CN1469937A - High strength magnesium alloy and its preparation method - Google Patents
High strength magnesium alloy and its preparation method Download PDFInfo
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- CN1469937A CN1469937A CNA008199914A CN00819991A CN1469937A CN 1469937 A CN1469937 A CN 1469937A CN A008199914 A CNA008199914 A CN A008199914A CN 00819991 A CN00819991 A CN 00819991A CN 1469937 A CN1469937 A CN 1469937A
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Abstract
The present invention provides high strength magnesium alloys consisting essentially of 3 SIMILAR 10 wt.% Zn, 0.25 SIMILAR 3.0 wt.%, and the balance of Mg and inevitable impurities, the high strength magnesium alloy further containing 1 SIMILAR 6 wt.% Al, 0.1 SIMILAR 4.0 wt.% Si, and 0.1 SIMILAR 2.0 wt.% Ca, in order to provide a high strength magnesium alloy having an improved hardness and strength, and an excellent elongation at an ambient temperature. In addition, the present invention provides a method for preparing the high strength magnesium alloy characterized in that a Zn-Mn mother alloy is added to a magnesium melt by a fluxless melting method, and process conditions for working and heat-treating an obtained cast material.
Description
Technical field
The present invention relates to high-strength magnesium alloy and the method that is used to prepare this magnesium alloy, more particularly, relate to a kind of by add specific alloying element or change comprise magnesium alloy that the processing condition of specific heat treatment obtain with and cheap working method, described magnesium alloy has the mechanical property that comprises intensity, hardness and extensibility of improvement, and has formability, high strength and the extensibility of improvement simultaneously.
Background technology
In magnesium alloy, Mg-Zn base alloy shows excellent time hardening.These alloys show quite high intensity and toughness, and have the advantage aspect workability and weldability.On the other hand, owing to interpolation Zn in Mg is easy to increase the formation of micropore in castingprocesses, thus be difficult for Mg-Zn base alloy is carried out the casting processing of for example die casting, thereby the basic alloy of Mg-Zn also has shortcoming.
And then there is restriction in this Mg-Zn base alloy aspect the raising intensity, and this is because compare with other magnesium alloy, is not easy to make the microtexture refinement by adding alloying element or overheated thermal treatment.This limitations restrict they use at coml.
In order to address these problems, obtained the achievement in research of in the Mg-Zn alloy, adding alloying element.The example of these achievements in research is as follows.
In nineteen forty-seven, J P Doan and G Ansel have proposed a kind of method, wherein, Zr is added in the Mg-Zn base alloy so that the grain-size of alloy is carried out refinement, thereby improve the intensity (J P Doan and G Ansel, Trans.AIME.vol 171 (1947), the 286-295 page or leaf) of alloy.Yet, in these methods, so be difficult in the molten mass of magnesium, add Zr owing to Zr has high-melting-point.
Add rare earth element in the Mg-Zn alloy, for example La, Ce or Nd or Th also are known.Known this method has can reduce the advantage that micropore formed and improved intensity at high temperature and improves weldability.Yet, compare with other magnesium alloy, because alloying element is very expensive, this method has slightly gesture of tangible cost.
In 1987, W Unsworth has reported with J F King can be by adding Cu refinement β 1 ' mutually in the Mg-Zn alloy, thereby improve the toughness of Mg-Zn, wherein β 1 ' is the main reinforcement precipitated phase of Mg-Zn alloy (W Unsworth and J F King mutually, MagnesiumTechnology, The Inst of Metal, 1987, the 25-35 pages or leaves).Yet although can slightly increase extensibility according to the amount of the element that is added, the interpolation of Zn and Cu has produced at ambient temperature the limited extensibility less than 10%.
The tensile properties of following table 1 expression coml casting alloy and wrought alloy.
Table 1
The characteristic of coml magnesium alloy
Composition (%) tensile properties
Surrender stretches and extends
Strength rate alloy A l Mn Th Zn Zr other (MPa) is (%) casting AZ91C-8.7 0.13-0.7--145 275 6EQ21A-----0 1.5Ag 195 235 2HK31A---3-0-105 220 8WE54A-----0 5.2Y 172 250 2ZC63A--0.25-6.0-2.7Cu 125 210 4ZE63A----5.8 0 2.6RE 190 300 10ZK61A----6.0 0-195 310 10 die casting AM60A-6.0 0.13----115 205 6AS41A-F 4.3 0.35---1.0Si 150 220 4AZ91A (MPa), B 9.0 0.13-0.7--150 230 3 extruding AZ80A-8.5--0.5--275 380 7M1A-F-1.2----180 255 12ZC71-F-0.5-1.0-6.5-1.2Cu 340 360 5HM31A--1.2 3---230 290 10ZK60A----5.5 0-305 365 11 sheet material AZ31B-3.0--1.0--220 290 15HK31A---3-0-200 255 9HM21A--0.6 2---170 235 11PE 3.3--0.7-----
With reference to table 1, can find to compare with the coml casting alloy, the coml wrought alloy shows higher yield strength, tensile strength and unit elongation usually.Yet,, still be difficult to make existing commerce to obtain the combination of high strength and high-elongation with wrought alloy even under the situation of these wrought alloys.That is, the high-strength alloy that shows above the high tensile of 300MPa exists its unit elongation to be difficult to surpass about 10% shortcoming.And there has been report to point out, under the situation of the alloy of interpolation Zn that shows excellent specific property aspect the intensity and Zr, in the preparation technology who adds Zr, had many restrictions.
U.S. Patent No. 4,997,622 disclose the characteristic of utilizing by the magnesium alloy of fast-curing process method preparation.According to this patent, magnesium alloy by fast-curing process method preparation shows yield strength, tensile strength and the unit elongation that has improved.Yet up-to-date result of study shows that with existing commerce alloy phase ratio, these alloys have very high tooling cost and limited application.
Summary of the invention
The purpose of this invention is to provide a kind of high-strength magnesium alloy, interpolation according to alloying element, this high-strength magnesium alloy shows in the refinement of microtexture and separates out improvement aspect the characteristic, enhancing aspect mechanical characteristics, for example hardness, intensity and unit elongation, and the improvement aspect formability, alloying element is compared more cheap with the element that is used for Mg-Zn base alloy traditionally.
Another object of the present invention provides a kind of method that is used to prepare high-strength magnesium alloy, described high-strength magnesium alloy is compared the unit elongation that shows obvious excellence with intensity, this method adopts optimum heat treatment conditions, and the present invention also is provided for the processing conditions of this preparation method's economy.
According to a scheme, the invention provides a kind of high-strength magnesium alloy, basic Zn by 3~10wt%, the Mn of 0.25~3.0wt%, surplus is that Mg and unavoidable impurities are formed.
This magnesium alloy may further include the Al of 1~6wt%.And this magnesium alloy may further include the Si of 0.1~4.0wt%, perhaps the combination of the Ca of the Si of 0.1~4.0wt% and 0.1~2.0wt%.Preferably, the content of Al is no more than the content of Zn.
Preferably, the content of Zn is 5.0~7.0wt%, and the content of Mn is 0.75~2.0wt%, and the content of Si is 1.5~3.0wt%, and the content of Ca is 0.3~1.0wt%.
Key character of the present invention is that Al is added in the Mg-Zn base alloy as alloying element, to obtain the reduction of yield strength, thereby produce the improvement of formability and the enhancing of work hardening capacity, thereby a kind of high-strength magnesium alloy with high strength and high-elongation is provided.
According to another scheme, the invention provides a kind of method that is used to prepare high-strength magnesium alloy, wherein, adding Mn in the molten mass of magnesium is to realize by add the Zn-Mn mother alloy in the molten mass of magnesium.
Preferably, has the Zn-Mn mother alloy that Mn content is 10~20wt% (Zn-10~20wt%Mn mother alloy) by in 670 to 720 ℃ temperature range, in the molten mass of magnesium, adding, and in the molten mass of magnesium, add Zn or add Zn, prepare high-strength magnesium alloy with the form of ingot casting with Al.Perhaps, can be preferably by in 670 to 720 ℃ temperature range, in the molten mass of magnesium, adding the mother alloy of Zn-10~20wt%Mn, and the Mg-Si mother alloy is added in the molten mass of magnesium, and add in the molten mass of magnesium with Al and/or Ca with Zn or with Zn, prepare high-intensity magnesium alloy with the form of ingot casting.
Preferably, the homogenizing that ingot casting can stand in 340 to 410 ℃ temperature range 6 to 12 hours is subsequently handled, to form blank.Blank can carry out mechanical workout to this blank preheat 30 minutes to 2 hours in 150 to 400 ℃ temperature range after.
More preferably, processed or quilt forges body can stand 24 to 96 hours ageing treatment first in 70 to 100 ℃ temperature range, and stands 48 hours in 150 to 180 ℃ temperature range subsequently or longer secondary ageing processing.
Before twice ageing treatment, can in 340 to 410 ℃ temperature range, carry out 6 to 12 hours solution heat treatment.Perhaps, before twice ageing treatment, can carry out 3 to 7% stretching.
The reason that the composition range of each alloying element that the present invention uses is limited in the above-mentioned scope is as follows:
Zinc(Zn):3~10wt%
Under 340 ℃, the maximum solid solution degree limit of Zn in the Mg matrix is 6.2wt%.Under the situation of adding 3.0wt% or more Zn in the Mg matrix, Zn forms the needle-like precipitated phase when through heat-treated, thereby shows aging hardening behavior.Usually the content of Zn is determined according to its solid solubility limit.When the Zn that adds near the about 5.0~7.0wt% of its maximum solid solution degree ultimate, may obtain maximum aging hardening behavior.Under common aging temp, when Zn content is not more than 3.0wt% corresponding to minimum solid solubility limit, because the formation of precipitated phase is insufficient, so be difficult to expect required precipitation strength phenomenon.On the other hand, when the addition of Zn be 10.0wt% or when higher, in the enhancing of separating out of crystal boundary place equilibrium phase.As a result, may produce the reduction of mechanical characteristics.Therefore according to the present invention, the content of Zn is limited in the scope of 3~10wt%, be preferably limited in the scope of 5.0~7.0wt%.
Manganese (Mn): 0.25~3.0wt%
Corresponding under 650 ℃ of the fusing point of Mg, the maximum solid solution degree limit of Mn in the Mg matrix is about 2.2wt%.At a lower temperature, the solid solubility limit of Mn descends rapidly, thereby Mn can be present in the form of α-Mn in the Mg matrix.Usually known, in magnesium alloy, when the addition of Mn is 0.1wt% or when higher, Mn is used to improve corrosion stability.The purpose of adding Mn is except improving corrosion stability, for example also is used to the purpose strengthened, can be used to improve the intensity of alloy product when its content is 0.25~2.0wt%, although its effect may change to some extent because the matrix alloy of alloy product is different.Especially, the inventor etc. test discovery, when the forging body stands ageing treatment after solution heat treatment, are present in the Mn that forges in the body and play the effect of the precipitated phase of refinement Mg-Zn binary alloy, thereby play the effect that improves intensity and improve unit elongation.According to this fact, the interpolation of Mn makes that alloy according to the present invention is strengthened.In this, according to the present invention the minimum content of Mn is defined as 0.25wt%.Consider the maximum solid solution degree limit of Mn and the treatment process that is adopted, adopt common melting process to be difficult to add a large amount of Mn.When adding 3.0wt% or more during the Mn of volume, Mn mainly exists in matrix with the form of α-Mn.Therefore, superfluous Mn causes unwanted results on the contrary for the not contribution of the characteristic of improving alloy aspect preparation cost.Therefore, according to the present invention, the content of Mn is limited in the scope of 0.25~3.0wt%, preferably in the scope of 0.75~2.0wt%.
Aluminium (Al): 1~6wt%
In the Mg matrix, Al shows the maximum solid solution degree limit of about 12wt% under 437 ℃.Knownly pass through the thermal treatment adopted, can in the Mg-Al binary alloy, form Mg
17Al
12Precipitated phase.Yet, according to interpolation and this Mg of Al of the present invention
17Al
12The formation of precipitated phase is irrelevant.According to the present invention, the interpolation of Al is used for improving the main strengthening phase of Mg-Zn-Mn base ternary alloy, that is, and and Mg-Zn base needle-like precipitated phase.Therefore, consider heat treated temperature range, the content of the scope of aging temp and the Zn that adds as main alloying element for example, the content of Al are determined the scope that produces the limited formation of Mg-Al base precipitated phase at one.Because in aging range, the solid solubility limit of Al in the Mg matrix is equivalent to about 1wt%, so the smallest limit of Al content is defined as 1.0wt%.In order to limit the formation of the Mg-Al base precipitated phase that content that amount surplus owing to Al surpassed Zn causes, the upper limit of Al content is confirmed as 6.0wt%.Simultaneously, when the addition of Al is significantly higher than the addition of Zn, form Mg-Al base precipitated phase, i.e. Mg
17Al
12The possibility of precipitated phase enlarges markedly.Under certain thermal treatment temp, this precipitated phase may be separated out in the grain boundary even in crystal grain inside thickly.Because this precipitated phase is highly brittle,, thereby cause strength degradation so this precipitated phase provides the path of fracture when alloy fracture aspect intensity.Thereby, wish the content of the content of Al less than Zn.The inventor etc. find by test, even do not carry out solution heat treatment to forging body, be present in the send as an envoy to effect of needle-like precipitated phase refinement of the Al performance of forging in the body, although and yield strength slightly descend, but can significantly improve tensile strength, especially improve unit elongation.Find that also the increase of Al content causes the decline of yield strength, causes the increase of tensile strength simultaneously.
Silicon (Si): 0.1~4.0wt%
Because silicon is difficult to be dissolved in the Mg matrix, so when adding in Mg as alloying element it, Si forms Mg
2The Si phase.If in preparation of forging body and heat treatment step its form and/or size are adjusted, this composition can provide dispersion-strengthened effect.The inventor finds by test, in the time of in Si being added to Mg-Zn-Al-Mn base quad alloy, can obtain above-mentioned required dispersion-strengthened effect.When the content of Si during less than 0.1wt%, the desired result that adds Si is difficult to realize.When the content of Si during, form thick Mg greater than 4.0wt%
2Si, thus the decline of unit elongation caused.In this regard, according to the present invention, the content of Si is limited in the scope of 0.1~4.0wt%, preferably is limited in the scope of 1.5~3.0wt%.
Calcium (Ca): 0.1~2.0wt%
Under the situation of the Mg alloy that contains Si,, improve Mg simultaneously by the grain-size that interpolation Ca can reduce alloy
2The form of Si phase.To this,, Ca is added in the Mg-Zn-Al-Mn alloy that contains Si according to the present invention.When Ca content was less than 0.1wt%, very difficult expectation can be observed Mg
2The Si phase improve effect.On the other hand, be 2.0wt%, when significantly having surpassed 516 ℃ during the maximum solid solution degree limit of the 1.34wt% of Ca in the Mg matrix, form Mg when the add-on of Ca
2The Ca precipitated phase.Because this Mg at the place, grain boundary
2The Ca precipitated phase is except improving Mg
2The effect of Si phase has also reduced intensity.The inventor etc. found through experiments, and when Ca content is 0.3~1.0wt%, can more effectively control the Mg that is formed in the Mg-Zn-Al-Mn alloy
2The form of Si phase, therefore and obtain the raising of intensity and unit elongation.In this regard, according to the present invention, the content of Ca is limited in the scope of 0.1~2.0wt%, and preferred in the scope of 0.3~1.0wt%.
In addition, should suitably limit the major impurity of Mg alloy, because they mainly have fatal detrimental action aspect the corrosion stability of alloy, rather than aspect the mechanical property of alloy.Common known impurity comprises: Fe, Ni and Cu.Although Cu has disadvantageous effect for corrosion stability in widely used Mg-Al base alloy, its not significantly effect in Mg-Zn base alloy according to the present invention.For Mg-Zn according to the present invention base alloy, Fe and Ni are considered to the impurity that need be limited its content.Usually, these impurity conservatively are limited to the maximum level of 0.005wt%.The disadvantageous effect that Fe causes can be eliminated by adding Mn.Under the situation of Mg alloy, by with the ratio of the content between Fe and the Mn, Fe/Mn is reduced to smaller or equal to 0.032, and the disadvantageous effect of Fe is minimized.Because mainly needs add Mn according to the present invention, as long as the content of Fe just can be eliminated the disadvantageous effect of Fe to corrosion stability effectively less than the conservative limit.Under the situation of Mg alloy, all the other impurity comprise Fe, Ni and Cu, and its total content is limited in the maximum level of 0.3wt% usually.
Adopt the preparation method of the present invention of no flux scorification (fluxless melting method), handled outside the above-mentioned specific composition, also has an important feature, promptly, owing to consider this fact in the magnesium that can not utilize the method that directly Mn is melted in the fused magnesium Mn to be added to fusing, so the form with the Zn-Mn mother alloy is added Mn, this is because Mn has very high fusing point.At the commitment of magnesium alloy development, adopt the method for adding Mn with the form of flux.Because there is incendiary danger in fused magnesium in being exposed to air the time, thus a kind of flux that fused magnesium and air are separated of being used for adopted, thus prevent incendiary danger.For this flux, the flux that adopts the Mn interpolation traditionally is so that add required Mn.In this case, Mn is deep in the melt by diffusion.In this method, to the addition existence restriction of Mn.And then, be difficult to control the content of impurity.Therefore, this method has produced relevant many difficulties with the preparation of required alloy.After no flux melting method is popularized, because the surperficial protected gas of melt covers, so the main interpolation of adopting the method for adding Mn to realize Mn with the form of Mg-Mn mother alloy.According to this method, in can preventing fused magnesium incendiary protective atmosphere, Mn is added in the fused magnesium that is heated to certain temperature, Mn is directly fusion under this temperature.Therefore, the Mg-Mn mother alloy can prepare separately.Adopt no flux scorification to prepare in the alloy, adopting the Mg-Mn mother alloy for preparing to add the Mn of aequum.Yet this method need dispose expensive melting unit, so that control given atmosphere.And, because magnesium at high temperature shows high-vapor-pressure, so in the preparation process of mother alloy, may lose a large amount of magnesium.Therefore, the increase of adopting the method for Mg-Mn mother alloy to produce the technology cost.After a series of test, discoveries such as the inventor are adopting no flux method to carry out alloy when preparing, and employing is added Mn in the fused magnesium method with the form of low-melting Zn-Mn mother alloy, can realize the interpolation of Mn effectively.According to this method, can eliminate a large amount of losses of magnesium melt incendiary possibility or material.Therefore, can realize the cheapness preparation of magnesium alloy.Can also be easily and control foreign matter content easily.
Preferably, be approximately 650 ℃ although consider the fusing point of magnesium, but under 670 ℃ temperature, could guarantee this fact of sufficient flowability of magnesium melt at least, the incendiary possibility increases this fact when surpassing 720 ℃ with the temperature of magnesium melt, the scope of the temperature limitation of the Zn-Mn mother alloy being added to the magnesium melt at 670 to 720 ℃.The Zn-Mn mother alloy is preferably that to have Mn content be Zn-10~20wt%Mn composition of 10 to 20wt%, so that fusing fully in the said temperature scope of magnesium melt.More preferably, in the process of the Zn-Mn mother alloy being added in the magnesium melt, stir.
Form with the Mg-Si mother alloy is added Si.Preferably, consider the high-melting-point of mother alloy and need be suppressed at the burning of magnesium bath surface, fix in 700 to 720 ℃ the scope adding temperature limit that Si carries out.In this case, in the process of adding mother alloy, more preferably stir.
Owing to lack zinc, so add Zn with Al individually.At this moment can add Ca selectively.Zn prepares at alloy and shows high vapour pressure under the employed temperature, preferably, carries out the interpolation of Zn after the stove process for cooling that the magnesium melt is carried out, so that reduce the Zn loss.Consider the flowability of magnesium melt, stove is cold can to proceed to about 670 ℃.More preferably in the process of adding these elements, stir.
Then, resulting Mg melt casting is become ingot casting.Preferably, after magnesium melt stove is as cold as 660 to 670 ℃, cast, produce heat from the Mg melt so that prevent as much as possible.
Preferably, the casting alloy ingot casting according to method for preparing is carried out homogenizing handles, with the segregation of eliminating issuable alloying element in castingprocesses and since the forging body that segregation causes in the ununiformity aspect the characteristic.Consider to make that the precipitated phase of i.e. Zn generation fully dissolves and produce the condition of required alloy thermostability, carries out 6 to 12 hours equal thermal treatment under 340 to 410 ℃ by main alloying element.
Then, ingot casting is formed blank to be extruded.Preferably, can be under 150 to 400 ℃ temperature preheating 30 minutes to 2 hours, then, in same temperature range, comprise the machining processes of extruding, rolling, forging, die forging and drawing.Usually, magnesium alloy does not have required workability at ambient temperature.Therefore, in order to obtain flawless forging body, magnesium alloy is carried out hot mechanical workout.According to the present invention, processing temperature is determined in the scope of the zero defect that can guarantee to forge body by test.
Preferably, under 70 to 100 ℃,, be right after after timeliness operation first, under 150 to 180 ℃ temperature, carried out 48 hours or the secondary ageing of longer time forging the timeliness first that body carried out 24 to 96 hours.At the main precipitated phase that is not higher than Mg-Zn base alloy, be to carry out ageing treatment first under the temperature of G, P district solvus temperature of β 1 phase, carry out secondary ageing under the temperature of aging temp first and handle being higher than then, this dual timeliness can make precipitated phase to improving the effect maximization of intensity.Therefore, according to the present invention, aging temp is limited in 70 to the 100 ℃ lower slightly scope of G, P district solvus temperature than common known β 1 ' phase first, and aging time is confirmed as being enough to wish hardness is brought up to for some time of required level first.And second aging temp is limited in 150 to 180 ℃ the scope.Under less than 150 ℃ second aging temp,, exist and the relevant problem of enforcement ageing treatment owing to need a large amount of time up to obtaining highest hardness.Surpass under 180 ℃ second aging temp at one, although can promptly obtain highest hardness, the highest hardness that is obtained but can not reach required level.
More preferably, before dual ageing treatment, under 340 to 410 ℃ temperature, carry out 6 to 12 hours solution heat treatment to forging body, described temperature range is corresponding with the temperature range that issuable precipitated phase in the course of processing can exist with the form of sosoloid, so that make precipitated phase to improving the effect maximization of intensity.Consider can make by main alloying element, be the condition that precipitated phase that Zn produces fully dissolves and obtain required alloy thermostability, the cycle of this temperature range and solution heat treatment is to determine according to the phasor of Mg-Zn binary system.
Simultaneously, more preferably, before dual ageing treatment, extend processing.Usually, according to before thermal treatment by the strain measured to the tension test of alloy, will be referred to strengthen the target alloy and elongation in the heat treatment process process of carrying out is limited in from elastic limit to maximum strength ultimate scope.Therefore, according to the present invention, elongation is limited in 3% to 7% the scope.
According to the present invention, compare with wrought alloy with existing commerce, can make and have, the cheap high-strength magnesium alloy that unit elongation improves with respect to intensity.That is, with of intensity maximum in the existing commercial extruded alloy of describing in the table 1, i.e. ZC71 alloy phase ratio, magnesium alloy of the present invention can show the unit elongation that improves with interest, and keeps simultaneously and strength level like the ZC71 alloy type.According to the present invention, do not adopt the alloying element of unmanageable costliness, for example radioelement is such as Th or the alloying element that has difficulties in the interpolation relevant with preparation technology, and for example Zr also can prepare high-intensity alloy.According to the present invention,,, can reduce the loss of material, and therefore reduce preparation cost so compare with the existing method of adding Mn with the form of Mg-Mn mother alloy because Mn adds with the form of Zn-Mn mother alloy.
The accompanying drawing summary
After reading following detailed description in conjunction with the accompanying drawings, above-mentioned purpose of the present invention and other feature and advantage will become clearer.
Fig. 1 a is the Photomicrograph of Mg-Zn base binary alloy squeezing prod (Z6);
Fig. 1 b and 1c are added with the Mg-Zn base alloy of Mn and the Photomicrograph of the squeezing prod of the Mg-Zn base alloy (ZM61 and ZAM621) that is added with Al and Mn;
Fig. 1 d and 1e are respectively the photos that shows of squeezing prod that is added with the Mg-Zn base alloy of Al, Mn and Si and is added with the Mg-Zn base alloy (ZAM631+2.5Si and ZAM631+2.5Si+0.4Ca) of Al, Mn, Si and Ca;
Fig. 2 is the graphic representation that is illustrated in the aging hardening behavior that Mg-Zn base binary alloy squeezing prod (Z6) shows in the ageing treatment process;
Fig. 3 is illustrated in the dual ageing treatment process, be added with the Mg-Zn base alloy extrusion (ZM61) of Mn and be added with the aging hardening behavior that the cast article of the basic alloy extrusion of Mg-Zn (ZAM621) of Al+Mn shows respectively, with in dual ageing treatment process, the graphic representation that the aging hardening behavior of the squeezing prod (Z6) of Mg-Zn base binary alloy is compared;
Fig. 4 is illustrated in the aging hardening behavior that the Mg-Zn base alloy extrusion (ZM61) that is added with Mn in the process of carrying out dual ageing treatment after the solution heat treatment and the cast article that is added with the Mg-Zn base alloy extrusion (ZAM621) of Al+Mn show respectively, the graphic representation of comparing with the aging hardening behavior of the basic binary alloy squeezing prod of Mg-Zn when carrying out identical processing (Z6).
Fig. 5 is the graphic representation of aging hardening behavior separately that is added with the Mg-Zn base alloy extrusion (ZAM631+2.5Si) of Al+Mn+Si and is added with the basic alloy extrusion of Mg-Zn (ZAM631+2.5Si+0.4Ca) of Al+Mn+Si+Ca in dual ageing treatment process;
Fig. 6 is that expression is added with the Mg-Zn base alloy extrusion (ZM61) of Mn and is added with the tensile properties that the cast article of the Mg-Zn base alloy extrusion (ZAM621) of Al+Mn shows at ambient temperature, the graphic representation of comparing with the tensile properties that the basic binary alloy squeezing prod of Mg-Zn (Z6) shows at ambient temperature;
Fig. 7 is the graphic representation of representing to be added with the Mg-Zn base alloy extrusion (ZAM631+2.5Si) of Al+Mn+Si respectively and being added with the tensile properties that the basic alloy extrusion of Mg-Zn (ZAM631+2.5Si+0.4Ca) of Al+Mn+Si+Ca shows at ambient temperature;
Fig. 8 is illustrated in after the dual ageing treatment, be added with the Mg-Zn base alloy extrusion (ZM61) of Mn and be added with the tensile properties that the cast article of the basic alloy extrusion of Mg-Zn (ZAM621) of Al+Mn shows respectively at ambient temperature, with after dual ageing treatment, the graphic representation that the tensile properties that Mg-Zn base binary alloy squeezing prod (Z6) shows is compared;
Fig. 9 is illustrated respectively in after the dual ageing treatment, is added with the Mg-Zn base alloy extrusion (ZAM631+2.5Si) of Al+Mn+Si and is added with the graphic representation of the tensile properties that the basic alloy extrusion of Mg-Zn (ZAM631+2.5Si+0.4Ca) of Al+Mn+Si+Ca shows;
Figure 10 is illustrated in solution heat treatment to carry out after the dual ageing treatment afterwards, be added with the Mg-Zn base alloy extrusion (ZM61) of Mn and be added with the tensile properties that the cast article of the basic alloy extrusion of Mg-Zn (ZAM621) of Al+Mn shows respectively at ambient temperature, the graphic representation of comparing with the tensile properties that Mg-Zn binary alloy squeezing prod (Z6) after carrying out identical processing shows at ambient temperature;
Figure 11 is illustrated in and carries out dual ageing treatment after 5% the extension processing and be added with the Mg-Zn base alloy extrusion (ZM61) of Mn later on and be added with the tensile properties that the cast article of the basic alloy extrusion of Mg-Zn (ZAM621) of Al+Mn shows respectively at ambient temperature, the graphic representation of comparing with the tensile properties that Mg-Zn binary alloy squeezing prod (Z6) when carrying out identical processing shows.
The best mode that carries out an invention
Now, describe in detail according to high-strength magnesium alloy of the present invention with reference to following embodiment
According to the present invention, preparation has the alloy casting product of predetermined component described in the following table 2 respectively.In the preparation of each alloy casting product, the fusing of unprocessed alloy and alloying element is to adopt no flux melts method to realize, in this method, with CO
2+ 0.5%SF
6Mixed gas is sprayed on the whole surface of melt with 2l/ minute flow velocity.In melting treatment, adopt Steel Crucible.Under 700 ℃ temperature, Mn is added in the melt with the form of Zn-15wt%Mn mother alloy.Then, utilize agitator that melt was stirred 5 minutes, be cooled to 670 ℃ with the cold form of stove then.In the refrigerative melt, add Zn separately or with Al, stirred then 2 minutes.Relating under the situation of adding Si, Si is added in the melt with the form of Mg-10wt%Si mother alloy.In this case, under 720 ℃, the gained melt was stirred 10 minutes.After agitating procedure was finished, the form cold with stove was cooled to 670 ℃ with melt.In the refrigerative melt, add Zn separately or with Al and/or Ca, stirred then 2 minutes.After this, the melt stove is chilled to 660 ℃.At last, with the crucible thorough impregnation in the water that keeps at ambient temperature.Like this, prepare the alloy casting product.
Table 2
The predetermined component of embodiment interalloy
Predetermined component (wt%) embodiment alloy Zn Al Mn Si Ca Mg
1 Z6 6----surplus
2 ZM60 6-0.5--surplus
3 ZM61 6-1--surplus
4 ZM62 6-1.5--surplus
5 ZAM611 61 1--surplus
6 ZAM621 62 1--surplus
7 ZAM631 63 1--surplus
8 ZAM641 64 1--surplus
9 ZAM661 66 1--surplus
10 ZAM631+2.5Si, 631 2.5-surplus
11 ZAM631+2.5Si+0.4Ca, 631 2.5 0.4 surpluses
In order to control the microtexture of each alloy casting product of preparation as mentioned above, the homogenizing of under 340 to 410 ℃ temperature the alloy cast article being carried out 12 hours is handled.Then the alloy casting product is formed blank, then, under 320 to 360 ℃ temperature, blank is carried out 30 minutes preheating.Utilize extrusion machine that this blank is pushed then, wherein, the temperature of blank reservoir and mould is set in 320 to 360 ℃.Like this, can prepare the extruded alloy product.
Fig. 1 a, 1b and 1c are respectively the Z6, the ZM61 that prepare as mentioned above and the Photomicrograph of ZAM621 alloy extrusion.Fig. 1 d and Fig. 1 e are respectively the Photomicrographs of ZAM631+2.5Si and ZAM631+2.5Si+0.4Ca alloy extrusion.With reference to Fig. 1 a to 1e, the Z6 alloy is traditional magnesium alloy, and its grain-size is approximately 22 μ m, and is respectively about 12 μ m and about 8 μ m according to the grain-size of ZM61 of the present invention and ZAM621 alloy.The grain-size of ZAM631+2.5Si and ZAM631+2.5Si+0.4Ca alloy is respectively about 12 μ m and about 6 μ m.
Therefore, can find that when the Mn with the 1wt% amount added in traditional Mg-Zn alloy, the microtexture grain-size of alloy reduced about 1/2.Can also find that be added with traditional Mg-Zn alloy of 1wt% and 2wt%Al, its grain-size reduces about 1/3.Under the situation of ZAM631+2.5Si+0.4Ca alloy, promptly when when the ZAM631+2.5Si alloy adds the Ca of 0.4wt%, the grain-size that it has about 6 μ m is equivalent to about 2/3 of ZAM621 alloy grain size.Therefore, can find that according to alloy of the present invention, for the alloy that adds Mn and Al, it is about 2/3 that the grain-size that obtains is reduced to, the alloy for add Si and Ca with Mn and Al is about 3/4.
Fig. 2 is illustrated in the ageing treatment process, the graphic representation of the aging hardening behavior that Mg-Zn base binary alloy squeezing prod (Z6) shows.To the Z6 alloy extrusion, carry out single ageing treatment and dual ageing treatment, to obtain improving of hardness and intensity respectively the biglyyest.The Z6 alloy extrusion carried out 48 hours timeliness first under 90 ℃, then, carry out 384 hours secondary ageing under 180 ℃, secondary ageing is to carry out under the condition of in the secondary ageing process variation of aging hardening behavior periodically being measured.In Fig. 2, expressed the variation of measured aging hardening behavior.With reference to Fig. 2,, can find to show the increase of highest hardness and obtain reducing of required time of highest hardness through the alloy of dual ageing treatment with alloy phase ratio through single ageing treatment.
Fig. 3 is illustrated in the dual ageing treatment process, be added with the Mg-Zn base alloy extrusion (ZM61) of Mn and be added with the aging hardening behavior that the cast article of the Mg-Zn base alloy extrusion (ZAM621) of Al+Mn shows respectively, the graphic representation of comparing with the aging hardening behavior that the squeezing prod (Z6) of the basic binary alloy of Mg-Zn in dual ageing treatment process shows.Under 70 ℃, respectively Z6, ZM61 and ZAM621 alloy extrusion are carried out 48 hours timeliness first, carry out 384 hours secondary ageing then under 150 ℃, secondary ageing is to carry out under the condition of in the secondary ageing process variation of aging hardening behavior periodically being measured.Expressed the variation of the aging hardening behavior of measuring among Fig. 3.Can find with reference to Fig. 3, with Z6 alloy phase ratio, the ZAM621 alloy of Al by adding 2wt% in the Z6 alloy and the Mn preparation of 1wt% is being squeezed and is showing hardness under the state and improved approximately 35%, and has improved about 20% being subjected to showing hardness under the state of maximum dual ageing treatment.Yet,,, do not have in the ag(e)ing process or almost do not show hardening effect although under squeezed state, show high rigidity by only in Z6, adding the ZM61 alloy that Mn prepares.And the highest hardness of ZM61 alloy is lower than the Z6 alloy.
Fig. 4 is illustrated in solution heat treatment to carry out in the process of dual ageing treatment afterwards, be added with the Mg-Zn base alloy extrusion (ZM61) of Mn and be added with the aging hardening behavior that the cast article of the Mg-Zn base alloy extrusion (ZAM621) of Al+Mn shows respectively, the graphic representation of comparing with the aging hardening behavior of the basic binary alloy squeezing prod of Mg-Zn when carrying out identical processing (Z6).Every kind of Z6, ZM61 and ZAM621 alloy extrusion at first stand 12 hours solution heat treatment under temperature remains on 380 to 410 ℃ condition.After the solution heat treatment, each alloy is carried out dual ageing treatment.In Fig. 4, expressed the aging hardening behavior of each alloy that produces by dual ageing treatment.Can find that with reference to Fig. 4 when when the Z6 alloy adds Mn separately or with Al, base table reveals the raising of hardness in age hardening is handled.The interpolation of one or more alloying elements based on highest hardness, can make hardness improve 10% or more.Especially, by only adding ZM61 alloy aging hardening characteristics that Mn prepares with significantly different at the aging hardening behavior that does not carry out before the dual ageing treatment showing under the heat-treat condition of solution heat treatment, hardness obtains significant the raising under described heat-treat condition.The highest hardness of ZM61 alloy with add ZAM621 alloy type that Al and Mn prepare simultaneously seemingly.
Fig. 5 is in dual ageing treatment process, is added with the Mg-Zn base alloy extrusion (ZAM631+2.5Si) of Al+Mn+Si and is added with the graphic representation of other aging hardening behavior of branch of the basic alloy extrusion of Mg-Zn (ZAM631+2.5Si+0.4Ca) of Al+Mn+Si+Ca.After extruding, under 70 ℃, respectively ZAM631+2.5Si and ZAM631+2.5Si+0.4CA alloy are carried out 48 hours timeliness first, 150 ℃ of secondary ageing of carrying out preset time, secondary ageing is to carry out under the condition of in the secondary ageing process variation of aging hardening behavior periodically being measured then.Can find with reference to Fig. 3 and Fig. 5, at alloy under 150 ℃ of conditions that stand maximum dual ageing treatment, it is about 12% that the hardness that can make the Ca that adds the Si of 2.5wt% and 0.4wt% to the ZAM631 alloy improves, and significantly reduce to obtain the required time of highest hardness.
Table 3
Alloy yield strength tensile strength unit elongation
(MPa) (MPa) (%)
Z6 126 292 28
ZM60 211 309 26
ZM61 223 313 26
ZM62 220 314 24
ZAM611 188 319 28
ZAM621 178 338 27
ZAM631 169 356 25
ZAM641 185 364 26
ZAM661 225 359 26
ZAM631+2.5Si 143 271 10
ZAM631+2.5Si+0.4Ca 150 371 16
Fig. 6 is that expression is added with the Mg-Zn base alloy extrusion (ZM61) of Mn and is added with the tensile properties that the cast article of the Mg-Zn base alloy extrusion (ZAM621) of Al+Mn shows respectively at ambient temperature, the graphic representation of comparing with the tensile properties that the basic binary alloy squeezing prod of Mg-Zn (Z6) shows at ambient temperature.Can find with reference to Fig. 6, separately or in the Z6 alloy, add Mn with Al and make the yield strength and the ultimate tensile strength that under squeezed state, show significantly improve.Adopting under the as-forged condition of extrusion process, alloy shows 25% or higher excellent unit elongation.Detailed result has been described in above-mentioned table 3.
Fig. 7 is that expression is added with the Mg-Zn base alloy extrusion (ZAM631+2.5Si) of Al+Mn+Si and is added with the graphic representation of the tensile properties that the basic alloy extrusion of Mg-Zn (ZAM631+2.5Si+0.4Ca) of Al+Mn+Si+Ca shows respectively at ambient temperature.Can find that with reference to Fig. 7 the Si of interpolation 2.5wt% and 0.4% Ca have produced the raising that shows ultimate tensile strength under the squeezed state in the ZAM631 alloy.Adopting under the as-forged condition of extrusion process, this alloy shows 16% or bigger excellent unit elongation.Detailed result has been described in above-mentioned table 3.
Table 4
Alloy yield strength tensile strength unit elongation
(MPa) (MPa) (%)
Z6 237 314 26
ZM60 248 305 26
ZM61 253 314 28
ZM62 248 307 24
ZAM611 281 344 23
ZAM621 265 360 25
ZAM631 245 385 27
ZAM641 255 387 22
ZAM661 256 355 22
ZAM631+2.5Si 265 317 7
ZAM631+2.5Si+0.4Ca 234 398 12
Fig. 8 is illustrated in after the dual ageing treatment, be added with the Mg-Zn base alloy extrusion (ZM61) of Mn and be added with the tensile properties that the cast article of the Mg-Zn base alloy extrusion (ZAM621) of Al+Mn shows respectively at ambient temperature, the graphic representation of comparing with the tensile properties that the basic binary alloy squeezing prod of Mg-Zn after dual ageing treatment (Z6) shows.Under 70 ℃, every kind of Z6, ZM61 and ZAM621 alloy carried out 48 hours timeliness first, under 150 ℃, carry out 96 hours secondary ageing then.The tensile properties of each alloy that shows after dual ageing treatment is illustrated among Fig. 8.Can find with reference to Fig. 8, compare that the information slip that relates to dual ageing treatment reveals the enhancing of each alloy yield strength and ultimate tensile strength with the situation that does not relate to dual ageing treatment.Can also find, show similar unit elongation respectively two kinds of situations.After the tension test of carrying out after dual ageing treatment, the tensile properties that each alloy shows is illustrated in the table 4.
Fig. 9 is illustrated respectively in after the dual ageing treatment, is added with the Mg-Zn base alloy extrusion (ZAM631+2.5Si) of Al+Mn+Si and is added with the graphic representation of the tensile properties that the basic alloy extrusion of Mg-Zn (ZAM631+2.5Si+0.4Ca) of Al+Mn+Si+Ca shows at ambient temperature.Under 70 ℃, each extruded alloy product carried out 48 hours timeliness first, under 150 ℃, carry out 24 hours secondary ageing then.The tensile properties of each alloy that shows after dual ageing treatment is illustrated among Fig. 9.Can find with reference to Fig. 9, the ZAM631+2.5Si for preparing of the mixture of the Ca of Si by in the ZAM631 alloy, adding 2.5wt% and Si that adds 2.5wt% and 0.4wt% and the squeezing prod of ZAM631+2.5Si+0.4Ca alloy respectively, with alloy phase ratio, obtain the effect that yield strength and ultimate tensile strength significantly improve without dual ageing treatment.Detailed result is illustrated in the table 4.
Can find that with reference to table 4 by adding the ZM61 alloy that Mn prepares to the Z6 alloy, Z6 compares with alloy, aspect tensile properties, show enhancing slightly owing to dual ageing treatment.By simultaneously adding the ZAM621 alloy that Al and Mn prepare, owing to dual ageing treatment shows intensity above the excellence of Z6 alloy to the Z6 alloy.Especially, the ZAM621 alloy shows the remarkable enhancing of ultimate tensile strength.Even after dual timeliness, all alloys still show excellent unit elongation.
Figure 10 is illustrated in after the dual ageing treatment of carrying out after the solution heat treatment, be added with the Mg-Zn base alloy extrusion (ZM61) of Mn and be added with the tensile properties that the cast article of the basic alloy extrusion of Mg-Zn (ZAM621) of Al+Mn shows respectively at ambient temperature, the graphic representation of comparing with the tensile properties that Mg-Zn binary alloy squeezing prod (Z6) after carrying out identical processing shows at ambient temperature.At first 12 hours solution heat treatment of experience under 380 to 410 ℃ temperature of each alloy Z6, ZM61 and ZAM621.After solution heat treatment, under 70 ℃, each alloy extrusion carried out 48 hours timeliness first, under 150 ℃, carry out 96 hours secondary ageing then.The tensile properties of each alloy that shows after dual ageing treatment is illustrated among Figure 10.Can find that with reference to Figure 10 when carrying out solution heat treatment before dual ageing treatment, the ZM61 alloy shows significantly improving of yield strength and ultimate tensile strength, show simultaneously and unit elongation like the Z6 alloy phase.Descend although ZAM621 alloy and ZM61 alloy phase ratio show yield strength, its aspect ultimate tensile strength with the ZM61 alloy phase seemingly.Especially, the ZMA621 alloy shows significantly improving of unit elongation.The tensile properties that each later alloy of the dual ageing treatment of carrying out after solution heat treatment shows at ambient temperature is illustrated in the following table 5.
Table 5
Alloy yield strength tensile strength unit elongation
(MPa) (MPa) (%)
Z6 252 310 16
ZM60 331 349 13
ZM61 344 363 15
ZM62 339 358 13
ZAM611 295 349 22
ZAM621 252 361 23
ZAM631 239 391 23
ZAM641 254 400 21
ZAM661 232 408 15
Simultaneously, to after just pushing each alloy extrusion being carried out the situation of dual ageing treatment, the situation that stands dual ageing treatment with alloy extrusion after carrying out solution heat treatment compares.Can find that on the basis of comparative result owing to carry out dual ageing treatment after solution heat treatment, the ZM61 alloy shows the remarkable enhancing of intensity, and Z6 and ZAM621 alloy show intensity under identical treatment condition enhancing slightly.Can also find that owing to carry out dual ageing treatment after solution heat treatment, Z6 and ZM61 alloy show the remarkable decline of unit elongation, even and the ZAM621 alloy still shows similar unit elongation after solution heat treatment.
Figure 11 be illustrated in 5% prolonged treatment after carry out dual ageing treatment and be added with the Mg-Zn base alloy extrusion (ZM61) of Mn later on and be added with the tensile properties that the cast article of the Mg-Zn base alloy extrusion (ZAM621) of Al+Mn shows at ambient temperature, the graphic representation that the tensile properties that the basic binary alloy squeezing prod of Mg-Zn (Z6) shows at ambient temperature when carrying out identical processing is compared.Each alloy extrusion of Z6, ZM61 and ZAM621 at first stand 5% prolonged treatment.After prolonged treatment, under 70 ℃, each extruded alloy product carried out 48 hours timeliness first, under 150 ℃, carry out 96 hours secondary ageing then.The tensile properties of each alloy that shows after dual ageing treatment is illustrated among Figure 11.Can find that with reference to Figure 11 compare with not carrying out prolonged treatment situation, the ZAM621 alloy shows the raising of intensity.The ZAM621 alloy also shows 20% or bigger unit elongation.Owing to carry out dual ageing treatment after prolonged treatment, all alloys in fact all show the raising of intensity.Particularly, when the ZAM621 alloy only stands prolonged treatmently, and stood solution heat treatment so that when obtaining the raising of intensity before dual ageing treatment, it shows and intensity like the ZM61 alloy type, and unit elongation significantly improves.After dual ageing treatment, carry out 5% prolonged treatment after, the tensile properties that each alloy shows at ambient temperature is illustrated in the following table 6.
Table 6
Alloy yield strength tensile strength unit elongation
(Mpa) (Mpa) (%)
Z6 298 336 19
ZM60 311 337 23
ZM61 314 347 24
ZM62 297 327 21
ZAM611 337 376 20
ZAM621 318 377 20
ZAM631 316 405 20
ZAM641 315 403 21
ZAM661 314 386 20
Industrial practicality
Can be clear from top explanation, by adding Mn separately or with Al to the Mg-Zn binary alloy, and in the Mg-Zn binary alloy, add Si separately or with Ca simultaneously, so that the forging body that preparation has the grain-size that reduces, and heat-treat or relate to heat treated processing treatment forging body, the invention provides and a kind ofly have hardness and intensity at ambient temperature and improve, and unit elongation enhanced magnesium alloy.
Although given an example disclosed the preferred embodiments of the present invention, it will be apparent to those skilled in the art that in claims disclosed like that, under situation about not departing from the scope of the present invention with purport, can carry out various changes, interpolation and substitute.
Claims (17)
1. high-strength magnesium alloy mainly is made up of the Mn of Zn, the 0.25~3.0wt% of 3~10wt% and the Mg and the unavoidable impurities of surplus.
2. high-strength magnesium alloy as claimed in claim 1 further comprises the Al of 1~6wt%.
3. high-strength magnesium alloy as claimed in claim 2 further comprises the Si of 0.1~4.0wt%.
4. high-strength magnesium alloy as claimed in claim 3 further comprises the Ca of 0.1~2.0wt%.
5. high-strength magnesium alloy as claimed in claim 2, wherein, the content of Al is no more than the content of Zn.
6. as any one described high-strength magnesium alloy in the claim 1 to 5, wherein the content of Zn is 5.0~7.0wt%.
7. as any one described high-strength magnesium alloy in the claim 1 to 5, wherein the content of Mn is 0.75~2.0wt%.
8. as claim 3 or 4 described high-strength magnesium alloys, wherein the content of Si is 1.5~3.0wt%.
9. high-strength magnesium alloy as claimed in claim 4, wherein the content of Ca is 0.3~1.0wt%.
10. a method for preparing as any one described high-strength magnesium alloy in the claim 1 to 9 wherein, is added Mn with the form of Zn-Mn mother alloy in the magnesium melt.
11. method as claimed in claim 10 may further comprise the steps:
Under 670 to 720 ℃ temperature, add Zn-10~20wt%Mn mother alloy to this magnesium melt;
Add Zn to this magnesium melt separately or with Al; And
The magnesium melt of gained is formed cast body.
12. method as claimed in claim 10 may further comprise the steps:
Under 670 to 720 ℃ temperature, add Zn-10~20wt%Mn mother alloy to this magnesium melt;
Add the Mg-Si mother alloy to this magnesium melt;
Add Zn to this magnesium melt separately or with Al and/or Ca; And
The magnesium melt of gained is formed cast body.
13. as claim 11 or 12 described methods, wherein, be to carry out under the magnesium melt condition that cold form has been cooled with stove separately or with the step that Al adds Zn, to reduce the loss of Zn, Zn shows high vapour pressure under the alloy preparation temperature.
14., further comprise step as claim 11 or 12 described methods:
The homogenizing of under 340 to 410 ℃ temperature cast body being carried out 6 to 12 hours is handled;
Make cast body form blank;
Under 150 to 400 ℃ temperature, blank is carried out 30 minutes to 2 hours preheating; And
Blank is processed, forged body thereby form.
15. method as claimed in claim 14 further comprises step:
Under 70 to 100 ℃ temperature to forging the timeliness first that body carried out 24 to 96 hours; And
Under 150 to 180 ℃ temperature to carrying out 48 hours or longer secondary ageing through the forging body of timeliness first.
16. method as claimed in claim 15 further comprises step:
Before dual timeliness, under the temperature of 340 to 410 ℃ of temperature, carry out 6 to 12 hours solution heat treatment to forging body.
17. method as claimed in claim 15 further comprises step:
Before dual timeliness, carry out 3% to 7% stretching to forging body.
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2000
- 2000-09-26 AT AT00966545T patent/ATE505567T1/en not_active IP Right Cessation
- 2000-09-26 DE DE60045848T patent/DE60045848D1/en not_active Expired - Lifetime
- 2000-09-26 CN CNB008199914A patent/CN100390313C/en not_active Expired - Lifetime
- 2000-09-26 AU AU7688400A patent/AU7688400A/en active Pending
- 2000-09-26 JP JP2002530813A patent/JP3891933B2/en not_active Expired - Lifetime
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- 2000-09-26 WO PCT/KR2000/001072 patent/WO2002027053A1/en active IP Right Grant
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CN111218594A (en) * | 2018-11-26 | 2020-06-02 | 内蒙金属材料研究所 | Magnesium-beryllium rare earth die-casting alloy and preparation method thereof |
CN110835702A (en) * | 2019-10-29 | 2020-02-25 | 天津东义镁制品股份有限公司 | Magnesium alloy template profile and preparation method thereof |
CN114318094A (en) * | 2021-12-20 | 2022-04-12 | 重庆大学 | Mn particle reinforced Mg-Zn composite material and preparation method thereof |
CN114703388A (en) * | 2022-04-12 | 2022-07-05 | 重庆大学 | Method for refining Mn-containing Mg-Zn-Al series cast magnesium alloy grains |
CN115044813A (en) * | 2022-04-29 | 2022-09-13 | 北京工业大学 | Low-cost high-strength magnesium alloy material and preparation method thereof |
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DE60045848D1 (en) | 2011-05-26 |
CA2423459C (en) | 2009-09-15 |
IL154897A0 (en) | 2003-10-31 |
ATE505567T1 (en) | 2011-04-15 |
AU7688400A (en) | 2002-04-08 |
JP2004510057A (en) | 2004-04-02 |
NO20031349D0 (en) | 2003-03-25 |
IL154897A (en) | 2009-12-24 |
JP3891933B2 (en) | 2007-03-14 |
EP1339888A1 (en) | 2003-09-03 |
EP1339888A4 (en) | 2005-03-16 |
AU2000276884B2 (en) | 2005-09-29 |
CA2423459A1 (en) | 2002-04-04 |
WO2002027053A1 (en) | 2002-04-04 |
EP1339888B1 (en) | 2011-04-13 |
NO20031349L (en) | 2003-05-23 |
CN100390313C (en) | 2008-05-28 |
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