CN104018049B - A kind of superplasticity magnesium alloy and preparation method thereof - Google Patents
A kind of superplasticity magnesium alloy and preparation method thereof Download PDFInfo
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Abstract
A kind of superplasticity magnesium alloy and preparation method thereof, belongs to magnesium alloy technical field.Following composition: selecting Zn, Er as main alloying elements, its addition is respectively 10～30wt.%Zn, 10～15wt.%Er, and Zn/Er ratio is 1～2, and surplus is Mg.It is prepared by smelting technology and extrusion process.This alloy is 0.5～5mm/min in initial strain rate, has good plasticity at 100～150 DEG C, has and present good superplasticity in the lower temperature range of 175～300 DEG C, is a kind of potential magnesium alloy materials that can be used for Superplastic Forming Techniques processing.
Description
Technical field
The present invention relates to a kind of low temperature superplasticity Mg-Zn-Er alloy and preparation method thereof, be specifically related to be become by certain alloy
Point, the preparation such as smelting technology and extruding condition.This alloy has significant superplasticity in lower temperature range, and it is potential to be that one has
Application prospect can the magnesium alloy materials of superplasticforming, belong to magnesium alloy technical field.
Background technology
21 century, shortage of resources and ecological deterioration become the matter of utmost importance affecting human kind sustainable development.Relative to day by day exhaustion
For various metals mineral resources, magnesium is with its abundant reserves more advantage on the effective environmental protection of resource is used.Equally, magnesium alloy
Have in fields such as automobile, track, electronics, space flight, aviation and defence and militaries as the lightest a kind of energy-conserving and environment-protective structural material
Extremely important industrial value and application prospect.The most in recent years, environmental pollution increases the weight of day by day, air quality severe exacerbation,
The requirement of automotive energy-saving emission-reducing is improved by society the most day by day.Magnesium alloy (such as series alloys such as AZ91 and AM60) is light as automobile
One of preferred material quantified, Successful utilization is on the multiple parts such as steering wheel, instrumental panel, gear box casing, pedal,
Alleviate automobile exhaust pollution problem to a certain extent.But, magnesium crystal structure is close-packed hexagonal, and under low temperature, plasticity is poor, adds
Work difficulty, greatly limit its extensive application in automobile manufacture industry.
Magnesium alloy Superplastic Forming Techniques can improve its crystallized ability, develop complex-shaped, size accurately, any surface finish
Alloy product, and then overcome the problem of processing difficulties under magnesium alloy low temperature.Initially, the main collection of magnesium alloy Study of Superplasticity in early days
In at crystal grain on superplastic impact, crystal grain can be divided on the research that Alloy during Superplastic affects following two aspect: (1) is carefully brilliant
Impact superplastic on magnesium alloy.Originally, the research in early days of magnesium alloy superplasticity is concentrated mainly on crystal grain refinement to superplastic shadow
Ring.Using Equal Channel Angular Pressing (ECAE), rapid solidification (RS) technology to prepare the grain size alloy less than 1 μm, this alloy has
There is the superplastic deformation ability of excellence.Further investigations have shown that, crystal grain refinement contributes to the realization of Alloy during Superplastic.Backofen
(AIME1969,245:1131-1132) develops the ZK60 alloy that grain size is 0.55 μm, 3.3 × 10-3s–1、270℃
Under conditions of elongation percentage (δ) reach more than 1000%.(2) coarse-grain impact superplastic on magnesium alloy.Deep exhibition along with research
Open, find that the magnesium alloy with texture of coarse crystal still has superplasticity.Wang Qudong (high-tech communication 2002,9:52-55) makes
Standby rolling state AZ91 alloy, crystallite dimension is 11 μm, and high temperature elongation percentage is 455%.Zhang Shichang (learn by Wuhan University Of Technology
Report 2008,31:547-551) crystallite dimension of As-extruded AZ31 alloy prepared is that the elongation percentage under 37.6 μm, high temperature is
214%.For the Superplasticity Phenomenon under coarse grain, research finds that the dynamic recrystallization occurred in plastic history is to improve to close
The main cause of gold plasticity, this is because the dynamic recrystallization occurred in plastic deformation causes texture of coarse crystal to disappear, defines
More tiny grain structure, can be obviously improved plasticity.
As can be seen here, either coarse grains or tiny, magnesium alloy is all (to include temperature, rate of deformation) under certain condition
Can have certain superplasticity, this also indicates that grain size is not the major influence factors limiting the actual application of magnesium alloy superplasticity.
Along with going deep into of research, find that a difficult problem for the restriction actual application of magnesium alloy Superplastic Technology at present is to improve production efficiency and reduce raw
Produce cost.This bottleneck can be attributed to: how (1) obtains (1 × 10 under high strain rate-2) superplasticity (δ 100%).
The superplasticforming speed improving magnesium alloy can reduce production cost, improves production efficiency, increases production scale, beneficially magnesium and closes
The popularization of gold Superplastic Forming Techniques.(2) superplasticity under cryogenic conditions how is obtained.The crystal structure of magnesium and alloy thereof is close
Arrange six sides, low temperature (> 220 DEG C) under the conditions of predominantly basal slip, slip system causes its plasticity the best less.Only in higher temperatures
The lower cylinder of degree and conical surface slip system can start, and improve the plasticity of magnesium alloy.But temperature is the highest, and to often lead to magnesium alloy crystal grain thick
Change, be degrading the mechanical property (intensity) of alloy, improve the processing cost of alloy simultaneously.Under exploitation low temperature, there is superplastic ability
The magnesium alloy of power is conducive to Superplastic Forming Techniques application in the magnesium alloy, reduces production cost, prevents grain coarsening simultaneously.
If two above problem not can solve, then necessarily limit the extensively application of magnesium alloy Superplastic Forming Techniques and promote.
It is especially noted that the application using Superplastic Forming Techniques to carry out industrialization magnesium-alloy material production at present is close to sky
In vain, the principal element of restriction magnesium alloy Superplastic Forming Techniques popularization and application is exactly the shortage of superplasticforming ability excellence magnesium alloy,
This shortage is mainly manifested in the following aspects: (1) superplastic research of magnesium alloy the most both at home and abroad be concentrated mainly on AZ,
The commercial magnesium alloy such as ZK.On the one hand, although such alloy is cheap, aboundresources, but the mechanical property of such alloy is relatively
Difference, especially its mechanical behavior under high temperature is worse, it is impossible to the parts used under the load-bearing parts preparing key or high temperature.
On the other hand, such alloy cannot also exist substantial amounts of low melting point the second phase (mainly Mg-Al, Mg-Zn phase) with avoiding,
They cannot function as effective stable particle and are present in alloy, the most softened under conditions of higher than 350 DEG C.Stable particle
Lack the roughening necessarily causing alloy grain under high-temp plastic processing conditions and the suppression to dynamic recrystallization (PSN mechanism), by
This seriously compromises the Large strain superplasticforming ability of such magnesium alloy.(2) current relevant Mg-Zn-RE (rare earth) alloy
The research of superplastic behavior the weakest, Relatively centralized is in Mg-Zn-Y system alloy, and to containing other beyond Y element
The research of Mg-Zn-RE system alloy is the most less.From the point of view of Yi Fangmian, containing stable I phase (Mg in Mg-Zn-RE alloy3Zn6RE)、
W phase (Mg2Zn3RE3) etc. ternary phase (they can under conditions of 450 DEG C stable existence).Magnesium alloy superplasticity is being processed
Time, these stable ternary phase particles are not only able to suppress grain coarsening, moreover it is possible to promote the generation refining alloy of dynamic recrystallization
Crystal grain, the change of these two aspects can be substantially improved the superplasticforming ability of magnesium alloy.On the other hand, these nascent ternary phases
Size is thick, skewness, has the trend of self embrittlement under the effect of stress, have impact on the superplasticforming ability of alloy.
Additionally, the crystal structure of particularly W phase is also poor with matrix lattice matching degree, under the effect of high temperature stress, the interface between them is not
Stablize and occur crackle to cause material failure.(3) last, grinding of current most of AZ, ZK, Mg-Zn-Y Alloy during Superplastic
Studying carefully and focus primarily upon superplastic deformation at a temperature of higher, its superplastic deformation temperature range is 300～450 DEG C.Relevant relatively low temperature
Superplastic deformation research under the conditions of degree is relatively fewer, and does not the most report the alloy the most i.e. with superplasticity ability
Material.
From the above analysis, need to be not limited to from source the restriction of AZ, ZK and Mg-Zn-Y alloy, widen super
The composition scope of design of plasticity magnesium alloy, uses manufacturing process reasonable, simple, effective to prepare the magnesium of Superplastic Technology processing
Alloy base substrate, and then design the magnesium alloy materials under novel high strain rate and low temperature with superplasticity ability.
Relating to a kind of new alloy and preparation method thereof in the present invention, main alloying component is Mg, Zn and Er.Zn and
Er is as main alloy element, and its addition is higher, respectively 10～30wt.%Zn, and 10～15wt.%Er, and have Zn/Er
Ratio is 1～2, and surplus is Mg.This alloying component be clearly distinguishable from current report containing I phase, the Mg-Zn-RE of W phase
(rare earth element such as RE=Y, Er, Gd) alloy (containing Zn more (general 3～9wt.%), and the addition of rare earth is less,
Generally below 5wt.%).In combination with hot extrusion technique condition etc., above-mentioned alloy extrusion is processed, and then obtain a kind of low temperature
Under the conditions of there is the Mg-Zn-Er alloy of superplasticity ability.Owing to the alloy in the present invention containing substantial amounts of Zn and Er element,
A large amount of thermodynamically stable ternary phase is caused to produce, it is suppressed that the formation of Mg-Zn equal thermodynamic instability the second phase.This be after
In the continuous course of processing, dynamic recrystallization is laid a good foundation.A large amount of thermodynamically stable ternary phases promote extrusion process process
In the generation of dynamic recrystallization, inhibit again the long main trend of recrystal grain simultaneously.Therefore, with the Mg-Zn-RE reported at present
Alloy is compared, and the novel Mg-Zn-Er alloy in the present invention can have superplasticity ability within the temperature range of low temperature.
Summary of the invention
The present invention relates to a kind of new alloy and preparation method thereof, it is provided that there is in a kind of low temperature range superplasticity ability
Magnesium alloy materials.Mg-Zn-Er alloy in the present invention, in its lower temperature range, the superplasticity ability of (175～250 DEG C) is excellent
Different, breach the deficiency of current Mg-Zn-RE alloy plasticity so that prepared by alloy, manufacturing process simplifies, its superplasticity ability
Prominent, it is can the magnesium alloy materials of superplasticforming under a kind of low temperature.
In order to obtain this superplasticity ability preferable Mg-Zn-Er alloy, present invention employs the alloy of following composition: select Zn,
Er is as main alloying elements, and its addition is respectively 10～30wt.%Zn, 10～15wt.%Er, and Zn/Er ratio is
1～2, surplus is Mg.
Preparation method comprises the steps:
(1) smelting technology:
The smelting technology of the present invention is, is melted by Mg-Er intermediate alloy in 720～750 DEG C of temperature ranges, after insulation 5～15min,
The bits such as the oxide skin stirring and removing aluminium alloy surface；Then, reduce smelting temperature to 680～720 DEG C, the most above-mentioned melting
During temperature difference it is 720 DEG C, then adds magnesium ingot, stir and after the sub-insulation 5～15min that removes the gred after it melts, continue to reduce
Low temperature, to 650～680 DEG C, is 680 DEG C during the most above-mentioned smelting temperature difference, then adds Zn, stir and remove the gred；Add
Big electric current, after temperature rises to 720～750 DEG C, stirs aluminium alloy, slagging-off.Finally, aluminium alloy is incubated at such a temperature,
Stand more than half an hour, treat that aluminium alloy is cooled to 700～720 DEG C and waters and cast from mould.
(2) extrusion process:
The circular ingot processed is positioned in the holding furnace of 250～400 DEG C, is incubated 2.5～6h, take out, uniform on its surface
Graphite, ingot casting is taken out be positioned in recipient subsequently, recipient is placed on extruder fixing, utilizes reverse extrusion
Alloy cast ingot is extruded by machine, and extrusion ratio is 10～16, and extrusion temperature is 250～350 DEG C, and extrusion speed is 1～5mm/min,
The extruded bars shrend immediately that will obtain.
The scale removal layers such as above-mentioned Mg-Er intermediate alloy, pure Zn and pure magnesium, and preferably carry out preheating insulation.
Containing 2 kinds of main ternary phases in the alloy of the present invention, one is Mg3Zn6Er phase, one is Mg2Zn3Er phase.
The substantive distinguishing features of the present invention and marked improvement:
1) being prepared for a kind of novel superplasticity lightweight magnesium alloy material, it is substantially distinguished from conventional Mg-Zn-RE alloy.
2) the controlled alloyage superplasticity abilities such as alloying component, smelting technology, extruding condition are controlled.
3) common casting, the Mg-Zn-Er alloy of extrusion process exploitation is used to have significant low temperature superplasticity.
4) preparation of this alloy, processing method are simple, it is not necessary to special installation and method can obtain the alloy material that superplasticity property is excellent
Material.
5) this alloy is 50～75% at the elongation percentage of 100～150 DEG C of temperature ranges, and the elongation percentage 175～300 DEG C of temperature ranges is
100～360%.Good superplasticity (elongation percentage (δ) >=100%) is possessed within the scope of low temperature.This alloy can be straight
Connect and shape for Superplastic Technology.
Detailed description of the invention
Below in conjunction with embodiment, the present invention will be further described, but the present invention is not limited to following example.
Embodiment 1
Now by scale removal layers such as Mg-Er intermediate alloy, pure Zn and pure magnesium, and weighing dispensing, wherein the content of Zn is 10%,
In prealloy, Zn/Er ratio is 1:1.The intermediate alloy split, pure Zn and pure magnesium are positioned in heating furnace and preheat,
Preheating temperature is 200 DEG C, is incubated 1h.Preheated intermediate alloy is transferred in mild steel crucible, and at SF6/CO2Mixing
Melting is carried out under gas shield.First, smelting temperature is set as 720 DEG C, treats alloy melting, be incubated 5min, then stir
And remove the oxide skin on aluminium alloy surface, and reduce furnace temperature subsequently to 680 DEG C, add Mg, stir after magnesium fusing and remove the gred, insulation
5min.Continuation reduction furnace temperature, to 650 DEG C, is added Zn, is stirred and remove the gred after fusing.Subsequently furnace temperature is risen to 720 DEG C, stirring
Aluminium alloy also removes the gred, and is incubated the most at such a temperature, and temperature retention time is 0.5h, then after aluminium alloy is cooled to 710 DEG C
Water and cast from mould.The ingot casting of acquisition is carried out machining, it is thus achieved that circular ingot, be placed on 250 DEG C of holding furnaces subsequently
In, to take out after insulation 2.5h, be uniformly coated with graphite on its surface, be positioned in recipient and carry out reverse extrusion, extrusion ratio is 10,
Extrusion temperature is 250 DEG C, and extrusion speed is 1.5mm/min, it is thus achieved that bar immediately shrend, and coolant-temperature gage is 75 DEG C.
Bar is processed, it is thus achieved that tensile sample.Under different temperatures, strain rate is 1mm/min, and the elongation percentage of alloy is:
150 DEG C: 27%
175 DEG C: 100%
200 DEG C: 110%
225 DEG C: 140%
250 DEG C: 360%
300 DEG C: 250%
Embodiment 2
Now by scale removal layers such as Mg-Er intermediate alloy, pure Zn and pure magnesium, and weigh dispensing.Zn/Er in prealloy
Ratio is 1.5:1, and wherein the content of Zn is 15%.It is positioned in heating furnace by the intermediate alloy split, pure Zn and pure magnesium
Row preheating, preheating temperature is 200 DEG C, is incubated 1h.Preheated intermediate alloy is transferred in mild steel crucible, and at SF6/CO2
Melting is carried out under mixed gas protected.First, smelting temperature is set as 730 DEG C, treats alloy melting, be incubated 10min, then
Stirring and remove the oxide skin on aluminium alloy surface, reduction furnace temperature is to 700 DEG C subsequently, adds Mg, stirs and remove the gred after magnesium fusing,
Insulation 5min.Continuation reduction furnace temperature, to 650 DEG C, is added Zn, is stirred and remove the gred after fusing.Subsequently furnace temperature is risen to 730 DEG C,
Stirring aluminium alloy also removes the gred, and is incubated the most at such a temperature, and temperature retention time is 1h, then treats that aluminium alloy is cooled to 720 DEG C
After water and cast from mould.The ingot casting of acquisition is carried out machining, it is thus achieved that circular ingot, be placed on 350 DEG C of insulations subsequently
In stove, taking out, be uniformly coated with graphite on its surface, be positioned in recipient and carry out reverse extrusion after insulation 5h, extrusion ratio is
16, extrusion temperature is 300 DEG C, and extrusion speed is 2.5mm/min, it is thus achieved that bar immediately shrend, and coolant-temperature gage is 75 DEG C.
Bar is processed, it is thus achieved that tensile sample.Under different temperatures, strain rate is 2mm/min, and the elongation percentage of alloy is:
150 DEG C: 75%
175 DEG C: 100%
200 DEG C: 140%
225 DEG C: 135%
250 DEG C: 250%
Embodiment 3
Now by scale removal layers such as Mg-Er intermediate alloy, pure Zn and pure magnesium, and weigh dispensing.Zn/Er in prealloy
Ratio is 2:1, and wherein the content of Zn is 30%.It is positioned in heating furnace by the intermediate alloy split, pure Zn and pure magnesium
Row preheating, preheating temperature is 200 DEG C, is incubated 1h.Preheated intermediate alloy is transferred in mild steel crucible, and at SF6/CO2
Melting is carried out under mixed gas protected.First, smelting temperature is set as 750 DEG C, treats alloy melting, be incubated 15min, then
Stirring and remove the oxide skin on aluminium alloy surface, reduction furnace temperature is to 720 DEG C subsequently, adds Mg, stirs and remove the gred after magnesium fusing,
Insulation 15min.Continuation reduction furnace temperature, to 680 DEG C, is added Zn, is stirred and remove the gred after fusing.Subsequently furnace temperature is risen to 740 DEG C,
Stirring aluminium alloy also removes the gred, and is incubated the most at such a temperature, and temperature retention time is 0.5h, then treats that aluminium alloy is cooled to 720 DEG C
After water and cast from mould.The ingot casting of acquisition is carried out machining, it is thus achieved that circular ingot, be placed on 400 DEG C of insulations subsequently
In stove, taking out, be uniformly coated with graphite on its surface, be positioned in recipient and carry out reverse extrusion after insulation 2.5h, extrusion ratio is
16, extrusion temperature is 320 DEG C, and extrusion speed is 1.5mm/min, it is thus achieved that bar immediately shrend, and coolant-temperature gage is 75 DEG C.
Bar is processed, it is thus achieved that tensile sample.Under different temperatures, strain rate is 2.5mm/min, the elongation percentage of alloy
For:
150 DEG C: 35%
175 DEG C: 60%
200 DEG C: 102%
225 DEG C: 149%
250 DEG C: 200%
300 DEG C: 235%
Embodiment 4
Now by scale removal layers such as Mg-Er intermediate alloy, pure Zn and pure magnesium, and weigh dispensing.Zn/Er in prealloy
Ratio is 1.2:1, and wherein the content of Zn is 12%.It is positioned in heating furnace by the intermediate alloy split, pure Zn and pure magnesium
Row preheating, preheating temperature is 200 DEG C, is incubated 1h.Preheated intermediate alloy is transferred in mild steel crucible, and at SF6/CO2
Melting is carried out under mixed gas protected.First, smelting temperature is set as 720 DEG C, treats alloy melting, be incubated 5min, then
Stirring and remove the oxide skin on aluminium alloy surface, reduction furnace temperature is to 680 DEG C subsequently, adds Mg, stirs and remove the gred after magnesium fusing,
Insulation 5min.Continuation reduction furnace temperature, to 650 DEG C, is added Zn, is stirred and remove the gred after fusing.Subsequently furnace temperature is risen to 720 DEG C,
Stirring aluminium alloy also removes the gred, and is incubated the most at such a temperature, and temperature retention time is 0.5h, then treats that aluminium alloy is cooled to 710 DEG C
After water and cast from mould.The ingot casting of acquisition is carried out machining, it is thus achieved that circular ingot, be placed on 250 DEG C of insulations subsequently
In stove, taking out, be uniformly coated with graphite on its surface, be positioned in recipient and carry out reverse extrusion after insulation 2.5h, extrusion ratio is
10, extrusion temperature is 250 DEG C, and extrusion speed is 1.5mm/min, it is thus achieved that bar immediately shrend, and coolant-temperature gage is 75 DEG C.
Bar is processed, it is thus achieved that tensile sample.Under different temperatures, strain rate is 1mm/min, and the elongation percentage of alloy is:
150 DEG C: 75%
175 DEG C: 100%
200 DEG C: 140%
225 DEG C: 176%
250 DEG C: 253%
300 DEG C: 280%
Claims (2)
1. a superplasticity magnesium alloy, it is characterised in that select Zn, Er as main alloying elements, its addition be respectively 10～
30wt.%Zn, 10～15wt.%Er, and Zn/Er ratio is 1～2, surplus is Mg；Alloy is 100～150 DEG C of humidity provinces
Between elongation percentage be 50～75%, the elongation percentage 175～300 DEG C of temperature ranges is 100～360%.
2. the method for a kind of superplasticity magnesium alloy of preparation claim 1, it is characterised in that comprise the following steps:
(1) smelting technology:
Smelting technology is, is melted by Mg-Er intermediate alloy in 720～750 DEG C of temperature ranges, and after insulation 5～15min, stirring is also
Remove the oxide skin bits on aluminium alloy surface；Then, reduction smelting temperature, to 680～720 DEG C, adds magnesium ingot, after it melts
Stir and after the sub-insulation 5～15min that removes the gred；Continuation reduction temperature, to 650～680 DEG C, is added Zn, is stirred and remove the gred；Strengthen electricity
Stream, after temperature rises to 720～750 DEG C, stirs aluminium alloy, slagging-off；Finally, aluminium alloy is incubated at such a temperature, stands
More than half an hour, treat that aluminium alloy is cooled to 700～720 DEG C and waters and cast from mould；
(2) extrusion process:
The circular ingot processed is positioned in the holding furnace of 250～400 DEG C, is incubated 2.5～6h, take out, uniform on its surface
Graphite, ingot casting is taken out be positioned in recipient subsequently, recipient is placed on extruder fixing, utilizes reverse extrusion
Alloy cast ingot is extruded by machine, and extrusion ratio is 10～16, and extrusion temperature is 250～350 DEG C, and extrusion speed is 1～5mm/min,
The extruded bars of acquisition is carried out immediately shrend.
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| CN104894447B (en) * | 2015-04-03 | 2017-06-16 | 北京工业大学 | The magnesium-rare earth and its preparation technology of a kind of stratiform/needle-like two-phase composite strengthening |
| CN108441731B (en) * | 2018-07-07 | 2020-01-17 | 中南大学 | Coarse-grain magnesium alloy plate with superplasticity and preparation method thereof |
| CN111070814B (en) * | 2019-12-31 | 2022-01-14 | 北京工业大学 | Sandwich structure metal material and preparation method thereof |
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| CN101235454A (en) * | 2008-03-07 | 2008-08-06 | 北京工业大学 | Quasi-crystal enhancement Mg-Zn-Er heat-resistant magnesium alloy and preparation method thereof |
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| CN102605227A (en) * | 2012-03-27 | 2012-07-25 | 北京工业大学 | Magnesium alloy reinforced by nano-quasi-crystal particles and preparation method of the alloy |
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| KR101225530B1 (en) * | 2003-11-26 | 2013-01-23 | 요시히토 카와무라 | High strength and high toughness magnesium alloy and method for production thereof |
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| CN101235454A (en) * | 2008-03-07 | 2008-08-06 | 北京工业大学 | Quasi-crystal enhancement Mg-Zn-Er heat-resistant magnesium alloy and preparation method thereof |
| CN101787481A (en) * | 2010-03-22 | 2010-07-28 | 北京工业大学 | Quasicrystal intermediate alloy containing Mg-Zn-Gd radical and preparation method thereof |
| CN102294553A (en) * | 2011-07-21 | 2011-12-28 | 北京工业大学 | Magnesium alloy brazing filler metal containing rare-earth element Er and preparation method thereof |
| CN102492883A (en) * | 2011-12-28 | 2012-06-13 | 东北大学 | Magnesium alloy possessing extruding characteristic at room temperature and method for preparing extrusion material |
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