CN108018438A - A kind of method that aluminothermic reduction prepares scandium bearing master alloy in elpasolite fused salt - Google Patents
A kind of method that aluminothermic reduction prepares scandium bearing master alloy in elpasolite fused salt Download PDFInfo
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- CN108018438A CN108018438A CN201711310655.9A CN201711310655A CN108018438A CN 108018438 A CN108018438 A CN 108018438A CN 201711310655 A CN201711310655 A CN 201711310655A CN 108018438 A CN108018438 A CN 108018438A
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- C22C1/00—Making non-ferrous alloys
- C22C1/12—Making non-ferrous alloys by processing in a semi-solid state, e.g. holding the alloy in the solid-liquid phase
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C1/00—Making non-ferrous alloys
- C22C1/02—Making non-ferrous alloys by melting
- C22C1/026—Alloys based on aluminium
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Abstract
A kind of method that aluminothermic reduction prepares scandium bearing master alloy in elpasolite fused salt, belongs to field of material technology, carries out according to the following steps：(1) anhydrous K F and anhydrous AlF3 is mixed；(2) Sc2O3 is added to be uniformly mixed；(3) salt-mixture is warming up to 720 ~ 1020 DEG C, keeps the temperature 30 ~ 60min；(4) reducing agent metallic aluminium is added, is heat-treated at 720 ~ 1020 DEG C, alloy component and electrolyte portion is isolated, scandium bearing master alloy is formed after alloy component condensation.Electrolyte system KFAlF3 solubility of the present invention is high；Sc contents reach national standard in the AlSc intermediate alloys of preparation；Using cheap scandium oxide as raw material, technique is simple, shortens scandium bearing master alloy preparation flow, reduces production cost.
Description
Technical field
The invention belongs to field of material technology, in more particularly to a kind of elpasolite fused salt aluminothermic reduction prepare among aluminium scandium
The method of alloy.
Background technology
Sc is the most effective alloy element found so far, and the addition of minor Sc can significantly improve alloy
Mechanical property, high-temperature behavior, corrosion resistance, welding performance and the anti-neutron irradiation damage performance of enhancing.In space flight and aviation, core
Reactor and communications and transportation etc. have wide application prospect.Since the fusing point of metal scandium is up to 1541 DEG C, chemical property
Vivaciously, when preparing aluminium-scandium alloy, scandium must be added in the form of intermediate alloy, thus Al-Sc intermediate alloys become prepare aluminium scandium
The key raw material of alloy.
At present, the preparation method of domestic and international Al-Sc intermediate alloys has to the method for mixing, fused salt electrolysis process and thermal reduction.
It is that metallic aluminium and the direct fusion of scandium are prepared into scandium bearing master alloy at high temperature to the method for mixing；In Al-Sc intermediate alloys
In preparation process, aluminium and scandium melt at high temperature, and uniform aluminium-scandium alloy is formed by being sufficiently stirred, after keeping the temperature enough time,
It is molded into the swage or copper mold of preheating；When producing Al-Sc intermediate alloys using this method, due to the fusing point of aluminium and scandium difference compared with
Greatly, aluminium and scandium are not easy uniformly to mix, and are segregated in the alloy of formation serious；In addition, prepare Al-Sc intermediate alloys using to mixing method
When, it is necessary to using simple metal scandium as raw material, the scaling loss of scandium is larger in preparation process, and the cost of alloy of preparation is higher.
Fused salt electrolysis process is usually using Sc2O3 as raw material, and the difference formed by electrolyte is roughly divided into three classes, and one kind is to contain
ScCl3 or ScF3 or ScCl3-ScF3 electrolyte systems, the solubility of Sc2O3 in the electrolyte is higher, using this electrolyte
When system is electrolysed, it can be electrolysed to obtain the Al-Sc intermediate alloys that Sc contents are 2 ~ 6%, but the preparation process of ScCl3 and ScF3 is all
Using Sc2O3 as raw material, increase production cost, in addition the hygroscopic deliquescence of ScCl3, the preparation and preservation of anhydrous ScCl3, which exist, to be stranded
Difficulty, is unsuitable for production application；Second class is nNaF-AlF3 electrolyte systems, and Sc2O3 is in nNaF-AlF3 electrolyte systems
Solubility is relatively low, further, since the deposition potential of Al3+ is than Sc3+ just, the Al3+ preferential discharges in electrolytic process in fused salt, are adopted
1% is respectively less than with the Al-Sc intermediate alloys amount containing Sc prepared in the electrolyte system, it is impossible to reaches the Al-Sc required in national standard
The requirement of intermediate alloy amount containing Sc 2%；Three classes are KF-AlF3 electrolyte systems, in the molten salt system, using the side of electrolysis
Method can not obtain the scandium bearing master alloy that amount containing Sc is 2%, being capable of electrolytic preparation after adding NaF in the electrolyte system
Obtain the scandium bearing master alloy that amount containing Sc is 1 ~ 5%.
Thermal reduction can be divided into vacuum-thermal method and antivacuum thermal reduction according to the difference of experiment condition;Vacuum Heat
For reduction method using ScF3 as raw material, experiment needs extra vacuum equipment, and experimentation is complex；Rather than vacuum-thermal method with
Al powder and Sc2O3 powder are raw material, and direct thermal reduction after mixing prepares scandium bearing master alloy, in the alloy prepared using method
Sc contents are less than 1%, contain reaction product Al2O3 and other impurities in alloy in addition.
The content of the invention
Aluminium-scandium alloy technology above shortcomings are prepared for various, the present invention provides aluminium in a kind of elpasolite fused salt
The method that thermal reduction prepares scandium bearing master alloy, using Sc2O3 cheap and easy to get as raw material, using elpasolite as fused salt, work
Skill flow is simple, and less pollution, cost is relatively low, is adapted to large-scale industrial production.
The method of the present invention carries out in accordance with the following steps：
1st, anhydrous K F and anhydrous AlF3 are mixed and made into fused salt, the molar ratio of wherein KF and AlF3 are 1.5 ~ 3.0；
2nd, Sc2O3 is added in fused salt and be uniformly mixed, salt-mixture is made, the addition of Sc2O3 is the 3 of KF and AlF3 gross masses
~ 9%；
3rd, salt-mixture is warming up to 720 ~ 1020 DEG C, 30 ~ 60min of insulation is completely melt material, forms melting mixing salt；
4th, reducing agent metallic aluminium is added into melting mixing salt, is heat-treated at 720 ~ 1020 DEG C, the recovery time is 0.5 ~ 3h,
Alloy component and electrolyte portion are isolated after reduction, scandium bearing master alloy is formed after alloy component condensation.
In above-mentioned step 3, salt-mixture heating is located in corundum crucible and is heated up.
In above-mentioned step 4, the dosage of reducing agent metallic aluminium is by the molar ratio of metallic aluminium and Sc2O3（16~40）:1.
The mass percent of scandium is 2 ~ 3% in above-mentioned scandium bearing master alloy.
The component of above-mentioned electrolyte portion includes KF, AlF3, the Al2O3 and unreacted Sc2O3 of reaction generation.
The reaction equation of above-mentioned reduction reaction institute foundation is：
8Al+Sc2O3=2Al3Sc+Al2O3；
In the above method, the dosage of reducing agent metallic aluminium is 2 ~ 5 times of theoretical amount.
Compared with prior art, present invention has the advantages that：
1st, Sc2O3 in electrolyte system KF-AlF3 solubility of the present invention compared with conventional aluminum electrolyte system NaF-AlF3
Larger raising, at 800 DEG C, solubility of the Sc2O3 in KF-AlF3 systems is up to 9.74%；
2nd, in the electrolyte system, Sc contents reach 2 ~ 3%, Neng Gouman in the Al-Sc intermediate alloys prepared using thermal reduction
Requirement in sufficient national standard in Al-Sc intermediate alloys to Sc contents；
3rd, for the present invention using cheap scandium oxide as raw material, technique is simple, shortens scandium bearing master alloy preparation flow, reduces life
Produce cost.
Brief description of the drawings
Fig. 1 is the method flow diagram signal that aluminothermic reduction prepares scandium bearing master alloy in a kind of elpasolite fused salt of the present invention
Figure.
Embodiment
The Sc2O3 purity selected in present example>99.999%.
The purity for the reducing agent metallic aluminium selected in present example is>99%.
KF and AlF3 in present example are analytical reagents purchased in market.
After intermediate alloy is made in the method for the present invention, using the method remelting of vacuum melting, water-cooled casting is waited until in aluminium scandium
Between alloy pig, drill through alloy sample, obtain alloy bits, using the content of aes determination wherein scandium element, scanning
Electron microscope shows that scandium Elemental redistribution is uniform in alloy.
Step 3 and 4 is to carry out under an argon atmosphere in the method for the present invention.
Embodiment 1
Anhydrous K F and anhydrous AlF3 are mixed and made into fused salt, the molar ratio of wherein KF and AlF3 are 1.5；
Sc2O3 is added in fused salt and is uniformly mixed, salt-mixture is made, the addition of Sc2O3 is the 3% of KF and AlF3 gross masses；
Salt-mixture is placed in corundum crucible and is warming up to 720 DEG C, insulation 60min is completely melt material, forms melting mixing
Salt；
Reducing agent metallic aluminium is added into melting mixing salt, dosage is 40 by the molar ratio of metallic aluminium and Sc2O3:1, Ran Hou
720 DEG C are heat-treated, and recovery time 3h isolates alloy component and electrolyte portion after reduction, alloy component is cold
Scandium bearing master alloy is formed after solidifying；The mass percent of scandium is 2.1% in scandium bearing master alloy；The component of electrolyte portion includes
KF, AlF3, the AlO3 and unreacted Sc2O3 of reaction generation.
Embodiment 2
With embodiment 1, difference is method：
（1）The molar ratio of KF and AlF3 is 1.8；
（2）The addition of Sc2O3 is the 9% of KF and AlF3 gross masses；
（3）Salt-mixture is warming up to 1020 DEG C, keeps the temperature 30min；
（4）It is 35 that metallic aluminium dosage, which is added, by the molar ratio of metallic aluminium and Sc2O3:1, heat-treated at 1020 DEG C, during reduction
Between be 0.5h；The mass percent of scandium is 2.33% in scandium bearing master alloy.
Embodiment 3
With embodiment 1, difference is method：
（1）The molar ratio of KF and AlF3 is 2.0；
（2）The addition of Sc2O3 is the 4% of KF and AlF3 gross masses；
（3）Salt-mixture is warming up to 800 DEG C, keeps the temperature 50min；
（4）It is 30 that metallic aluminium dosage, which is added, by the molar ratio of metallic aluminium and Sc2O3:1, heat-treated at 800 DEG C, the recovery time
For 2.5h；The mass percent of scandium is 2.47% in scandium bearing master alloy.
Embodiment 4
With embodiment 1, difference is method：
（1）The molar ratio of KF and AlF3 is 2.5；
（2）The addition of Sc2O3 is the 8% of KF and AlF3 gross masses；
（3）Salt-mixture is warming up to 980 DEG C, keeps the temperature 35min；
（4）It is 25 that metallic aluminium dosage, which is added, by the molar ratio of metallic aluminium and Sc2O3:1, heat-treated at 980 DEG C, the recovery time
For 1h；The mass percent of scandium is 2.67% in scandium bearing master alloy.
Embodiment 5
With embodiment 1, difference is method：
（1）The molar ratio of KF and AlF3 is 2.8；
（2）The addition of Sc2O3 is the 5% of KF and AlF3 gross masses；
（3）Salt-mixture is warming up to 900 DEG C, keeps the temperature 40min；
（4）It is 20 that metallic aluminium dosage, which is added, by the molar ratio of metallic aluminium and Sc2O3:1, heat-treated at 900 DEG C, the recovery time
For 1.5h；The mass percent of scandium is 2.82% in scandium bearing master alloy.
Embodiment 6
With embodiment 1, difference is method：
（1）The molar ratio of KF and AlF3 is 3.0；
（2）The addition of Sc2O3 is the 6% of KF and AlF3 gross masses；
（3）Salt-mixture is warming up to 950 DEG C, keeps the temperature 45min；
（4）It is 16 that metallic aluminium dosage, which is added, by the molar ratio of metallic aluminium and Sc2O3:1, heat-treated at 950 DEG C, the recovery time
For 1.5h；The mass percent of scandium is 3% in scandium bearing master alloy.
Claims (5)
1. a kind of method that aluminothermic reduction prepares scandium bearing master alloy in elpasolite fused salt, it is characterised in that according to the following steps
Carry out：
（1）Anhydrous K F and anhydrous AlF3 are mixed and made into fused salt, the molar ratio of wherein KF and AlF3 are 1.5 ~ 3.0；
（2）Sc2O3 is added in fused salt and is uniformly mixed, salt-mixture is made, the addition of Sc2O3 is KF and AlF3 gross masses
3~ 9%；
（3）Salt-mixture is warming up to 720 ~ 1020 DEG C, 30 ~ 60min of insulation is completely melt material, forms melting mixing salt；
（4）Reducing agent metallic aluminium is added into melting mixing salt, is heat-treated at 720 ~ 1020 DEG C, the recovery time for 0.5 ~
3h, isolates alloy component and electrolyte portion, scandium bearing master alloy is formed after alloy component condensation after reduction.
2. the method that aluminothermic reduction prepares scandium bearing master alloy in a kind of elpasolite fused salt according to claim 1, its
It is characterized in that step（3）In, salt-mixture heating is located in corundum crucible and is heated up.
3. the method that aluminothermic reduction prepares scandium bearing master alloy in a kind of elpasolite fused salt according to claim 1, its
It is characterized in that step（4）In, the dosage of reducing agent metallic aluminium is by the molar ratio of metallic aluminium and Sc2O3（16~40）:1.
4. the method that aluminothermic reduction prepares scandium bearing master alloy in a kind of elpasolite fused salt according to claim 1, its
The mass percent of scandium is 2 ~ 3% in scandium bearing master alloy described in being characterized in that.
5. the method that aluminothermic reduction prepares scandium bearing master alloy in a kind of elpasolite fused salt according to claim 1, its
Being characterized in that the component of the electrolyte portion includes KF, AlF3, the Al2O3 and unreacted Sc2O3 of reaction generation.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112746191A (en) * | 2020-12-30 | 2021-05-04 | 贵州华科铝材料工程技术研究有限公司 | Preparation method of mixed Sc-Zr aluminum alloy |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106381408A (en) * | 2016-09-26 | 2017-02-08 | 东北大学 | Method for preparing aluminum-scandium intermediate alloy by thermally reducing aluminum in elpasolite fused salt |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106381408A (en) * | 2016-09-26 | 2017-02-08 | 东北大学 | Method for preparing aluminum-scandium intermediate alloy by thermally reducing aluminum in elpasolite fused salt |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112746191A (en) * | 2020-12-30 | 2021-05-04 | 贵州华科铝材料工程技术研究有限公司 | Preparation method of mixed Sc-Zr aluminum alloy |
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