CN102653829B - Preparation method of AlSc alloy - Google Patents
Preparation method of AlSc alloy Download PDFInfo
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- CN102653829B CN102653829B CN 201210155381 CN201210155381A CN102653829B CN 102653829 B CN102653829 B CN 102653829B CN 201210155381 CN201210155381 CN 201210155381 CN 201210155381 A CN201210155381 A CN 201210155381A CN 102653829 B CN102653829 B CN 102653829B
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Abstract
The invention relates to the technical field of alloy preparation, and specifically relates to a preparation method of an AlSc alloy. The preparation method comprises the following steps of: placing a compounding reducer aluminium strontium alloy on the bottom of a crucible, then uniformly mixing raw material strontia and a fluxing agent ice stone as well as sodium chloride, covering on the upper part of the aluminium strontium alloy, wherein the weight ratio of the components is as follows: strontia to sodium chloride to aluminium strontium alloy is equal to (4-15): (100-140): (60-100): (80-120); then heating the crucible to ensure the temperature to achieve 800-1110 DEGC, carrying out reducing reaction for 30-120 minutes, and generating an AlSc alloy liquid; and finally ensuring the AlSc alloy liquid to enter a module for casting to prepare an AlSc alloy pig. The preparation method provided by the invention takes Sc2O3 which is cheap and easy to get as a raw material, and does not need fluoridation or chlorination; the process is simple and reliable, the preparation method has no pollution, the cost is low, the scandium quantity contained in the alloy is higher, the vertical collection efficiency of scandium is 60%-85%, and the preparation method is suitable for large-scale industry production.
Description
Technical field
The present invention relates to the alloy preparing technical field, be specifically related to a kind of preparation method of aluminum scandium alloy.
Background technology
Aluminum scandium alloy is a kind of high-performance aluminium alloy, and the high performance of aluminium alloy has several approach, and wherein the microalloying highly malleablized is the Disciplinary Frontiers of high-performance aluminium alloy research over nearly 20 years.So-called microalloying highly malleablized typically refers to adds mass percent or compound adding in aluminium alloy so as to increasing substantially a kind of technology of alloy strength and toughness less than 0.5% trace element.Scandium is added in aluminium and aluminium alloy as a kind of transition element and rare earth element, significantly thereby refinement cast alloy crystal grain, raising recrystallization temperature improve intensity and the toughness of aluminium alloy, and can significantly improve the effect of weldability, thermotolerance, corrosion stability, thermostability and the anti-neutron irradiation damage of aluminium alloy.Therefore, aluminum scandium alloy is considered to space flight and aviation of new generation, naval vessel, weapons high-performance aluminium alloy structured material.
Al-Sc alloy preparation method commonly used has:
1, to the method for mixing:
To produce the traditional method of Al-Sc master alloy to the method for mixing.To the method for mixing be a certain proportion of High Purity Scandium Metal is wrapped with aluminium foil after, mix under argon shield in the aluminium liquid of fusing, the insulation enough time is cast in swage or water cooled copper mould after fully stirring, and can make the Al-Sc master alloy.Can make to the method for mixing the Al-Sc master alloy that contains Sc2%～11%, principle and technique are all simple, but Sc and Al fusing point differ greatly, and molten aluminium need be heated to higher temperature, is difficult to be made into ingredient stability, the Al-Sc master alloy product that is evenly distributed.It is raw material that the method for mixing is needed expensive metal Sc, can not avoid the scaling loss of metal Sc, causes the casting yield of metal Sc not high, causes cost higher, and this has limited the application of this method;
2, fused salt electrolysis process:
At Na
3AlF
6-KCl – NaCl-ScF
3, ScCl
3-KCl – NaCl, Na
3AlF
6-LiF-Sc
2O
3Logical argon shield in system, 850～1100 ℃ of temperature, graphite cathode carries out fused salt electrolysis.But this method processing requirement is high, and current efficiency is 65%～80%, and the corrodibility of villiaumite is serious, the easy corrosion failure of electrolyzer and electrode materials.Fused salt electrolysis process also is in the laboratory study stage at present, has a lot of problems to need further research;
3, scandium fluoride vacuum aluminum hot reducing method:
This method is take scandium fluoride as raw material, and activated aluminum powder is reductive agent, reduces under vacuum condition.With aluminium powder and ScF
3Put into corundum crucible after mixed compaction, then be placed in the reactor that quartzy material is made, vacuumize, under 900～920 ℃, thermal reduction 30～600min, ScF
3Transformation efficiency be 87%～92%.The master alloy that this method obtains is very inhomogeneous, and the content of ingot bottom exceeds 1.5～5 times than top, thus must remelting in argon shield, the rate of recovery that scandium enters master alloy only 70%;
4, the direct thermit reduction of Scium trioxide:
The main points of this method are take the powdery Scium trioxide as raw material, and it is mixed with activated aluminum powder, make bead and afterwards it are immersed in the aluminium liquid of melting, aluminium liquid is as reductive agent, and aluminium powder is as dispersion agent, at high temperature, Scium trioxide is reduced into metal scandium, and Sc enters and forms the Al-Sc master alloy in aluminium liquid.This method operational path is simple, but weak point is to carry out in atmosphere, if bead does not have abundant compacting during batch mixing, the part air that wherein contains forms Sc in reaction
2O
3, Al
2O
3N, η Al
2O
3Deng impurity, the casting yield of the purity of master alloy and metal Sc still remains further to be improved;
5, the thermit reduction of Scium trichloride:
At first with Sc
2O
3Use dissolving with hydrochloric acid, then evaporation and the standby anhydrous ScCl of Dehydration
3, vacuumize with 900 ℃ of applying argon gas under go out scandium with the magnesium reduction metal, and then collect with aluminium, generate the Al-Mg-Sc master alloy.But anhydrous ScCl
3Be difficult to preparation, and the easy moisture absorption, be difficult to preserve, the research of still needing of reduction mechanism and technique is difficult to carry out industrial-scale production.
Summary of the invention
The objective of the invention is the deficiency for the prior art existence, provide a kind of preparation method of aluminum scandium alloy, with Sc cheap and easy to get
2O
3Be raw material, need not to fluoridize or chlorination, simple and reliable process, pollution-free, cost is low, and alloy to contain the scandium amount higher, the direct yield of scandium can carry out large-scale commercial production 60%～85%.
The technical scheme that realizes the object of the invention is to carry out as follows:
At first the complex reducing agent al-sr alloy is positioned over crucible bottom, then raw material Scium trioxide and flux sodium aluminum fluoride, sodium-chlor are mixed, and be covered in al-sr alloy top, each component proportion is by weight: Scium trioxide: sodium aluminum fluoride: sodium-chlor: al-sr alloy=(4～15): (100～140): (60～100): (80～120): then heating crucible makes its temperature reach 800～1110 ℃, carry out reduction reaction 30～120min, generate aluminum scandium alloy liquid; At last aluminum scandium alloy liquid is entered the mould casting, make the aluminum scandium alloy ingot;
Described crucible is alumina crucible or plumbago crucible;
The proportioning of described complex reducing agent al-sr alloy is by weight: aluminium: strontium=(16～24): (1～5);
In the aluminum scandium alloy of preparation, each compositions in weight percentage is: scandium: 1～3%, and scandium+aluminium〉99%.
Compared with prior art, characteristics of the present invention and beneficial effect thereof are:
1. contain Sc:1～3wt%, Sc+Al in the aluminum scandium alloy of the present invention's preparation〉99wt%, contain a small amount of Sr, Si, Fe, Ca, difference＜0.05wt%;
2. the inventive method technique is simple, and is pollution-free, and production cost is low, and raw material sources are wide, and reaction equilibrium constant is high, and alloy scandium content is higher, and foreign matter content is low, excellent property;
3. the aluminum scandium alloy of the inventive method preparation is applicable to the additive of various aluminium alloys and other alloys, can significantly improve the mechanical property of alloy.
Embodiment
Below in conjunction with embodiment, the present invention is elaborated, but protection scope of the present invention is not limited only to following embodiment: embodiment 1: with proportioning be by weight at first: aluminium: the complex reducing agent al-sr alloy of strontium=24:1 is positioned over bottom alumina crucible or plumbago crucible, then raw material Scium trioxide and flux sodium aluminum fluoride, sodium-chlor are mixed, and being covered in al-sr alloy top, each component proportion is by weight: Scium trioxide: sodium aluminum fluoride: sodium-chlor: al-sr alloy=4:100:60:80; Then heating crucible makes its temperature reach 800 ℃, carries out reduction reaction 120min, generates aluminum scandium alloy liquid; At last aluminum scandium alloy liquid is entered the mould casting, make the aluminum scandium alloy ingot, after testing, alloying constituent is by weight percentage: scandium: 1%, and scandium+aluminium is 99.1%.
Embodiment 2: with proportioning be by weight at first: aluminium: the complex reducing agent al-sr alloy of strontium=16:5 is positioned over bottom alumina crucible or plumbago crucible, then raw material Scium trioxide and flux sodium aluminum fluoride, sodium-chlor are mixed, and being covered in al-sr alloy top, each component proportion is by weight: Scium trioxide: sodium aluminum fluoride: sodium-chlor: al-sr alloy=15:140:100:120; Then heating crucible makes its temperature reach 1110 ℃, carries out reduction reaction 30min, generates aluminum scandium alloy liquid; At last aluminum scandium alloy liquid is entered the mould casting, make the aluminum scandium alloy ingot, after testing, alloying constituent is by weight percentage: scandium: 3%, and scandium+aluminium is 99.7%.
Embodiment 3: with proportioning be by weight at first: aluminium: the complex reducing agent al-sr alloy of strontium=20:3 is positioned over bottom alumina crucible or plumbago crucible, then raw material Scium trioxide and flux sodium aluminum fluoride, sodium-chlor are mixed, and being covered in al-sr alloy top, each component proportion is by weight: Scium trioxide: sodium aluminum fluoride: sodium-chlor: al-sr alloy=8:120:81:100; Then heating crucible makes its temperature reach 1000 ℃, carries out reduction reaction 60min, generates aluminum scandium alloy liquid; At last aluminum scandium alloy liquid is entered the mould casting, make the aluminum scandium alloy ingot, after testing, alloying constituent is by weight percentage: scandium: 2%, and scandium+aluminium is 99.5%.
Claims (3)
1. the preparation method of an aluminum scandium alloy, it is characterized in that carrying out as follows: at first the complex reducing agent al-sr alloy is positioned over crucible bottom, then raw material Scium trioxide and flux sodium aluminum fluoride, sodium-chlor are mixed, and being covered in al-sr alloy top, each component proportion is by weight: Scium trioxide: sodium aluminum fluoride: sodium-chlor: al-sr alloy=(4～15): (100～140): (60～100): (80～120); Then heating crucible makes its temperature reach 800～1110 ℃, carries out reduction reaction 30～120min, generates aluminum scandium alloy liquid; At last aluminum scandium alloy liquid is entered the mould casting, make the aluminum scandium alloy ingot;
The proportioning of described complex reducing agent al-sr alloy is by weight: aluminium: strontium=(16～24): (1～5).
2. the preparation method of a kind of aluminum scandium alloy according to claim 1, is characterized in that described crucible is alumina crucible or plumbago crucible.
3. the preparation method of a kind of aluminum scandium alloy according to claim 1, in the aluminum scandium alloy that it is characterized in that preparing, each compositions in weight percentage is: scandium: 1～3%, scandium+aluminium〉99%.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104388713A (en) * | 2014-10-31 | 2015-03-04 | 三祥新材股份有限公司 | Preparation method of aluminum-zirconium alloy |
Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| AU2013201572B2 (en) * | 2013-03-15 | 2014-12-11 | Commonwealth Scientific And Industrial Research Organisation | Production of Aluminium-Scandium Alloys |
| CN105803235B (en) * | 2014-12-30 | 2018-03-16 | 有研稀土新材料股份有限公司 | Preparation method, scandium bearing master alloy and the aluminium-scandium alloy of scandium bearing master alloy |
| ES2774075T3 (en) * | 2015-04-22 | 2020-07-16 | Obshchestvo S Ogranichennoy Otvetstvennostyu Obedinennaya Kompaniya Rusal Inzhenerno Tekh Tsentr | Production procedure of an aluminum alloy and scandium |
| CN107868877B (en) * | 2017-11-03 | 2020-01-31 | 郑州大学 | Method for preparing aluminum-scandium alloy by adopting segmented countercurrent reduction method |
| US10988830B2 (en) | 2018-01-16 | 2021-04-27 | Scandium International Mining Corporation | Scandium master alloy production |
| US11384412B2 (en) | 2018-01-16 | 2022-07-12 | Scandium International Mining Corporation | Direct scandium alloying |
| CN116024443B (en) * | 2023-03-30 | 2023-06-20 | 湖南东方钪业股份有限公司 | Recovery method of scandium metal |
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| WO2003042418A1 (en) * | 2001-11-12 | 2003-05-22 | Sergei Vladimirovich Makhov | Method for producing an aluminium-scandium foundry alloy and a flux for producing said aluminium-scandium foundry alloy |
| CN1605641A (en) * | 2004-11-09 | 2005-04-13 | 湖南稀土金属材料研究院 | Method for preparation of aluminum scandium alloy by alumino-thermic reduction method |
| CN101709394A (en) * | 2009-12-11 | 2010-05-19 | 清华大学 | Preparation method of aluminum-scandium master alloy |
| CN102337406A (en) * | 2011-09-26 | 2012-02-01 | 河北四通新型金属材料股份有限公司 | Method for preparing aluminum-scandium intermediate alloy by using aluminothermic reduction method |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2003042418A1 (en) * | 2001-11-12 | 2003-05-22 | Sergei Vladimirovich Makhov | Method for producing an aluminium-scandium foundry alloy and a flux for producing said aluminium-scandium foundry alloy |
| CN1605641A (en) * | 2004-11-09 | 2005-04-13 | 湖南稀土金属材料研究院 | Method for preparation of aluminum scandium alloy by alumino-thermic reduction method |
| CN101709394A (en) * | 2009-12-11 | 2010-05-19 | 清华大学 | Preparation method of aluminum-scandium master alloy |
| CN102337406A (en) * | 2011-09-26 | 2012-02-01 | 河北四通新型金属材料股份有限公司 | Method for preparing aluminum-scandium intermediate alloy by using aluminothermic reduction method |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104388713A (en) * | 2014-10-31 | 2015-03-04 | 三祥新材股份有限公司 | Preparation method of aluminum-zirconium alloy |
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