CN104694975A - Electrolyte for preparing aluminum-scandium intermediate alloy - Google Patents

Electrolyte for preparing aluminum-scandium intermediate alloy Download PDF

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Publication number
CN104694975A
CN104694975A CN201510137947.1A CN201510137947A CN104694975A CN 104694975 A CN104694975 A CN 104694975A CN 201510137947 A CN201510137947 A CN 201510137947A CN 104694975 A CN104694975 A CN 104694975A
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alf
scandium
ionogen
master alloy
aluminium
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田忠良
赖延清
胡勋
张凯
杨树
李劼
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Central South University
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Central South University
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    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25C—PROCESSES FOR THE ELECTROLYTIC PRODUCTION, RECOVERY OR REFINING OF METALS; APPARATUS THEREFOR
    • C25C3/00—Electrolytic production, recovery or refining of metals by electrolysis of melts
    • C25C3/36—Alloys obtained by cathodic reduction of all their ions

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Abstract

The invention relates to an electrolyte for preparing an aluminum-scandium intermediate alloy. The electrolyte mainly comprises Na3AlF6, K3AlF6, Li3AlF6, AlF3, CaF2, MgF2, Al2O3 and a scandium compound. The scandium compound is one or more of Sc2O3, ScF3 and ScCl3. An electrolyte fused salt system serves as a basic electrolyte for preparing the aluminum-scandium intermediate alloy in an electrolysis mode, and the solubility of the scandium compound in the electrolyte can be maintained from 6.0 percent to 10.0 percent at the temperature of superheat degree of 5-20 DEG C. Compared with a traditional electrolyte for preparing the aluminum-scandium intermediate alloy, the solubility of the scandium compound for preparing the aluminum-scandium intermediate alloy is increased by 1.0-5.0 percent, the scandium content of the aluminum-scandium intermediate alloy prepared in the electrolysis mode is higher than 2 percent and is increased by 0.5-2.5 percent compared with traditional electrolysis, the requirement for preparing the aluminum-scandium intermediate alloy with the high scandium content of molten salt electrolysis can be met completely, and a foundation is laid for producing high-performance aluminum-scandium alloy on a large scale.

Description

A kind of ionogen preparing aluminium-bearing master alloy
Technical field
The invention discloses a kind of ionogen preparing aluminium-bearing master alloy, specifically relate to the ionogen that aluminium-bearing master alloy is prepared in a kind of fused salt electrolysis, belong to fused salt electrolysis technical field.
Background technology
Metal scandium is the alterant and the most effective recrystallize inhibitor of processing work in-process that aluminium alloy casting grain structure is the strongest.Mo-bearing granitoid is because significantly can improving the over-all properties (as higher intensity (>750MPa), higher toughness (modulus of elasticity can more than l00GPa), stronger corrosion resisting property etc.) of conventional aluminum alloy and being widely used in the fields such as aerospace industries, military industry, civilian industry.
Because the chemical property of metal scandium is active, and the fusing point of metal scandium and the aluminium difference greatly (fusing point of scandium: 1541 DEG C, the fusing point of aluminium: 660 DEG C), when producing Mo-bearing granitoid, scandium must add with the form of master alloy (as Al-Sc, Mg-Sc or Al-Mg-Sc etc.).Research shows, for the aluminium-bearing master alloy of scandium content about 2%, scandium is with Al wherein 3sc intermetallic compound exists, and its fusing point is about 800 DEG C, close to the fusing point of metallic aluminium, is convenient to the production of aluminum scandium alloy.Therefore, the aluminium-bearing master alloy containing scandium amount 2% becomes the key raw material producing Mo-bearing granitoid.
With compared with the method for mixing, metallothermics, fused salt electrolysis process is prepared aluminium-bearing master alloy and is had that production cost is low, product uniform ingredients and easily control, easily realize the advantages such as continuous large-scale production and enjoy the concern of domestic and international investigators.From fused salt electrolysis plastome, research work concentrates on muriate and fluorochemical two class.When taking molten chloride as ionogen, electrolysis raw material adopts metal chloride, due to the utilization ways not good to the chlorine produced, easily causes severe contamination to environment, and raw material ScCl 3preparation flow is long, and equipment is complicated, and production cost is high.
And when taking fluorochemical as ionogen, following a few class can be divided into again: (1) Sc 2o 3-ScF 3-nNaFAlF 3system; (2) Sc 2o 3-ScF 3-LiF system; (3) Sc 2o 3-ScF 3-NaF system; (4) KF-AlF 3-Sc 2o 3system.Wherein, when adopting first three to plant electrolyte system, due to low (as Sc containing scandium raw material solubleness in the melt 2o 3at nNaFAlF 3-ScF 3solubleness in molten salt system is generally lower than 5%), institute's scandium content in product aluminium-bearing master alloy that obtains is low and can not meet the demands; And the specific conductivity of the 4th kind of potassium cryolite melt is low.Therefore, developing a kind of Novel electrolytic plastome to having high-solvency containing scadium compound, is the key that high scandium content aluminium-bearing master alloy is produced in fused salt electrolysis.
Summary of the invention
The object of the invention is the deficiency that exists for prior art and a kind of reasonable mixture ratio of components is provided, improves containing the ionogen preparing aluminium-bearing master alloy of scadium compound solubleness.Adopt ionogen of the present invention, when fused salt electrolysis process prepares aluminium-bearing master alloy, aluminium-bearing master alloy the product being not less than 2% containing scandium amount can be obtained, meet the requirement that the aluminium-bearing master alloy of high scandium content is prepared in fused salt electrolysis, for scale operation high-performance aluminum scandium alloy lays the foundation.
A kind of ionogen preparing aluminium-bearing master alloy of the present invention, comprises following component and forms by mass percentage:
Na 3AlF 6，10％-50％；
K 3AlF 6，10％-40％；
Li 3AlF 6，0.5％-10％；
AlF 3，10％-30％；
CaF 2，0.5％-5％；
MgF 2，0.5％-5％；
Al 2O 3，0.5％-5％；
Containing scadium compound, 0.5%-10%, each constituent mass percent and be 100%.
A kind of ionogen preparing aluminium-bearing master alloy of the present invention, comprises following component and forms by mass percentage:
Na 3AlF 6，15％-50％；
K 3AlF 6，15％-35％；
Li 3AlF 6，2％-9％；
AlF 3，10％-25％；
CaF 2，1％-5％；
MgF 2，1％-5％；
Al 2O 3，0.5％-4％；
Containing scadium compound, 2%-10%, each constituent mass percent and be 100%.
A kind of ionogen preparing aluminium-bearing master alloy of the present invention, comprises following component and forms by mass percentage:
Na 3AlF 6，20％-50％；
K 3AlF 6，20％-32％；
Li 3AlF 6，3％-9％；
AlF 3，10％-23％；
CaF 2，1.5％-4.5％；
MgF 2，1.5％-4.5％；
Al 2O 3，0.8％-3％；
Containing scadium compound, 4%-10%, each constituent mass percent and be 100%.
A kind of ionogen preparing aluminium-bearing master alloy of the present invention, comprises following component and forms by mass percentage:
Na 3AlF 6，25％-45％；
K 3AlF 6，22％-30％；
Li 3AlF 6，4％-8％；
AlF 3，10％-21％；
CaF 2，2％-4％；
MgF 2，2％-4％；
Al 2O 3，0.9％-1.5％；
Containing scadium compound, 6%-10%, each constituent mass percent and be 100%.
A kind of ionogen preparing aluminium-bearing master alloy of the present invention, the described scadium compound that contains is selected from Sc 2o 3, ScF 3, ScCl 3in one or more.
A kind of ionogen preparing aluminium-bearing master alloy of the present invention, each constituent mass percentage composition is: Na 3alF 638%, K 3alF 624%, Li 3alF 67%, AlF 319%, CaF 23%, MgF 23%, Al 2o 31%, Sc 2o 35%, when melt temperature is 880 DEG C, Sc 2o 3solubleness in this ionogen reaches 8.76%.
A kind of ionogen preparing aluminium-bearing master alloy of the present invention, each constituent mass percentage composition is: Na 3alF 637%, K 3alF 627%, Li 3alF 66%, AlF 318%, CaF 24%, MgF 22%, Al 2o 32%, ScF 34%, when melt temperature is 905 DEG C, ScF 3solubleness in this ionogen reaches 7.48%.
A kind of ionogen preparing aluminium-bearing master alloy of the present invention, each constituent mass percentage composition is: Na 3alF 646%, K 3alF 625.5%, Li 3alF 64%, AlF 311%, CaF 22%, MgF 24%, Al 2o 31.5%, ScCl 36%, when melt temperature is 940 DEG C, ScCl 3solubleness in this ionogen reaches 9.87%.
A kind of ionogen preparing aluminium-bearing master alloy of the present invention, each constituent mass percentage composition is: Na 3alF 637%, K 3alF 623%, Li 3alF 67%, AlF 318%, CaF 23%, MgF 23%, Al 2o 31%, Sc 2o 35%, ScF 33%, when melt temperature is 875 DEG C, Sc 2o 3, ScF 3solubleness in this ionogen reaches 5.73%, 3.34% respectively.
A kind of ionogen preparing aluminium-bearing master alloy of the present invention, each constituent mass percentage composition is: Na 3alF 636%, K 3alF 624%, Li 3alF 68%, AlF 319%, CaF 22%, MgF 22%, Al 2o 32%, Sc 2o 33%, ScF 32%, ScCl 32%, when melt temperature is 886 DEG C, Sc 2o 3, ScF 3, ScCl 3solubleness in this ionogen reaches 3.36%, 3.14%, 3.47% respectively.
The present invention is owing to adopting said components proportioning, K 3alF 6effectively can improve the solubleness containing scadium compound; Li 3alF 6can electrolytic conductivity be improved, reduce K 3alF 6on the impact that electrolyte conductivity reduces; CaF 2and MgF 2electrolytical interfacial property etc. can be improved.Thus while improving containing scadium compound in the electrolyte solubleness, do not affect the change of other physicochemical property of melt.
The ionogen preparing aluminium-bearing master alloy of the present invention's design, under the electrolysis temperature of superheating temperature 5 DEG C-20 DEG C, can keep containing the solubleness of scadium compound in this ionogen is 6.0%-10.0%.Compared with the ionogen preparing aluminium-bearing master alloy with traditional electrolyte, containing scadium compound, in the present invention, the solubleness prepared in the ionogen of aluminium-bearing master alloy improves 1.0%-5.0%, and in the aluminium-bearing master alloy of electrolytic preparation, scandium content improves 0.5%-2.5%.
The present invention compared with prior art, has following beneficial effect:
1. a kind of electrolyte system preparing aluminium-bearing master alloy provided by the invention, compared with traditional electrolyte matter, increases containing the solubleness of scadium compound in this system.Such as, Na is worked as 3alF 6, K 3alF 6, Li 3alF 6, AlF 3, CaF 2, MgF 2, Al 2o 3mass percent is in the electrolyte 40:25:8:20:3:3:1, when melt temperature is 870 DEG C, and Sc 2o 3solubleness in this ionogen improves about 3.57%, ScF 3solubleness in this ionogen improves about 2.67%, ScCl 3solubleness in this ionogen improves about 4.54%, reaches 8.61%, 7.36% and 9.33% respectively.
2. a kind of electrolyte system preparing aluminium-bearing master alloy provided by the invention, compared with traditional electrolyte matter, adopts the scandium content in the aluminium-bearing master alloy of this system Electrowinning to improve.Such as, at electrolysis temperature 950 DEG C and cathode current density 1.5A/cm 2under condition, as Sc in ionogen 2o 3concentration be 6%, Al 2o 3concentration when being 2%, in the aluminium-bearing master alloy of Electrowinning, scandium content reaches 3.04%, compared with traditional electrolyte matter, improves about 1.54%.
In sum, instant component reasonable ratio, can effectively to improve containing scadium compound solubleness, adopt ionogen of the present invention, when fused salt electrolysis process prepares aluminium-bearing master alloy, aluminium-bearing master alloy the product being not less than 2% containing scandium amount can be obtained, under electrolyte body of the present invention ties up to the temperature of superheating temperature 5 DEG C-20 DEG C, can keep containing the solubleness of scadium compound in this ionogen is 6.0%-10.0%.Compared with the ionogen preparing aluminium-bearing master alloy with traditional electrolyte, the solubleness prepared in aluminium-bearing master alloy ionogen in the present invention containing scadium compound improves 1.0%-5.0%, scandium content in the aluminium-bearing master alloy of electrolytic preparation improves 0.5%-2.5%, meet the requirement that the aluminium-bearing master alloy of high scandium content is prepared in fused salt electrolysis, for scale operation high-performance aluminum scandium alloy lays the foundation.
Embodiment
Below in conjunction with embodiment, the present invention is described in further detail, but is not restricted to the protection domain of invention.
In the embodiment of the present invention, the mode adopting isothermal supersaturation method to combine with x-ray fluorescence spectrometry instrument obtains containing scadium compound solubleness in the melt; After adopting Inductively Coupled Plasma Atomic Emission Spectrometry instrument (ICP-AES) to analyze electrolysis obtain scandium content in aluminium-bearing master alloy.
Embodiment 1
The ionogen compositing formula preparing aluminium-bearing master alloy is: Na 3alF 6, 38%; K 3alF 6, 32%; Li 3alF 6, 8%; AlF 3, 12%; CaF 2, 3%; MgF 2, 3%; Al 2o 3, 1%; Sc 2o 3, 3%.At 929 DEG C of temperature, Sc 2o 3solubleness in this ionogen reaches 8.85%, at cathode current density 1.5A/cm 2under condition Electrowinning aluminium-bearing master alloy in scandium content be 2.03%.
Embodiment 2
The ionogen compositing formula preparing aluminium-bearing master alloy is: Na 3alF 6, 41%; K 3alF 6, 24%; Li 3alF 6, 5%; AlF 3, 18%; CaF 2, 4%; MgF 2, 2%; Al 2o 3, 2%; ScF 3, 4%.At 926 DEG C of temperature, ScF 3solubleness in this ionogen reaches 7.96%, at cathode current density 1.5A/cm 2under condition Electrowinning aluminium-bearing master alloy in scandium content be 2.21%.
Embodiment 3
The ionogen compositing formula preparing aluminium-bearing master alloy is: Na 3alF 6, 28%; K 3alF 6, 26%; Li 3alF 6, 9%; AlF 3, 22%; CaF 2, 2%; MgF 2, 4%; Al 2o 3, 3%; ScCl 3, 6%.At 870 DEG C of temperature, ScCl 3solubleness in this ionogen reaches 9.63%, at cathode current density 1.5A/cm 2under condition Electrowinning aluminium-bearing master alloy in scandium content be 2.57%.
Embodiment 4
The ionogen compositing formula preparing aluminium-bearing master alloy is: Na 3alF 6, 39%; K 3alF 6, 25.5%; Li 3alF 6, 6%; AlF 3, 18%; CaF 2, 1%; MgF 2, 1%; Al 2o 3, 1.5%; Sc 2o 3, 5%; ScF 3, 3%.At 920 DEG C of temperature, Sc 2o 3and ScF 3solubleness sum in this ionogen reaches 8.47%, at cathode current density 1.5A/cm 2under condition Electrowinning aluminium-bearing master alloy in scandium content be 3.25%.
Embodiment 5
The ionogen compositing formula preparing aluminium-bearing master alloy is: Na 3alF 6, 41%; K 3alF 6, 23%; Li 3alF 6, 3%; AlF 3, 18%; CaF 2, 2%; MgF 2, 2%; Al 2o 3, 2%; Sc 2o 3, 3%; ScF 3, 2.5%, ScCl 3, 3.5%.At 916 DEG C of temperature, Sc 2o 3, ScF 3and ScCl 3solubleness sum in this ionogen reaches 9.48%, at cathode current density 1.5A/cm 2under condition Electrowinning aluminium-bearing master alloy in scandium content be 2.17%.
Embodiment 6
The ionogen compositing formula preparing aluminium-bearing master alloy is: Na 3alF 6, 38%; K 3alF 6, 24%; Li 3alF 6, 7%; AlF 3, 19%; CaF 2, 3%; MgF 2, 3%; Al 2o 3, 1%; Sc 2o 3, 5%; At 880 DEG C of temperature, Sc 2o 3solubleness in this ionogen reaches 8.76%, at cathode current density 1.5A/cm 2under condition Electrowinning aluminium-bearing master alloy in scandium content 2.32%.
Embodiment 7
The ionogen compositing formula preparing aluminium-bearing master alloy is: Na 3alF 6, 37%; K 3alF 6, 27%; Li 3alF 6, 6%; AlF 3, 18%; CaF 2, 4%; MgF 2, 2%; Al 2o 3, 2%; ScF 3, 4%; At 905 DEG C of temperature, ScF 3solubleness in this ionogen reaches 7.48%, at cathode current density 1.5A/cm 2under condition Electrowinning aluminium-bearing master alloy in scandium content 2.18%.
Embodiment 8
The ionogen compositing formula preparing aluminium-bearing master alloy is: Na 3alF 6, 46%; K 3alF 6, 25.5%; Li 3alF 6, 4%; AlF 3, 11%; CaF 2, 2%; MgF 2, 4%; Al 2o 3, 1.5%; ScCl 3, 6%; At 940 DEG C of temperature, ScCl 3solubleness in this ionogen reaches 9.87%; At cathode current density 1.5A/cm 2under condition Electrowinning aluminium-bearing master alloy in scandium content 2.25%.
Embodiment 9
The ionogen compositing formula preparing aluminium-bearing master alloy is: Na 3alF 6, 37%; K 3alF 6, 23%; Li 3alF 6, 7%; AlF 3, 18%; CaF 2, 3%; MgF 2, 3%; Al 2o 3, 1%; Sc 2o 3, 5%; ScF 3, 3%; At 875 DEG C of temperature, Sc 2o 3, ScF 3solubleness in this ionogen reaches 5.73%, 3.34% respectively; At cathode current density 1.5A/cm 2under condition Electrowinning aluminium-bearing master alloy in scandium content 3.15%.
Embodiment 10
The ionogen compositing formula preparing aluminium-bearing master alloy is: Na 3alF 6, 36%; K 3alF 6, 24%; Li 3alF 6, 8%; AlF 3, 19%; CaF 2, 2%; MgF 2, 2%; Al 2o 3, 2%; Sc 2o 3, 3%; ScF 3, 2%; ScCl 3, 2%; At 886 DEG C of temperature, Sc 2o 3, ScF 3, ScCl 3solubleness in this ionogen reaches 3.36%, 3.14%, 3.47% respectively; At cathode current density 1.5A/cm 2under condition Electrowinning aluminium-bearing master alloy in scandium content 3.68%.
Data from above embodiment obtains: adopt ionogen of the present invention, when fused salt electrolysis process prepares aluminium-bearing master alloy, scandium amount is contained all higher than 2% in the aluminium-bearing master alloy product obtained, meet the requirement that the aluminium-bearing master alloy of high scandium content is prepared in fused salt electrolysis, for scale operation high-performance aluminum scandium alloy lays the foundation.

Claims (10)

1. prepare an ionogen for aluminium-bearing master alloy, comprise following component and form by mass percentage:
Na 3AlF 6，10％-50％；
K 3AlF 6，10％-40％；
Li 3AlF 6，0.5％-10％；
AlF 3，10％-30％；
CaF 2，0.5％-5％；
MgF 2，0.5％-5％；
Al 2O 3，0.5％-5％；
Containing scadium compound, 0.5%-10%, each constituent mass percent and be 100%.
2. a kind of ionogen preparing aluminium-bearing master alloy according to claim 1, comprises following component and forms by mass percentage:
Na 3AlF 6，15％-50％；
K 3AlF 6，15％-35％；
Li 3AlF 6，2％-9％；
AlF 3，10％-25％；
CaF 2，1％-5％；
MgF 2，1％-5％；
Al 2O 3，0.5％-4％；
Containing scadium compound, 2%-10%, each constituent mass percent and be 100%.
3. a kind of ionogen preparing aluminium-bearing master alloy according to claim 1, comprises following component and forms by mass percentage:
Na 3AlF 6，20％-50％；
K 3AlF 6，20％-32％；
Li 3AlF 6，3％-9％；
AlF 3，10％-23％；
CaF 2，1.5％-4.5％；
MgF 2，1.5％-4.5％；
Al 2O 3，0.8％-3％；
Containing scadium compound, 4%-10%, each constituent mass percent and be 100%.
4. a kind of ionogen preparing aluminium-bearing master alloy according to claim 1, comprises following component and forms by mass percentage:
Na 3AlF 6，25％-45％；
K 3AlF 6，22％-30％；
Li 3AlF 6，4％-8％；
AlF 3，10％-21％；
CaF 2，2％-4％；
MgF 2，2％-4％；
Al 2O 3，0.9％-1.5％；
Containing scadium compound, 6%-10%, each constituent mass percent and be 100%.
5. a kind of ionogen preparing aluminium-bearing master alloy according to claim 1-4 any one, is characterized in that, the described scadium compound that contains is selected from Sc 2o 3, ScF 3, ScCl 3in one or more.
6. a kind of ionogen preparing aluminium-bearing master alloy according to claim 5, each constituent mass percentage composition is: Na 3alF 638%, K 3alF 624%, Li 3alF 67%, AlF 319%, CaF 23%, MgF 23%, Al 2o 31%, Sc 2o 35%.
7. a kind of ionogen preparing aluminium-bearing master alloy according to claim 5, each constituent mass percentage composition is: Na 3alF 637%, K 3alF 627%, Li 3alF 66%, AlF 318%, CaF 24%, MgF 22%, Al 2o 32%, ScF 34%.
8. a kind of ionogen preparing aluminium-bearing master alloy according to claim 5, each constituent mass percentage composition is: Na 3alF 646%, K 3alF 625.5%, Li 3alF 64%, AlF 311%, CaF 22%, MgF 24%, Al 2o 31.5%, ScCl 36%.
9. a kind of ionogen preparing aluminium-bearing master alloy according to claim 5, each constituent mass percentage composition is: Na 3alF 637%, K 3alF 623%, Li 3alF 67%, AlF 318%, CaF 23%, MgF 23%, Al 2o 31%, Sc 2o 35%, ScF 33%.
10. a kind of ionogen preparing aluminium-bearing master alloy according to claim 5, each constituent mass percentage composition is: Na 3alF 636%, K 3alF 624%, Li 3alF 68%, AlF 319%, CaF 22%, MgF 22%, Al 2o 32%, Sc 2o 33%, ScF 32%, ScCl 32%.
CN201510137947.1A 2015-03-26 2015-03-26 Electrolyte for preparing aluminum-scandium intermediate alloy Pending CN104694975A (en)

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WO2019083471A3 (en) * 2017-03-21 2019-06-06 Minertek Mineral Teknolojileri Madencilik Sanayi Ve Ticaret Anonim Sirketi A production method for scandium metal or al-sc alloys using electrolysis method from scandium salt mixtures prepared by adding of cacl2 and/or mgcl2 compounds to scf3 compound obtained from scandium compound in the form of (nh4)2nascf6
CN112534074A (en) * 2018-03-15 2021-03-19 Fea材料有限责任公司 Method for producing aluminum-scandium alloy
JP2021515851A (en) * 2018-03-15 2021-06-24 インフィニアム インコーポレイテッド Manufacturing method of aluminum-scandium alloy
JP7361058B2 (en) 2018-03-15 2023-10-13 エフイーエー マテリアルズ エルエルシー Method for producing aluminum-scandium alloy

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Application publication date: 20150610