from the inlet to the outlet, the three sections are all of frustum structures, the length of the first section is 10mm, the length of the second section is 20mm, and the length of the third section is 7mm; the diameter of the inlet end face of the first section is 30mm, the diameter of the inlet end face of the second section is 20mm, and the diameter of the inlet end face of the third section is 15mm.
5. The method for preparing the Mg-RE based high temperature resistant high performance magnesium alloy according to claim 3, wherein the raw materials in step 1 comprise Mg with a purity of 99.99wt.%, sn with a purity of 99.9wt.% and Y intermediate alloy with Mg-30 wt.%.
6. The method for preparing the Mg-RE based high-temperature-resistant high-performance magnesium alloy according to claim 5, wherein the raw materials are firstly ground to remove the surface oxide skin before smelting in the step 2; at SF 6 And CO 2 Heating to 720-730 ℃ under the protective atmosphere, adding pure Sn and Mg-30Y intermediate alloy after the magnesium ingot is completely melted, preserving the temperature for 10-15 min, stirring and fishing slag after melting;
then casting is carried out at 710-720 ℃.
7. The preparation method of the Mg-RE based high-temperature-resistant high-performance magnesium alloy according to claim 3, wherein the heat treatment temperature in the step 3 is 500 ℃ and the heat treatment time is 8-10 h.
8. The method for preparing Mg-RE based high-temperature-resistant high-performance magnesium alloy according to claim 6, wherein the SF is 6 And CO 2 Is 1.99.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB903584A (en) * | 1959-08-05 | 1962-08-15 | Magnesium Elektron Ltd | Magnesium base alloys |
| CN104060140A (en) * | 2014-07-10 | 2014-09-24 | 重庆大学 | High temperature oxidation resistant magnesium alloy |
| CN111321333A (en) * | 2020-03-06 | 2020-06-23 | 西南交通大学 | Heat-resistant magnesium alloy and preparation method thereof |
| CN114438384A (en) * | 2020-11-02 | 2022-05-06 | 宝钢金属有限公司 | Low-cost high-toughness flame-retardant magnesium alloy and preparation method of extrusion material thereof |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB903584A (en) * | 1959-08-05 | 1962-08-15 | Magnesium Elektron Ltd | Magnesium base alloys |
| CN104060140A (en) * | 2014-07-10 | 2014-09-24 | 重庆大学 | High temperature oxidation resistant magnesium alloy |
| CN111321333A (en) * | 2020-03-06 | 2020-06-23 | 西南交通大学 | Heat-resistant magnesium alloy and preparation method thereof |
| CN114438384A (en) * | 2020-11-02 | 2022-05-06 | 宝钢金属有限公司 | Low-cost high-toughness flame-retardant magnesium alloy and preparation method of extrusion material thereof |
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| Title |
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| 徐春杰等: "热处理对Mg-3Sn-1Y合金显微组织及显微硬度的影响", 《中国有色金属学报》 * |
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