CN100532605C - Magnesium-zinc-scandium alloy and method for preparing same - Google Patents
Magnesium-zinc-scandium alloy and method for preparing same Download PDFInfo
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- CN100532605C CN100532605C CNB2007100563995A CN200710056399A CN100532605C CN 100532605 C CN100532605 C CN 100532605C CN B2007100563995 A CNB2007100563995 A CN B2007100563995A CN 200710056399 A CN200710056399 A CN 200710056399A CN 100532605 C CN100532605 C CN 100532605C
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Abstract
The invention relates to a magnesium-zinc-scandium alloy and a preparation method thereof, in particular to an mg-based alloy with high zinc content and low scandium content in a magnesium-zinc-rare earth system and a preparation method thereof. The mg-based alloy of the invention contains 10.5wt to 11.5wt percent of Zn, 0.95wt to 1.05wt percent of Sc, less than 0.05wt percent of the total amount of impurity elements of Fe, Ni, Cu and Si, and the residual is Mg. The alloy has the advantage of good high temperature performance and is beneficial for the recovery, the recurrent and the efficient utilization. At the high temperature of 280 DEG C, the tensile strengths of the series alloys of the invention are all larger than 100MPa.
Description
Technical field
The present invention relates to magnesium-zincium-rare earth is Alloy And Preparation Method.Particularly relate to Magnuminium of high-content zinc, low levels scandium in a kind of magnesium-zincium-rare earth system and preparation method thereof.
Background technology
In light alloy, add scandium (Sc) in particularly aluminium base, the magnesium base light alloy, can obtain high anticorrosive, high strength, high weldability, wide operation temperature area and the good light alloy of over-all properties, be widely used in high-tech sectors such as empty sky always.This has benefited from Sc is that atomic radius and Al, Mg are the most approaching in 17 kinds of rare earth elements (RE), and has under the room temperature in advantages such as Mg or Al solid solubility are big; But because Sc is the rare earth element the most rare in the 17 middle-weight rare earths elements, that market value is the most expensive, metal Sc usage quantity in alloy is also very limited.
In aluminium base or Magnuminium, how to add minimum Sc as far as possible and reach best effect, be the important problem in science in this area research or the production always.In last century, Sc is controlled at 0.15-0.25wt% usually at the aluminum base alloy addition, and has developed novel aluminium based alloy system.Enter this century, Sc develops to high density at the aluminium alloy addition, even reaches 2.15wt%; Because the progress of magnesium alloy surface treatment, such as technology such as differential arc oxidation or brush platings, Sc adds in Magnuminium and also receives much attention, the Mg-Sc alloy in addition that receives publicity simultaneously is as functional materials.
About rare earths such as Sc minimum addition and mechanism of action in light alloy, 1940 United States Patent (USP) trademark offices disclose 2,219, No. 056 patent that is entitled as " Magnuminium " of German inventor Sauerwald application.This patent content and this contriver are identical substantially at 305, No. 172 (series number) patent contents of German application in November, 1938.Its INVENTION IN GENERAL discloses: 1. if use Rare Earth Y fining metal magnesium crystal grain, the minimum addition of Rare Earth Y is 0.1wt%, just can obtain obvious thinning effect; 2. if by the grain refining effect, promote magnesium alloy mechanical property, then the minimum addition of Y is controlled at about 0.3wt%; 3. if attempt with Rare Earth Y as strengthening element, promote magnesium alloy mechanical property by precipitation strength, then the addition of Y is controlled at more than the 2.5wt%, until 10wt%.This invention is at present can be from patent retrieval channel, " tracing to the source " invention that retrieves Mg-RE binary alloy system the earliest and Mg-Zn-RE system " presoma " invention.Because rare earth (Sc, Y, La ... amount to 17 kinds) the chemical property similarity of element, this invention is to the invention of the present invention all interior descendants, in aluminium base or Magnuminium, add rare earth element, comprise and add Sc, principle and aspect such as quantity reference is provided.Obviously, this reference can not constitute the restriction to magnesium-zinc of the present invention-scandium ternary alloy novelty.
1997, United States Patent (USP) trademark office disclosed No. 5624632 patents of invention that are entitled as " comprising the aluminum magnesium alloy production of dispersoid particle " that Alcoa submits to.Extremely empty day field, various countries is paid close attention to, and is exclusively used in empty day sophisticated equipment.Mysterious " SCC " (stress corrosion cracking) alloy further obtains open in this patent; " SCC " alloy that the insider pays close attention to always is that high anti-stress-corrosion cracking, work-ing life are the alloy of the empty day domain-specific of 20-40.This invents announcement: for Al-Mg-Sc base alloy composition: adopt the alloy of Al-6.5wt%Mg-0.23wt%Sc-0.09wt%Zr, its density is 0.0943Ib/cu in (2.61g/cm
3), tensile strength is 64.6ksi. (445.4MPa), elongation 12%, doing the stress corrosion dehiscence resistant result of experiment that exposed in 180 days according to ASTM G-47 standard is 0/3, the test of other various performances is also very excellent.This invention produces useful prompting at magnesium/aspects such as scandium interaction to the present invention.Obviously, this aluminum base alloy is not construed as limiting Magnuminium of the present invention " three property ".
During the 1999-2001, disclose 4 patents to produce the well-known German Daimler-Chrysler stock company (Daimler Chrysler AG) of " benz " car altogether in Patent Office of the People's Republic of China and United States Patent (USP) trademark office, these 4 patents are added 0.15wt%Sc with protection in aluminum base alloy Al-(5-6wt%) Mg-0.15wt%Sc-(0.05-0.15wt%) Zr basic ingredient is that core, emphasis disclose: keeping the Mn/Sc ratio behind the interpolation Mn is 2; Adding the 0.15wt%Sc insufficient section can be by multiple rare earth substitutional relation such as Dy, Gd and effect etc.These 4 patents comprise: Patent Office of the People's Republic of China: 1. be entitled as the aluminium-magnesium alloy of corrosion-resistant, high Mg content " be specially adapted to that automobile is used, new to weld, " number 99801195.9 patents, 2. be entitled as " be specially adapted to aerospace applications, new weld, the aluminium-magnesium alloy of corrosion-resistant, high Mg content " No. 99801242.4 patents, 3. be entitled as " be specially adapted to communications and transportation, can weld, corrosion-resistant aluminium-magnesium alloy " No. 99801414.1 patents; 4. being entitled as of United States Patent (USP) trademark office " be specially adapted to that automobile is used, can weld, the aluminium-magnesium alloy of corrosion-resistant, high Mg content " 6,315, No. 948 patents.This invention at aspects such as Mn/Sc compare to Zn/Sc of the present invention than useful promptings such as generations.Obviously, this aluminium basely is not construed as limiting Magnuminium of the present invention " three property " yet.
During the 2001-2003, a German branch office (DeutschlandGmbH) of European aviation defence and space flight company (EADS) discloses 2 patents altogether in United States Patent (USP) trademark office.The claimed content of these two patents and above-mentioned German Daimler-4 patents of Chrysler stock company is basic identical, promptly adds the high-magnesium aluminum alloy of 0.15wt% left and right sides Sc in the aluminum base alloy.These 2 patents are: disclosed being entitled as of calendar year 2001 " be specially adapted to communications and transportation, can weld, corrosion resistant Al-Mg alloy " 6,258, No. 318 patents, disclosed being entitled as in 2003 " be specially adapted to aerospace applications, new weld, the aluminium-magnesium alloy of corrosion-resistant, high Mg content " 6,531, No. 004 patents.Equally, this aluminum base alloy is not construed as limiting Magnuminium of the present invention " three property ".
During the 2001-2004, United States Patent (USP) trademark office discloses U.S. pistol professional production company-Smith; (the SMITH of Wei Sen company; WESSON CORP) 2 that are applied for are entitled as " containing the scandium-aluminium alloy gun " patent, and its patent No. is respectively 20010054247 and 20040010917.Two patents mainly apply for protecting Sc and the Zn of 7.5wt%-8.3wt% and the aluminium alloy of other a small amount of strengthening element that adds 0.05wt%-0.15wt% in aluminum base alloy.This invention for empty day field contain scandium-aluminium alloy be on active service the back, utilize recovery article to be processed into light-weighted high-grade revolver (Revolvers) or other type pistol provides fine resources effective utilization thinking, also the Mg-Zn-Sc alloy designs for the high Zn of the present invention, low Sc provides coherent reference.Equally, this aluminum base alloy is not construed as limiting Magnuminium of the present invention " three property " yet.
During the 2003-2004, Patent Office of the People's Republic of China disclosed to find AB in 2003
5No. 01804203.1 patent of invention that is entitled as " metal hydride battery material with high storage capacity " that the dutch royal N.V. Philips' Optical Lamp Ltd., Co of well-known various countries such as type hydrogen-storage alloy submits to, this invention discloses: consist of Sc
0.347-Mg
0.647-Pd
0.006-H
XHydrogen-storage alloy in battery, show the electrochemical specific capacity of 980mAh/g.
United States Patent (USP) trademark office disclosed 6,821, No. 676 patents of invention that are entitled as " heavy body Metal hydrogen-storing material " that dutch royal N.V. Philips' Optical Lamp Ltd., Co submits in 2004, and this invention discloses: consist of Sc
0.3-Mg
0.7And Sc
0.2-Mg
0.8Weight ratio capacity be respectively 1508mAh/g and 1652mAh/g, than LaNi commonly used
5Capacity exceeds 4 times.
The invention of above-mentioned Philips company contains with how preventing that aspects such as " hydrogen embrittlements " has useful prompting in Sc, the melting of Mg metal alloy, the course of processing the present invention, obviously, this invention that belongs to " functional materials " can not constitute the restriction of the patent of the present invention " three property " that belongs to " structured material ".
2003, United States Patent (USP) trademark office disclosed No. 20030029526 patents that are entitled as " with elevated temperature heat moulding and accurate brilliant enhanced Magnuminium and preparation method thereof " that the Korea S inventor submits to.This invents announcement: ((it is 30% accurate crystalline phase that 0.4 ~ 6.9wt%) Y system, suitable alloying constituent can obtain to contain volume fraction to 2.7 ~ 22wt%) Zn-for Mg-.The novelty of this invention is to utilize accurate brilliant enhancing and obtains very well results.But the Magnuminium of this invention high Zn content belongs to the alloy in the Mg-Zn-Y system, and is first-class variant in series with the Mg-Zn-Sc alloy of high Zn content of the present invention, obviously do not constitute novelty restriction of the present invention.
2006, Patent Office of the People's Republic of China discloses No. 200610084150.0 patents of invention that are entitled as " high temperature aluminium alloys " that U.S. United Technologies Corp. submits to, Sc and the Ni of 8.4wt% and the aluminium alloy of other strengthening element of 2.15wt% added in this invention in aluminum base alloy based on protection, and disclose: consist of Al-8.4wt%Ni-2.15wt%Sc-8.5wt%Gd-2.5wt%Y or alloys such as Al-8.4wt%Ni-2.15wt%Sc-8.8wt%Gd-2.5wt%Zr or Al-8.4wt%Ni-2.15wt%Sc-9.0wt%Hf-4.5wt%Gd, be the wide operation temperature area that can use to about 650 ℉ (343 ℃) temperature at about-420 ℉ (251 ℃), over-all properties is good, be to be adapted at the aluminium alloy that was widely used in the field in empty day, man-made satellite such as around-the-moon flight, fly to run into subzero low temperature below-100 ℃ to " back of the body day face " (solar direction space dorsad), and " meeting a day face " runs into high temperature more than above freezing+100 ℃, obviously, the alloy of this wide operation temperature area is essential; This invention has also disclosed the possibility that this alloy is applied to aircraft or the concrete component of rocket.This invention produces useful prompting to aspects such as Sc utilizations rationally to the present invention in Sc effect, the wide operation temperature area design of alloy, but the aluminum base alloy of this invention obviously is not construed as limiting Magnuminium of the present invention " three property " yet.
2006-2007, patent and trademark office and Patent Office of the People's Republic of China disclose the Japanese inventor (Kawamura of Kawamura Yoshihito; Yoshihito) etc. multinomial relevant patent.Comprise: 1. 2006 United States Patent (USP) trademark office disclosed being entitled as " magnesium alloy and production method thereof " No. 20060065332 patents, 2. No. 20070102072 patents of in May, 2007 United States Patent (USP) trademark office disclosed being entitled as " high-strength-toughness magnesium alloy and preparation method thereof ", 3. No. 20070125464 patents of in June, 2007 United States Patent (USP) trademark office disclosed being entitled as " high-strength-toughness magnesium alloy and production method thereof ", 4. No. 20070169859 patents of in July, 2007 United States Patent (USP) trademark office disclosed being entitled as " high-strength-toughness magnesium alloy and production method thereof ", 5. in August, 2007 China Patent Office is disclosed is entitled as No. 200580032675.3 patents of invention of " high-intensity high-tenacity metal and manufacture method thereof ", 6. No. 20070204936 patents of in September, 2007 United States Patent (USP) trademark office disclosed being entitled as " magnesium alloy ".In above-mentioned 6 patents, such as Mg-4.4wt%Zn-3wt%Y-0.3wt%Zr, Mg-7.6wt%Zn-1.7wt%Y etc., in the invention of this series at aspects such as Zn/RE compare to Zn/Sc of the present invention than useful promptings such as generations.But it is alloy or other rare earth metal that the Magnuminium of this invention high Zn content belongs to Mg-Zn-Y, variant on series with the Mg-Zn-Sc alloy of high Zn content of the present invention, does not obviously constitute novelty restriction of the present invention.
2007; Patent Office of the People's Republic of China discloses No. 200710099819.8 patents of invention that are entitled as " a kind of casting heat-resistant magnesium alloy " that Chinese Aluminium Co., Ltd submits to; this patent application protection " Mg-(0.3～0.8wt%) Sc-(5～10wt%) Gd-(0.5～1.0wt%) Mn system "; this invention discloses: for the alloy that consists of Mg-0.3Sc-10Gd-1Mn; under 300 ℃, its tensile strength is that 186.23MPa, yield strength are 142.77MPa, elongation 6.91%.The high Sc of this invention, the design of high Gd magnesium alloy are compared with high Sc of the present invention, high Zn magnesium alloy, obviously, have very big-difference at aspects such as affiliated alloy series, alloy compositions formations; Though can produce useful prompting, novelty of the present invention etc. be not construed as limiting.
In a word, do not see patent disclosure and bibliographical information with the present invention in many-sided closely-related patents such as compositions.
Summary of the invention
The object of the present invention is to provide a kind of magnesium-zinc-scandium alloy and preparation method thereof.
Magnesium-zinc-scandium alloy of the present invention specifically consists of: contain the Zn of 10.5wt%-11.5wt% in the Magnuminium, and the Sc of 0.95wt%-1.05wt%, the total amount of impurity element Fe, Ni, Cu and Si is less than 0.05wt%%, and all the other are Mg; It is formed skeleton symbol and is expressed as: Mg-(10.5-11.5) Zn-(0.95-1.05) Sc.
Magnesium-zinc-scandium alloy preparation method's of the present invention step and condition are as follows:
With purity is that 99.9% Mg ingot, 99.5% Zn ingot, 99.5% Mg-Sc intermediate alloy ingot are alloy raw material; Wherein, to account for the master alloy weight percent be 2.3% to the Sc in the Mg-Sc intermediate alloy ingot;
Mg ingot, Zn ingot and intermediate alloy ingot raw material through cut apart, oil removing, drying and scale removal make raw material block; Carry out weighing according to the quality proportioning, raw material block is dipped in molten salt pool hang that to join smelting temperature behind the fused salt be in 800 ℃ the smelting furnace, the extension fused salt dips in institute, and to select the NaCl:KCl mol ratio for use be that 1:3, purity are the fused salt mixt of chemical pure NaCl and KCl;
Order of addition(of ingredients) in smelting furnace is: metal M g piece, Metal Zn piece and Mg-Sc master alloy piece, and the crucible of this smelting furnace is a plumbago crucible; It is the fused salt mixt of chemical pure NaCl and KCl that protective material molten chloride composition dips in extension fused salt composition identical mol ratio 1 to 3, purity with the shove charge raw material block; All furnace charges melt the back and stirred 2 minutes, and alloy left standstill 15 minutes, adopt casting process, and teeming temperature is at 760 ℃, and casting mold uses preheating stainless steel metal mould, and preheating temperature obtains magnesium-zinc-scandium alloy at 250 ℃.
Preparation method's advantage of the present invention is:
1, the method with simple and easy handling obtains the good alloy of high-temperature behavior.Under 280 ℃ high temperature, series alloy tensile strength of the present invention all surpasses 100MPa.
2, containing alloy designs that Sc is about 1wt% helps alloy and utilizes.Show: alloy of the present invention use retired after, melt down melting when being converted to other composition alloy, Sc content downward modulation space is bigger; Reason is to contain the Sc content about the most 0.15wt% of being of scandium alloy.
Description of drawings
Fig. 1 is the typical XRD figure of Mg-11wt%Zn-1.0wt%Sc cast alloy of the present invention.
Fig. 2 is the figure of typical organization of optical photograph under the Mg-11wt%Zn-1.0wt%Sc cast alloy low power of the present invention.
Fig. 3 is the figure of typical organization of optical photograph under the Mg-11wt%Zn-1.0wt%Sc cast alloy high power of the present invention.
Embodiment
Embodiment 1:
Composition according to Mg-11.5wt%Zn-1.05wt%Sc carries out raw material mass mixture ratio, and Mg is a surplus.Material purity used in this formula is: 99.9% Mg ingot, 99.5% Zn ingot and 99.5% Mg-Sc rare earth intermediate alloy ingot; Wherein to account for the master alloy weight percent be 2.3% to the rare earth Sc in the Mg-Sc rare earth intermediate alloy ingot.
Mg ingot, Zn ingot and intermediate alloy ingot raw material through cut apart, oil removing, drying and scale removal obtain block material; According to the concrete weighing of quality proportioning, raw material block dipped in molten salt pool hang that to join smelting temperature behind the fused salt be in 800 ℃ the smelting furnace, it dips in the extension fused salt, and to select constitutive molar ratio 1 to 3, purity for use be the fused salt mixt of chemical pure NaCl/3KCl; The addition sequence of its furnace charge is followed successively by: metal M g piece, Metal Zn piece and Mg-Sc master alloy piece; The crucible of this smelting furnace is a plumbago crucible; Protective material molten chloride composition and shove charge alloy dip in that to hang the fused salt composition identical, promptly still be the fused salt mixt of the NaCl/3KCl of constitutive molar ratio 1 to 3, this protective material muriate fused salt mixt to the smelting furnace addition be metal and alloy furnace charge summation 8wt%, and for after following the rare earth intermediate alloy piece closely the interpolation;
All furnace charges melt the back and stirred 2 minutes, and alloy left standstill 15 minutes, 250 ℃ of casting stainless steel metal die preheating temperatures; Teeming temperature is 760 ℃; Alloy liquid obtains the Mg-11.5wt%Zn-1.05wt%Sc alloy after casting aside salt, in the metal die of pushing off the slag cast preheating, alloy room temperature and pyritous as cast condition tensile strength, yield strength and elongation are listed in table 1.
Main mechanical property under the table 1:Mg-11.5wt%Zn-1.05wt%Sc alloy differing temps
| Probe temperature ℃ | Tensile strength MPa | Yield strength MPa | Elongation % |
| Room temperature | 225 | 161 | 4.9 |
| 200 | 173 | 142 | 13.8 |
| 280 | 118 | 99 | 4.4 |
Embodiment 2:
Composition according to Mg-11.5wt%Zn-1.05wt%Sc carries out raw material mass mixture ratio, and Mg is a surplus.With the alloy of forming among the alloy replacing embodiment 1 that consists of Mg-11wt%Zn-1.0wt%Sc.All the other operations are with embodiment 1, and alloy room temperature and pyritous as cast condition tensile strength, yield strength and elongation are listed in table 2.
Main mechanical property under the table 2:Mg-11wt%Zn-1.0wt%Sc alloy differing temps
| Probe temperature ℃ | Tensile strength MPa | Yield strength MPa | Elongation % |
| Room temperature | 227 | 163 | 4.7 |
| 200 | 175 | 144 | 15.0 |
| 280 | 120 | 102 | 4.6 |
Embodiment 3:
Composition according to Mg-11.5wt%Zn-1.05wt%Sc carries out raw material mass mixture ratio, and Mg is a surplus.With the alloy of forming among the alloy replacing embodiment 1 that consists of Mg-10.5wt%Zn-0.95wt%Sc.All the other operations are with embodiment 1, and alloy room temperature and pyritous as cast condition tensile strength, yield strength and elongation are listed in table 3.
Main mechanical property under the table 3:Mg-10.5wt%Zn-0.95wt%Sc alloy differing temps
| Probe temperature ℃ | Tensile strength MPa | Yield strength MPa | Elongation % |
| Room temperature | 226 | 162 | 4.8 |
| 200 | 174 | 143 | 14.0 |
| 280 | 119 | 100 | 4.3 |
Claims (2)
1, a kind of magnesium-zinc-scandium alloy is characterized in that, it consists of: contain the Zn of 10.5wt%-11.5wt% in the Magnuminium, and the Sc of 0.95wt%-1.05wt%, the total amount of impurity element Fe, Ni, Cu and Si is less than 0.05wt%, and all the other are Mg; It is formed skeleton symbol and is expressed as: Mg-(10.5-11.5) Zn-(0.95-1.05) Sc.
2, the preparation method of a kind of magnesium-zinc-scandium alloy as claimed in claim 1 is characterized in that, step and condition are:
With purity is that 99.9% Mg ingot, 99.5% Zn ingot, 99.5% Mg-Sc intermediate alloy ingot are alloy raw material; Wherein, to account for the master alloy weight percent be 2.3% to the Sc in the Mg-Sc intermediate alloy ingot;
Mg ingot, Zn ingot and intermediate alloy ingot raw material through cut apart, oil removing, drying and scale removal make raw material block; Carry out weighing according to the quality proportioning, raw material block is dipped in molten salt pool hang that to join smelting temperature behind the fused salt be in 800 ℃ the smelting furnace, the extension fused salt dips in institute, and to select the NaCl:KCl mol ratio for use be that 1:3, purity are the fused salt mixt of chemical pure NaCl and KCl;
Order of addition(of ingredients) in smelting furnace is: metal M g piece, Metal Zn piece and Mg-Sc master alloy piece, and the crucible of this smelting furnace is a plumbago crucible; It is the fused salt mixt of chemical pure NaCl and KCl that protective material molten chloride composition dips in extension fused salt composition identical mol ratio 1 to 3, purity with the shove charge raw material block; All furnace charges melt the back and stirred 2 minutes, and alloy left standstill 15 minutes, adopt casting process, and teeming temperature is at 760 ℃, and casting mold uses preheating stainless steel metal mould, and preheating temperature obtains magnesium-zinc-scandium alloy at 250 ℃.
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| CN100532605C true CN100532605C (en) | 2009-08-26 |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20030029526A1 (en) * | 2001-04-11 | 2003-02-13 | Kim Do Hyang | Quasicrystalline phase-reinforced Mg-based metallic alloy with high warm and hot formability and method of making the same |
| CN1475592A (en) * | 2003-07-11 | 2004-02-18 | 武汉理工大学 | High Zinc aluminium rare earth magnesium alloy |
| CN1488773A (en) * | 2003-09-05 | 2004-04-14 | 郑州大学 | Rare-earth-containg high-zinc-magnesium alloy and preparing method thereof |
| US20070102072A1 (en) * | 2003-11-26 | 2007-05-10 | Yoshihito Kawamura | High strength and high toughness magnesium alloy and method of producing the same |
-
2007
- 2007-12-06 CN CNB2007100563995A patent/CN100532605C/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20030029526A1 (en) * | 2001-04-11 | 2003-02-13 | Kim Do Hyang | Quasicrystalline phase-reinforced Mg-based metallic alloy with high warm and hot formability and method of making the same |
| CN1475592A (en) * | 2003-07-11 | 2004-02-18 | 武汉理工大学 | High Zinc aluminium rare earth magnesium alloy |
| CN1488773A (en) * | 2003-09-05 | 2004-04-14 | 郑州大学 | Rare-earth-containg high-zinc-magnesium alloy and preparing method thereof |
| US20070102072A1 (en) * | 2003-11-26 | 2007-05-10 | Yoshihito Kawamura | High strength and high toughness magnesium alloy and method of producing the same |
Non-Patent Citations (1)
| Title |
|---|
| 微量Sc元素对AZ91镁合金组织性能的影响. 王斌等.铸造，第54卷第5期. 2005 * |
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