CN104109786B - A kind of magnesium alloy and preparation method thereof - Google Patents

A kind of magnesium alloy and preparation method thereof Download PDF

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CN104109786B
CN104109786B CN201310140235.6A CN201310140235A CN104109786B CN 104109786 B CN104109786 B CN 104109786B CN 201310140235 A CN201310140235 A CN 201310140235A CN 104109786 B CN104109786 B CN 104109786B
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alloy
magnesium alloy
ingot
magnesium
preparation
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CN104109786A (en
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李绍青
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BYD Co Ltd
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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
    • C22C1/00—Making non-ferrous alloys
    • C22C1/02—Making non-ferrous alloys by melting
    • 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
    • C22C23/02—Alloys based on magnesium with aluminium 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

Abstract

The invention provides a kind of magnesium alloy, on the basis of the gross mass of magnesium alloy, described magnesium alloy contains following components: the Al of 2.5 3.5 wt%, the Zn of 0.4 1.5wt%, the Mn of 0.15 0.5wt%, the In of 1 3wt%, the Sr of 0.2 1.4wt%, surplus is magnesium.Present invention also offers the preparation method of this magnesium alloy.The magnesium alloy of the present invention has good elevated temperature strength.

Description

A kind of magnesium alloy and preparation method thereof
Technical field
The invention belongs to field of magnesium alloy field, particularly relate to a kind of magnesium alloy and preparation method thereof.
Background technology
Magnesium and magnesium alloy are 21 century lightweighting materials, and magnesium alloy has light specific gravity, specific strength and specific stiffness height, resistance because of it Buddhist nun's property, heat conductivity, machinability and castability are good, the most also have that electromagnetic shielding capability is strong, an aboundresources and easily reclaiming Etc. series of advantages, its development and application receives more and more attention, and becomes one of the structural metallic materials of " the youngest ". It is applied on the structural member in the fields such as Aero-Space, automobile, transportation, can substantially alleviate weight, save fuel oil consumption.
The application of traditional magnesium alloy mainly produces product with casting techniques such as molding, die casting, but product easily occurs The defects such as coarse grains, tissue looseness, component segregation and mechanical property are on the low side, it is impossible to give full play to the performance advantage of magnesium alloy. At present, the most all attaching great importance to the research and development of wrought magnesium alloy, wrought magnesium alloy refers to available to extrude, rolls, forges With the magnesium alloy of the plastic molding method such as punching press processing, compared with cast magnesium alloy, the crystal grain of wrought magnesium alloy is tiny, segregation-free And Micro porosity, there is excellent combination property.
But, although current wrought magnesium alloy plasticity is preferable, but room temperature and elevated temperature strength are relatively low on the low side with creep resistance, It is difficult to meet Aeronautics and Astronautics, weapons and civil car field to high tough, high-fire resistance and the light structures material of high creep strength The requirement of material, therefore a kind of high-strength heat-resisting magnesium alloy of exploitation is extremely important.
Summary of the invention
The present invention solves the technical problem that magnesium alloy elevated temperature strength of the prior art is low, it is provided that a kind of elevated temperature strength is high Magnesium alloy and preparation method thereof.
The invention provides a kind of magnesium alloy, on the basis of the gross mass of magnesium alloy, described magnesium alloy contains following components: The Sr of the In of the Mn of the Zn of the Al of 2.5-3.5 wt%, 0.4-1.5wt%, 0.15-0.5wt%, 1-3wt%, 0.2-1.4wt%, surplus For magnesium.
Present invention also offers a kind of magnesium alloy preparation method, the method comprises the following steps: raw material magnesium alloy melted Alloying obtains magnesium alloy liquation, is then shaped, and obtains described magnesium alloy；Described raw material magnesium alloy comprises: magnesium ingot, aluminum Ingot, zinc ingot metal, indium ingot, aluminum manganese intermediate alloy ingot and aluminium-strontium master alloy ingot；The weight percent of each component in described magnesium alloy Ratio is: the In of the Mn of the Zn of the Al of 2.5-3.5 wt%, 0.4-1.5wt%, 0.15-0.5wt%, 1-3wt%, 0.2-1.4wt%'s Sr, surplus is magnesium.
The present invention, by adding metallic element indium and metallic element strontium, defines the good In of heat stability2Sr granule phase, This phase Dispersed precipitate, in the intracrystalline of alloy and grain boundaries, enhances matrix and crystal boundary effectively, so that alloy strength and heat-resisting Property improve.
Detailed description of the invention
In order to make technical problem solved by the invention, technical scheme and beneficial effect clearer, below in conjunction with Embodiment, is further elaborated to the present invention.Should be appreciated that specific embodiment described herein is only in order to explain The present invention, is not intended to limit the present invention.
One magnesium alloy of the present invention, on the basis of the gross mass of magnesium alloy, described magnesium alloy contains following components: 2.5- The Sr of the In of the Mn of the Zn of the Al of 3.5 wt%, 0.4-1.5wt%, 0.15-0.5wt%, 1-3wt%, 0.2-1.4wt%, surplus is Magnesium.
The present invention, by adding metallic element indium and metallic element strontium, defines the good In of heat stability2Sr granule phase, This phase Dispersed precipitate, in the intracrystalline of alloy and grain boundaries, enhances matrix and crystal boundary effectively, so that alloy strength and heat-resisting Property improve.Metallic element indium defines the InMn higher than matrix fusing point with the manganese in alloy3(910 DEG C) granule phase, makes alloy draw Grain Boundary Sliding when stretching effectively is suppressed, so that the thermostability of alloy is improved.The interpolation of metallic element indium simultaneously is also Effectively change β (Mg17Al12) form of phase and crystallite dimension, it is effectively improved alloy high-temp intensity.Metallic element strontium, It is possible not only to crystal grain thinning, is combined generation Al simultaneously with Al4The heat-resisting phase of Sr, thus it is effectively improved intensity and thermostability.
According to magnesium alloy provided by the present invention, in order to obtain high-temperature behavior more preferably wrought magnesium alloy, it is preferable that with magnesium On the basis of the gross mass of alloy, described magnesium alloy contains following components: the Zn of the Al of 2.8-3.2 wt%, 0.8-1.2wt%, The Sr of the In of the Mn of 0.25-0.35wt%, 1.5-2.5wt%, 0.5-1.0wt%, surplus is magnesium.
Preferably, described magnesium alloy also includes that impurity, described impurity element are at least one in Fe, Cu, Ni.More preferably Ground, on the basis of the gross mass of described magnesium alloy, the content of Fe is less than 0.004 wt %, and the content of Cu is less than 0.004 The content of wt %, Ni is less than 0.002 wt %.
Present invention also offers a kind of magnesium alloy preparation method, the method comprises the following steps: raw material magnesium alloy melted Alloying obtains magnesium alloy liquation, is then shaped, and obtains described magnesium alloy；Described raw material magnesium alloy comprises: magnesium ingot, aluminum Ingot, zinc ingot metal, indium ingot, aluminum manganese intermediate alloy ingot and aluminium-strontium master alloy ingot；The weight percent of each component in described magnesium alloy Ratio is: the In of the Mn of the Zn of the Al of 2.5-3.5 wt%, 0.4-1.5wt%, 0.15-0.5wt%, 1-3wt%, 0.2-1.4wt%'s Sr, surplus is magnesium.
According to preparation method provided by the present invention, in order to remove the moisture in raw material, prevent in fusion process, water and magnesium Reaction produces blast.Preferably, by magnesium ingot, aluminium ingot, zinc ingot metal, indium ingot, aluminum manganese intermediate alloy before the method is additionally included in and melts Ingot and aluminium-strontium master alloy ingot carry out baking step.
According to preparation method provided by the present invention, in order to reduce the product of impurity, it is preferable that described molten alloyization walks Suddenly, after for first magnesium ingot, aluminium ingot, zinc ingot metal, indium ingot all being melted, aluminum manganese intermediate alloy and aluminium-strontium master alloy are added to all Melted.
According to preparation method provided by the present invention, in order to prevent magnesium from burning when melted, it is preferable that described molten alloy Change step to carry out under gas and coverture protective condition；Described gas is SF6；Described coverture is calcium chloride or sodium chloride.
Preferably, before molten alloy, adding end flux in the feed, the content of flux of the described end is that magnesium alloy is total The 1.5-2.5 wt% of quality.
Preparation method provided by the present invention, described forming method has no particular limits, and can be commonly used in the art Various forming methods, as forging, extrude and roll in one.
Preparation method provided by the present invention, in order to reduce the generation of impurity, it is preferable that at the aftershaping of molten alloy Include removing the impurity removal step in aluminium alloy before.It is highly preferred that described removal step is under argon includes, at alloy Liquid surface adds refining agent, stands and remove impurity after aluminium alloy alloying.
The preparation of the magnesium alloy of the present invention can use the most conventional process for smelting magnesium alloy, and wherein, smelting technology uses Existing get the raw materials ready → melt → step of refine → cast, existing by concrete for each step of the preparation method of wrought magnesium alloy of the present invention Details are as follows:
Step 1, get the raw materials ready: 1) raw material: be ready to the pure magnesium ingot (purity >=99.9wt%) of formula ratio, fine aluminium ingot (purity >= 99.9 wt%), pure zinc ingot (purity >=99.9 wt%), pure indium ingot (purity >=99.9wt%), in aluminum manganese intermediate alloy ingot and aluminum strontium Between alloy pig.
2) flux: end flux, coverture and refining agent, all can use existing for end flux prepared by magnesium alloy, Coverture and refining agent, such as: coverture RJ-6, refining agent RJ-5.
Step 2, be dried: the raw material of preparation is dried process, and wherein, Mg, Al, Zn, In are 100 DEG C ± 10 DEG C temperature Lower drying, and AlMn intermediate alloy and Al-Sr intermediate alloy are dried at a temperature of 150 DEG C ± 10 DEG C, the effect of drying be in order to Removing the moisture in raw material, prevent in fusion process, water produces blast with reactive magnesium.
Step 3, molten alloy: in whole fusion process, continue to be passed through SF6 gas in crucible and protect, first Crucible is preheated to 200-250 DEG C, load weighted magnesium ingot, aluminium ingot, zinc ingot metal, indium ingot are put in crucible and added the heating of end flux Fusing, the consumption of end flux accounts for the 1.5-2.5 wt% of quality of furnace charge, after magnesium ingot, aluminium ingot, zinc ingot metal, indium ingot all melt, adds Enter the most load weighted aluminum manganese intermediate alloy and aluminium-strontium master alloy, continue heating, after alloy fully melts, stir, system Obtaining liquation in the middle of magnesium alloy, the time of whole fusion process controls at 2-6H, and the final temperature of magnesium alloy liquation controls 670-720℃.Whole fusion process is sprinkled into the most equably coverture with prevent burning, spread the rule of coverture It is: not making metal surface open combustion, addition is the least, it is possible to cover molten surface, and the consumption of coverture accounts for furnace charge The 0.3-0.5wt% of quality；Because the activity of magnesium is high, heat in atmosphere, oxidizable scaling loss, and in the molten state, without covering During agent protection, the burning that meeting is violent.Thus whole fusion process needs to carry out under SF6 gas shield, and need to be sprinkled into cover Lid agent.
Step 4, refine: in magnesium alloy liquation, be passed through argon protect, the most uniform on the surface of magnesium alloy liquation Being sprinkled into refining agent and carry out refine, and use mechanical agitation, the consumption of refining agent accounts for the 1.5-2.5wt% of quality of furnace charge, then rises Temperature, temperature controls at 720-730 DEG C, and the time controls at 30-45min, makes the metal of addition the most preferably close Aurification；Standing cooling after end, time of repose controls at 10-30min, and temperature controls, at 660-680 DEG C, to make flux and field trash Sedimentation, makes alloy more homogenization, obtains magnesium alloy fused mass.
Step 5, cast: the magnesium alloy fused mass after refine is injected in mould, the demoulding after molding, prepare magnesium alloy cast rod, Cast condition be: at a temperature of 660-680 DEG C, and carry out in protective atmosphere, protective atmosphere be usually SF6, CO2, N2, SO2 or mixed gas protected atmosphere.
Step 6, extruded: according to the requirement of extrusion process, the homogenization that magnesium alloy cast rod first carries out 10-12H is moved back Fire processes, then under conditions of extrusion die is preheated to 350-450 DEG C, magnesium alloy cast rod is placed in recipient, installs mould, Being extruded by extruder, finally prepare extruded bar from magnesium alloy, wherein, extrusion temperature controls at 300-450 DEG C, extrusion ratio Controlling at 10:1-100:1, extrusion speed controls at 2m/min-10m/min.
Below in conjunction with specific embodiment, the present invention is described in detail.
Embodiment 1
Step is as follows:
1, dry: by ready raw material: in the middle of pure magnesium, fine aluminium, pure zinc, pure indium (purity all >=99.9 wt%), aluminum strontium Alloy and aluminum manganese intermediate alloy, carry out drying and processing, and wherein Mg, Al, Zn, In are dried at a temperature of 100 DEG C, and closes in the middle of AlMn Gold and Al-Sr intermediate alloy are then dried at a temperature of 150 DEG C.
2, melting: in whole fusion process, continues to be passed through SF6 gas in resistance crucible and protects, first by resistance Crucible is preheated to 200 DEG C, sprinkles appropriate refining agent RJ-5 and coverture RJ-6 at crucible wall and bottom, is then placed in weighing Good 93.6wt%Mg, 2.7%wtAl, 1.1wt%Zn, 1.5wt%In ingot, continues heating, treats that Mg, Al, Zn, In ingot is complete After portion's fusing, add at a temperature of 680 DEG C and weighed AlMn intermediate alloy that Fe content is 0.3wt% and content of strontium is The Al-Sr intermediate alloy of 0.5wt% and frequently uniformly spread lower coverture RJ-6；Treat AlMn intermediate alloy and Al-Sr intermediate alloy All after fusing, stir, be incubated 5min simultaneously；Add refining agent RJ-5 and carry out refine, during refine, refining agent Addition is furnace charge amount about 10%, be sufficiently stirred for after addition, stand 5min, then heat to 720 DEG C insulation 30min, then Lower the temperature 680 DEG C and stand 15min, finally pour in the swage that preheating temperature is 250 DEG C, prepare magnesium alloy cast rod.
3, extruding: according to extrusion process requirement, the homogenizing annealing that magnesium alloy cast rod first carries out 10-12H processes, and will Under conditions of extrusion die is preheated to 400 DEG C, carrying out extrudate on extruder, wherein extrusion temperature controls at 350 DEG C, squeezes Pressure ratio controls at 10:1, and extrusion speed controls at 3m/min, obtains extruded bar from magnesium alloy A1.
Embodiment 2
Magnesium alloy extrusion stick A2 is prepared according to the method for embodiment 1.Difference is, in magnesium alloy, the mass fraction of strontium is 0.80wt%。
Embodiment 3
Magnesium alloy extrusion stick A3 is prepared according to the method for embodiment 1.Difference is, in magnesium alloy, the mass fraction of strontium is 1.0wt%。
Embodiment 4
Magnesium alloy extrusion stick A4 is prepared according to the method for embodiment 1.Difference is, in magnesium alloy, the mass fraction of indium is 2.0wt%。
Embodiment 5
Magnesium alloy extrusion stick A5 is prepared according to the method for embodiment 1.Difference is, in magnesium alloy, the mass fraction of indium is 2.0wt%, and the mass fraction of strontium is 0.8wt%.
Embodiment 6
Magnesium alloy extrusion stick A6 is prepared according to the method for embodiment 1.Difference is, in magnesium alloy, the mass fraction of indium is 2.0wt%, and the mass fraction of strontium is 1.0wt%.
Embodiment 7
Magnesium alloy extrusion stick A7 is prepared according to the method for embodiment 1.Difference is, in magnesium alloy, the mass fraction of indium is 2.5wt%, and the mass fraction of strontium is 0.5wt%.
Embodiment 8
Magnesium alloy extrusion stick A8 is prepared according to the method for embodiment 1.Difference is, in magnesium alloy, the mass fraction of Al is The mass fraction of 3.2wt%, Zn be the mass fraction of 1.2wt%, Mn be 0.35wt%, the mass fraction of indium is 2.5wt%, and strontium Mass fraction is 0.8wt%.
Embodiment 9
Magnesium alloy extrusion stick A9 is prepared according to the method for embodiment 1.Difference is, in magnesium alloy, the mass fraction of Al is The mass fraction of 2.8wt%, Zn be the mass fraction of 0.8wt%, Mn be 0.25wt%, the mass fraction of indium is 2.5wt%, and strontium Mass fraction is 1.0wt%.
Embodiment 10
Magnesium alloy extrusion stick A10 is prepared according to the method for embodiment 1.Difference is, in magnesium alloy, the mass fraction of Al is The mass fraction of 2.5wt%, Zn be the mass fraction of 0.4wt%, Mn be 0.15wt%, the mass fraction of indium is 1wt%, and the matter of strontium Amount mark is 0.2wt%.
Embodiment 11
Magnesium alloy extrusion stick A11 is prepared according to the method for embodiment 1.Difference is, in magnesium alloy, the mass fraction of Al is The mass fraction of 3.5wt%, Zn be the mass fraction of 1.5wt%, Mn be 0.5wt%, the mass fraction of indium is 3wt%, and the matter of strontium Amount mark is 1.4wt%.
Comparative example 1
Magnesium alloy extrusion stick CA1 is prepared according to the method for embodiment 1.Difference is, does not add indium and strontium.
Performance test
1, chemical composition,
Magnesium alloy extrusion stick CA1ization prepared by magnesium alloy extrusion stick A1-A9 embodiment prepared and comparative example 1 Learn composition detection (ICP test), the results are shown in Table 1.
2, strength character test
Magnesium alloy extrusion stick CA1 prepared by magnesium alloy extrusion stick A1-A9 embodiment prepared and comparative example 1 exists respectively Carry out yield strength in the case of room temperature, 100 DEG C, 200 DEG C and 300 DEG C and tensile strength is tested (by omnipotent mechanics machine Test), the results are shown in Table 2.
Table 1
。
Table 2
。
From Table 2, it can be seen that after with the addition of metallic element indium and strontium in alloy, room temperature strength and the high temperature of alloy are strong Degree has promoted, and wherein elevated temperature strength promotes more apparent；Illustrate that the magnesium alloy of the present invention has good elevated temperature strength.
The foregoing is only presently preferred embodiments of the present invention, not in order to limit the present invention, all essences in the present invention Any amendment, equivalent and the improvement etc. made within god and principle, should be included within the scope of the present invention.

Claims (12)

1. a magnesium alloy, it is characterised in that on the basis of the gross mass of magnesium alloy, described magnesium alloy contains following components: The Sr of the In of the Mn of the Zn of the Al of 2.5-3.5 wt%, 0.4-1.5wt%, 0.15-0.5wt%, 1-3wt%, 0.2-1.4wt%, surplus For magnesium.
Magnesium alloy the most according to claim 1, it is characterised in that on the basis of the gross mass of magnesium alloy, described magnesium alloy Containing following components: the In of the Mn of the Zn of the Al of 2.8-3.2 wt%, 0.8-1.2wt%, 0.25-0.35wt%, 1.5-2.5wt%, The Sr of 0.5-1.0wt%, surplus is magnesium.
Magnesium alloy the most according to claim 1, it is characterised in that described magnesium alloy also includes impurity, described impurity element For at least one in Fe, Cu, Ni.
Magnesium alloy the most according to claim 3, it is characterised in that on the basis of the gross mass of described magnesium alloy, Fe contains Amount is less than 0.004 wt % less than 0.004 wt %, the content of Cu, and the content of Ni is less than 0.002 wt %.
5. a magnesium alloy preparation method, it is characterised in that the method comprises the following steps: by raw material magnesium alloy molten alloy Obtain magnesium alloy liquation, be then shaped, obtain described magnesium alloy；Described raw material magnesium alloy comprises: magnesium ingot, aluminium ingot, zinc ingot metal, Indium ingot, aluminum manganese intermediate alloy ingot and aluminium-strontium master alloy ingot；In described magnesium alloy, the percentage by weight of each component is: 2.5- The Sr of the In of the Mn of the Zn of the Al of 3.5 wt%, 0.4-1.5wt%, 0.15-0.5wt%, 1-3wt%, 0.2-1.4wt%, surplus is Magnesium.
Preparation method the most according to claim 5, it is characterised in that the method is additionally included in magnesium ingot, aluminum before melting Ingot, zinc ingot metal, indium ingot, aluminum manganese intermediate alloy ingot and aluminium-strontium master alloy ingot carry out baking step.
Preparation method the most according to claim 5, it is characterised in that described molten alloy step is first by magnesium ingot, aluminum After ingot, zinc ingot metal, indium ingot all melt, add aluminum manganese intermediate alloy and aluminium-strontium master alloy to the most melted.
Preparation method the most according to claim 5, it is characterised in that described molten alloy step is at gas and coverture Carry out under protective condition；Described gas is SF6；Described coverture is calcium chloride or sodium chloride.
Preparation method the most according to claim 5, it is characterised in that before molten alloy, adds at the end in the feed Flux, the 1.5-2.5 wt% that content is magnesium alloy gross mass of flux of the described end.
Preparation method the most according to claim 5, it is characterised in that during described forming method is for forging, extruding and roll One.
11. preparation methoies according to claim 5, it is characterised in that included before the aftershaping of molten alloy Except the impurity removal step in aluminium alloy.
12. preparation methoies according to claim 11, it is characterised in that described removal step is under argon shield, Aluminium alloy surface adds refining agent, stands and remove impurity after aluminium alloy alloying.
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CN102226242A (en) * 2011-06-22 2011-10-26 重庆大学 Melting method for magnesium alloy containing high reactivity elements

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