CN111893409B - High-energy-absorption superfine crystal magnesium alloy and preparation method thereof - Google Patents

High-energy-absorption superfine crystal magnesium alloy and preparation method thereof Download PDF

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CN111893409B
CN111893409B CN202010776978.2A CN202010776978A CN111893409B CN 111893409 B CN111893409 B CN 111893409B CN 202010776978 A CN202010776978 A CN 202010776978A CN 111893409 B CN111893409 B CN 111893409B
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magnesium alloy
energy
absorption
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crystal
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CN111893409A (en
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杨续跃
张宇修
王春雨
霍庆欢
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Central South University
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Central South University
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    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22FCHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
    • C22F1/00Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
    • C22F1/06Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of magnesium or alloys based thereon
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B21MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
    • B21JFORGING; HAMMERING; PRESSING METAL; RIVETING; FORGE FURNACES
    • B21J5/00Methods for forging, hammering, or pressing; Special equipment or accessories therefor
    • B21J5/002Hybrid process, e.g. forging following casting
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C1/00Making non-ferrous alloys
    • C22C1/02Making non-ferrous alloys by melting
    • C22C1/03Making non-ferrous alloys by melting using master alloys
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C23/00Alloys based on magnesium
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C23/00Alloys based on magnesium
    • C22C23/04Alloys based on magnesium with zinc or cadmium as the next major constituent

Abstract

The invention provides a preparation method of a high-energy-absorption ultrafine-crystal magnesium alloy, which comprises the following steps: homogenizing the as-cast magnesium alloy to obtain homogenized magnesium alloy; forging the homogenized magnesium alloy at 440-530 ℃ to obtain a forged magnesium alloy; annealing the forged magnesium alloy to obtain an annealed magnesium alloy; extruding the annealed magnesium alloy at 100-150 ℃ to obtain the high-energy-absorption superfine crystal magnesium alloy; the high-energy-absorption superfine crystal magnesium alloy is Mg-Mn-RE magnesium alloy or Mg-Mn-Zn magnesium alloy; the sum of the mass percentages of Mn and RE/Zn in the high-energy-absorption superfine crystal magnesium alloy is not more than 2%. The invention designs the Mg-Mn-RE or Mg-Mn-Zn alloy with low alloying content, combines the high-temperature forging and low-temperature extrusion process, and utilizes the dynamic precipitation, dynamic recrystallization and grain boundary segregation and clustering behaviors of solid solution atoms in low-temperature forming to realize high energy absorption.

Description

High-energy-absorption superfine crystal magnesium alloy and preparation method thereof
Technical Field
The invention belongs to the technical field of magnesium alloy processing, and particularly relates to a high-energy-absorption superfine crystal magnesium alloy and a preparation method thereof.
Background
The magnesium alloy has the advantages of small density, high specific strength, excellent vibration damping performance, electromagnetic shielding performance, excellent machining performance and the like, and is an ideal material with light structure. The magnesium alloy extruded tube is an important bulk product form for producing deformed magnesium alloy structural members, can be widely applied to civil fields such as bicycles, wheelchairs, beach chairs, outdoor furniture, sports equipment and the like, and can also be widely applied to the fields such as aerospace, war industry and the like.
The impact absorption work of the magnesium alloy under high-speed impact load is generally represented by the area enclosed by the stress-strain curve of the magnesium alloy, and the greater the absorption work is, the stronger the energy absorption and impact load resistance of the magnesium alloy is. Therefore, the improvement of the room temperature plasticity by refining the grains is a key factor for effectively improving the energy absorption and impact damage resistance of the magnesium alloy. At present, the high-energy-absorption superfine crystal magnesium alloy is generally prepared by adopting severe plastic deformation processes such as equal-channel angular extrusion, high-pressure torsion, repeated creasing-straightening and the like, and due to the poor plastic deformation capability of the magnesium alloy, the severe plastic deformation process can cause the problems of uneven texture, strong deformation texture and the like of the magnesium alloy, so that the ductility of the material is reduced, and the energy absorption performance is further reduced. Therefore, the preparation method needs to be improved to improve the ductility of the superfine crystal magnesium alloy so as to realize high energy absorption of the magnesium alloy.
Disclosure of Invention
The invention aims to provide a high-energy-absorption superfine crystal magnesium alloy and a preparation method thereof. The high-energy-absorption ultrafine-crystal magnesium alloy prepared by the preparation method provided by the invention has high ductility and further has a high energy-absorption effect.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a preparation method of a high-energy-absorption ultrafine-crystal magnesium alloy, which comprises the following steps:
(1) homogenizing the as-cast magnesium alloy to obtain homogenized magnesium alloy;
(2) forging the homogenized magnesium alloy obtained in the step (1) at 440-530 ℃ to obtain a forged magnesium alloy;
(3) annealing the forged magnesium alloy obtained in the step (2) to obtain an annealed magnesium alloy;
(4) extruding the annealed magnesium alloy obtained in the step (3) at 100-150 ℃ to obtain the high-energy-absorption superfine crystal magnesium alloy;
the high-energy-absorption superfine crystal magnesium alloy is Mg-Mn-RE magnesium alloy or Mg-Mn-Zn magnesium alloy; the sum of the mass percentages of Mn and RE/Zn in the high-energy-absorption superfine crystal magnesium alloy is not more than 2%.
Preferably, the RE comprises at least one of Ce and Nd.
Preferably, the mass content of Mn in the high-energy-absorption ultrafine-crystal magnesium alloy is not more than 1%.
Preferably, the temperature of the homogenization treatment in the step (1) is 440-520 ℃, and the time of the homogenization treatment is 10-24 h.
Preferably, the total deformation amount of the forging in the step (2) is 20-40%.
Preferably, the temperature for forging in the step (2) is 460-510 ℃.
Preferably, the annealing temperature in the step (3) is 400-460 ℃, and the annealing time is 1-3 h.
Preferably, the extrusion ratio of the extrusion in the step (4) is 20: 1-25: 1.
preferably, the extrusion speed in the step (4) is 10-30 mm/s.
The invention also provides the high-energy-absorption superfine crystal magnesium alloy prepared by the preparation method in the technical scheme.
The invention provides a preparation method of a high-energy-absorption ultrafine-crystal magnesium alloy, which comprises the following steps: homogenizing the as-cast magnesium alloy to obtain homogenized magnesium alloy; forging the homogenized magnesium alloy at 440-530 ℃ to obtain a forged magnesium alloy; annealing the forged magnesium alloy to obtain an annealed magnesium alloy; extruding the annealed magnesium alloy at 100-150 ℃ to obtain the high-energy-absorption superfine crystal magnesium alloy; the high-energy-absorption superfine crystal magnesium alloy is Mg-Mn-RE magnesium alloy or Mg-Mn-Zn magnesium alloy; the sum of the mass percentages of Mn and RE/Zn in the high-energy-absorption superfine crystal magnesium alloy is not more than 2%. The invention designs the Mg-Mn-RE or Mg-Mn-Zn alloy with low alloying element content by components, and combines high-temperature forging to eliminate casting defects, component segregation, second phase and the like in an as-cast structure, homogenize the structure, and effectively improve the dynamic recrystallization nucleation rate and dynamic precipitation during low-temperature extrusion; then annealing treatment is carried out to eliminate internal stress, and finally low-temperature extrusion is carried out, because the solid solution amounts of Mn, RE and Zn in the Mg matrix are all in a supersaturated state, a large amount of second phases containing Mn, RE and Zn can be dynamically precipitated from a supersaturated solution in the extrusion deformation process, so that more nucleation points are provided for dynamic recrystallization, the recrystallization degree is improved, the grain boundary can be pinned, the grain boundary movement is hindered, the growth of recrystallized grains is inhibited, and an ultrafine crystal structure with uniform grains is obtained; the trace RE/Zn element can promote the segregation or cluster copolymerization of Mn solid solution atoms on a crystal boundary, thereby coordinating the sliding or rotation of the crystal boundary, improving the ductility of the magnesium alloy at room temperature, fundamentally solving the problems of finer crystal grains and poorer ductility, and finally preparing the high-energy-absorption superfine crystal magnesium alloy. The results of the embodiment show that the grains of the magnesium alloy prepared by the preparation method provided by the invention are refined to 1-3 mu m, and the ductility at room temperature reaches 40-50%; compared with the common AZ31 magnesium alloy, the absorption work of the impact test is improved by 3-5 times.
Drawings
FIG. 1 is a process flow diagram of a preparation method of the high energy absorption ultrafine crystal magnesium alloy;
FIG. 2 is a graph showing the variation of solid solubility of solid-solutionizing elements in the magnesium alloy of the present invention with extrusion temperature.
Detailed Description
The invention provides a preparation method of a high-energy-absorption ultrafine-crystal magnesium alloy, which comprises the following steps:
(1) homogenizing the as-cast magnesium alloy to obtain homogenized magnesium alloy;
(2) forging the homogenized magnesium alloy obtained in the step (1) at 440-530 ℃ to obtain a forged magnesium alloy;
(3) annealing the forged magnesium alloy obtained in the step (2) to obtain an annealed magnesium alloy;
(4) extruding the annealed magnesium alloy obtained in the step (3) at 100-150 ℃ to obtain the high-energy-absorption superfine crystal magnesium alloy;
the high-energy-absorption superfine crystal magnesium alloy is Mg-Mn-RE magnesium alloy or Mg-Mn-Zn magnesium alloy; the sum of the mass percentages of Mn and RE/Zn in the high-energy-absorption superfine crystal magnesium alloy is not more than 2%.
In the invention, the high-energy-absorption ultrafine-crystal magnesium alloy is an Mg-Mn-RE magnesium alloy or an Mg-Mn-Zn magnesium alloy. In the present invention, the RE includes at least one of Ce and Nd.
In the invention, the sum of the mass percentages of Mn and RE/Zn in the high-energy-absorption ultrafine-crystal magnesium alloy is not more than 2%, preferably 1-2%, and more preferably 1.4-1.8%. In the invention, the mass content of Mn in the high-energy-absorption ultrafine-crystal magnesium alloy is preferably not more than 1%, and more preferably 0.5-0.9%. In the invention, the RE/Zn mass content in the high-energy-absorption ultrafine-crystal magnesium alloy is preferably not more than 1%, and more preferably 0.5-0.9%. In the invention, trace RE/Zn element can promote Mn solid solution atoms to be partially aggregated or cluster copolymerized on a grain boundary, thereby coordinating the sliding of the grain boundary or the rotation of crystal grains, improving the room temperature ductility of the high-energy-absorption superfine crystal magnesium alloy, fundamentally solving the problems of finer crystal grains and poorer ductility and further preparing the high-ductility high-energy-absorption superfine crystal magnesium alloy.
The cast magnesium alloy is homogenized to obtain homogenized magnesium alloy. In the invention, the homogenization treatment can dissolve the alloy phase, eliminate dendrite segregation, make the components in the magnesium alloy uniform and is beneficial to material processing and molding.
In the invention, the components of the as-cast magnesium alloy are the same as those of the high-energy-absorption ultrafine-crystal magnesium alloy.
In the present invention, the as-cast magnesium alloy is preferably prepared by the following operations: smelting by taking pure Mg, Mg-Mn intermediate alloy and Mg-RE intermediate alloy/pure Zn as raw materials to obtain a melt; and cooling the melt to the casting temperature for semi-continuous casting to obtain the as-cast magnesium alloy.
The invention uses pure Mg, Mg-Mn intermediate alloy and Mg-RE intermediate alloy/pure Zn as raw materials to carry out smelting, thus obtaining the melt. In the present invention, the temperature of the melting is preferably 720 to 740 ℃, more preferably 725 to 730 ℃. In the present invention, the melting is preferably performed under a protective atmosphere. The gas of the protective atmosphere is not particularly limited in the present invention, and a protective gas known to those skilled in the art may be used. The sources of the pure Mg, the Mg-Mn intermediate alloy, the Mg-RE intermediate alloy and the pure Zn are not particularly limited in the invention, and the commercially available products well known to those skilled in the art can be adopted.
In the present invention, the smelting preferably includes: pure Mg is heated and melted, and then Mg-Mn intermediate alloy and Mg-RE intermediate alloy/pure Zn are added in sequence.
After obtaining the melt, the invention preferably cools the melt to the casting temperature for semi-continuous casting to obtain the as-cast magnesium alloy. In the present invention, the casting temperature is preferably 700 ℃. In the present invention, the electromagnetic frequency of the semi-continuous casting is preferably 40Hz to 45Hz, more preferably 42Hz to 44 Hz; the casting speed of the semi-continuous casting is preferably 150 mm/min-200 mm/min, and more preferably 160 mm/min-180 mm/min; the preferable cooling water amount of the semi-continuous casting is 10-20 m3More preferably 16 to 18 m/h3H is used as the reference value. In the invention, the semi-continuous casting has high crystallization speed, can improve the intragranular structure of the cast ingot, reduce the regional segregation of chemical components and improve the mechanical property of the cast ingot; the metal casting system is improved, the oxide inclusions and metal impurities are reduced, and the purity of the metal is improved; the compactness of the cast ingot is improved, and the looseness of the central part of the cast ingot is reduced.
In the invention, the temperature of the homogenization treatment is preferably 440-520 ℃, and more preferably 460-500 ℃; the time for the homogenization treatment is preferably 10 to 24 hours, and more preferably 15 to 20 hours. In the invention, when the temperature and time of the homogenization treatment are in the above ranges, the dendrite segregation can be further eliminated, the uniformity degree of the magnesium alloy components is improved, and the processing and molding of the material are further facilitated.
After obtaining the homogenized magnesium alloy, forging the homogenized magnesium alloy at 440-530 ℃ to obtain a forged magnesium alloy. In the invention, the forging temperature is preferably 460-510 ℃, and more preferably 480-500 ℃. In the present invention, the forging preferably employs a single pass deformation; the total deformation amount of the forging is preferably 20-40%, and more preferably 30-35%. In the invention, the homogenized magnesium alloy is forged at high temperature, so that the casting defects, component segregation and secondary equinox in an as-cast structure can be eliminated, the structure is homogenized, and the dynamic recrystallization nucleation rate and dynamic precipitation during low-temperature extrusion are improved, thereby improving the recrystallization degree and obtaining an ultrafine grain structure with uniform grains.
After obtaining the forged magnesium alloy, annealing the forged magnesium alloy to obtain the annealed magnesium alloy. In the invention, the annealing temperature is preferably 400-460 ℃, more preferably 430-450 ℃, and even more preferably 440 ℃. In the invention, the annealing time is preferably 1-3 h, and more preferably 1.5-2 h. According to the invention, the annealing treatment of the forged magnesium alloy can eliminate the internal stress generated in high-temperature forging, and avoid influencing the performance of the magnesium alloy.
After the annealed magnesium alloy is obtained, extruding the annealed magnesium alloy at 100-150 ℃ to obtain the high-energy-absorption superfine crystal magnesium alloy. In the invention, the extrusion temperature is preferably 120-140 ℃, and more preferably 130 ℃. In the present invention, the extrusion ratio of the extrusion is preferably 20: 1-25: 1, more preferably 22: 1-24: 1. in the present invention, the extrusion is preferably a single-pass extrusion. In the invention, the extrusion speed is preferably 10-30 mm/s, and more preferably 15-25 mm/s. In the invention, the extrusion speed is in the range, so that the annealed magnesium alloy can generate higher deformation heat in a shorter time to perform more sufficient dynamic recrystallization, the structure uniformity is better, the elongation is higher, and the internal stress is reduced continuously. In the invention, the solid solution amounts of Mn, RE and Zn in the Mg matrix are all in a supersaturated state, a large amount of second phases containing Mn, RE and Zn can be dynamically precipitated from the supersaturated solid solution in the low-temperature extrusion deformation process, more nucleation points are provided for dynamic recrystallization, the recrystallization degree is improved, grain boundaries can be pinned, the movement of the grain boundaries is hindered, the growth of recrystallized grains is inhibited, and an ultrafine crystal structure with uniform grains is obtained.
In the invention, the process flow diagram of the preparation method of the high-energy-absorption ultrafine-crystal magnesium alloy is shown in fig. 1, and the cast magnesium alloy is subjected to homogenization treatment, high-temperature forging, annealing treatment and low-temperature extrusion in sequence to obtain the high-energy-absorption ultrafine-crystal magnesium alloy.
The invention designs the Mg-Mn-RE or Mg-Mn-Zn alloy with low alloying element content by components, and combines high-temperature forging to eliminate casting defects, component segregation, second phase and the like in an as-cast structure, homogenize the structure, and effectively improve the dynamic recrystallization nucleation rate and dynamic precipitation during low-temperature extrusion; then annealing treatment is carried out to eliminate internal stress, and finally low-temperature extrusion is carried out, while the solid solubility of solid solution elements such as Mn, RE and Zn in the magnesium alloy is obviously reduced along with the reduction of temperature (as shown in figure 2, and figure 2 is a change curve of the solid solubility of the solid solution elements in the magnesium alloy along with the extrusion temperature), because the solid solubility of Mn, RE and Zn in the Mg matrix is in a supersaturated state, a large amount of second phases containing Mn, RE and Zn can be dynamically precipitated from a supersaturated solid solution in the extrusion deformation process, not only more nucleation points are provided for dynamic recrystallization, thereby improving the recrystallization degree, but also grain boundary pinning, hindering the movement of the grain boundary and inhibiting the growth of recrystallized grains, and an ultrafine crystal structure with uniform grains is obtained; the trace RE/Zn element can promote the segregation or cluster copolymerization of Mn solid solution atoms on a crystal boundary, thereby coordinating the sliding or the rotation of the crystal grain boundary, improving the room temperature ductility of the high-energy-absorption superfine crystal magnesium alloy, fundamentally solving the problems of finer crystal grains and poorer ductility, and finally preparing the high-energy-absorption superfine crystal magnesium alloy.
The preparation method provided by the invention can be used for preparing the Mg-Mn-RE magnesium alloy or the Mg-Mn-Zn magnesium alloy, and has the advantages of wide application range and low requirement on equipment; and the magnesium alloy mainly contains a relatively cheap Mn element, and rare earth element/non-rare earth element Zn is added in a trace amount, so that the effects of purifying a melt and improving the toughness are achieved, and the light advantage of the magnesium alloy is damaged very little.
The preparation method provided by the invention improves the plastic deformation capacity of the magnesium alloy by utilizing high-temperature forging cogging, avoids deformation damage in the low-temperature extrusion process, can prepare the ultrafine-crystal magnesium alloy, improves the ductility, and solves the technical problem of contradiction between grain refinement and ductility reduction; the preparation method has the advantages of reasonable process, simple process and low cost, can be used for preparing long magnesium alloys and large magnesium alloys, widens the industrial application of the magnesium alloys, and has good application prospects in the fields of aerospace, rail transit and the like.
The invention also provides the high-energy-absorption superfine crystal magnesium alloy prepared by the preparation method in the technical scheme.
The high-energy-absorption ultrafine-crystal magnesium alloy provided by the invention not only realizes grain refinement, but also has high ductility, and solves the technical problem of contradiction between grain refinement and ductility reduction.
The technical solution of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. It is to be understood that the described embodiments are merely exemplary of the invention, and not restrictive of the full scope of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
The method comprises the following steps: heating a pure magnesium ingot to 720 ℃ in a protective gas atmosphere for melting, sequentially adding an Mg-Mn intermediate alloy, finally adding an Mg-Ce intermediate alloy, cooling the melt to 700 ℃ for semi-continuous casting to obtain an as-cast magnesium alloy Mg-0.9Mn-0.5Ce, wherein the electromagnetic frequency is 40Hz, the casting speed is 160mm/min, and the cooling water amount is 16m3/h;
Step two: homogenizing the as-cast magnesium alloy obtained in the step one at 500 ℃ for 24h to obtain homogenized magnesium alloy:
step three: forging the homogenized magnesium alloy obtained in the second step at 500 ℃ to obtain a forged magnesium alloy, wherein the forging is single-pass deformation, and the total deformation is 35%;
step four: annealing the forged magnesium alloy obtained in the third step at 430 ℃ for 1h to obtain an annealed magnesium alloy;
step five: extruding the annealed magnesium alloy obtained in the fourth step at 120 ℃, wherein the extrusion is performed in a single pass, and the extrusion ratio is 24: 1, the extrusion speed is 15mm/s, and the high-energy-absorption superfine crystal magnesium alloy with the grain size of 3 mu m is obtained.
Room temperature compression and impact test are carried out on the high energy absorption superfine crystal magnesium alloy, and the room temperature compression and the high speed impact strain rate are respectively 3 multiplied by 10-3s-1And 1X 103s-1The room temperature elongation of Mg-0.9Mn-0.5Ce magnesium alloy reaches 40%, and the absorption power of an impact test is improved by 3 times compared with that of the common AZ31 magnesium alloy。
Example 2
The method comprises the following steps: heating a pure magnesium ingot to 730 ℃ in a protective gas atmosphere for melting, sequentially adding Mg-Mn intermediate alloy and Mg-Nd intermediate alloy, cooling the melt to 700 ℃ for semi-continuous casting to obtain the as-cast magnesium alloy Mg-0.9Mn-0.5Nd, wherein the electromagnetic frequency is 45Hz, the casting speed is 180mm/min, and the cooling water amount is 16m3/h;
Step two: homogenizing the cast magnesium alloy obtained in the step one at 520 ℃ for 24 hours to obtain homogenized magnesium alloy:
step three: forging the homogenized magnesium alloy obtained in the second step at 500 ℃ to obtain a forged magnesium alloy, wherein the forging is single-pass deformation, and the total deformation is 40%;
step four: annealing the forged magnesium alloy obtained in the third step at 430 ℃ for 1.5h to obtain an annealed magnesium alloy;
step five: extruding the annealed magnesium alloy obtained in the fourth step at 120 ℃, wherein the extrusion is performed in a single pass, and the extrusion ratio is 22: 1, the extrusion speed is 15mm/s, and the high-energy-absorption superfine crystal magnesium alloy with the grain size of 1 mu m is obtained.
Room temperature compression and impact test are carried out on the high energy absorption superfine crystal magnesium alloy, and the room temperature compression and the high speed impact strain rate are respectively 3 multiplied by 10-3s-1And 1X 103s-1The room-temperature elongation of the Mg-0.9Mn-0.5Nd magnesium alloy reaches 47%, and the absorption work of an impact test is improved by 3.5 times compared with that of the common AZ31 magnesium alloy.
Example 3
The method comprises the following steps: heating a pure magnesium ingot to 730 ℃ in a protective gas atmosphere for melting, sequentially adding Mg-Mn intermediate alloy and Mg-Nd intermediate alloy, cooling the melt to 700 ℃ for semi-continuous casting to obtain the as-cast magnesium alloy Mg-0.9Mn-0.9Nd, wherein the electromagnetic frequency is 45Hz, the casting speed is 180mm/min, and the cooling water amount is 16m3/h;
Step two: homogenizing the cast magnesium alloy obtained in the step one at 520 ℃ for 24 hours to obtain homogenized magnesium alloy:
step three: forging the homogenized magnesium alloy obtained in the second step at 510 ℃ to obtain a forged magnesium alloy, wherein the forging is single-pass deformation, and the total deformation is 35%;
step four: annealing the forged magnesium alloy obtained in the third step at 450 ℃ for 2h to obtain an annealed magnesium alloy;
step five: extruding the annealed magnesium alloy obtained in the fourth step at 130 ℃, wherein the extrusion is performed in a single pass, and the extrusion ratio is 22: 1, the extrusion speed is 15mm/s, and the high-energy-absorption superfine crystal magnesium alloy with the grain size of 2 mu m is obtained.
Room temperature compression and impact test are carried out on the high energy absorption superfine crystal magnesium alloy, and the room temperature compression and the high speed impact strain rate are respectively 3 multiplied by 10-3s-1And 1X 103s-1The room-temperature elongation of the Mg-0.9Mn-0.9Nd magnesium alloy reaches 45%, and the absorption work of an impact test is improved by 4 times compared with that of the common AZ31 magnesium alloy.
Example 4
The method comprises the following steps: heating a pure magnesium ingot to 720 ℃ in a protective gas atmosphere for melting, sequentially adding Mg-Mn intermediate alloy and pure Zn ingot, cooling the melt to 700 ℃ for semi-continuous casting to obtain as-cast magnesium alloy Mg-0.9Mn-0.5Zn, wherein the electromagnetic frequency is 40Hz, the casting speed is 160mm/min, and the cooling water amount is 16m3/h;
Step two: homogenizing the as-cast magnesium alloy obtained in the step one at 460 ℃ for 24h to obtain homogenized magnesium alloy:
step three: forging the homogenized magnesium alloy obtained in the second step at 460 ℃ to obtain a forged magnesium alloy, wherein the forging is single-pass deformation, and the total deformation is 35%;
step four: annealing the forged magnesium alloy obtained in the third step at 400 ℃ for 2h to obtain an annealed magnesium alloy;
step five: extruding the annealed magnesium alloy obtained in the fourth step at 100 ℃, wherein the extrusion is performed in a single pass, and the extrusion ratio is 24: 1, the extrusion speed is 15mm/s, and the high-energy-absorption superfine crystal magnesium alloy with the grain size of 1 mu m is obtained.
Room temperature compression and impact test are carried out on the high energy absorption superfine crystal magnesium alloy, and the room temperature compression and the high speed impact strain rate are respectively 3 multiplied by 10-3s-1And 1X 103s-1The room temperature elongation of the Mg-0.9Mn-0.5Zn magnesium alloy reaches 50%, and the absorption power of an impact test is improved by 5 times compared with that of the common AZ31 magnesium alloy.
Example 5
The method comprises the following steps: heating a pure magnesium ingot to 720 ℃ in a protective gas atmosphere for melting, sequentially adding Mg-Mn intermediate alloy, finally adding pure Zn ingot, cooling the melt to 700 ℃ for semi-continuous casting to obtain as-cast magnesium alloy Mg-0.9Mn-0.9Zn, wherein the electromagnetic frequency is 40Hz, the casting speed is 160mm/min, and the cooling water amount is 16m3/h;
Step two: homogenizing the as-cast magnesium alloy obtained in the step one at 440 ℃ for 24h to obtain homogenized magnesium alloy:
step three: forging the homogenized magnesium alloy obtained in the second step at 440 ℃ to obtain a forged magnesium alloy, wherein the forging is single-pass deformation, and the total deformation is 35%;
step four: annealing the forged magnesium alloy obtained in the third step at 400 ℃ for 1.5h to obtain an annealed magnesium alloy;
step five: extruding the annealed magnesium alloy obtained in the fourth step at 100 ℃, wherein the extrusion is performed in a single pass, and the extrusion ratio is 24: 1, the extrusion speed is 15mm/s, and the high-energy-absorption superfine crystal magnesium alloy with the grain size of 1.5 mu m is obtained.
Room temperature compression and impact test are carried out on the high energy absorption superfine crystal magnesium alloy, and the room temperature compression and the high speed impact strain rate are respectively 3 multiplied by 10-3s-1And 1X 103s-1The room temperature elongation of the Mg-0.9Mn-0.9Zn magnesium alloy reaches 48%, and the absorption power of an impact test is improved by 4 times compared with that of the common AZ31 magnesium alloy.
From the examples 1-5, the crystal grains of the magnesium alloy prepared by the preparation method provided by the invention are refined to 1-3 μm, and the ductility at room temperature reaches 40-50%; compared with the common AZ31 magnesium alloy, the absorption power of the impact test is improved by 3-5 times, which shows that the high-energy-absorption superfine crystal magnesium alloy prepared by the preparation method provided by the invention has high ductility.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.

Claims (9)

1. A preparation method of a high-energy-absorption superfine crystal magnesium alloy comprises the following steps:
(1) homogenizing the as-cast magnesium alloy to obtain homogenized magnesium alloy;
(2) forging the homogenized magnesium alloy obtained in the step (1) at 440-530 ℃ to obtain a forged magnesium alloy;
(3) annealing the forged magnesium alloy obtained in the step (2) to obtain an annealed magnesium alloy;
(4) extruding the annealed magnesium alloy obtained in the step (3) at 100-150 ℃ to obtain the high-energy-absorption superfine crystal magnesium alloy;
the high-energy-absorption superfine crystal magnesium alloy is Mg-Mn-RE magnesium alloy or Mg-Mn-Zn magnesium alloy; the sum of the mass percentages of Mn and RE/Zn in the high-energy-absorption superfine crystal magnesium alloy is not more than 2%;
the temperature of the homogenization treatment in the step (1) is 440-520 ℃, and the time of the homogenization treatment is 10-24 h;
and (3) forging in the step (2) adopts single-pass deformation.
2. The production method according to claim 1, wherein the RE includes at least one of Ce and Nd.
3. The preparation method according to claim 1, wherein the mass content of Mn in the high-energy-absorption ultrafine-crystal magnesium alloy is not more than 1%.
4. The method according to claim 1, wherein the total deformation amount of the forging in the step (2) is 20 to 40%.
5. The production method according to claim 1 or 4, wherein the temperature of forging in the step (2) is 460 to 510 ℃.
6. The preparation method according to claim 1, wherein the annealing temperature in the step (3) is 400-460 ℃ and the annealing time is 1-3 h.
7. The production method according to claim 1, wherein the extrusion ratio in the step (4) is 20: 1-25: 1.
8. the method according to claim 1 or 7, wherein the extrusion speed in the step (4) is 10 to 30 mm/s.
9. The high-energy-absorption ultrafine-crystal magnesium alloy prepared by the preparation method of any one of claims 1 to 8.
CN202010776978.2A 2020-08-05 2020-08-05 High-energy-absorption superfine crystal magnesium alloy and preparation method thereof Active CN111893409B (en)

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CN115011824B (en) * 2022-06-30 2023-05-23 中南大学 High-strength and high-creep-resistance magnesium alloy and preparation method and application thereof

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