CN114855042B - High-strength-plasticity Mg-Al-Sn alloy and preparation method thereof - Google Patents
High-strength-plasticity Mg-Al-Sn alloy and preparation method thereof Download PDFInfo
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Abstract
The present invention providesA high-strength-plasticity Mg-Al-Sn alloy and a preparation method thereof belong to the field of metal materials, and the alloy consists of the following components; according to the mass percentage: al:3-12%, sn:0.5-4%, ca:0.1-3%, inevitable impurities less than or equal to 0.02%, and the balance of magnesium. The refined and spheroidized CaMgSn, mgAlCa and Mg are obtained by the processes of melting, refining, sub-rapid solidification, large stirring friction deformation and the like 17 Al 12 When the second phase is equal, uniform and fine grains are obtained at the same time, and the obtained magnesium alloy has high strength and plasticity, wherein the room-temperature elongation is more than or equal to 30 percent. The invention solves the problem that coarse second phases such as CaMgSn, mgAlCa and the like in Mg-Al-Sn magnesium alloy are difficult to refine, omits high-temperature long-time solution treatment, is green and energy-saving, has simple and reliable preparation process, and provides an effective path for the industrialized production of the magnesium alloy.
Description
Technical Field
The invention belongs to the technical field of metal materials, and particularly relates to a high-strength-plasticity Mg-Al-Sn alloy and a preparation method thereof.
Background
Magnesium alloys have been widely used in a variety of industrial fields due to their advantages of light weight. However, the coarse second phase in the magnesium alloy can be used as a crack source in the deformation process, so that cracks are induced to be initiated in advance, and the matrix is cut, so that the plasticity of the alloy is reduced, and the material can fail in advance. Thus refining the second phase of the magnesium alloy is crucial to the alloy application and the prior art discloses the following methods for refining the second phase of the magnesium alloy: firstly, a refiner containing rare earth components is added, the refiner has higher selectivity for the alloy, only part of second phases in the alloy can be refined, and the addition of the rare earth refiner obviously increases the cost of the alloy; secondly, the second phase is promoted to be redissolved through high-temperature long-time solid solution heat treatment so as to refine the second phase. However, the heating process of high-temperature long-time solid solution is complex in process, so that the cost is obviously increased, and meanwhile, the environmental burden is increased due to the use of a large amount of electric energy; and thirdly, the second phase is refined by adopting large deformation modes such as equal channel angular extrusion, high-pressure torsion and the like, but the effect is not ideal, and the large deformation process is only suitable for the stage of preparing small samples in a laboratory and cannot realize large-batch industrial production. Therefore, the development of a high-strength plastic magnesium alloy with short flow, low energy consumption, production cost saving and refined and spheroidized second phase is a technical problem which needs to be solved at present.
Disclosure of Invention
In order to solve the technical problem, the invention provides a high-strength-plasticity Mg-Al-Sn alloy which comprises the following components in parts by weight: the alloy consists of the following components: by mass percent, al:3-12%, sn:0.5-4%, ca:0.1-3%, and inevitable impurities less than or equal to 0.02%; the balance being magnesium;
the alloy is prepared by the following method:
(1) In CO 2 And SF 6 Under the protection of mixed gas or commercialized flux II, keeping pure magnesium, pure aluminum, pure tin and magnesium-calcium intermediate alloy at 660-740 ℃ for 1-5 hours, blowing inert gas for refining, stirring and keeping the temperature for 3-40 minutes to obtain magnesium alloy melt;
(2) Pouring the magnesium alloy melt obtained in the step (1) into a vibration-assisted water-cooling copper mould to obtain an alloy cast ingot, and cutting and polishing to obtain a magnesium alloy plate with a smooth surface;
(3) Processing the magnesium alloy plate obtained in the step (2) by adopting a stirring and friction tool at the temperature of 10-50 ℃ to obtain high-strength plastic Mg-Al-Sn alloy; the friction stir tool is as follows: the rotating speed is 400-3000rpm, the feeding speed is 40-250mm/min, the length of the friction stir tool is 1-10mm, and the pressing amount of the friction stir tool is 0.1-1.5mm; the inclination angle between the friction stir tool and the magnesium alloy plate is 1-10 degrees;
the average size of the second phase of the Mg-Al-Sn alloy obtained in the step (3) is 0.3-1.0 mu m.
Further, CO described in step (1) 2 And SF 6 Mixed gas, by volume, of CO 2 :SF 6 Is 50.
Further, the magnesium-calcium master alloy in the step (1) is one of Mg-20Ca, mg-25Ca and Mg-30 Ca.
Further, the inert gas in the step (1) is one of argon, neon or helium.
Further, the vibration-assisted water-cooling copper mold in the step (2): can realize sub-rapid solidification, and the solidification cooling rate is 10-400K/s.
Further, the vibration-assisted water-cooling copper mold in the step (2): the vibration amplitude is 1-3mm, and the vibration frequency is 15-100Hz.
Further, the rotating speed in the step (3) is 600-2000rpm.
Further, the feeding speed in the step (3) is 50-200mm/min.
Further, the pressing amount in the step (3) is 0.2-0.8mm.
Further, the inclination angle of the friction stir tool and the magnesium alloy sheet material in the step (3) is 1-4 degrees.
Compared with the prior art, the invention is characterized in that:
in order to effectively solve the problem that the coarse second phase in the magnesium alloy is difficult to refine, particularly when the Mg-Al-Sn alloy contains Ca element, a large amount of large-size and sharp-angled coarse second phase containing Ca element is generated, so that the second phase of the Ca-alloyed Mg-Al-Sn alloy is more difficult to refine. The invention effectively solves the technical problems through the interaction between alloy components and the synergistic effect of the process, and obtains the following excellent effects: firstly, the large-size second phase is crushed to form spherical and fine CaMgSn phase, mgAlCa phase and Al phase which are uniformly dispersed and distributed 2 Ca phase and Mg 17 Al 12 Phases, the average size of these spherical and fine second phases being 0.3 to 1.0 μm, while achieving the effect of second phase refinement and spheroidization; secondly, the magnesium matrix crystal grains can be obviously refined, so that the crystal grain size can be refined to 0.6-1 mu m; thirdly, the inventionObviously, the plasticity index of the obtained Mg-Al-Sn alloy is far higher than that of the Mg-Al-Sn alloy obtained in the prior art. Compared with the prior art, the method has the advantages that the high strength is kept and the average elongation is improved by 45% or more than the prior art on the premise of saving the production cost of raw materials, simplifying the production process and energy consumption and obviously shortening the flow.
Drawings
FIG. 1 is an SEM photograph of a Mg-4Al-2Sn-0.6Ca magnesium alloy obtained in step (3) of example 3.
Detailed Description
Example 1
The Mg-4Al-1Sn-2.5Ca alloy (calculated by mass percent, 4 percent of Al, 1 percent of Sn, 2.5 percent of Ca, less than or equal to 0.02 percent of unavoidable impurities and the balance of magnesium) is prepared by the following steps;
(1) In CO 2 And SF 6 Under the protection of mixed gas of (2), according to the volume ratio of CO 2 :SF 6 Keeping the temperature of pure magnesium, pure aluminum, pure tin and Mg-20Ca intermediate alloy at 710 ℃ for 3 hours, blowing argon gas into the bottom of the melt for refining, stirring and keeping the temperature for 30 minutes to obtain a magnesium alloy melt, wherein the temperature is 250 ℃;
(2) Pouring the magnesium alloy melt obtained in the step (1) into a vibration-assisted water-cooling copper mould, casting under the conditions of vibration amplitude of 2mm, vibration frequency of 30Hz and solidification cooling rate of 350K/s to obtain an alloy ingot, and cutting and polishing to obtain a magnesium alloy plate with a smooth surface;
(3) Processing the magnesium alloy plate obtained in the step (2) by adopting a stirring and friction tool at the temperature of 20 ℃ to finally obtain Mg-4Al-1Sn-2.5Ca alloy; wherein the friction stir processing parameters are as follows: the rotation speed of the friction stir tool is 1800rpm, the feed speed of the friction stir tool is 100mm/min, the length of the friction stir tool is 3.5mm, the pressing amount of the friction stir tool is 0.5mm, and the inclination angle between the friction stir tool and the magnesium alloy plate is 2 degrees;
the Mg-4Al-1Sn-2.5Ca alloy obtained in the step (3) has a better spheroidizing effect of a second phase of the magnesium alloy, the average size of the second phase is 0.3-0.45 mu m, the average grain size is 0.7 mu m, and the average elongation is 36%.
Example 2
The preparation method of the Mg-8Al-3Sn-1Ca alloy (according to the mass percentage, 8 percent of Al, 3 percent of Sn, 1 percent of Ca, less than or equal to 0.02 percent of unavoidable impurities and the balance of magnesium) comprises the following steps of;
(1) In CO 2 And SF 6 Under the protection of mixed gas of (A) and (B), according to the volume ratio of CO 2 :SF 6 Keeping the temperature of pure magnesium, pure aluminum, pure tin and Mg-30Ca intermediate alloy at a temperature of 690 ℃ for 4 hours, blowing neon at the bottom of the melt for refining, stirring, keeping the temperature for 25 minutes, and obtaining a magnesium alloy melt;
(2) Pouring the magnesium alloy melt obtained in the step (1) into a vibration-assisted water-cooling copper mould, casting under the conditions of vibration amplitude of 2mm, vibration frequency of 60Hz and solidification cooling rate of 100K/s to obtain an alloy ingot, and cutting and polishing to obtain a magnesium alloy plate with a smooth surface;
(3) Processing the magnesium alloy plate obtained in the step (2) by adopting a stirring and friction tool at 35 ℃ to finally obtain Mg-8Al-3Sn-1Ca alloy; wherein the friction stir processing parameters are as follows: the rotating speed of the friction stir tool is 1000rpm, the feeding speed of the friction stir tool is 120mm/min, the length of the friction stir tool is 5mm, the pressing amount of the friction stir tool is 0.2mm, and the inclination angle between the friction stir tool and the magnesium alloy plate is 3 degrees;
in the Mg-8Al-3Sn-1Ca alloy obtained in the step (3), the second phase of the magnesium alloy has better spheroidization effect, the average size of the second phase is 0.6-0.9 mu m, the average grain size is 0.85 mu m, and the average elongation is 34%.
Example 3
The Mg-4Al-2Sn-0.6Ca alloy (calculated by mass percent, 4 percent of Al, 2 percent of Sn, 0.6 percent of Ca, less than or equal to 0.02 percent of unavoidable impurities and the balance of magnesium) is prepared by the following steps;
(1) In CO 2 And SF 6 Under the protection of mixed gas of (A) and (B), according to the volume ratio of CO 2 :SF 6 Keeping the temperature of pure magnesium, pure aluminum, pure tin and Mg-20Ca intermediate alloy at the temperature of 700 ℃ for 2 hours at 150;
(2) Pouring the magnesium alloy melt obtained in the step (1) into a vibration-assisted water-cooling copper mould, casting under the conditions of vibration amplitude of 2mm, vibration frequency of 30Hz and solidification cooling rate of 120K/s to obtain an alloy ingot, and cutting and polishing to obtain a magnesium alloy plate with a smooth surface;
(3) Processing the magnesium alloy plate obtained in the step (2) by adopting a stirring and friction tool at room temperature to finally obtain Mg-4Al-2Sn-0.6Ca alloy; wherein the friction stir processing parameters are as follows: the rotating speed of the friction stir tool is 800rpm, the feeding speed of the friction stir tool is 100mm/min, the length of the friction stir tool is 3mm, the pressing amount of the friction stir tool is 0.3mm, and the inclination angle between the friction stir tool and the magnesium alloy plate is 2 degrees;
the Mg-4Al-2Sn-0.6Ca alloy obtained in the step (3) can be seen from the attached figure 1: the second phase of the magnesium alloy has good spheroidizing effect and is uniformly dispersed, and the second phase realizes good refining effect, the average second phase size is 0.5-0.8 mu m, the average grain size is 0.9 mu m, and the average elongation is 35%.
Comparative example 1
A method for refining a CaMgSn phase in Mg-Sn-Ca based magnesium alloy by adding Sr, which is disclosed in CN101985713A by Yangmbo et al, by adding 0.05% Sr as a refiner (in mass%: mg:94.95%, sn:3%, ca:2%, sr: 0.05%) to Mg-3Sn-2Ca alloy, and by making the area of the CaMgSn phase from 545 μm 2 Thinning the mixture to 216 mu m 2 According to the patent, the average size of the second phase is refined from 26 μm to 16 μm through calculation, and the average elongation is improved from 1.9% to 2.2%.
Comparative example 2
An article entitled "Hot formation floor of Mg-2Sn-2Ca alloy in as-cast condition and after catalysis and homology" published in J.A.A. by K.P. Rao et al, J.A. 8.2012, volumes 552, pages 444-450, in which an as-cast Mg-2Sn-2Ca alloy is solution treated at 450 ℃ for 5 hours, and the second phase of CaMgSn after solution treatment is compared with the second phase of CaMgSn in the ingot, the results show that: the size and the appearance of the second phase are not changed, and the size of the CaMgSn second phase is 50 mu m after the solution treatment.
Comparative example 3
An article entitled "Enhanced precipitation straightening of Mg-Al-Sn-Ca alloy by multidirectional rolling" disclosed in the 9 th month 2021, 19 volume of Materialia journal, p 101185, by Li Shigang et Al, in which an extruded Mg-2Al-0.8Sn-0.5Ca alloy was subjected to a solution treatment at 420 ℃ for 2 hours, followed by a solution treatment at 490 ℃ for 2 hours, followed by four-pass rolling at 300 ℃ of 15%, 20%, 30% and 45%, followed by annealing at 275 ℃ for 8 minutes to finally obtain a multi-directionally rolled Mg-2Al-0.8Sn-0.5Ca alloy, crushing the large-size second phase to micron and submicron sizes, measuring the average second phase size to 1.3 μm, the average grain size to 2.6 μm, and the average elongation to 23.4%, was disclosed by Li Shigang et Al, 9.1.
As can be seen by comparative examples 1 to 3: the larger the content of added Ca element, the larger the second phase size, with the second phase size of comparative example 3 being the smallest; examples 1-3 compared to comparative example 3, all examples of the invention have a higher calcium content than comparative example 3, calculated according to the prior art: the sizes of the second phases in examples 1-3 of the invention are all higher than the size of comparative example 3, but through the comparison, the sizes of the second phases in examples 1-3 are far smaller than the sizes of the second phases disclosed in comparative example 3, and compared with comparative examples 1-3, the refining effect of the second phase of the invention is obviously improved; in addition, the grain size obtained by the invention is smaller than that disclosed in comparative examples 1-3, and the plasticity of the Mg alloy finally obtained by the invention is higher than that of the alloy disclosed in comparative example 3. Compared with the comparative example, the invention simultaneously obtains 3 beneficial effects of refining the spheroidized second phase, refining the crystal grains and improving the plasticity of the alloy through the interaction between elements and the synergistic effect of the process, and compared with the prior art, the alloy structure and the performance of the invention both obtain unexpected technical effects.
In addition, the technical effects of simultaneously realizing the second phase refining, spheroidizing and grain size refining of the magnesium alloy are not given by the comparative example and the prior art; the invention also obtains the excellent technical effect of 45 percent or more of magnesium alloy plasticity than that obtained by the prior art.
To sum up: the invention realizes the technical effects of the second phase refinement, spheroidization and grain size refinement of the magnesium alloy simultaneously through the interaction between elements and the synergistic effect of the process; the invention also achieves the excellent technical effect of magnesium alloy plasticity which is higher than that obtained by the prior art.
Table 1 shows the second phase size, grain size and room temperature elongation of the magnesium alloys obtained in examples 1 to 3 and comparative examples 1 to 3
Claims (10)
1. A high-strength-plasticity Mg-Al-Sn alloy is characterized in that: the alloy consists of the following components: by mass percent, al:3-12%, sn:0.5-4%, ca:0.1 to 3 percent of the total weight of the composition, and less than or equal to 0.02 percent of inevitable impurities; the balance being magnesium;
the alloy is prepared by the following method:
(1) In CO 2 And SF 6 Under the protection of mixed gas or commercialized flux II, keeping pure magnesium, pure aluminum, pure tin and magnesium-calcium intermediate alloy at 660-740 ℃ for 1-5 hours, blowing inert gas for refining, stirring and keeping the temperature for 3-40 minutes to obtain magnesium alloy melt;
(2) Pouring the magnesium alloy melt obtained in the step (1) into a vibration-assisted water-cooling copper mould to obtain an alloy cast ingot, and cutting and polishing to obtain a magnesium alloy plate with a smooth surface;
(3) Processing the magnesium alloy plate obtained in the step (2) by adopting a stirring and friction tool at the temperature of 10-50 ℃ to obtain high-strength plastic Mg-Al-Sn alloy; the friction stir tool is as follows: the rotating speed is 400-3000rpm, the feeding speed is 40-250mm/min, the length of the friction stir tool is 1-10mm, and the pressing amount of the friction stir tool is 0.1-1.5mm; the inclination angle between the friction stir tool and the magnesium alloy plate is 1-10 degrees;
the average size of the second phase of the Mg-Al-Sn alloy obtained in the step (3) is 0.3-1.0 μm.
2. High strength plastic according to claim 1A Mg-Al-Sn alloy characterized by: CO described in step (1) 2 And SF 6 Mixed gas, by volume, of CO 2 :SF 6 Is 50.
3. The high-strength plastic Mg-Al-Sn alloy as claimed in claim 1, wherein: the magnesium-calcium intermediate alloy in the step (1) is one of Mg-20Ca, mg-25Ca or Mg-30 Ca.
4. A high strength and ductility Mg-Al-Sn alloy according to claim 1, wherein: the inert gas in the step (1) is one of argon, neon or helium.
5. A high strength and ductility Mg-Al-Sn alloy according to claim 1, wherein: the vibration-assisted water-cooling copper mould in the step (2): can realize sub-rapid solidification, and the solidification cooling rate is 10-400K/s.
6. A high strength and ductility Mg-Al-Sn alloy according to claim 1, wherein: the vibration-assisted water-cooling copper mould in the step (2): the vibration amplitude is 1-3mm, and the vibration frequency is 15-100Hz.
7. A high strength and ductility Mg-Al-Sn alloy according to claim 1, wherein: the rotating speed in the step (3) is 600-2000rpm.
8. The high-strength plastic Mg-Al-Sn alloy as claimed in claim 1, wherein: the feeding speed in the step (3) is 50-200mm/min.
9. A high strength and ductility Mg-Al-Sn alloy according to claim 1, wherein: the pressing amount in the step (3) is 0.2-0.8mm.
10. A high strength and ductility Mg-Al-Sn alloy according to claim 1, wherein: the inclination angle between the friction stir tool in the step (3) and the magnesium alloy plate is 1-4 degrees.
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