CN110468317A - Magnesium alloy and preparation method thereof with excellent temperature-room type plasticity - Google Patents

Magnesium alloy and preparation method thereof with excellent temperature-room type plasticity Download PDF

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CN110468317A
CN110468317A CN201910433326.6A CN201910433326A CN110468317A CN 110468317 A CN110468317 A CN 110468317A CN 201910433326 A CN201910433326 A CN 201910433326A CN 110468317 A CN110468317 A CN 110468317A
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magnesium alloy
temperature
alloy
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CN110468317B (en
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钱亚锋
赵言辉
方明
赵建峰
孙志阳
吴洋
苏晓华
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National Quality Supervision And Inspection Center For Magnesium And Magnesium Alloys
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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
    • 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
    • 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
    • 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 present invention provides a kind of magnesium alloy with excellent temperature-room type plasticity, it is characterized in that, the magnesium alloy is Mg-Bi-Gd-Mn magnesium alloy, its component is by weight percentage are as follows: Bi 1~3%, Gd 1.5~4%, Gd >=1.5%, Mn 0.05~0.15%, surplus is Mg, and wherein Bi/Gd content ratio is 0.25~2.Elongation percentage can achieve 40% or more to the alloy at room temperature, show excellent temperature-room type plasticity, be a kind of magnesium alloy materials that potentially can be used for further temperature-room type plasticity processing or the processing of superplastic forming technology；In addition, the alloy shows excellent flame retardant property in casting and heat treatment process.

Description

Magnesium alloy and preparation method thereof with excellent temperature-room type plasticity
Technical field
The present invention relates to metal material and metal material processing field more particularly to a kind of magnesium with excellent temperature-room type plasticity Alloy and preparation method thereof.
Background technique
The energy, material and information are three big pillars of human social development.With the consumption that is becoming tight the day of the resources such as iron ore, And energy-saving and emission-reduction situation is increasingly serious, developing and utilizing resourceful mg-based material is inexorable trend.In metal material In, magnesium density is about 1.74g/cm3, it is the 2/3 of aluminium alloy, the 1/4 of steel, magnesium alloy has density small, specific strength, specific stiffness Higher, effectiveness is good, and damping shock absorption is good, is easy the series of advantages such as recycling and reusing, is known as " 21st century Green metal engineering material " has wide application in fields such as aerospace, weaponry, telecommunications and communications and transportation Prospect.But absolute intensity is lower, and corrosion resistance is poor, and the reasons such as room temperature forming capacity difference greatly limit magnesium and its alloy as novel The application of green material.
In terms of high-temperature-room type plasticity magnesium alloy exploitation, since the crystal structure of magnesium and its most alloys is solid matter six Square, predominantly basal slip, slip system cause its plasticity bad less under the conditions of low temperature (220 DEG C of <), and are easily squeezing or rolling Fibrous texture or plate texture are formed in the process, and the further plastic deformation ability of alloy is made to be deteriorated.Only cylinder at relatively high temperatures Sliding and conical surface slip system can start, and improve the plasticity of magnesium alloy.But magnesium temperature is too high, and to often lead to magnesium alloy crystal grain thick Change, is degrading the mechanical property (intensity) of alloy, while improving alloy processing cost.Have under exploitation room temperature or lower temperature The magnesium alloy of superior plasticity ability is advantageously implemented the plastic processing of magnesium alloy at low temperature or even at room temperature, enhances product performance Quality, while the costs such as energy consumption for reducing production are greatly facilitated magnesium and its alloy as novel green material and hand in automobile, track The extensive use in the fields such as logical, aviation.Therefore, the magnesium alloy of high-temperature-room type plasticity is developed for further deforming by cold plasticity Magnesium alloy strength is improved, and then the application field for expanding magnesium alloy is of great significance.
In recent years, with being increasingly urgent to transport facility lightweight requirements, have a lot of research work and pass through respectively Kind of method prepares high-temperature-room type plasticity magnesium alloy, gradually has some high-temperature-room type plasticity magnesium alloys to developed successively both at home and abroad.
Patent document 1 (publication number: CN102061414A) discloses a kind of high plastic magnesium alloy and preparation method thereof, at Be divided into: Al:0.5-2%, Mn:2%, Ca:0.02-0.1%, surplus are magnesium, and room temperature elongation percentage can achieve 25%.The alloy Cost is relatively low, but elongation percentage is still relatively low.
Patent document 2 (publication number: CN101381831A) discloses a kind of high plastic magnesium alloy, magnesium, zinc, zirconium in the alloy Ratio be respectively 80-83%, 12-15%, 2-8%, and account for Li that mass ratio is 23-27%, account for total mass ratio 7-9%'s Manganese, the yttrium for accounting for total mass ratio 4-6%.By melting, heat treatment and extruding, Alloy At Room Temperature elongation percentage 42-49 is made.But in alloy There is a large amount of Li, fusion process needs first to vacuumize or the protection of logical argon gas, needs strict control oxygen content.Another aspect alloy In have a large amount of Y rare earth element and Li, cause the raising of cost of alloy.
Patent document 3 (publication number: CN102925771A) discloses a kind of High-room-temperaturductility ductility magnesium alloy material and its preparation Method: Li 1.0-5.0% by mass percentage, Al 2.5-3.5%, Zn 0.7-1.3%, Mn 0.2-0.5%, impurity≤ 0.3%, magnesium surplus.Pass through pure lithium and AZ31 magnesium alloy melting system under conditions of vacuumizing and being passed through inert gas that will be formulated , elongation percentage is between 14-31% under gained Alloy At Room Temperature.Alloy smelting process is complicated, and whole room temperature elongation percentage is still inclined It is low.
The related invention of these existing related high-temperature-room type plasticities, possessed temperature-room type plasticity is still relatively low, is preferably full Sufficient consumer electronics, automobile and other industries are to high-strength magnesium alloy low cost, easy processing, high performance requirement, and there is an urgent need to develop energy out The magnesium alloy materials with excellent temperature-room type plasticity enough are prepared with simple process of manufacture, this also will greatly expand magnesium Alloy has great economy and society meaning in the following further popularization and application.
Summary of the invention
The purpose of the present invention is being directed to this low main problem of existing magnesium alloy temperature-room type plasticity, provide a kind of with excellent room Warm plasticity has both novel magnesium alloy of excellent fire-retardancy and preparation method thereof simultaneously.The alloy is a kind of Mg-Bi-Gd-Mn conjunction Gold, in this alloy system, with extremely simple manufacturing process, so that it may the excellent wrought magnesium alloy of temperature-room type plasticity is obtained, Room temperature elongation percentage reaches 50% or more, while having excellent flame retardant property.
One aspect of the present invention, provides a kind of magnesium alloy with excellent temperature-room type plasticity, which is Mg-Bi-Gd- Mn magnesium alloy, component is by weight percentage are as follows: Bi 1~3%, Gd 1.5~4%, Gd >=1.5%, Mn 0.05~ 0.15%, surplus Mg, wherein Bi/Gd content ratio is 0.25~2.
Another aspect of the present invention provides a kind of preparation method of magnesium alloy with excellent temperature-room type plasticity, the preparation Method the following steps are included:
1) it ingredient: using pure Mg ingot, pure Bi block, Mg-Gd intermediate alloy and Mg-Mn intermediate alloy as raw material, is wanted according to right The weight percent of each component of magnesium alloy described in asking 1 carries out ingredient；
2) melting: 700~730 DEG C of furnace temperature of setting puts the pure Mg ingot of preheating when furnace temperature is warming up to set temperature Enter in the crucible of smelting furnace, after its fusing, the Mg-Gd intermediate alloy of the pure Bi block of preheating and preheating is added to magnesium respectively and is melted In liquid；Then smelting temperature is increased to 750~760 DEG C, and keeps the temperature 5~15 minutes, is then stirred 3~10 minutes, is stood 3~10 Minute, Mg-Mn intermediate alloy is added, and keep the temperature 5~15 minutes, then stirs 3~10 minutes, furnace temperature is reduced to 740~750 DEG C, 3~10 minutes are stood, is passed through argon gas 1~3 minute and carries out refining degassing processing；Stand 3~10 minutes；
3) it casts: the magnesium alloy fused mass after melting is cast in corresponding mold, as-cast magnesium alloy is made；
4) it is heat-treated: solution heat treatment is carried out to as-cast magnesium alloy obtained in step 3), wherein heat treatment temperature is 470 ~510 DEG C, the time is 7~12 hours；
5) ingot casting after solution treatment in step 4) is cut into corresponding blank and removed the peel；
6) extrusion process: temperature is squeezed needed for the blank that step 5) obtains is heated within 30 minutes, is put into extruding In cylinder, extrusion deformation processing is carried out, extrusion deformation speed is 0.1~20m/min, and extrusion ratio is 10~40, and squeezing temperature is 270 ~450 DEG C, finally obtain the Mg-Bi-Gd-Mn wrought magnesium alloy.
Preferably, the preparation method of high-toughness casting magnesium alloy according to the present invention, the Mg-Gd intermediate alloy are Mg-30Gd intermediate alloy；
Preferably, the preparation method of high-toughness casting magnesium alloy according to the present invention, the Mg-Mn intermediate alloy are Mg-5Mn intermediate alloy.
Preferably, the preparation method of high-toughness casting magnesium alloy according to the present invention, the CO2/SF6 mixed gas group At preferably volume ratio CO2: SF6=100: 1.
Preferably, the preparation method of high-toughness casting magnesium alloy according to the present invention, in step 2), the pure Mg ingot Preheating temperature is 200~300 DEG C, and the preheating temperature of the pure Bi block is 50~70 DEG C, the preheating temperature of the Mg-Gd intermediate alloy Degree is 200~300 DEG C.
Preferably, the preparation method of high-toughness casting magnesium alloy according to the present invention, the fusion process in step 2) be CO2/SF6Mixed gas protected lower progress.
Preferably, the preparation method of high-toughness casting magnesium alloy according to the present invention, the heat treatment of step 4) further include: use 40~80 DEG C of warm water are quenched.
Preferably, the preparation method of high-toughness casting magnesium alloy according to the present invention, the entire heat treatment process of step 4) It is not necessarily to gas shield.
Preferably, the casting process of the preparation method of high-toughness casting magnesium alloy according to the present invention, step 3) is not necessarily to gas Body protection.
Compared with prior art, the invention has the following beneficial effects:
1) magnesium alloy of the invention cooperates the use of a small amount of Mn element using Bi, GD element as main alloying elements, leads to Simple alloying means are crossed, in casting process, in situ generated BiGd phase and Mg3Bi2Phase, the two competitive growth, suppression It makes and mutual excessively grows up；Both second phases are not fractured into micron order by the part for being dissolved into matrix in extrusion process Dispersed precipitate provides a large amount of phase interface on matrix after grain, promotes dynamic recrystallization, while dynamically analysing with thermal deformation process The equally distributed Mg of nanoscale disperse out3Bi2Phase collective effect, effectively pin crystal boundary hinder the movement of dislocation, and inhibition is tied again Jingjing grain length is big, so that deformed alloy has uniformly tiny perfect recrystallization tissue；On the other hand, it is partially dissolved into base The Bi element and Gd element of body can change the axis ratio of α-Mg phase in alloy, so that more slip systems are excited in extrusion process, Weak non-basal plane texture is formd in the alloy, avoids the generation of strong basis plane texture.In summary crystal grain and the refinement of the second phase, The effect of texture optimization etc., so that room temperature superplastic deformation magnesium alloy is developed in the alloy series, room temperature (25 DEG C) 43% or more stretch percentage elongation.
2) alloy of the present invention has excellent flame retardant property simultaneously, does not have to need to protect in casting stage and heat treatment stages Gas is protected, the stability of alloy production process had both been ensure that, and had reduced processing cost, and in turn avoided the combustion in alloy use process Burning problem.
3) Mg in alloy of the present invention3Bi2Phase (823 DEG C of fusing point) and BiGd phase fusing point with higher, allow alloy to exist Thermal processing distortion is carried out at higher temperature, to reduce Deformation Resistance, improves processing or production efficiency.
4) magnesium alloy preparation process of the present invention is simple, breaches big plasticity required by most of high-temperature-room type plasticity magnesium alloys Deformation etc. special processing method come obtain small grains so that improve plasticity limitation, existing magnesium alloy extrusion equipment all can be right It carries out Continuous maching production, is not necessarily to additional improvement, and the requirement to production equipment is low.
Detailed description of the invention
Fig. 1 is the microscopic structure that the direction of extrusion is parallel to according to the magnesium alloy of the embodiment of the present invention 1.
Fig. 2 is the microscopic structure that the direction of extrusion is parallel to according to the magnesium alloy of the embodiment of the present invention 2
Fig. 3 is the microscopic structure that the direction of extrusion is parallel to according to the magnesium alloy of the embodiment of the present invention 3.
Specific embodiment
(technical solution) of the invention is described further below by specific embodiments and the drawings, following embodiment is equal Implemented under premised on technical solution of the present invention, the detailed implementation method and specific operation process are given, but this hair Bright protection scope is not limited to the following embodiments.
The temperature-room type plasticity of magnesium alloy and grain size in alloy, grain uniformity, the type of the second phase, size, quantity, point The texture type of cloth and alloy is closely related.High plastic magnesium alloy needs control and obtains uniformly tiny grain structure, and one As by thermal deformation process occur dynamic recrystallization reach.Squeezing etc. in hot procedures, coarse second meet by Broken refinement, and Dispersed precipitate further increases the mechanical property of alloy in magnesium alloy substrate.Dynamic recrystallization crystal grain If grow up and be suppressed, be easily obtained small grains.And the second phase with preferable thermal stability, it can be in extrusion process Middle promotion dynamic recrystallization forming core, inhibits growing up for recrystal grain.Extrusion magnesium alloy is frequently present of stronger basal plane texture, leads Causing the temperature-room type plasticity of alloy reduces, and alloy can be excited to activate more slip systems under external force by the texture of optimized alloy, To improve the plastic deformation ability of alloy.
For magnesium alloy of the invention using Bi and GD as main alloying elements, which is Mg-Bi-Gd-Mn magnesium alloy, Component (wt%) by weight percentage are as follows: Bi 1~3%, Gd 1.5~4%, Gd >=1.5%, Mn 0.05~0.15%, surplus For Mg, wherein Bi/Gd content ratio is 0.25~2.
In the present invention, complicated object occurs under melt temperature and ambient condition for Mg, Bi, GD, Mn in alloy melt Physicochemical reaction in situ generated the BiGd phase of high thermal stability in process of setting, and the Mg in part Bi element and alloy is raw At Mg3Bi2Phase.The competitive growth of two kinds of object phases avoids Mg3Bi2Excessively growing up for phase, is not dissolved in extrusion process into base The second of body is met be fractured into micron particles after Dispersed precipitate on matrix, a large amount of phase interface is provided, promotes dynamic again Crystallization, while the equally distributed Mg of nanoscale disperse with Dynamic Precipitation in thermal deformation process3Bi2Phase collective effect, effectively pin Crystal boundary hinders the movement of dislocation, and recrystal grain is inhibited to grow up, so that deformed alloy is tied again completely with uniformly tiny Crystalline substance tissue；The joint of Gd element, Bi element and Mn element exists so that the axis ratio of α-Mg is changed in alloy, to change Deformation mechanism of the alloy under power effect during (extruding), forms weak non-basal plane texture in the alloy, avoids strong fibre The presence for tieing up texture, so that the texture of alloy after extruding is optimized.
In the following, the preparation method of the magnesium alloy with excellent temperature-room type plasticity of the invention is described.
1) ingredient: using pure Mg ingot, pure Bi block, Mg-Gd intermediate alloy and Mg-Mn intermediate alloy as raw material, according to magnesium alloy The weight percent of each component be Bi 1~3%, Gd 1.5~4%, Gd >=1.5%, Mn 0.05~0.15%, surplus is Mg (wherein Bi/Gd content ratio is 0.25~2) carries out ingredient.
2) melting: 700~730 DEG C of furnace temperature of setting puts the pure Mg ingot of preheating when furnace temperature is warming up to set temperature Enter in the crucible of smelting furnace, after its fusing, the Mg-Gd intermediate alloy of the pure Bi block of preheating and preheating is added to magnesium respectively and is melted In liquid；Then smelting temperature is increased to 750~760 DEG C, and keeps the temperature 5~15 minutes, is then stirred 3~10 minutes, is stood 3~10 Minute, Mg-Mn intermediate alloy is added, and keep the temperature 5~15 minutes, then stirs 3~10 minutes, furnace temperature is reduced to 740~750 DEG C, 3~10 minutes are stood, is passed through argon gas 1~3 minute and carries out refining degassing processing；Stand 3~10 minutes.
Relatively uniform stabilization when alloy melting of the present invention, since the fusing point (271.3 DEG C) of master alloying element Bi is lower, very It is easy to keep alloy melt uniform；Simultaneously because the joint with the presence of Gd element and Bi element in the magnesium alloy, plays good Fire retardation, melt are also more stable.
3) it casts: the magnesium alloy fused mass after melting is cast in corresponding mold, as-cast magnesium alloy is made.
4) it is heat-treated: solution heat treatment being carried out to as-cast magnesium alloy obtained in step 3), wherein solution heat treatment temperature It is 470~510 DEG C, the time is 7~12 hours.
5) ingot casting after solution treatment in step 4) is cut into corresponding blank and removed the peel.
6) extrusion process: temperature is squeezed needed for the blank that step 5) obtains is heated within 30 minutes, is put into extruding In cylinder, extrusion deformation processing is carried out, extrusion deformation speed is 0.1~20m/min, and extrusion ratio is 10~40, and squeezing temperature is 270 ~450 DEG C, finally obtain the Mg-Bi-Gd-Mn wrought magnesium alloy.
Alloy of the invention is after solid solution, extrusion molding, and elongation percentage is greater than 40% under room temperature (25 DEG C).
In the following, choosing three kinds of alloying component Mg-2Bi-3Gd-0.06Mn (wt%) (alloy 1), Mg-1.5Bi-1.5Gd- 0.08Mn (alloy 2), Mg-1Bi-1.5Gd-0.05Mn (wt%) (alloy 3) are used as typical example, carry out to the present invention detailed Explanation.
Technical solution according to the invention, with pure Mg (99.8wt%) ingot, pure Bi (99wt%) block, Mg-30Gd (Gd element Actually detected content is 30.03wt%) intermediate alloy and Mg-5Mn (the actually detected content of Mn is 4.98wt%) intermediate alloy It is smelting that low-cost magnesium alloy ingot casting is made for alloyed feedstock；Case will be put by the blank of solution treatment and peeling processing Be heated rapidly to squeeze 300 DEG C of temperature in formula resistance furnace, then using extrusion process by magnesium alloy blank deformation processing at bar, Extrusion speed is 5m/min, and extrusion ratio 36, bar is using air-cooled after extruding.And Mechanics Performance Testing is carried out to extruded bars, Embodiment and the room-temperature mechanical property test result of comparative example A Z31 are shown in Table 1.
Embodiment 1
(1) design choose Mg-2Bi-3Gd-0.06Mn (wt%) alloying component proportion at magnesium alloy, preparation method include with Lower step:
1) ingredient: using pure Mg ingot, pure Bi block, Mg-30Gd intermediate alloy and Mg-5Mn intermediate alloy as raw material, by table After the pretreatment of face (such as removal dirt, oxide skin etc., following embodiment is same), ingredient is carried out by above-mentioned target component；
2) melting: setting 700~730 DEG C of furnace temperature (such as 700 DEG C) will be preheating to when furnace temperature is warming up to predetermined temperature 200 DEG C of pure Mg ingot is put into the crucible of smelting furnace, after its fusing, will be preheating to 50 DEG C of pure Bi block respectively, is preheating to 200 DEG C Mg-Gd intermediate alloy be added in magnesium melt；Then smelting temperature is increased to 750~760 DEG C (such as 750 DEG C), and is protected Then temperature 10 minutes stirs 5 minutes, stand 5 minutes, Mg-5Mn intermediate alloy is added, and keep the temperature 10 minutes, then stirs 5 points Furnace temperature is reduced to 740~750 DEG C (such as 740 DEG C) by clock, stands 10 minutes, is passed through and is carried out within argon gas 2 minutes at refining degasification Reason；Stand 10 minutes.Entire fusion process is in CO2/SF6Mixed gas protected lower progress.
3) it casts: the magnesium alloy fused mass after standing is cast in corresponding mold, as-cast magnesium alloy is made；Wherein, should Casting process is not necessarily to gas shield.
4) Homogenization Treatments: with alloy cast ingot obtained by stove heating step 3) to 480 DEG C, and this temperature 12 hours into Then sample was put into 50 DEG C of warm water and is quenched, wherein the heating-up time of above-mentioned heating process by row Homogenization Treatments It is 60 minutes；Entire heat treatment process undesirable gas protection, carries out under burner hearth nature atmosphere.
5) machine: turnery processing removes the oxide layer on alloy cast ingot surface obtained by step 4), and is processed into suitable extruding The size of processing；
6) extrusion process: with extruder by alloy extrusion obtained by step 5) at bar, main technologic parameters when extruding: blank 300 DEG C of temperature, 300 DEG C of extrusion cylinder temperature, 300 DEG C of mold temperature, extrusion speed 7m/min, extrusion ratio 36 adds deformation blank Heat 30 minutes squeezes 300 DEG C of temperature needed for reaching, squeeze wood uses air-cooled cooling, that is, obtains the magnesium with excellent temperature-room type plasticity Alloy material.
(2) alloy performance test and Analysis on Microstructure
The extrusion magnesium alloy bar obtained from the preparation method by the embodiment 1 intercepts the sample of a length of 85mm, processing It is 6mm at diameter, the pole shape tensile sample of a length of 35mm of gauge length carries out tension test, tensile speed under room temperature (25 DEG C) 1mm/min, the axis direction of sample pole and the extruding grain direction of material are identical.Measure the tension of magnesium alloy of the present invention Intensity is 175.9MPa, and yield strength 117.6MPa, elongation percentage is 40.8% (table 1).Magnesium alloy obtained by the embodiment has Very big room temperature elongation percentage.Fig. 1 is that Mg-2Bi-3Gd-0.06Mn (wt%) magnesium alloy obtained by the present embodiment is parallel to extruding The displaing micro tissue topography in direction can also be seen that dynamic completely has occurred in extrusion process and ties again for alloy from the metallographic microscope Crystalline substance, second-phase dispersion are distributed in matrix.This is also that the alloy has the reason of superhigh intensity.
Embodiment 2
(1) design chooses Mg-1.5Bi-1.5Gd-0.08Mn (wt%) alloying component proportion into magnesium alloy, preparation method packet Include following steps:
1) ingredient: using pure Mg ingot, pure Bi block, Mg-30Gd intermediate alloy and Mg-5Mn intermediate alloy as raw material, by table (such as removal dirt, oxide skin etc.) after the pretreatment of face, ingredient is carried out by above-mentioned target component；
2) melting: setting 700~730 DEG C of furnace temperature (such as 720 DEG C) will be preheating to when furnace temperature is warming up to predetermined temperature 200 DEG C of pure Mg ingot is put into the crucible of smelting furnace, after its fusing, will be preheating to 50 DEG C of pure Bi block respectively, is preheating to 200 DEG C Mg-Gd intermediate alloy be added in magnesium melt；Then smelting temperature is increased to 750~760 DEG C (such as 755 DEG C), and is protected Then temperature 10 minutes stirs 5 minutes, stand 5 minutes, Mg-5Mn intermediate alloy is added, and keep the temperature 10 minutes, then stirs 5 points Furnace temperature is reduced to 740~750 DEG C (such as 740 DEG C) by clock, stands 10 minutes, is passed through and is carried out within argon gas 2 minutes at refining degasification Reason；Stand 10 minutes.Entire fusion process is in CO2/SF6Mixed gas protected lower progress；
3) it casts: the magnesium alloy fused mass after standing is cast in corresponding mold, as-cast magnesium alloy is made；The casting Cheng Wuxu gas shield；
4) Homogenization Treatments: with alloy cast ingot obtained by stove heating step 3) to 480 DEG C, and this temperature 12 hours into Then sample was put into 50 DEG C of warm water and is quenched, wherein the heating-up time of above-mentioned heating process by row Homogenization Treatments It is 60 minutes；Entire heat treatment process undesirable gas protection, carries out under burner hearth nature atmosphere.
5) machine: turnery processing removes the oxide layer on alloy cast ingot surface obtained by step 4), and is processed into suitable extruding The size of processing；
6) extrusion process: with extruder by alloy extrusion obtained by step 5) at bar, main technologic parameters when extruding: blank 300 DEG C of temperature, 300 DEG C of extrusion cylinder temperature, 300 DEG C of mold temperature, extrusion speed 5m/min, extrusion ratio 36 adds deformation blank Heat 30 minutes squeezes 300 DEG C of temperature needed for reaching, squeeze wood uses air-cooled cooling, that is, obtains the magnesium with excellent temperature-room type plasticity Alloy material.
(2) alloy performance test and Analysis on Microstructure
The extrusion magnesium alloy bar obtained from the preparation method by the embodiment 2 intercepts the sample of a length of 85mm, adds Work is 6mm at diameter, and the pole shape tensile sample of a length of 35mm of gauge length carries out tension test under room temperature (25 DEG C), stretches speed 1mm/min is spent, the axis direction of sample pole and the extruding grain direction of material are identical.Measure the anti-of magnesium alloy of the present invention Tensile strength is 169.4MPa, and yield strength 113.2MPa, elongation percentage is 42.5% (table 1).The tool of magnesium alloy obtained by the embodiment There is very big room temperature elongation percentage.Fig. 2 is that Mg-1.5Bi-1.5Gd-0.08Mn (wt%) magnesium alloy obtained by the present embodiment is parallel In the displaing micro tissue topography of the direction of extrusion, it is completely dynamic to can also be seen that alloy has occurred in extrusion process from the metallographic microscope State recrystallization, second-phase dispersion are distributed in matrix.
Embodiment 3
(1) design chooses Mg-1Bi-1.5Gd-0.05Mn (wt%) alloying component proportion into magnesium alloy, and preparation method includes Following steps:
1) ingredient: using pure Mg ingot, pure Bi block, Mg-30Gd intermediate alloy and Mg-5Mn intermediate alloy as raw material, by table (such as removal dirt, oxide skin etc.) after the pretreatment of face, ingredient is carried out by above-mentioned target component；
2) melting: setting 700~730 DEG C of furnace temperature (such as 730 DEG C) will be preheating to when furnace temperature is warming up to predetermined temperature 200 DEG C of pure Mg ingot is put into the crucible of smelting furnace, after its fusing, will be preheating to 50 DEG C of pure Bi block respectively, is preheating to 200 DEG C Mg-Gd intermediate alloy be added in magnesium melt；Then smelting temperature is increased to 750~760 DEG C (such as 760 DEG C), and is protected Then temperature 10 minutes stirs 5 minutes, stand 5 minutes, Mg-5Mn intermediate alloy is added, and keep the temperature 10 minutes, then stirs 5 points Furnace temperature is reduced to 740~750 DEG C (such as 750 DEG C) by clock, stands 10 minutes, is passed through and is carried out within argon gas 2 minutes at refining degasification Reason；Stand 10 minutes.Entire fusion process is in CO2/SF6Mixed gas protected lower progress；
3) it casts: the magnesium alloy fused mass after standing is cast in corresponding mold, as-cast magnesium alloy is made；Casting process Without gas shield；
4) Homogenization Treatments: with alloy cast ingot obtained by stove heating step 3) to 480 DEG C, and this temperature 12 hours into Then sample is put into 50 DEG C of warm water and is quenched by row Homogenization Treatments, wherein the heating-up time is 60 minutes；Entire heat The protection for the treatment of process undesirable gas, carries out under burner hearth nature atmosphere.
5) machine: turnery processing removes the oxide layer on alloy cast ingot surface obtained by step 4), and is processed into suitable extruding The size of processing；
6) extrusion process: with extruder by alloy extrusion obtained by step 5) at bar, main technologic parameters when extruding: blank 300 DEG C of temperature, 300 DEG C of extrusion cylinder temperature, 300 DEG C of mold temperature, extrusion speed 7m/min, extrusion ratio 36 adds deformation blank Heat 30 minutes squeezes 300 DEG C of temperature needed for reaching, squeeze wood uses air-cooled cooling, that is, obtains the magnesium with excellent temperature-room type plasticity Alloy material.
(2) alloy performance test and Analysis on Microstructure
The sample of a length of 85mm is intercepted from the extrusion magnesium alloy bar obtained according to the preparation method of the present embodiment 3, is processed It is 6mm at diameter, the pole shape tensile sample of a length of 35mm of gauge length carries out tension test, tensile speed under room temperature (25 DEG C) 1mm/min, the axis direction of sample pole and the extruding grain direction of material are identical.Measure the tension of magnesium alloy of the present invention Intensity is 165.3MPa, and yield strength 101.4MPa, elongation percentage is 43.4% (table 1).Magnesium alloy obtained by the embodiment has Very big room temperature elongation percentage.Fig. 3 is parallel to crowded for Mg-1Bi-1.5Gd-0.05Mn (wt%) magnesium alloy obtained by the present embodiment The displaing micro tissue topography for pressing direction, it can also be seen that, the reality similar to embodiment 1 and 2 alloy of embodiment from the metallographic microscope It applies an alloy and complete dynamic recrystallization has occurred in extrusion process, second-phase dispersion is distributed in matrix.
Comparative example
Comparative example is a kind of current commercial extrusion magnesium alloy: Mg-2.8Al-0.9Zn-0.3Mn (wt%) AZ31 magnesium alloy. It is 223.7MPa that comparative example (obtains) tensile strength under processing conditions same as Example 2, and yield strength 203.5MPa prolongs Stretching rate is 20.2% (table 1).Comparison as it can be seen that novel magnesium alloy room temperature elongation percentage of the invention have compared to comparative example alloy it is extremely aobvious The promotion of work.
The room-temperature mechanical property test result of 1 embodiment of table and comparative example
Raw material used in above-described embodiment and equipment pass through well known approach and obtain, and operating procedure used is this What those skilled in the art can grasp.In addition, each numerical value provided in above-mentioned preparation method is only example, the present invention is not It is limited to this.
Magnesium alloy according to the present invention with excellent temperature-room type plasticity, due to having Gd element and Bi element in the magnesium alloy Joint exists, and plays good fire retardation, and melt is also more stable, and the alloy is after solid solution, extrusion molding, room temperature (25 DEG C) Lower elongation percentage is greater than 40%.
In addition, magnesium alloy of the invention has excellent flame retardant property simultaneously, in casting stage and heat treatment stages Do not have to need protective gas, both ensure that the stability of alloy production process, reduced processing cost, in turn avoiding alloy makes With combustion problem in the process.
In addition, magnesium alloy preparation process of the present invention is simple, breach big required by most of high-temperature-room type plasticity magnesium alloys Plastic deformation etc. special processing method come obtain small grains so that improve plasticity limitation, existing magnesium alloy extrusion equipment is all Continuous maching production can be carried out to it, be not necessarily to additional improvement, the requirement to production equipment is low
Novel high-temperature-room type plasticity antiflaming magnesium alloy of the invention, has both excellent temperature-room type plasticity and flame retardant property, process Economic cost and environmental cost it is small, in use can to avoid the hidden danger of burning, can be used as communications and transportation, aviation boat It, computer, communication and consumer electronics product components materials'use.
The above embodiments merely illustrate the technical concept and features of the present invention, and its object is to allow the ordinary skill of this field Personnel understand the contents of the present invention and implement accordingly, and it is not intended to limit the scope of the present invention.It is all smart according to the present invention The equivalent transformation or modification that refreshing essence is done, should be covered by the protection scope of the present invention.

Claims (10)

1. a kind of magnesium alloy with excellent temperature-room type plasticity, which is characterized in that the magnesium alloy is Mg-Bi-Gd-Mn magnesium alloy, Component is by weight percentage are as follows: Bi 1~3%, Gd 1.5~4%, Gd >=1.5%, Mn 0.05~0.15%, surplus Mg, Wherein Bi/Gd content ratio is 0.25~2.
2. a kind of preparation method of the magnesium alloy with excellent temperature-room type plasticity, which is characterized in that the preparation method includes following Step:
1) ingredient: using pure Mg ingot, pure Bi block, Mg-Gd intermediate alloy and Mg-Mn intermediate alloy as raw material, according to claim 1 institute The weight percent of each component for the magnesium alloy stated carries out ingredient；
2) melting: the pure Mg ingot of preheating is put into molten by 700~730 DEG C of furnace temperature of setting when furnace temperature is warming up to set temperature In the crucible of furnace, after its fusing, the Mg-Gd intermediate alloy of the pure Bi block of preheating and preheating is added to magnesium melt respectively In；Then smelting temperature is increased to 750~760 DEG C, and keeps the temperature 5~15 minutes, is then stirred 3~10 minutes, is stood 3~10 points Clock is added Mg-Mn intermediate alloy, and keeps the temperature 5~15 minutes, then stirs 3~10 minutes, furnace temperature is reduced to 740~750 DEG C, 3~10 minutes are stood, is passed through argon gas 1~3 minute and carries out refining degassing processing；Stand 3~10 minutes；
3) it casts: the magnesium alloy fused mass after melting is cast in corresponding mold, as-cast magnesium alloy is made；
4) be heat-treated: to as-cast magnesium alloy obtained in step 3) carry out solution heat treatment, wherein heat treatment temperature be 470~ 510 DEG C, the time is 7~12 hours；
5) ingot casting after solution treatment in step 4) is cut into corresponding blank and removed the peel；
6) extrusion process: squeezing temperature, be put into extrusion cylinder needed for the blank that step 5) obtains is heated within 30 minutes, Extrusion deformation processing is carried out, extrusion deformation speed is 0.1~20m/min, and extrusion ratio is 10~40, and squeezing temperature is 270~450 DEG C, finally obtain the Mg-Bi-Gd-Mn wrought magnesium alloy.
3. the preparation method of high-toughness casting magnesium alloy according to claim 2, which is characterized in that in the Mg-Gd Between alloy be Mg-30Gd intermediate alloy.
4. the preparation method of high-toughness casting magnesium alloy according to claim 2, which is characterized in that in the Mg-Mn Between alloy be Mg-5Mn intermediate alloy.
5. the preparation method of high-toughness casting magnesium alloy according to claim 2, which is characterized in that the CO2/SF6 Mixed gas composition is preferably volume ratio CO2: SF6=100: 1.
6. the preparation method of high-toughness casting magnesium alloy according to claim 2, which is characterized in that in step 2), institute The preheating temperature for stating pure Mg ingot is 200~300 DEG C, and the preheating temperature of the pure Bi block is 50~70 DEG C, is closed among the Mg-Gd The preheating temperature of gold is 200~300 DEG C.
7. the preparation method of high-toughness casting magnesium alloy according to claim 2, which is characterized in that the melting in step 2) Process is in CO2/SF6Mixed gas protected lower progress.
8. the preparation method of high-toughness casting magnesium alloy according to claim 2, which is characterized in that the heat treatment of step 4) Further include: it is quenched with 40~80 DEG C of warm water.
9. the preparation method of high-toughness casting magnesium alloy according to claim 2, which is characterized in that the entire heat of step 4) Treatment process is not necessarily to gas shield.
10. the preparation method of high-toughness casting magnesium alloy according to claim 2, which is characterized in that the casting of step 3) Process is not necessarily to gas shield.
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