CN102628133A - Magnesium-aluminum based alloy - Google Patents
Magnesium-aluminum based alloy Download PDFInfo
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- CN102628133A CN102628133A CN2012100221823A CN201210022182A CN102628133A CN 102628133 A CN102628133 A CN 102628133A CN 2012100221823 A CN2012100221823 A CN 2012100221823A CN 201210022182 A CN201210022182 A CN 201210022182A CN 102628133 A CN102628133 A CN 102628133A
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- grain
- magnalium
- refining agent
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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
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
- B22D27/00—Treating the metal in the mould while it is molten or ductile ; Pressure or vacuum casting
- B22D27/20—Measures not previously mentioned for influencing the grain structure or texture; Selection of compositions therefor
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- 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
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Abstract
The present invention relates to magnesium-aluminum based alloys having a small grain size and to a method of their production. The alloys are particularly useful in casting applications. The alloys comprise a grain refiner, the grain refiner having the chemical formula: Mg 100-x-y-z Al x C y R z wherein R is an element selected from the group consisting of silicon, calcium, strontium or a rare earth element, x is from 10 to 60 At.%, y is from 5 to 50 At.%, and z is from 0 to 20 At.%, provided that x+y+z is less than 100 At.%.
Description
Technical field
The present invention relates to a kind of magnalium and preparation method thereof with little grain-size.This alloy is particularly useful for foundry applications.
The exploitation of magnesiumalloy is generally space industry the performance requirement that lightweight material improves constantly is driven.The reason that magnesiumalloy is paid attention to by planners so just is that it has low density, is merely 2/3rds of aluminium.This also is that magnesiumalloy is widely used in casting and the major reason of forged article.
In recent years, the further requirement owing to high antiseptic property has obtained suitable progress in the improvement of novel magnesium alloy.Because the improvement aspect mechanical characteristics and antiseptic property, magnesiumalloy receives more attention day by day in aerospace and other special application fields.
Background technology
The suitability of magnesiumalloy tends to owing to less grain-size improves.Little grain-size can make magnesiumalloy have better mechanical property and structural uniformity usually, thereby has better machining property, good heat resistanceheat resistant cutting performance and more excellent extrudability ability.Have at present many products through strand is pushed, rolling and forged mode produces.Therefore, the fine grain size of magnesiumalloy not only helps improving the processing characteristics of as cast condition product in casting, also helps to improve the suitability for secondary processing of product.
Magnesiumalloy can be divided into two big types usually: not aluminiferous and aluminiferous magnesiumalloy.Not aluminiferous alloy mainly refers to contain zinc or passes through the alloy that zirconium is improved crystal grain, for example ZE41, ZK60, WE43 and EZ33.In these alloys, grain-size can be controlled or reduces through the mode of adding zirconium.Yet; The special crystal grain improvement effect of zirconium is containing for example AM50 of aluminum magnesium alloy; But unable to get up effect among AM60 and the AZ91, this is to form stable intermetallic phase owing to aluminium and zirconium can be easy to interact, it is just inoperative as magnesiumalloy crystal grain nucleator unfortunately.Therefore, still need develop for the suitable grain-refining agent of magnalium.
State-of-the-art
Up to now, the method for existing multiple magnalium crystal grain thinning is able to exploitation.
In crossing by the use of thermal means, magnesiumalloy is heated to its more than fusing point about 150 to 250 ℃, under this temperature, keeps 5 to 15 minutes, is cooled to pouring temperature afterwards rapidly.Its grain refining mechanism is considered to the heterogeneous nucleation effect through the Al-Mn-Fe compound.In the process of crossing by the use of thermal means, several essential characteristics have been observed.The first, need be more than pouring temperature certain TR could bring into play the effect of grain refining to greatest extent.The second, also be vital condition from the quick cooling of temperature of superheat to pouring temperature and of short duration hold-time for forming fine-grain.Owing to need high temperature, the energy consumption of this method is quite high, and is preventing melt oxidation and inspection and safeguarding that aspect such as casting ladle also has suitable cost.
The carbon inoculation technique is the main and effective crystal fining method that present another kind is used for magnalium.The committed step of this method just is carbon is incorporated in the molten magnesium metal.Its grain refining mechanism is considered to: reacting through carbon in the compound and the aluminium in the melt forms aluminium carbide (Al
4C
3) heterogeneous nucleogenesis.In commercial run, be to add C
7Cl
6As grain-refining agent, but owing to can produce a large amount of obnoxious flavoures, this method no longer is allowed to use.In addition, inorganic carbon, for example graphite is rare, carbon and paraffin also are studied as grain-refining agent.Yet their grain refining effect is quite limited.
In the Elfinal method, iron(ic)chloride is added in the melt at about 760 ℃, and said melt kept under this temperature 30 to 60 minutes, thereby forms the Al-Mn-Fe compound gradually, and this compound is considered to have the grain refining effect.Yet there is report to point out that in order to obtain notable effect of crystal grain thinning, manganese content must be higher than certain dividing value.The problem of this method is the deterioration of the local element corrosion resistance that effect causes of Fe and Mn.
Above method is for example being described in the following document to some extent: Lee et al.Metallurgical andMaterials Transactions, Vol.31A, 2000, pages 2805-2906.
In brief, also there are not a kind of gratifying means that are used to improve the grain refining of as cast condition magnalium up to now.Therefore, the object of the present invention is to provide the modification method of a kind of magnalium type alloy grain refinement.
Summary of the invention
In first aspect, the invention provides a kind of magnalium that contains grain-refining agent, said grain-refining agent has following chemical formula:
Mg
100-x-y-zAl
xC
yR
z
Wherein, R is the element that is selected from silicon, calcium, strontium or cohort that REE constitutes, and x is 10 to 60At.%, and y is 5 to 50At.%, and z is 0 to 20At.%, and condition is that x+y+z is less than 100At.%.Preferably x is 20 to 50At.%; Further preferably y is 10 to 35At.%; And further preferably z be 1 to 20At.%.
Preferably, said REE is selected from lanthanum, cerium, neodymium, samarium, europium or mishmetal.
Magnalium preferably comprises grain-refining agent and its add-on is 0.1 to 2% weight of said alloy initial weight.Said magnalium can be any traditional alloy that contains magnesium and aluminium.Preferably, said magnalium is selected from magnalium zinc alloy or magnalium manganese alloy; More preferably, said alloy is selected from AM50, AM60, AM201, AZ10, AZ31, AZ63, the cohort that AZ80 and AZ91 constituted.
In second aspect, the method that the present invention also provides a kind of preparation to have the magnalium of fine-grain, it comprises the alloy that contains magnesium and aluminium is melted under protective atmosphere, and adds the grain-refining agent with following chemical formula to the magnalium melt:
Mg
100-x-y-zAl
xC
yR
z
Wherein, R is the element that is selected from silicon, calcium, strontium or cohort that REE constitutes, and x is 10 to 60At.%, and y is 5 to 50At.%, and z is 0 to 20At.%, condition be x+y+z less than 100At.%, and allow alloy graining.Preferably, said REE is selected from the cohort that lanthanum, cerium, neodymium, samarium, europium or mishmetal constitute.
Magnalium preferably includes grain-refining agent and its add-on is 0.1 to 2% weight of alloy initial weight.Said magnalium can be any traditional alloy that contains magnesium and aluminium.Said magnalium preferably is selected from the cohort that magnalium zinc alloy and magnalium manganese alloy are constituted, and more preferably, said alloy is selected from AM50, AM60, AM201, AZ10, AZ31, AZ63, AZ80, AZ91, AE44, AE42, AJ53, the cohort that AS41 and AS42 constituted.
Preferably, the magnalium that contains the fusing of grain-refining agent is to cast before the alloy graining letting.Preferably said shielding gas comprises for example rare gas element, for example helium or argon gas.More preferably, said shielding gas is argon gas and SF
6Mixture.
Said grain-refining agent preferably prepares through high energy milling.Because grain-refining agent has relative high melt point, high energy milling is the effective ways that prepare suitable grain-refining agent through solid state reaction.
Said grain-refining agent joins can adopt in the magnalium melt to be similar to zirconium is joined the not mode of aluminiferous magnesiumalloy.Then, ready fining agent just is added into and serves as nucleator in the magnesium alloy fused mass.
When preparing grain-refining agent, should preferably consider following processing parameter through high energy milling:
Preferably grinding rate is 600 to 1300rpm, more preferably is 800 to 1100rpm.
In process of lapping, said shielding gas preferably should be continuously or is upgraded to prevent in said process of lapping magnesium and/or aluminium oxidized off and on.If shielding gas is intermittent the renewal, the update times of shielding gas described in the process of lapping is preferably 3 times at least, more preferably at least 5 times.
Preferably, in process of lapping, adopt mill ball by zirconium white or plow-steel manufacturing to reduce the detrimentally affect that iron was produced.In ball mill, the ratio of ball and powder is preferably 5: 1 to 10: 1, more preferably 6: 1 to 8: 1.Milling time preferably is chosen as 4 to 8 hours, more preferably is 5 to 7 hours.Hold-time before process of lapping begins preferably is chosen as 1 to 4 hour, more preferably is 1 to 3 hour.
When adopting high energy milling to prepare grain-refining agent, raw materials used preferably choice of powder form.Adopt high energy milling to prepare the raw materials used particle diameter of grain-refining agent and be preferably 100 μ m to 400 μ m, more preferably 250 μ m to 350 μ m.The purity that is used to prepare the raw material of grain-refining agent is preferably 99% to 99.999%, and more preferably 99.9% to 99.99%.
Particle diameter after said grain-refining agent grinds is preferably 0.1nm to 50nm, more preferably 0.1nm to 10nm.
Grain-refining agent according to the present invention is especially effective for cast magnesium alloy.The alloy of this kind comprises, such as gravitational casting magnalium, die casting magnalium, semi-solid casting magnalium, rheocasting magnalium and continuous casting magnalium.
Have in the method for magnalium of fine-grain in preparation, the temperature of molten alloy be preferably 720 ℃ or on, to prevent the fractional condensation of grain-refining agent nanoparticle.Said temperature is high more, realizes that the time of grain refining is just short more.Yet, consider may the ignite material of molten state of too high temperature, so temperature of fusion is preferably 720 ℃ to 760 ℃, more preferably about 750 ℃.
The content that adds the grain-refining agent of cast magnesium alloy to is preferably 0.1% to 2% weight, more preferably 0.5% to 1.5% weight.When the content of its interpolation was lower than 0.1% weight, the grain refining effect may be not enough.When the content of its interpolation was higher than 2% weight, remaining grain-refining agent might influence the performance of magnesiumalloy.
Said melt preferably should stir to obtain the alloy that homogeneous phase distributes.Stirring velocity is preferably 150rpm to 300rpm, more preferably 150rpm to 250rpm.Churning time is preferably 10min to 60min, more preferably 20min to 40min.
After adding grain-refining agent, being arranged one period hold-time, is favourable for the grain refinement process of cast magnesium alloy.The said hold-time is preferably 10min to 90min, more preferably 30min to 60min.
To describe some embodiment of the present invention below.But be interpreted as, the present invention is not limited to following listed examples.
Description of drawings
Fig. 1 (a)-(c) is the microscopic optical structure of the grain refining effect that is presented at 750 ℃ of original state powder that add magnesium-3wt.% duraluminum to.What Fig. 1 (a) showed is magnesium-3wt.% duraluminum.That Fig. 1 (b) shows is the grain-refining agent Mg that contains 1wt.%
0.3Al
0.4C
0.15Ca
0.15Magnesium-3wt.% duraluminum, and milling time is 20 hours.Churning time during fusion is 30 minutes.That Fig. 1 (c) shows is the grain-refining agent Mg that contains 1wt.%
0.3Al
0.4C
0.15RE
0.15Magnesium-3wt.% duraluminum, and milling time is 20 hours.Churning time during fusion is 30 minutes.
Fig. 2 is the microscopic optical structure that is presented at the grain refining effect of 750 ℃ of original state powder that add magnesium-3wt.% duraluminum to.What Fig. 2 (a) showed is to contain 0.5wt.%Mg
0.3Al
0.4C
0.15RE
0.15The magnesium of grain-refining agent-3wt.% duraluminum, and milling time is 20 hours.What Fig. 2 (b) showed is to contain 0.8wt.%Mg
0.3Al
0.4C
0.15RE
0.15The magnesium of grain-refining agent-3wt.% duraluminum, and milling time is 20 hours.What Fig. 2 (c) showed is to contain 1wt.%Mg
0.3Al
0.4C
0.15RE
0.15The magnalium of grain-refining agent-3wt.% alloy, and milling time is 20 hours.
Fig. 3 shows the average grain size and the Mg of magnesium-3wt.% duraluminum
0.3Al
0.4C
0.15RE
0.15Relation between the grain refining agent content, wherein milling time is 20 hours.When adding the grain-refining agent of 1.5wt.%, the grain-size that is obtained is minimum.
Fig. 4 shows the average grain size and the Mg of magnesium-3wt.% duraluminum
0.3Al
0.4C
0.15RE
0.15Relation between the milling time of grain-refining agent.Mg wherein
0.3Al
0.4C
0.15RE
0.15Content be 1.0wt.%.Grind 20 hours situation, the institute's alloy grain size that obtains minimum at grain-refining agent.
Fig. 5 is presented at the Mg that adds different content
0.3Al
0.4C
0.15Ca
0.15Grain-refining agent and milling time is 20 hours a situation, the average grain size of magnesium-3wt.% duraluminum.
Embodiment 1
The preparation of grain-refining agent:
In the present embodiment, the powder constituent before grinding is listed in table 1, and wherein unit is " atom% " (atomic percent).
Table 1
Adopt cylindrical cylinder of steel to prepare grain-refining agent.Too high and oxidized owing to temperature in process of lapping in order to prevent powder, use pure argon to carry out filling for 5 times and sweeps with excluding air.Grinding rate is 1000rpm.Select zirconia ball for use, and the ratio of ball and powder is 8: 1.Milling time is 5 to 20 hours (seeing table 1).Carry out continuously in order to make to be reflected between the different powder, the hold-time between twice grinding operation is 2 hours.In process of lapping, can not open crucible cover.The composition of gained sample is seen table 1 after the different milling times.
The grain refining technological process of magnalium:
In the present embodiment, adopted magnesium-3wt.% duraluminum to study the effect of novel grain-refining agent.Through 400 ℃ of preheatings 700 the gram pure magnesium in steel crucibles in 750 ℃ of fusings.SF
6With the mixed gas of argon gas as shielding gas.Then, 300 gram fine aluminiums of preheating are added in the melt, then, spend melt was stirred in 15 minutes.The grain-refining agent of particle diameter less than 20nm joined in the melt.In melt, add the operation triplicate of grain-refining agent.After adding grain-refining agent, said melt was continued to stir 30 minutes.Then, after keeping 30 minutes, carry out the casting of alloy.Grain morphology with the observation by light microscope casting alloy.Average grain size to each sample is measured.
Fig. 1 (a)-(c) is the microscopic optical structure of the grain refining effect that is presented at 750 ℃ of original state powder that add magnesium-3wt.% duraluminum to.It is thus clear that grain-size reduces with the adding of different grain-refining agents.
Fig. 2 is the microscopic optical structure that is presented at the grain refining effect of 750 ℃ of original state powder that add magnesium-3wt.% duraluminum to.Grain-size reduces with the content increase of grain-refining agent.Detailed numerical is as shown in Figure 3.In the situation of the grain-refining agent that adds 1.5wt.%, the value of the grain-size that obtains is minimum.Minimum average grain size is 67 μ m.
Fig. 4 shows the average grain size and the Mg of magnesium-3wt.% duraluminum
0.3Al
0.4C
0.15RE
0.15Relation between the milling time of grain-refining agent.In 20 hours situation of grain-refining agent grinding, the grain-size that is obtained in the alloy is minimum.
Embodiment 2
The preparation of grain-refining agent:
In the present embodiment, the powder constituent before grinding is listed in table 2, and wherein unit is " atom% " (atomic percent).
Table 2
Adopt cylindrical cylinder of steel to prepare grain-refining agent.Too high and oxidized owing to temperature in process of lapping in order to prevent powder, use pure argon to carry out filling for 5 times and sweeps with excluding air.Grinding rate is 1000rpm.Select zirconia ball for use, and the ratio of ball and powder is 8: 1.Milling time is 5 to 20 hours (seeing table 2).Carry out continuously in order to make to be reflected between the different powder, the hold-time between twice grinding operation is 2 hours.In process of lapping, can not open crucible cover.The composition of gained sample is seen table 2 after the different milling times.
The grain refining technological process of magnalium:
In the present embodiment, adopted magnesium-3wt.% duraluminum to study the effect of novel grain-refining agent.Through 400 ℃ of preheatings 700 the gram pure magnesium in steel crucibles in 750 ℃ of fusings.SF
6With the mixed gas of argon gas as shielding gas.300 gram fine aluminiums of preheating are added in the melt of magnesiumalloy.Then, spending 15 minutes stirs gained liquid.The grain-refining agent of particle diameter less than 20nm joined in the liquid.In melt, add the operation triplicate of grain-refining agent.After adding grain-refining agent, said melt was continued to stir 30 minutes.Then, after keeping 30 minutes, carry out the casting of alloy.Grain morphology with the observation by light microscope casting alloy.Average grain size to each sample is measured.
Be added with the grain-refining agent Mg of 1wt.%
0.3Al
0.4C
0.15Ca
0.15The typical microstructure of magnesium-3wt.% duraluminum shown in Fig. 1 (b).With magnesium-3wt.% duraluminum relatively, crystal grain is by refinement significantly after the interpolation of this fining agent.Fig. 5 shows average grain size and adds grain-refining agent Mg in magnesium-3wt.% duraluminum to
0.3Al
0.4C
0.15Ca
0.15Content between mutual relationship.Grain-size reduces with the content increase of fining agent.When the fining agent that adds surpassed 1wt.%, grain-size just tended towards stability.
Claims (11)
1. a magnalium contains grain-refining agent, and the chemical formula of said grain-refining agent is:
Mg
100-x-y-zAl
xC
yR
z
Wherein, R is selected from the element of silicon, calcium, strontium and cohort that REE constitutes, and x is 10 to 60At.%, and y is 5 to 50At.%, and z is 0 to 20At.%, and condition is that x+y+z is less than 100At.%.
2. magnalium according to claim 1, it comprises the said grain-refining agent that addition is 0.1% to 2% weight of said magnalium initial weight.
3. magnalium according to claim 1, wherein said REE is selected from the cohort that lanthanum, cerium, neodymium, samarium, europium and mishmetal constitute.
4. magnalium according to claim 1, wherein said magnalium are selected from the cohort that magnalium zinc alloy and magnalium manganese alloy are constituted.
5. magnalium according to claim 4, wherein said alloy is selected from AM50, AM60, AM201, AZ10, AZ31, AZ63, AZ80, AZ91, AE44, AE42, AJ53, the cohort that AS41 and AS42 constituted.
6. method for preparing the magnalium that contains trickle crystal grain; It comprises the alloy that contains magnesium and aluminium is melted in the shielding gas atmosphere; And will join in the magnalium of said fusing, and make said alloy graining according to each described grain-refining agent in the claim 1 to 6.
7. method according to claim 6, the magnalium that wherein contains the said fusing of said grain-refining agent was cast before making said alloy graining.
8. method according to claim 6, wherein said shielding gas comprises argon gas.
9. method according to claim 6, wherein said shielding gas further comprises SF
6
10. method according to claim 6, wherein said grain-refining agent are the abrasive dusts that has less than the 50nm particle size.
11. method according to claim 6 wherein after adding said grain-refining agent, stirs the magnalium of said fusing 10 to 60 minutes.
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
EP11152825.3A EP2481822B1 (en) | 2011-02-01 | 2011-02-01 | Magnesium-aluminum based alloy with grain refiner |
EP11152825 | 2011-02-01 |
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CN102628133A true CN102628133A (en) | 2012-08-08 |
CN102628133B CN102628133B (en) | 2015-07-08 |
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US (1) | US20120195789A1 (en) |
EP (1) | EP2481822B1 (en) |
CN (1) | CN102628133B (en) |
CA (1) | CA2765465A1 (en) |
ES (1) | ES2424005T3 (en) |
Cited By (2)
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CN112030049A (en) * | 2020-07-14 | 2020-12-04 | 中国石油天然气股份有限公司 | Controllable dissolution magnesium alloy material and preparation method thereof |
CN112921225A (en) * | 2021-02-16 | 2021-06-08 | 河南工学院 | Aluminum-coated nano Al for Mg-Al alloy4C3Granular grain refiner and preparation method thereof |
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US8126190B2 (en) | 2007-01-31 | 2012-02-28 | The Invention Science Fund I, Llc | Targeted obstrufication of an image |
US20070276757A1 (en) * | 2005-07-01 | 2007-11-29 | Searete Llc, A Limited Liability Corporation Of The State Of Delaware | Approval technique for media content alteration |
US8910033B2 (en) | 2005-07-01 | 2014-12-09 | The Invention Science Fund I, Llc | Implementing group content substitution in media works |
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US9065979B2 (en) | 2005-07-01 | 2015-06-23 | The Invention Science Fund I, Llc | Promotional placement in media works |
US9092928B2 (en) | 2005-07-01 | 2015-07-28 | The Invention Science Fund I, Llc | Implementing group content substitution in media works |
US9215512B2 (en) | 2007-04-27 | 2015-12-15 | Invention Science Fund I, Llc | Implementation of media content alteration |
CN104087804B (en) * | 2014-07-28 | 2016-09-07 | 胡贤晨 | A kind of creep resistance Dow metal and preparation method thereof |
CN115198128A (en) * | 2022-07-08 | 2022-10-18 | 宝胜(宁夏)线缆科技有限公司 | Zero-carbon manufacturing process for high-quality regenerated aluminum-silicon alloy |
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CN101135013A (en) * | 2007-10-11 | 2008-03-05 | 武汉理工大学 | Magnesium and magnesium alloy composite grain refiner and method for making same |
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CN1151293C (en) * | 2002-11-25 | 2004-05-26 | 山东大学 | Fining agent used for magnesium alloy and its preparation method |
US8016957B2 (en) * | 2006-02-03 | 2011-09-13 | GM Global Technology Operations LLC | Magnesium grain-refining using titanium |
CN101774013B (en) * | 2010-02-26 | 2012-05-23 | 华南理工大学 | Composite grain finer for Mg-Al alloy and preparation method thereof |
-
2011
- 2011-02-01 ES ES11152825T patent/ES2424005T3/en active Active
- 2011-02-01 EP EP11152825.3A patent/EP2481822B1/en not_active Not-in-force
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2012
- 2012-01-18 US US13/352,632 patent/US20120195789A1/en not_active Abandoned
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CN101135013A (en) * | 2007-10-11 | 2008-03-05 | 武汉理工大学 | Magnesium and magnesium alloy composite grain refiner and method for making same |
Cited By (3)
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CN112030049A (en) * | 2020-07-14 | 2020-12-04 | 中国石油天然气股份有限公司 | Controllable dissolution magnesium alloy material and preparation method thereof |
CN112921225A (en) * | 2021-02-16 | 2021-06-08 | 河南工学院 | Aluminum-coated nano Al for Mg-Al alloy4C3Granular grain refiner and preparation method thereof |
CN112921225B (en) * | 2021-02-16 | 2022-06-21 | 河南工学院 | Aluminum-coated nano Al for Mg-Al alloy4C3Granular grain refiner and preparation method thereof |
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US20120195789A1 (en) | 2012-08-02 |
EP2481822A1 (en) | 2012-08-01 |
CA2765465A1 (en) | 2012-08-01 |
ES2424005T3 (en) | 2013-09-26 |
CN102628133B (en) | 2015-07-08 |
EP2481822B1 (en) | 2013-05-08 |
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