CN113881878B - Preparation process of Mg-Al-Ca magnesium alloy forging - Google Patents
Preparation process of Mg-Al-Ca magnesium alloy forging Download PDFInfo
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- CN113881878B CN113881878B CN202111170653.0A CN202111170653A CN113881878B CN 113881878 B CN113881878 B CN 113881878B CN 202111170653 A CN202111170653 A CN 202111170653A CN 113881878 B CN113881878 B CN 113881878B
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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
- C22C23/02—Alloys based on magnesium with aluminium as the next major constituent
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
- B21J—FORGING; HAMMERING; PRESSING METAL; RIVETING; FORGE FURNACES
- B21J5/00—Methods for forging, hammering, or pressing; Special equipment or accessories therefor
- B21J5/06—Methods for forging, hammering, or pressing; Special equipment or accessories therefor for performing particular operations
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- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
- C21D1/00—General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering
- C21D1/26—Methods of annealing
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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
- C22F1/002—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
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Abstract
The invention discloses a preparation process of a Mg-Al-Ca magnesium alloy forging, which comprises the following steps: A. processing Mg-Al-Ca magnesium alloy into a cubic ingot blank with the side length of 60-200 mm; B. carrying out homogenization annealing treatment on the ingot blank, wherein the annealing process comprises the following steps: keeping the temperature at 320-360 ℃ for 4-6h, heating to 400-420 ℃ and keeping the temperature for 25-30h; C. after the homogenization annealing treatment, taking out the ingot blank, air-cooling to the initial forging temperature of 340-360 ℃, carrying out drawing length type cooling free forging on a hydraulic press, wherein the temperature of an upper chopping board and a lower chopping board is 300-350 ℃, the reduction speed is 400-500mm/min, the forging is carried out for 10-16 times, the pass true strain is 0.1-0.2, the accumulated true strain is 1.6-2.4, and the forging finishing temperature is 210-240 ℃; D. immediately quenching after forging, wherein the water temperature is 40-70 ℃; by adopting the process, intermediate annealing is not needed during forging, and aging treatment is not needed after forging, so that the process flow is obviously shortened, the production efficiency is improved, and the production cost is reduced; and the prepared Mg-Al-Ca series alloy forging has high strength and good plasticity, and meets the performance requirements of magnesium alloy structural members in the fields of aerospace and automobile industry.
Description
Technical Field
The invention relates to the field of magnesium alloy deformation processing, in particular to a short-process preparation process of a Mg-Al-Ca magnesium alloy forging.
Background
The magnesium alloy has the advantages of low density, high specific strength, good damping and shock-absorbing properties, easy recovery and the like, and shows wide development prospects in the fields of national defense and military industry, aerospace, automobile industry and the like. Among them, the Mg-Al-Ca series alloy has larger market and dosage compared with other magnesium alloys because of lower raw material cost and good matching of strength and plasticity. However, compared with rare earth magnesium alloy, aluminum alloy and steel structural materials, the strength and plasticity of Mg-Al-Ca series alloy are far insufficient, which seriously restricts the popularization and application of the alloy.
The fine grain strengthening is the main strengthening mechanism of Mg-Al-Ca series alloy, because the alloy has a close-packed hexagonal structure, the constant K value in the Hall-Petch relation of the alloy is far higher than that of metal materials (such as aluminum alloy, copper alloy and the like) with other structures, and when the recrystallization is sufficient, the uniform microstructure can also effectively relieve stress concentration so as to improve the plasticity of the material. Precipitation strengthening is another strengthening mechanism of Mg-Al-Ca series alloy, precipitates are formed in the alloy by aging heat treatment to block dislocation movement, and the shape and the size of the aging precipitates are determined by aging heat treatment system, which has great influence on the strength and the plasticity of the alloy.
Therefore, in order to improve the comprehensive mechanical properties of the Mg-Al-Ca alloy, the growth of crystal grains caused by intermediate annealing and other processes should be avoided as much as possible in the deformation processing process, and the aging treatment is adopted after the deformation so as to introduce the precipitation strengthening effect. Partial scholars propose a process route of pre-aging treatment before deformation, and achieve the refinement of the sizes of grains and a second phase at the same time by means of the induction action of aging precipitation relative to recrystallization and the crushing action of deformation on a precipitated phase, thereby improving the mechanical property. However, the deformation temperature is limited to the aging temperature range (200 ℃) in the process of deforming after pre-aging, and the process is mostly suitable for extruding the stress state of three-dimensional compression, and the process is easy to crack during forging, obviously improves the deformation resistance and increases the tonnage and the loss of equipment. In addition, the process still comprises the steps of aging treatment, cooling after heat treatment and heating before deformation, and the process flow cannot be shortened.
Disclosure of Invention
The invention provides a simple short-flow forging process for large-scale industrial production of Mg-Al-Ca magnesium alloy, and provides a short-flow preparation process of a Mg-Al-Ca magnesium alloy forging, wherein the specific technical scheme is as follows.
A preparation process of a Mg-Al-Ca magnesium alloy forging piece is characterized by comprising the following steps: the Mg-Al-Ca magnesium alloy comprises the following components in percentage by mass: 7.5-9.0%, ca:0.3-0.5%, fe is less than or equal to 0.01%, ni is less than or equal to 0.0015%, be is less than or equal to 0.001%, and the balance is Mg, wherein the preparation process comprises the following steps:
A. processing Mg-Al-Ca magnesium alloy into a cubic ingot blank with the side length of 60-200 mm;
B. carrying out homogenization annealing treatment on the ingot blank, wherein the annealing process comprises the following steps: keeping the temperature at 320-360 ℃ for 4-6h, heating to 400-420 ℃ and keeping the temperature for 25-30h;
C. after the homogenization annealing treatment, taking out the ingot blank, air-cooling to the initial forging temperature of 340-360 ℃, carrying out drawing length type cooling free forging on a hydraulic press, wherein the temperature of an upper chopping board and a lower chopping board is 300-350 ℃, the reduction speed is 400-500mm/min, the forging is carried out for 10-16 times, the pass true strain is 0.1-0.2, the accumulated true strain is 1.6-2.4, and the forging finishing temperature is 210-240 ℃;
D. quenching treatment is carried out immediately after the forging is finished, and the water temperature is 40-70 ℃.
Preferably, in the step C, the surface temperature of the ingot blank in the initial forging pass is 345-355 ℃.
Wherein, the drawing type temperature reduction free forging of the step C is as follows: any two groups of parallel surfaces of the cubic ingot blank rotate by 90 degrees in turn and are pressed, the other group of parallel surfaces are not forged all the time, and the ingot blank is continuously drawn out.
Preferably, the surface temperature of the ingot at the last forging in step C is 210-235 ℃.
And D, wherein the room-temperature yield strength of the quenched forging in the drawing direction in the step D is larger than or equal to 270MPa, the tensile strength of the quenched forging in the drawing direction is larger than or equal to 370MPa, and the elongation after fracture is larger than or equal to 6%.
In the above scheme, the purpose of homogenizing the square ingot is to eliminate dendrite segregation, promote the uniformity of components, remove residual pressure and the like, so as to improve the formability of the ingot blank.
And taking out the ingot blank after the homogenization treatment, and air-cooling to 340-360 ℃ (the initial forging temperature), wherein the temperature is near the solidus of the magnesium alloy, so that the rapid dynamic precipitation is facilitated, and the synergistic operation of the recrystallization and the dynamic precipitation process is achieved. And immediately performing drawing type temperature reduction free forging on an oil press after the temperature is reached. The temperature of the upper chopping block and the lower chopping block is 300-350 ℃ to prevent the heat from being lost too quickly. The pressing speed is 400mm/min-500mm/min. Any two groups of parallel surfaces (X/Y surfaces) of the cubic ingot blank are sequentially and alternately rotated by 90 degrees to be pressed, the other group of parallel surfaces (Z surfaces) are not forged all the time, the normal direction (Z axis) of the other group of parallel surfaces is drawn out in the forging process, and XYZ is three axial directions in a Cartesian coordinate system. Each forging is called 1 pass, 10-16 passes of total forging are carried out, the true strain amount of each pass is controlled to be 0.1-0.2, annealing treatment is not carried out between two adjacent passes, therefore, the deformation temperature of the next pass is always lower than that of the previous pass, continuous cooling forging is realized, the accumulated true strain is 1.6-2.4, and the final forging temperature is controlled to be 210-240 ℃. By adopting the combination of the temperature, the pass and the deformation, the recrystallized grains can be obviously refined, the magnesium alloy can be dynamically precipitated in the forging process, the dynamically precipitated second phase is fine and dispersed, and the forging piece is not fractured due to the over-low temperature. Through the control of the forging process, the Mg-Al-Ca magnesium alloy realizes the organic combination of recrystallization grain refinement and dynamic precipitation in the forging process, not only improves the mechanical property of the magnesium alloy, but also omits the aging process after deformation in the prior art and shortens the preparation flow.
The main advantages of the invention are: provides a forging process of a short-flow high-strength Mg-Al-Ca magnesium alloy forging. The traditional heat treatment and forging processes are organically integrated, and the large-size Mg-Al-Ca series alloy forging with high strength and high plasticity is successfully prepared. The process does not need a temperature rise and preservation link before forging, intermediate annealing is not needed in the forging process, and aging treatment is not needed after forging, so that the process flow is greatly shortened, the production efficiency is improved, the production cost is reduced, and the process is suitable for large-scale industrial production. Through a cooling forging process, a large number of spherical dynamic precipitated phases which are dispersed and distributed are generated while the grains of the Mg-Al-Ca magnesium alloy are refined, and the Mg-Al-Ca series alloy forging with excellent performance is obtained by utilizing the synergistic effect of fine grain strengthening, precipitation strengthening and work hardening.
Drawings
FIG. 1 is a scanning electron microscopy microstructure of the Mg-Al-Ca alloy forging of example 1;
FIG. 2 is an age hardness change curve for the Mg-Al-Ca alloy forging of example 1;
FIG. 3 is a scanning electron microscope microstructure of the Mg-Al-Ca alloy forging of comparative example 1;
FIG. 4 is a scanning electron microscope microstructure of the Mg-Al-Ca alloy forging of comparative example 2;
FIG. 5 is a scanning electron microscope microstructure of an aged Mg-Al-Ca alloy forging of comparative example 3;
FIG. 6 is a scanning electron microscope microstructure of an aged Mg-Al-Ca alloy forging of comparative example 4.
Detailed Description
According to the invention, a large number of comparison experiments are carried out by adjusting the forging process parameters. The invention is further illustrated by the following examples. The examples are for illustrating the present invention and not for limiting the present invention, and the modifications of the process of the present invention based on the idea of the present invention are within the protection scope of the present invention.
Example 1
Carrying out homogenizing annealing on a cubic ingot with the side length of 60mm, wherein the mass percentage content of the ingot is Mg-8.0Al-0.4Ca. The homogenizing annealing system is that the temperature is kept at 360 ℃ for 4h, then the temperature is raised to 415 ℃ for 26h, the temperature is cooled to 350 ℃, then drawing type cooling free forging is carried out on an oil press, the temperature of an upper chopping board and a lower chopping board is 334 ℃, and the pressing speed is 450mm/min. The total forging is carried out for 12 times, the true strain capacity of each pass is 0.2, the accumulated true strain is 2.4, the temperature of the forging is 240 ℃, the quenching treatment is carried out in water at 60 ℃ immediately after the forging, the room-temperature tensile mechanical properties of the component along the drawing direction (Z axis) are shown in a table 1, a scanning picture is shown in a figure 1, and the aging hardness change at 175 ℃ after the forging is shown in a figure 2.
Example 2: for a cubic ingot with the side length of 100mm, the mass percentage content of the ingot is Mg-7.5Al-0.3Ca.
The homogenizing annealing system comprises keeping the temperature at 320 deg.C for 6h, heating to 400 deg.C, keeping the temperature for 30h, air cooling to 355 deg.C, and performing drawing type cooling free forging on an oil press at 345 deg.C and a pressing speed of 400mm/min. The total forging is carried out for 16 times, the true strain capacity of each time is 0.1, the accumulated true strain is 1.6, the forging finishing temperature is 210 ℃, the quenching treatment is carried out in water at 45 ℃ immediately after the forging, and the room-temperature tensile mechanical properties of the member along the drawing direction (Z axis) are listed in Table 1.
Example 3: for a cubic ingot with the side length of 200mm, the mass percentage content of the ingot is Mg-9.0Al-0.5Ca.
The homogenizing annealing system comprises keeping the temperature at 350 deg.C for 6h, heating to 420 deg.C, keeping the temperature for 25h, air cooling to 345 deg.C, and performing drawing type cooling free forging on an oil press at the temperature of 350 deg.C for upper and lower chopping boards and the pressing speed of 500mm/min. The total forging is carried out for 14 times, the true strain capacity of each time is 0.15, the cumulative true strain is 2.1, the temperature of the forging end is 235 ℃, the quenching treatment is carried out in water at 50 ℃ immediately after the forging, and the room-temperature tensile mechanical properties of the component along the drawing direction (Z axis) are listed in table 1.
Comparative example 1: for a cubic ingot with the side length of 60mm, the mass percentage content of the ingot is Mg-8.0Al-0.4Ca. Keeping the temperature at 360 ℃ for 4h, heating to 415 ℃ for 26h, cooling to 350 ℃ in air, and performing drawing type cooling free forging on an oil press, wherein the temperature of an upper chopping board and a lower chopping board is 338 ℃, and the pressing speed is 450mm/min. The total forging is carried out for 4 times, the true strain quantity of each time is 0.2, the accumulated true strain is 0.8, the forging finishing temperature is 308 ℃, the quenching treatment is carried out in water at 60 ℃ immediately after the forging, the room-temperature tensile mechanical properties of the component along the drawing direction (Z axis) are listed in a table 1, and a scanning photograph shows that the component is shown in an attached figure 3.
Comparative example 2: for a cubic ingot with the side length of 100mm, the mass percentage content of the ingot is Mg-7.7Al-0.3Ca. The homogenizing annealing system comprises keeping the temperature at 320 deg.C for 6h, heating to 400 deg.C, keeping the temperature for 28h, cooling to 380 deg.C in air, and performing drawing type cooling free forging on an oil press at 352 deg.C for upper and lower chopping boards at a pressing speed of 400mm/min. The total forging is carried out for 16 times, the true strain quantity of each time is 0.1, the accumulated true strain is 1.6, the temperature of the final forging is 280 ℃, the quenching treatment is carried out in water at 45 ℃ immediately after the forging, the room-temperature tensile mechanical properties of the component along the drawing direction (Z axis) are listed in a table 1, and a scanning photograph shows that figure 4 is attached.
Comparative example 3: the forging in the comparative example 1 is subjected to aging treatment, the aging system is that the temperature is kept at 175 ℃ for 20h, the room-temperature tensile mechanical properties of the aged sample along the drawing direction (Z axis) are listed in Table 1, and the scanning photo shows that figure 5 is attached.
Comparative example 4: the forging of example 1 was aged by maintaining at 175 ℃ for 20 hours, the room temperature tensile mechanical properties of the aged samples along the elongation direction (Z axis) are shown in table 1, and the scanning photograph is shown in fig. 6.
TABLE 1 mechanical Properties of magnesium alloy structural members in examples and comparative examples
It can be seen from FIG. 1 that a large amount of spherical dynamic precipitates are dispersedly distributed after forging Mg-Al-Ca magnesium alloys, and it can be seen from Table 1 that the tensile mechanical properties after forging Mg-Al-Ca magnesium alloys of examples 1 to 3 are significantly better than those of comparative examples 1 to 4.
As can be seen from FIG. 2, the Mg-Al-Ca magnesium alloy of example 1, which was subjected to aging treatment after forging, did not improve its hardness, but rather decreased its hardness. In addition, in the case of combining example 1 and comparative example 4, the tensile mechanical properties of the Mg-Al-Ca magnesium alloy of example 1 were also degraded by aging after forging. FIG. 6 is a scanning photograph of the magnesium alloy of comparative example 4 after aging treatment, and the Mg-Al-Ca magnesium alloy of example 1 after forging did not precipitate a new age-precipitated phase and did not produce age hardening effect, but rather annihilated dislocations and coarsened dynamic precipitated phases occurred during aging, resulting in a decrease in strength. Obviously, the dispersed spherical dynamic precipitated phase formed by controlling the forging process is more beneficial to improving the mechanical property of the Mg-Al-Ca magnesium alloy. Therefore, by adopting the scheme of the embodiment 1-3 of the invention, the mechanical property of the Mg-Al-Ca magnesium alloy is improved, the aging treatment process after forging can be cancelled, the process flow is shortened, and the production efficiency is improved.
With reference to fig. 1 and 3, by comparing example 1 with comparative example 1, the forging pass is less, the accumulated strain amount is insufficient, and the effect of refining grains and generating dynamic precipitated phases of the Mg-Al-Ca magnesium alloy is difficult to achieve; as shown in FIG. 5, the Mg-Al-Ca magnesium alloy of comparative example 1, which was forged and then subjected to aging treatment, produced a large amount of acicular precipitates, which were disadvantageous in improving the tensile mechanical properties of the Mg-Al-Ca magnesium alloy, as compared to the spherical dynamic precipitates; meanwhile, by comparing example 2 and comparative example 2, as shown in fig. 4, the Mg-Al-Ca magnesium alloy of comparative example 2 has a high forging temperature (initial forging temperature and final forging temperature), although dynamic precipitation occurs, the distribution of precipitated phases is not uniform and discontinuous, which is not favorable for improving the tensile mechanical properties in a forged state.
The embodiments of the present invention are described above with reference to the drawings, and the embodiments and features of the embodiments of the present invention may be combined with each other without conflict. The present invention is not limited to the above-described embodiments, which are only illustrative and not restrictive, and those skilled in the art can make many modifications without departing from the spirit and scope of the invention as defined in the appended claims.
Claims (5)
1. A preparation process of a Mg-Al-Ca magnesium alloy forging is characterized by comprising the following steps: the Mg-Al-Ca magnesium alloy comprises the following components in percentage by mass: 7.5-9.0%, ca:0.3-0.5%, fe is less than or equal to 0.01%, ni is less than or equal to 0.0015%, be is less than or equal to 0.001%, and the balance is Mg, wherein the preparation process comprises the following steps:
A. processing Mg-Al-Ca magnesium alloy into a cubic ingot blank with the side length of 60-200 mm;
B. carrying out homogenization annealing treatment on the ingot blank, wherein the annealing process comprises the following steps: keeping the temperature at 320-360 ℃ for 4-6h, heating to 400-420 ℃ and keeping the temperature for 25-30h;
C. after the homogenization annealing treatment, taking out the ingot blank, air-cooling to the initial forging temperature of 340-360 ℃, carrying out drawing-length type cooling free forging on a hydraulic press, wherein the temperature of an upper chopping board and a lower chopping board is 300-350 ℃, the reduction speed is 400-500mm/min, the forging is carried out for 10-16 times, the annealing treatment is not carried out between two adjacent times, the true strain of each time is 0.1-0.2, the cumulative true strain is 1.6-2.4, and the final forging temperature is 210-240 ℃;
D. immediately quenching after forging, wherein the water temperature is 40-70 ℃.
2. A process for preparing a Mg-Al-Ca magnesium alloy forging as claimed in claim 1, wherein in step C, the surface temperature of the ingot in the initial forging pass is 345-355 ℃.
3. The process for preparing the Mg-Al-Ca magnesium alloy forging piece according to claim 1, wherein the drawing-out type cooling free forging of the step C comprises the following steps: any two groups of parallel surfaces of the cubic ingot blank are sequentially and alternately rotated by 90 degrees to be pressed, the other group of the remaining parallel surfaces are not forged all the time, and the ingot blank is continuously drawn out.
4. The process for preparing a Mg-Al-Ca magnesium alloy forging according to claim 1, wherein the surface temperature of the ingot blank at the last forging in step C is 210 to 235 ℃.
5. The preparation process of the Mg-Al-Ca magnesium alloy forging according to claim 1, wherein the room-temperature yield strength of the forging after quenching in the step D along the drawing direction is not less than 270MPa, the tensile strength is not less than 370MPa, and the elongation after fracture is not less than 6%.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2011099140A (en) * | 2009-11-05 | 2011-05-19 | National Institute Of Advanced Industrial Science & Technology | Magnesium alloy and method for producing the same |
| CN103786031A (en) * | 2014-01-18 | 2014-05-14 | 中南大学 | Process for forming moderately-strong heat-resisting magnesium alloy die-forged piece |
| CN105951012A (en) * | 2016-06-27 | 2016-09-21 | 湖南航天新材料技术研究院有限公司 | Variable-temperature forging strengthening process for low-alloyed magnesium alloy |
| CN107841696A (en) * | 2017-10-12 | 2018-03-27 | 中南大学 | A kind of preparation method of ultra-fine grained magnesium alloy |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103789583B (en) * | 2014-01-22 | 2016-06-08 | 北京科技大学 | Quick aging response type Al-Mg-Si-Cu-Zn system Alloy And Preparation Method |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2011099140A (en) * | 2009-11-05 | 2011-05-19 | National Institute Of Advanced Industrial Science & Technology | Magnesium alloy and method for producing the same |
| CN103786031A (en) * | 2014-01-18 | 2014-05-14 | 中南大学 | Process for forming moderately-strong heat-resisting magnesium alloy die-forged piece |
| CN105951012A (en) * | 2016-06-27 | 2016-09-21 | 湖南航天新材料技术研究院有限公司 | Variable-temperature forging strengthening process for low-alloyed magnesium alloy |
| CN107841696A (en) * | 2017-10-12 | 2018-03-27 | 中南大学 | A kind of preparation method of ultra-fine grained magnesium alloy |
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