CN110629058A - Preparation method of aluminum-scandium alloy - Google Patents
Preparation method of aluminum-scandium alloy Download PDFInfo
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- CN110629058A CN110629058A CN201810661064.4A CN201810661064A CN110629058A CN 110629058 A CN110629058 A CN 110629058A CN 201810661064 A CN201810661064 A CN 201810661064A CN 110629058 A CN110629058 A CN 110629058A
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- LUKDNTKUBVKBMZ-UHFFFAOYSA-N aluminum scandium Chemical compound [Al].[Sc] LUKDNTKUBVKBMZ-UHFFFAOYSA-N 0.000 title claims abstract description 157
- 229910000542 Sc alloy Inorganic materials 0.000 title claims abstract description 152
- 238000002360 preparation method Methods 0.000 title claims abstract description 22
- SIXSYDAISGFNSX-UHFFFAOYSA-N scandium atom Chemical compound [Sc] SIXSYDAISGFNSX-UHFFFAOYSA-N 0.000 claims abstract description 158
- 229910052706 scandium Inorganic materials 0.000 claims abstract description 155
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 114
- 238000002844 melting Methods 0.000 claims abstract description 112
- 230000008018 melting Effects 0.000 claims abstract description 112
- 229910052751 metal Inorganic materials 0.000 claims abstract description 111
- 239000002184 metal Substances 0.000 claims abstract description 111
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 76
- 239000000725 suspension Substances 0.000 claims abstract description 49
- 238000001816 cooling Methods 0.000 claims abstract description 39
- 238000003723 Smelting Methods 0.000 claims abstract description 35
- 230000001681 protective effect Effects 0.000 claims abstract description 10
- 239000012298 atmosphere Substances 0.000 claims abstract description 7
- 238000000034 method Methods 0.000 claims description 45
- 238000010309 melting process Methods 0.000 claims description 35
- 238000004321 preservation Methods 0.000 claims description 31
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 12
- 239000007789 gas Substances 0.000 claims description 10
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- 229910052786 argon Inorganic materials 0.000 claims description 6
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- 229910052724 xenon Inorganic materials 0.000 claims description 3
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 claims description 3
- 238000005204 segregation Methods 0.000 abstract description 11
- 239000012535 impurity Substances 0.000 abstract description 10
- 239000000463 material Substances 0.000 abstract description 9
- 239000002994 raw material Substances 0.000 abstract description 7
- 238000005516 engineering process Methods 0.000 abstract description 5
- 238000002425 crystallisation Methods 0.000 abstract description 4
- 230000008025 crystallization Effects 0.000 abstract description 4
- 230000002829 reductive effect Effects 0.000 abstract description 4
- 238000009835 boiling Methods 0.000 abstract description 3
- 239000012300 argon atmosphere Substances 0.000 description 13
- 239000000956 alloy Substances 0.000 description 11
- 229910045601 alloy Inorganic materials 0.000 description 10
- 230000000052 comparative effect Effects 0.000 description 9
- 239000000203 mixture Substances 0.000 description 6
- 238000005260 corrosion Methods 0.000 description 5
- 230000007797 corrosion Effects 0.000 description 5
- 239000000843 powder Substances 0.000 description 5
- 230000008569 process Effects 0.000 description 5
- 230000009467 reduction Effects 0.000 description 5
- 150000003839 salts Chemical class 0.000 description 5
- 229910000838 Al alloy Inorganic materials 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 4
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 4
- 238000005868 electrolysis reaction Methods 0.000 description 4
- 230000007613 environmental effect Effects 0.000 description 4
- 229910002804 graphite Inorganic materials 0.000 description 4
- 239000010439 graphite Substances 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- 238000005245 sintering Methods 0.000 description 4
- 238000010183 spectrum analysis Methods 0.000 description 4
- 238000002474 experimental method Methods 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- OEKDNFRQVZLFBZ-UHFFFAOYSA-K scandium fluoride Chemical compound F[Sc](F)F OEKDNFRQVZLFBZ-UHFFFAOYSA-K 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 239000004411 aluminium Substances 0.000 description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 2
- 238000005266 casting Methods 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000009616 inductively coupled plasma Methods 0.000 description 2
- 230000000670 limiting effect Effects 0.000 description 2
- 229910052763 palladium Inorganic materials 0.000 description 2
- 238000004663 powder metallurgy Methods 0.000 description 2
- HYXGAEYDKFCVMU-UHFFFAOYSA-N scandium(III) oxide Inorganic materials O=[Sc]O[Sc]=O HYXGAEYDKFCVMU-UHFFFAOYSA-N 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- KLZUFWVZNOTSEM-UHFFFAOYSA-K Aluminum fluoride Inorganic materials F[Al](F)F KLZUFWVZNOTSEM-UHFFFAOYSA-K 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 description 1
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 1
- 229910020549 KCl—NaCl Inorganic materials 0.000 description 1
- 229910017665 NH4HF2 Inorganic materials 0.000 description 1
- 229910018096 ScF3 Inorganic materials 0.000 description 1
- 229910001514 alkali metal chloride Inorganic materials 0.000 description 1
- -1 aluminium-scandium Chemical compound 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 238000007872 degassing Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 239000012025 fluorinating agent Substances 0.000 description 1
- 239000011737 fluorine Substances 0.000 description 1
- 229910052731 fluorine Inorganic materials 0.000 description 1
- 230000004907 flux Effects 0.000 description 1
- 239000011888 foil Substances 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- 230000005012 migration Effects 0.000 description 1
- 238000013508 migration Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 238000001953 recrystallisation Methods 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- PUZPDOWCWNUUKD-UHFFFAOYSA-M sodium fluoride Chemical compound [F-].[Na+] PUZPDOWCWNUUKD-UHFFFAOYSA-M 0.000 description 1
- 238000005477 sputtering target Methods 0.000 description 1
- 239000013077 target material Substances 0.000 description 1
- 238000003466 welding Methods 0.000 description 1
Classifications
-
- 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
- C22C1/026—Alloys based on aluminium
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C21/00—Alloys based on aluminium
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Manufacture And Refinement Of Metals (AREA)
- Physical Vapour Deposition (AREA)
Abstract
The application relates to a preparation method of an aluminum-scandium alloy, which comprises the following steps: and in a protective gas atmosphere, melting metal scandium by adopting vacuum suspension melting, preserving heat, adding metal aluminum for melting, preserving heat, and cooling to obtain the aluminum-scandium alloy. According to the preparation method of the aluminum-scandium alloy, metal scandium and metal aluminum are used as raw materials, a vacuum suspension smelting technology is adopted, crucible material pollution is avoided in the preparation process, impurities cannot be introduced, the cost is low, the environment is protected, the heat is preserved after the metal scandium is melted, the impurities with low boiling points are fully volatilized, and the prepared aluminum-scandium alloy is extremely low in impurity content; and slowly adding metal aluminum to melt, and then preserving heat, so that the aluminum element and the scandium element are uniformly distributed during crystallization, and the segregation degree is reduced.
Description
Technical Field
The invention relates to the technical field of aluminum alloy materials, in particular to a preparation method of an aluminum-scandium alloy.
Background
The scandium metal has the functions of refining grains, inhibiting alloy recrystallization, improving corrosion resistance and the like in the aluminum alloy, and can obviously improve the strength, plasticity, high-temperature performance, corrosion resistance, welding performance and the like of the alloy. Therefore, the aluminum scandium alloy is considered as a new generation of high-performance aluminum alloy structural material for aerospace, ships and weapons. In addition, researches show that the aluminum scandium film deposited by the aluminum scandium alloy target material not only can keep the conductivity equivalent to that of high-purity aluminum, but also can improve the corrosion resistance, and particularly can obviously inhibit electromigration and stress migration. Therefore, aluminum scandium alloy palladium is also considered as a new-generation wiring material for large-scale integrated circuits. In conclusion, the aluminum-scandium alloy has a wide application prospect in high-tech fields such as aerospace, electronic information technology and the like due to the excellent performance of the aluminum-scandium alloy. With the rapid development of science and technology, the research on key materials in China is more and more important, and the demand of high-performance and high-quality aluminum-scandium alloy is also greater and greater.
The traditional preparation method of the aluminum-scandium alloy mainly comprises a counter doping method, a molten salt electrolysis method, an aluminothermic reduction method and a powder metallurgy method.
The opposite doping method comprises the steps of wrapping a certain proportion of metal scandium with an aluminum foil, doping the metal scandium into molten aluminum under the protection of argon, preserving heat for enough time, fully stirring, and injecting into an iron mold or a water-cooled copper mold to obtain the aluminum-scandium intermediate alloy. However, the aluminum scandium compound formed by the method has coarse grains and very serious composition segregation.
Lava electrolysis method mainly on Na3AlF6-KCl-NaCl-ScF3Or ScCl3-KCl-NaCl or Na3AlF6-LiF-Sc2O3Introducing argon gas into the system for protection, and carrying out molten salt electrolysis on a graphite cathode at the temperature of 850-1100 ℃ to prepare the aluminum-scandium alloy. The prior art discloses a fused salt electrolysis method of aluminum-scandium master alloy, which comprises the step of using fluoride fused salt M in a prebaked anode fused salt electrolytic cell with point-type blanking3AlF6-AlF3Is a basic electrolyte system, alumina and scandium-containing compound are used as raw materials, and an independent blanking mode is adoptedMetallic aluminium and metallic scandium are electrolytically separated from different cathode regions in an electrolytic cell and alloyed, so that an aluminium-scandium master alloy with a scandium content of 1.5-3.0% and a total aluminium and scandium content of more than 99% is obtained. However, the method has the advantages of high process requirement, low current efficiency (65-80%), serious corrosion of villiaumite, easy corrosion failure of an electrolytic cell and an electrode material, high energy consumption, high cost and environmental friendliness.
The preparation of the aluminum-scandium alloy by the aluminothermic reduction method mainly comprises a scandium fluoride vacuum aluminothermic reduction method and a scandium fluoride direct aluminothermic reduction method. The method comprises the steps of filling raw materials of scandium fluoride and aluminum into a graphite crucible, then placing the graphite crucible into a vacuum reactor, vacuumizing at low temperature for degassing, vacuumizing to-0.1 MPa, heating to melt the aluminum, heating to 1100-1350 ℃, continuously stirring, controlling the temperature until the surface of a melt is clear, and then cooling and casting to obtain the aluminum-scandium alloy. However, the higher the scandium content of the aluminum-scandium alloy obtained by the method, the more serious the composition segregation is, and fluorine element is also introduced. In addition, the prior art discloses a method for preparing aluminum-scandium alloy by aluminothermic reduction, which takes powdery scandium oxide as a raw material and NH4HF2NaF and alkali metal chloride as fluorinating agent, fluxing agent and flux, and aluminum as reducing agent, heating to 850-1100 deg.C in alumina or graphite crucible, and casting to obtain alloy ingot. The mass content of scandium in the alloy ingot is 1% -3%, the sum of the mass contents of scandium and aluminum is more than 99%, and the yield of scandium is more than 80%. Therefore, the method can only prepare the aluminum-scandium alloy with low scandium content, and impurities are introduced in the preparation process, so that the method has large limitation.
The powder metallurgy method is an aluminum-scandium intermediate alloy obtained by fully and uniformly mixing high-purity metal scandium powder and aluminum powder in a certain proportion, pressing and forming the mixture, and then carrying out sintering and other heat treatment processes under the protection of argon. The prior art discloses a preparation method of an aluminum-scandium alloy target blank, and the method adopts a powder sintering method to prepare the aluminum-scandium alloy target blank containing 0.1-15% of scandium. In addition, the prior art discloses an aluminum-scandium alloy target blank and a preparation method thereof, wherein the method adopts a powder sintering method to prepare an aluminum-scandium alloy palladium blank containing 16-50% of scandium. In addition, the prior art discloses an aluminum-scandium alloy with high scandium content and a preparation method thereof, and the method adopts a powder sintering method to prepare the aluminum-scandium alloy with 55% -70% scandium content. However, the methods all need expensive metal powder as a raw material, so that the cost is high, the metal scandium powder and the aluminum powder are easy to oxidize, the oxygen content is high, the purity of the product is influenced, and the density of the alloy is difficult to reach the density of the alloy prepared by smelting.
Therefore, the research of finding a preparation method of the aluminum-scandium alloy with high purity, low segregation, low cost and environmental protection is important.
Disclosure of Invention
Accordingly, there is a need for a method for preparing an aluminum-scandium alloy with high purity, low segregation, low cost and environmental protection.
A preparation method of an aluminum-scandium alloy comprises the following steps:
and in a protective gas atmosphere, melting metal scandium by adopting vacuum suspension melting, preserving heat, adding metal aluminum for melting, preserving heat, and cooling to obtain the aluminum-scandium alloy.
In one embodiment, the method further comprises the following steps:
and repeatedly carrying out melting steps of melting the aluminum-scandium alloy by adopting vacuum suspension melting, then preserving heat, adding metal aluminum for melting, then preserving heat and cooling, wherein in the repeated melting process of the aluminum-scandium alloy, the mass of the metal aluminum added in each melting process does not exceed 180% of the mass of the metal scandium, and the aluminum-scandium alloy with the scandium mass content of more than 30% is obtained.
In one embodiment, the method further comprises the following steps:
repeatedly carrying out melting steps of melting the aluminum-scandium alloy by adopting vacuum suspension melting, then preserving heat, adding metal aluminum for melting, then preserving heat and cooling, wherein in the repeated melting process of the aluminum-scandium alloy, the mass of the metal aluminum added in each melting process does not exceed 180% of the mass of the metal scandium, until the aluminum-scandium alloy with the scandium mass content of 30% is obtained;
and (2) repeatedly melting the aluminum-scandium alloy with the scandium mass content of 30% by adopting vacuum suspension melting, then preserving heat, adding metal aluminum for melting, then preserving heat and cooling, wherein in the repeated melting process of the aluminum-scandium alloy with the scandium mass content of 30%, the mass of the metal aluminum added in each melting process is not more than 150% of the mass of the metal scandium until the aluminum-scandium alloy with the scandium mass content of more than 15% and less than 30% is obtained.
In one embodiment, the method further comprises the following steps:
repeatedly carrying out melting steps of melting the aluminum-scandium alloy by adopting vacuum suspension melting, then preserving heat, adding metal aluminum for melting, then preserving heat and cooling, wherein in the repeated melting process of the aluminum-scandium alloy, the mass of the metal aluminum added in each melting process does not exceed 180% of the mass of the metal scandium, until the aluminum-scandium alloy with the scandium mass content of 30% is obtained;
repeatedly melting the aluminum-scandium alloy with the scandium mass content of 30% by adopting vacuum suspension melting, then preserving heat, adding metal aluminum for melting, then preserving heat and cooling, wherein in the repeated melting process of the aluminum-scandium alloy with the scandium mass content of 30%, the mass of the metal aluminum added in each melting process does not exceed 150% of the mass of the metal scandium, until the aluminum-scandium alloy with the scandium mass content of 15% is obtained;
and repeatedly melting the aluminum-scandium alloy with the scandium mass content of 15% by adopting vacuum suspension melting, then preserving heat, adding metal aluminum for melting, then preserving heat and cooling, wherein in the repeated melting process of the aluminum-scandium alloy with the scandium mass content of 15%, the mass of the metal aluminum added in each melting process does not exceed 130% of the mass of the metal scandium, until the aluminum-scandium alloy with the scandium mass content of less than 15% is obtained.
In one embodiment, the protective gas is argon, xenon, or nitrogen.
In one embodiment, the current of the coil for vacuum suspension smelting is 100-200A, and the output power of the power supply is 45-110 KW.
In one embodiment, the heat preservation time after the metal scandium vacuum suspension smelting is melted is 10-25 minutes.
In one embodiment, the time for heat preservation after the metal aluminum is added and melted is 10-25 minutes.
According to the preparation method of the aluminum-scandium alloy, metal scandium and metal aluminum are used as raw materials, a vacuum suspension smelting technology is adopted, crucible material pollution is avoided in the preparation process, impurities cannot be introduced, the cost is low, the environment is protected, heat is preserved after the metal scandium is melted, the impurities with low boiling points are fully volatilized, and the prepared aluminum-scandium alloy is extremely low in impurity content; and slowly adding metal aluminum to melt, and then preserving heat, so that the aluminum element and the scandium element are uniformly distributed during crystallization, and the segregation degree is reduced.
Drawings
FIG. 1 is a diagram of a spectrum analysis of an aluminum-scandium alloy prepared in example 1;
fig. 2 is a diagram of the energy spectrum analysis of the aluminum-scandium alloy prepared in example 2.
Detailed Description
In order that the invention may be more fully understood, a more particular description of the invention will now be rendered by reference to specific embodiments thereof that are illustrated in the appended drawings. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used in the description of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. As used herein, the term "and/or" includes any and all combinations of one or more of the associated listed items.
The method for preparing an aluminum-scandium alloy according to an embodiment includes the following steps S110:
s110, in a protective gas atmosphere, melting metal scandium in a vacuum suspension manner, preserving heat, adding metal aluminum to melt, preserving heat, and cooling to obtain the aluminum-scandium alloy, wherein the mass of the metal aluminum is not more than 180% of that of the metal scandium.
In the present embodiment, the metallic scandium is high-purity scandium having a purity of 99.9% or more, and the metallic aluminum is high-purity aluminum having a purity of 99.9% or more.
It can be understood that metallic scandium and metallic aluminum are lower in cost than metallic scandium powder and metallic aluminum powder.
Further, the protective gas is argon, xenon or nitrogen.
Specifically, the vacuum suspension smelting adopts a suspension type cold crucible smelting method.
Furthermore, the current of the coil for vacuum suspension smelting is 100-200A, and the output power of the power supply is 45-110 KW.
Further, the heat preservation time after the metal scandium is melted in a vacuum suspension smelting mode is 10-25 minutes. And the heat preservation time after the metal aluminum is added and melted is 10-25 minutes.
The preparation method of the aluminum-scandium alloy can prepare the aluminum-scandium alloy with scandium mass content of more than 35.7%.
The method for preparing an aluminum-scandium alloy according to an embodiment includes steps S210 to S220 of:
s210, in a protective gas atmosphere, melting metal scandium in a vacuum suspension manner, preserving heat, adding metal aluminum to melt, preserving heat, and cooling to obtain the aluminum-scandium alloy, wherein the mass of the metal aluminum is not more than 180% of that of the metal scandium.
S220, repeatedly melting the aluminum-scandium alloy by adopting vacuum suspension melting, then preserving heat, adding metal aluminum for melting, then preserving heat and cooling, wherein in the repeated melting process of the aluminum-scandium alloy, the mass of the metal aluminum added in each melting process does not exceed 180% of the mass of the metal scandium, and the aluminum-scandium alloy with the scandium mass content of more than 30% is obtained.
It is understood that an aluminum-scandium alloy having a scandium content of 35.7% by mass or more is obtained in step S210. Therefore, an aluminum-scandium alloy having a scandium content of 35.7% by mass or more is prepared, and the step S220 described above can be omitted.
In addition, in the process of repeatedly smelting the aluminum-scandium alloy, the mass of the metallic aluminum added in each smelting can be added according to an upper limit value (180% of the mass of the metallic scandium) until the addition is finished, the mass of the metallic aluminum added in each smelting can be controlled to be lower than 180% of the mass of the metallic scandium until the addition is finished, or the metallic aluminum can be added irregularly as long as the mass of the metallic aluminum added in each smelting is controlled to be not more than 180% of the mass of the metallic scandium.
For example, in an aluminum-scandium alloy with a scandium content of 30% by mass, the mass of the metallic aluminum added in the first melting may be 180% of the scandium mass, and the mass of the metallic aluminum added in the second melting may be 53.3% of the scandium mass.
Alternatively, the mass of the metallic aluminum added in the first melting may be 100% of the mass of scandium, the mass of the metallic aluminum added in the second melting may be 100% of the mass of scandium, and the mass of the metallic aluminum added in the third melting may be 33.3% of the mass of scandium.
Alternatively, the mass of the metallic aluminum added in the first melting may be 50% of the mass of scandium, the mass of the metallic aluminum added in the second melting may be 150% of the mass of scandium, and the mass of the metallic aluminum added in the third melting may be 133% of the mass of scandium.
The aluminum-scandium alloy can be used for preparing the aluminum-scandium alloy with the scandium mass content of more than 30%.
The method for producing an aluminum-scandium alloy according to an embodiment includes steps S310 to S330:
s310, in a protective gas atmosphere, melting metal scandium in a vacuum suspension manner, preserving heat, adding metal aluminum to melt, preserving heat, and cooling to obtain the aluminum-scandium alloy, wherein the mass of the metal aluminum is not more than 180% of that of the metal scandium.
And S320, repeatedly melting the aluminum-scandium alloy by adopting vacuum suspension melting, then preserving heat, adding metal aluminum for melting, then preserving heat and cooling, wherein in the repeated melting process of the aluminum-scandium alloy, the mass of the metal aluminum added in each melting process does not exceed 180% of the mass of the metal scandium, until the aluminum-scandium alloy with the scandium mass content of 30% is obtained.
S330, repeatedly melting the aluminum-scandium alloy with 30% of scandium by vacuum suspension melting, then preserving heat, adding metal aluminum for melting, preserving heat and cooling, wherein in the repeated melting process of the aluminum-scandium alloy with 30% of scandium by mass, the mass of the metal aluminum added in each melting process does not exceed 150% of the mass of the metal scandium until the aluminum-scandium alloy with 15% or more and less than 30% of scandium by mass is obtained.
The preparation method of the aluminum-scandium alloy can be used for preparing the aluminum-scandium alloy with the mass content of scandium being more than or equal to 15% and less than 30%.
The method for preparing an aluminum-scandium alloy according to an embodiment includes steps S410 to S440 of:
s410, in a protective gas atmosphere, melting metal scandium in a vacuum suspension manner, preserving heat, adding metal aluminum to melt, preserving heat, and cooling to obtain the aluminum-scandium alloy, wherein the mass of the metal aluminum is not more than 180% of that of the metal scandium.
And S420, repeatedly melting the aluminum-scandium alloy by adopting vacuum suspension melting, then preserving heat, adding metal aluminum for melting, then preserving heat and cooling, wherein in the repeated melting process of the aluminum-scandium alloy, the mass of the metal aluminum added in each melting process does not exceed 180% of the mass of the metal scandium, and the aluminum-scandium alloy with the scandium mass content of 30% is obtained.
S430, repeatedly melting the aluminum-scandium alloy with the scandium mass content of 30% by adopting vacuum suspension melting, then preserving heat, adding metal aluminum for melting, preserving heat and cooling, wherein in the process of repeatedly melting the aluminum-scandium alloy with the scandium mass content of 30%, the mass of the metal aluminum added in each melting process does not exceed 150% of the mass of the metal scandium, until the aluminum-scandium alloy with the scandium mass content of 15% is obtained.
S440, repeatedly melting the aluminum-scandium alloy with the scandium mass content of 15% by adopting vacuum suspension melting, then preserving heat, adding metal aluminum for melting, preserving heat and cooling, wherein in the repeated melting process of the aluminum-scandium alloy with the scandium mass content of 15%, the mass of the metal aluminum added in each melting process does not exceed 130% of the mass of the metal scandium, and the aluminum-scandium alloy with the scandium mass content of less than 15% is obtained.
The preparation method of the aluminum-scandium alloy can be used for preparing the aluminum-scandium alloy with scandium mass content less than 15%.
The preparation method of the aluminum-scandium alloy has the advantages of simple process, short flow, high efficiency, low cost and environmental protection. The method is characterized in that metal scandium and metal aluminum are used as raw materials, a vacuum suspension smelting technology is adopted, crucible material pollution is avoided in the preparation process, impurities cannot be introduced, the temperature is kept after the metal scandium is melted, the impurities with lower boiling points are fully volatilized, and the content of the prepared aluminum-scandium alloy impurities is extremely low; and adding metal aluminum for melting, and then preserving heat, so that the aluminum element and the scandium element are uniformly distributed during crystallization, and the segregation degree is reduced.
In addition, the aluminum-scandium alloy with any scandium content can be prepared by repeatedly smelting the aluminum-scandium alloy and controlling the quality of the metallic aluminum added each time, and the metallic aluminum is added in multiple times by repeatedly smelting, so that the distribution uniformity of scandium and aluminum during crystallization is further improved, and the segregation degree is reduced.
The scandium content in the aluminum-scandium alloy prepared by the method can be in the range of 0.1-99%, the sum of the scandium and the aluminum is more than 99.9%, and the deviation of the scandium content is in the range of +/-0.5%.
The aluminum-scandium alloy prepared by the method has high density, small grain size and uniform components, and can be applied to high-performance aluminum alloy structural materials for aerospace, ships and weapons and high-performance sputtering targets for large-scale integrated circuits, semiconductor chips and micro-nano electronic devices.
The following are specific examples.
(1) Preparing materials: 300g of metallic scandium, 99.9% of purity, 1063g of metallic aluminum, 99.99% of purity.
(2) Smelting: and in an argon atmosphere, carrying out vacuum suspension smelting and melting on metal scandium, then carrying out heat preservation for 10 minutes, slowly adding 540g of metal aluminum, carrying out heat preservation for 20 minutes after melting, and cooling to obtain the aluminum-scandium alloy with scandium mass content of 35.7%.
(3) Smelting: and in an argon atmosphere, carrying out vacuum suspension melting on aluminum-scandium alloy with the scandium mass content of 35.7%, then carrying out heat preservation for 10 minutes, slowly adding 160g of metal aluminum, carrying out heat preservation for 20 minutes after melting, and cooling to obtain the aluminum-scandium alloy with the scandium mass content of 30%.
(4) Smelting: in an argon atmosphere, carrying out vacuum suspension melting and heat preservation for 10 minutes on an aluminum-scandium alloy with scandium mass content of 30%, slowly adding 363g of metallic aluminum for melting, carrying out heat preservation for 20 minutes, and cooling to obtain the aluminum-scandium alloy with scandium mass content of 22%.
The aluminum-scandium alloy with scandium content of 22% prepared in example 1 was detected by ICP-OES (inductively coupled plasma emission spectrometer) and scanning electron microscope.
Through detection, the sum of the mass contents of aluminum and scandium in the aluminum-scandium alloy prepared in example 1 is 99.95%, the deviation of the mass content of scandium is-0.46%, and the results of energy spectrum analysis refer to fig. 1 and table 1.
TABLE 1
Example 2
(1) Preparing materials: 300g of metallic scandium, 99.9% of purity, 3450g of metallic aluminum, 99.99% of purity.
(2) Smelting: and in an argon atmosphere, carrying out vacuum suspension smelting and melting on metal scandium, then carrying out heat preservation for 10 minutes, slowly adding 540g of metal aluminum, carrying out heat preservation for 20 minutes after melting, and cooling to obtain the aluminum-scandium alloy with scandium mass content of 35.7%.
(3) Smelting: and in an argon atmosphere, carrying out vacuum suspension melting on aluminum-scandium alloy with the scandium mass content of 35.7%, then carrying out heat preservation for 10 minutes, slowly adding 160g of metal aluminum, carrying out heat preservation for 20 minutes after melting, and cooling to obtain the aluminum-scandium alloy with the scandium mass content of 30%.
(4) Smelting: in an argon atmosphere, carrying out vacuum suspension melting and heat preservation for 10 minutes on an aluminum-scandium alloy with the scandium mass content of 30%, slowly adding 450g of metallic aluminum for melting, carrying out heat preservation for 20 minutes, and cooling to obtain the aluminum-scandium alloy with the scandium mass content of 20.7%.
(5) Smelting: in an argon atmosphere, carrying out vacuum suspension melting and melting on an aluminum-scandium alloy with scandium content of 20.7%, then carrying out heat preservation for 10 minutes, slowly adding 450g of metallic aluminum, carrying out heat preservation for 20 minutes, and cooling to obtain the aluminum-scandium alloy with scandium content of 15.7%.
(6) Smelting: in an argon atmosphere, carrying out vacuum suspension melting and melting on an aluminum-scandium alloy with scandium content of 15.7%, then carrying out heat preservation for 10 minutes, slowly adding 100g of metallic aluminum, carrying out heat preservation for 20 minutes, and cooling to obtain the aluminum-scandium alloy with scandium content of 15%.
(7) Smelting: in an argon atmosphere, carrying out vacuum suspension melting and heat preservation for 10 minutes on an aluminum-scandium alloy with the scandium mass content of 15%, slowly adding 390g of metallic aluminum, carrying out heat preservation for 20 minutes after melting, and cooling to obtain the aluminum-scandium alloy with the scandium mass content of 12.6%.
(8) Smelting: in an argon atmosphere, carrying out vacuum suspension melting and heat preservation for 10 minutes on an aluminum-scandium alloy with scandium mass content of 12.6%, slowly adding 390g of metallic aluminum, carrying out heat preservation for 20 minutes after melting, and cooling to obtain the aluminum-scandium alloy with scandium mass content of 10.8%.
(9) Smelting: in an argon atmosphere, carrying out vacuum suspension melting and melting on an aluminum-scandium alloy with scandium content of 10.8%, then carrying out heat preservation for 10 minutes, slowly adding 390g of metallic aluminum, carrying out heat preservation for 20 minutes after melting, and cooling to obtain the aluminum-scandium alloy with scandium content of 9.5%.
(10) Smelting: in an argon atmosphere, carrying out vacuum suspension melting and melting on an aluminum-scandium alloy with scandium content of 9.5%, then carrying out heat preservation for 10 minutes, slowly adding 390g of metallic aluminum, carrying out heat preservation for 20 minutes after melting, and cooling to obtain the aluminum-scandium alloy with scandium content of 8.4%.
(11) Smelting: in an argon atmosphere, carrying out vacuum suspension melting and melting on an aluminum-scandium alloy with scandium content of 8.4%, then carrying out heat preservation for 10 minutes, slowly adding 190g of metallic aluminum, carrying out heat preservation for 20 minutes, and cooling to obtain the aluminum-scandium alloy with scandium content of 8%.
The aluminum-scandium alloy with scandium content of 8% prepared in example 2 was detected by ICP-OES (inductively coupled plasma emission spectrometer) and scanning electron microscope.
Through detection, the sum of the mass contents of aluminum and scandium in the aluminum-scandium alloy prepared in example 2 is 99.98%, the deviation of the mass content of scandium is 0.37%, and the results of energy spectrum analysis refer to fig. 2 and table 2.
TABLE 2
Comparative example 1
Comparative example 1 is substantially the same as example 2 except that 3450g of metallic aluminum in comparative example 1 was added in its entirety in step (2), and steps (3) to (11) were omitted.
Experiments show that 3450g of metallic aluminum is doped into metallic scandium at one time, so that the composition segregation is very serious, the metal layering phenomenon is obvious, and good uniformity cannot be achieved even after repeated smelting.
Comparative example 2
Comparative example 2 is substantially the same as example 2 except that in comparative example 2 2750g of metallic aluminum was added in the entirety in step (4), and steps (5) to (11) were omitted.
Experiments show that 2750g of metal aluminum is doped into 30% of aluminum-scandium alloy in one step, so that the composition segregation is very serious, the metal layering phenomenon is obvious, and the good uniformity cannot be achieved even after repeated smelting.
Comparative example 3
Comparative example 3 is substantially the same as example 2 except that in comparative example 3 1750g of metallic aluminum was added in its entirety in step (7), and steps (8) to (11) were omitted.
Experiments show that 1750g of metal aluminum is completely heavy to 15% of aluminum-scandium alloy at one time, the composition segregation is very serious, the metal layering phenomenon is obvious, and good uniformity cannot be achieved even after repeated smelting.
The technical features of the embodiments described above may be arbitrarily combined, and for the sake of brevity, all possible combinations of the technical features in the embodiments described above are not described, but should be considered as being within the scope of the present specification as long as there is no contradiction between the combinations of the technical features.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.
Claims (8)
1. The preparation method of the aluminum-scandium alloy is characterized by comprising the following steps of:
in a protective gas atmosphere, melting metal scandium by adopting vacuum suspension melting, then preserving heat, adding metal aluminum for melting, preserving heat, and cooling to obtain an aluminum-scandium alloy;
the mass of the metallic aluminum is not more than 180% of the mass of the metallic scandium.
2. The method of producing an aluminum-scandium alloy according to claim 1, further comprising the steps of:
and repeatedly carrying out melting steps of melting the aluminum-scandium alloy by adopting vacuum suspension melting, then preserving heat, adding metal aluminum for melting, then preserving heat and cooling, wherein in the repeated melting process of the aluminum-scandium alloy, the mass of the metal aluminum added in each melting process does not exceed 180% of the mass of the metal scandium, and the aluminum-scandium alloy with the scandium mass content of more than 30% is obtained.
3. The method of producing an aluminum-scandium alloy according to claim 1, further comprising the steps of:
repeatedly carrying out melting steps of melting the aluminum-scandium alloy by adopting vacuum suspension melting, then preserving heat, adding metal aluminum for melting, then preserving heat and cooling, wherein in the repeated melting process of the aluminum-scandium alloy, the mass of the metal aluminum added in each melting process does not exceed 180% of the mass of the metal scandium, until the aluminum-scandium alloy with the scandium mass content of 30% is obtained;
and (2) repeatedly melting the aluminum-scandium alloy with the scandium mass content of 30% by adopting vacuum suspension melting, then preserving heat, adding metal aluminum for melting, then preserving heat and cooling, wherein in the repeated melting process of the aluminum-scandium alloy with the scandium mass content of 30%, the mass of the metal aluminum added in each melting process is not more than 150% of the mass of the metal scandium until the aluminum-scandium alloy with the scandium mass content of more than 15% and less than 30% is obtained.
4. The method of producing an aluminum-scandium alloy according to claim 1, further comprising the steps of:
repeatedly carrying out melting steps of melting the aluminum-scandium alloy by adopting vacuum suspension melting, then preserving heat, adding metal aluminum for melting, then preserving heat and cooling, wherein in the repeated melting process of the aluminum-scandium alloy, the mass of the metal aluminum added in each melting process does not exceed 180% of the mass of the metal scandium, until the aluminum-scandium alloy with the scandium mass content of 30% is obtained;
repeatedly melting the aluminum-scandium alloy with the scandium mass content of 30% by adopting vacuum suspension melting, then preserving heat, adding metal aluminum for melting, then preserving heat and cooling, wherein in the repeated melting process of the aluminum-scandium alloy with the scandium mass content of 30%, the mass of the metal aluminum added in each melting process does not exceed 150% of the mass of the metal scandium, until the aluminum-scandium alloy with the scandium mass content of 15% is obtained;
and repeatedly melting the aluminum-scandium alloy with the scandium mass content of 15% by adopting vacuum suspension melting, then preserving heat, adding metal aluminum for melting, then preserving heat and cooling, wherein in the repeated melting process of the aluminum-scandium alloy with the scandium mass content of 15%, the mass of the metal aluminum added in each melting process does not exceed 130% of the mass of the metal scandium, until the aluminum-scandium alloy with the scandium mass content of less than 15% is obtained.
5. The method of any one of claims 1 to 4, wherein the protective gas is argon, xenon or nitrogen.
6. The method for preparing the aluminum-scandium alloy according to any one of claims 1 to 4, wherein a coil current of the vacuum suspension smelting is 100 to 200A, and a power output is 45 to 110 KW.
7. The method for preparing the aluminum-scandium alloy according to any one of claims 1 to 4, wherein the time for heat preservation after the metal scandium is melted by vacuum suspension melting is 10 to 25 minutes.
8. The method for preparing the aluminum-scandium alloy according to any one of claims 1 to 4, wherein the time for holding the temperature after the metal aluminum is added and melted is 10 to 25 minutes.
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| CN113684456A (en) * | 2021-08-25 | 2021-11-23 | 湖南稀土金属材料研究院有限责任公司 | La-Ti alloy target and preparation method thereof |
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| CN107868888A (en) * | 2017-12-15 | 2018-04-03 | 广州宇智科技有限公司 | A kind of aluminium-scandium alloy with extremely excellent die casting performance |
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| CN107868888A (en) * | 2017-12-15 | 2018-04-03 | 广州宇智科技有限公司 | A kind of aluminium-scandium alloy with extremely excellent die casting performance |
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| CN111647858B (en) * | 2020-06-03 | 2022-09-06 | 先导薄膜材料（广东）有限公司 | Preparation method of aluminum-scandium alloy target material |
| CN113684456A (en) * | 2021-08-25 | 2021-11-23 | 湖南稀土金属材料研究院有限责任公司 | La-Ti alloy target and preparation method thereof |
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