CN108913924B - Method for preparing aluminum-scandium intermediate alloy by using low-grade scandium oxide - Google Patents
Method for preparing aluminum-scandium intermediate alloy by using low-grade scandium oxide Download PDFInfo
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Abstract
The invention relates to a method for preparing an aluminum-scandium intermediate alloy by using low-grade scandium oxide. Firstly, scandium oxide, aluminum ingot and solvent are mixed according to the mass ratio of (2-4): (20-35): (0.01-0.1), then, placing scandium oxide and a solvent into a ball mill for ball milling and uniform mixing, then, taking out a mixed material, placing the mixed material into a non-vacuum medium-frequency induction furnace, inserting an aluminum ingot into the mixed material of scandium oxide and the solvent for thermite reduction reaction, scattering a slag-removing agent for slag removal, vertically casting a molten material after the thermite reduction reaction, rapidly cooling to obtain an aluminum-scandium intermediate alloy ingot, and finally, carrying out surface treatment and detection packaging to obtain the aluminum-scandium intermediate alloy. The solvent disclosed by the invention can reduce the purity requirement of scandium oxide from 99.9% to 60-95%, and can obviously reduce the unit cost of the raw material scandium oxide, so that the price of the product aluminum-scandium intermediate alloy is reduced, the final preparation of low-price aluminum-scandium alloy is facilitated, and the application of the aluminum-scandium alloy in the fields of automobiles, railways and aerospace crafts is promoted.
Description
Technical Field
The invention belongs to the technical field of metal alloy preparation, and particularly relates to a method for preparing an aluminum-scandium intermediate alloy by using low-grade scandium oxide.
Background
The aluminum-scandium alloy has special excellent performance in aluminum alloy and is applied to aerospace industry as a structural material. The application of aluminum-scandium alloys has been previously greatly limited due to the high cost of raw materials. In recent years, with the development of scandium smelting technology, the cost of scandium raw materials is greatly reduced, and the development of the technology for preparing aluminum-scandium alloy is gradually mature, so that the processing and preparation cost of the aluminum-scandium alloy is gradually reduced. The research has been conducted by domestic research institutes, and if the cost of the aluminum-scandium alloy reaches 400 yuan/Kg, the aluminum-scandium alloy can be possibly applied to structural components of automobiles. The fields of urban subways, high-speed rails, hypersonic airplanes, unmanned planes and the like are huge potential markets in future.
The most classical production method of aluminum-scandium alloys is a metal-pairing method, i.e. the prepared pure metal scandium is added into molten high-temperature liquid aluminum metal, and then the molten high-temperature liquid aluminum metal is slowly and fully melted, and then is stirred to form a uniform aluminum-scandium intermediate alloy. However, the method has high production cost and does not have practical significance for industrial production popularization and application. The current production method is to prepare the aluminum-scandium alloy by directly reducing scandium oxide with aluminum. The scandium oxide cost of the method is reduced by more than 90% compared with the cost of the pure metal scandium of the classical metal-pair doping method, meanwhile, the serious segregation of scandium in the alloy can be avoided, and the industrial production of the aluminum-scandium alloy can be realized.
Although the cost of scandium oxide is lower than that of pure scandium metal, the general aluminothermic method for preparing the aluminum-scandium master alloy requires that the purity of scandium oxide reaches 99-99.9%, the price of scandium oxide with the purity of 99.9% in the current domestic market is 10000 yuan/Kg, the price of scandium oxide with the purity of 95% is 5000-6000 yuan/Kg, and the price of low-grade scandium oxide with the purity of 60-70% is lower to 2000-3000 yuan/Kg, but the current production method cannot directly utilize the low-grade scandium oxide with the purity of 60-70% to prepare the aluminum-scandium metal alloy. In addition, the high-purity scandium oxide is generally adopted to prepare the aluminum-scandium master alloy, and no better solvent is used for assisting melting, so that the raw materials can reach a molten state only at a very high temperature, the energy consumption is higher, and the production cost is higher due to the need of vacuum condition or inert gas protection.
Therefore, the method for preparing the aluminum-scandium intermediate alloy by using the low-grade scandium oxide is developed, the aluminum-scandium intermediate alloy is prepared by using the low-price scandium oxide with the purity of 60-70%, the energy consumption of raw material heating is reduced, a non-vacuum or inert gas environment is adopted, the preparation cost of the aluminum-scandium intermediate alloy is further reduced, the application range of the aluminum-scandium intermediate alloy is expanded, and the aluminum-scandium alloy is made of an excellent material
Chinese patent (CN 201610463339.4) a method for preparing an aluminum-scandium master alloy with fine intermetallic compound particles and (CN 200910242633.2) a method for preparing an aluminum-scandium master alloy both adopt a reduction method to prepare the aluminum-scandium alloy, but both use fluorides and chlorides, which cause environmental pollution.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a method for preparing an aluminum-scandium master alloy by using low-grade scandium oxide.
In order to achieve the purpose, the invention adopts the following technical scheme:
a method for preparing an aluminum-scandium master alloy by using low-grade scandium oxide comprises the following steps:
(1) mixing materials: mixing silicon dioxide, magnesium oxide, aluminum oxide, polyethylene glycol 2000 and kerosene to prepare a solvent,
(2) weighing raw materials: scandium oxide, aluminum ingot and solvent are mixed according to the mass ratio (2-4): (20-35): (0.01-0.1), weighing, putting the solvent and scandium oxide into a ball mill, performing ball milling and mixing uniformly, and taking out a mixed material of the scandium oxide and the solvent;
(3) charging and heating: the method comprises the following steps of (1) loading a mixed material of scandium oxide and a solvent into a non-vacuum medium-frequency induction furnace, inserting an aluminum ingot into the mixed material of scandium oxide and the solvent, and heating at a uniform acceleration power of 50-100W/min;
(4) aluminothermic reduction: when the temperature rises to 660-680 ℃, keeping the heating power constant, melting the mixed material of the aluminum ingot, the scandium oxide and the solvent, carrying out an aluminothermic reduction reaction on the aluminum ingot and the scandium oxide in a molten state, and keeping the temperature at 660-680 ℃ for 10-30 min to ensure that the reaction is complete;
(5) removing slag on the surface: sodium sulfite powder, sodium carbonate powder, vermiculite and primary amine crystals are mixed according to the mass ratio of 1: (1-2): (1-2): (2-3) mixing, and crushing to obtain powder with the particle size of 40-100 meshes to obtain a slag-removing agent; uniformly spreading a slag removing agent on the surface of the molten material for removing slag;
(6) and (3) heat preservation casting: continuing to keep the temperature of 660-680 ℃, starting a stirring paddle of the non-vacuum intermediate frequency induction furnace to stir the molten material, simultaneously vertically casting the molten material after the aluminothermic reduction reaction, and rapidly cooling the molten material to normal temperature by using circulating water after the casting is finished to obtain an aluminum-scandium intermediate alloy ingot;
(7) surface treatment: polishing the cooled aluminum-scandium intermediate alloy ingot by using a grinding wheel machine, and removing salt slag remaining on the surface to obtain an aluminum-scandium intermediate alloy;
(8) detecting and packaging: sampling and detecting the aluminum-scandium intermediate alloy, and packaging after the detection is qualified.
The solvent is prepared from (5-10) by mass: 1: (2-4): (0.1-0.5): (0.02-0.05) silicon dioxide, magnesium oxide, aluminum oxide, polyethylene glycol 2000 and kerosene.
Preferably, the purity of the scandium oxide is 60-95%.
Preferably, the purity of the scandium oxide is 60-70%.
Preferably, the solvent is a mixture of 6: 1: 2: 0.2: 0.04 parts of silica, magnesia, alumina, polyethylene glycol 2000 and kerosene.
Preferably, the weight ratio of scandium oxide to aluminum ingot to solvent is 3: 28: 0.03 weight.
Preferably, the primary amine crystal is one or a combination of more of decyl primary amine crystal, dodecyl primary amine crystal, coconut alkyl primary amine crystal, tetradecyl primary amine crystal, hexadecyl primary amine crystal, octadecyl primary amine crystal, palmityl primary amine crystal and soybean oil-based primary amine crystal.
Preferably, the ball milling conditions are that the temperature is 90-200 ℃, the rotating speed is 400-600 rpm, and the time is 10-30 min.
Preferably, the rotation speed of the stirring is 50-200 rpm.
Preferably, the temperature of the circulating water is 4-15 ℃, and the cooling speed is 150-200 ℃/min.
The principle of the invention is as follows:
the invention develops the fluxing salt system and the proportion, weakens the intermolecular force in the scandium oxide crystal when the temperature is raised and heated, reduces the melting point, and reduces the heat energy required for reaching the molten state; polyethylene glycol 2000 and kerosene in a solvent are used as a coupling agent and a lubricant during ball milling and mixing, so that the uniformity of the mixed material is improved, fluxing salt molecules can better enter the inside of scandium oxide crystals, the damage to the crystal structure of scandium oxide is facilitated, and meanwhile, the polyethylene glycol 2000 and the kerosene which are proportioned by the method are easy to volatilize during high-temperature ball milling, and cannot enter the subsequent aluminum-scandium master alloy preparation link to influence the product quality; the charging and heating are carried out at a uniform acceleration power of 50-100W/min, all the raw materials are uniformly heated, the same temperature can be kept, and the uniformity of raw material melting is improved; aluminothermic reduction at 660-680 DEG CFirstly, the melting point of the raw materials is reduced by the solvent, and secondly, the impurity elements cannot be melted and added into the aluminum-scandium master alloy to cause pollution by keeping the lower temperature, so that the purity of the product is improved; the stirring of the stirring paddle can improve the uniformity of the materials during heat preservation casting, reduce the segregation degree to be less than or equal to 0.1 percent, and quickly cool the materials by circulating water to reduce intermetallic compounds Al3And the sedimentation of Sc avoids the segregation of components due to slow cooling, and improves the uniformity of the aluminum-scandium alloy.
Aluminum is a relatively active metal, and slag inclusion and gas absorption of oxides are easily formed during smelting, so that the physical performance and the corrosion resistance of the product are reduced, and therefore, a slag removing agent is required to be used for degassing and deslagging in the smelting process of the aluminum alloy. Generally, a layer of thick scum is generated on the surface of aluminum and aluminum alloy after refining, but the scum generated by the aluminum-scandium alloy prepared by the method is less, and a good effect can be achieved by using a small amount of slag-striking agent. This application uses sodium sulfite, sodium carbonate, vermiculite, primary amine as the slagging-off agent, meets high temperature inflation, softens, and three kinds of former substances all have the hydroscopicity. Common slag removing agents are all chloride and fluoride, and cause pollution to the environment. The sodium sulfite can remove samples in the molten liquid, the sodium carbonate removes sulfur, the vermiculite absorbs water to expand to agglomerate slag, the primary amine can generate inert gas nitrogen at high temperature to discharge impurities and gas in the molten liquid, and the primary amine has cohesiveness and can agglomerate the slag together to be convenient to remove.
The invention has the following advantages and positive effects:
(1) the solvent disclosed by the invention can reduce the purity requirement of scandium oxide from 99.9% to 60-95%, and can obviously reduce the unit cost of the raw material scandium oxide, so that the price of the product aluminum-scandium intermediate alloy is reduced, the final preparation of low-price aluminum-scandium alloy is facilitated, and the application of the aluminum-scandium alloy in the fields of automobiles, railways and aerospace crafts is promoted.
(2) The scandium recovery rate is more than or equal to 90%, the mass percent of scandium in the aluminum-scandium intermediate alloy is stabilized at 1.8-2.2%, the segregation degree is less than or equal to 0.1%, the alloy fracture structure is compact, slag and other impurities are very few, and the product quality is excellent.
(3) The solvent provided by the invention can obviously reduce the melting point of scandium oxide, reduce heating energy consumption, shorten the heat preservation time, and simultaneously reduce the production cost of the aluminum-scandium intermediate alloy without adopting a vacuum environment or inert gas protection.
(4) The invention has the advantages of low cost, simple process, short production period and good market prospect of products, and is suitable for large-scale industrial production.
Detailed Description
The present invention is described below with reference to examples, which are not intended to limit the present invention, in order to prepare an aluminum-scandium master alloy from low-grade scandium oxide.
Example 1
(1) Mixing materials: mixing silicon dioxide, magnesium oxide, aluminum oxide, polyethylene glycol 2000 and kerosene in a ratio of 6: 1: 2: 0.2: 0.04 to prepare a solvent;
(2) weighing raw materials: scandium oxide with the purity of 60%, aluminum ingot and solvent are mixed according to the mass ratio of 3: 28: 0.03, putting the solvent and scandium oxide with the purity of 60% into a ball mill for ball milling and uniformly mixing, wherein the temperature is 130 ℃, the rotating speed is 450rpm, and the time is 20 min, and then taking out the mixed material of the scandium oxide and the solvent;
(3) charging and heating: the mixed material of scandium oxide and solvent is loaded into a non-vacuum intermediate frequency induction furnace, an aluminum ingot is inserted into the mixed material of scandium oxide and solvent, and the temperature is raised with the uniform acceleration power of 80W/min;
(4) aluminothermic reduction: when the temperature is raised to 670 ℃, the heating power is kept constant, so that the mixed material of the aluminum ingot, the scandium oxide and the solvent is melted, the aluminum ingot and the scandium oxide are subjected to aluminothermic reduction reaction in a molten state, and the temperature is kept at 680 ℃ for 25 min to ensure that the reaction is complete;
(5) removing slag on the surface: sodium sulfite powder, sodium carbonate powder, vermiculite, decyl primary amine crystal and dodecyl primary amine crystal are mixed according to the mass ratio of 1: 2: 1: 2: 1, mixing, and crushing to powder with the particle size of 100 meshes to prepare a slag removing agent; uniformly spreading a slag removing agent on the surface of the molten material for removing slag;
(6) and (3) heat preservation casting: continuing to keep the temperature at 660 ℃, starting a stirring paddle of the non-vacuum intermediate frequency induction furnace to stir the molten material at the stirring speed of 100rpm, simultaneously carrying out vertical casting on the molten material after the thermite reduction reaction, and after the casting is finished, rapidly cooling the molten material to normal temperature at the speed of 180 ℃/min by using circulating water at 10 ℃ to obtain an aluminum-scandium intermediate alloy ingot;
(7) surface treatment: polishing the cooled aluminum-scandium intermediate alloy ingot by using a grinding wheel machine, and removing salt slag remaining on the surface to obtain an aluminum-scandium intermediate alloy;
(8) detecting and packaging: sampling and detecting the aluminum-scandium intermediate alloy, and packaging after the detection is qualified.
The Al-Sc master alloy with an average scandium content of 1.93% was analyzed by ICP-AES, and the scandium recovery rate was 93.68%.
Example 2:
(1) mixing materials: mixing silicon dioxide, magnesium oxide, aluminum oxide, polyethylene glycol 2000 and kerosene in a ratio of 8: 1: 3: 0.3: 0.02 mass ratio to prepare a solvent;
(2) weighing raw materials: scandium oxide with the purity of 70%, aluminum ingot and solvent are mixed according to the mass ratio of 2: 31: 0.06, putting the solvent and scandium oxide with the purity of 70% into a ball mill for ball milling and uniformly mixing, wherein the temperature is 150 ℃, the rotating speed is 500rpm, and the time is 30min, and then taking out the mixed material of the scandium oxide and the solvent;
(3) charging and heating: the mixed material of scandium oxide and solvent is loaded into a non-vacuum intermediate frequency induction furnace, an aluminum ingot is inserted into the mixed material of scandium oxide and solvent, and the temperature is raised with uniform acceleration power of 90W/min;
(4) aluminothermic reduction: when the temperature is raised to 660 ℃, the heating power is kept constant, so that the mixed material of the aluminum ingot, the scandium oxide and the solvent is melted, the aluminum ingot and the scandium oxide are subjected to aluminothermic reduction reaction in a molten state, and the temperature is kept at 67 ℃ for 10 min to ensure that the reaction is complete;
(5) removing slag on the surface: sodium sulfite powder, sodium carbonate powder, vermiculite, coconut alkyl primary amine crystals, tetradecyl primary amine crystals and hexadecyl primary amine crystals are mixed according to the mass ratio of 1: 1: 2: 1: 0.5: 0.5, and crushing the mixture into powder with the particle size of 80 meshes to prepare the slag removing agent; uniformly spreading a slag removing agent on the surface of the molten material for removing slag;
(6) and (3) heat preservation casting: continuing to keep the temperature at 680 ℃, starting a stirring paddle of the non-vacuum intermediate frequency induction furnace to stir the molten material at the stirring speed of 120rpm, simultaneously vertically casting the molten material after the thermite reduction reaction, and rapidly cooling the molten material to normal temperature at the speed of 150 ℃/min by using circulating water at 8 ℃ after the casting is finished to obtain an aluminum-scandium intermediate alloy ingot;
(7) surface treatment: polishing the cooled aluminum-scandium intermediate alloy ingot by using a grinding wheel machine, and removing salt slag remaining on the surface to obtain an aluminum-scandium intermediate alloy;
(8) detecting and packaging: sampling and detecting the aluminum-scandium intermediate alloy, and packaging after the detection is qualified.
By ICP-AES analysis, the recovery rate of scandium was 92.38% for the aluminum-scandium master alloy with the average scandium content of 1.98%.
Example 3:
(1) mixing materials: mixing silicon dioxide, magnesium oxide, aluminum oxide, polyethylene glycol 2000 and kerosene in a ratio of 10: 1: 4: 0.1: 0.05, preparing a solvent by mixing;
(2) weighing raw materials: scandium oxide with the purity of 95%, aluminum ingot and solvent are mixed according to the mass ratio of 4: 22: 0.05, putting the solvent and scandium oxide with the purity of 95% into a ball mill for ball milling and uniformly mixing, wherein the temperature is 100 ℃, the rotating speed is 600rpm, and the time is 25 min, and then taking out the mixed material of the scandium oxide and the solvent;
(3) charging and heating: the mixed material of scandium oxide and solvent is loaded into a non-vacuum intermediate frequency induction furnace, an aluminum ingot is inserted into the mixed material of scandium oxide and solvent, and the temperature is raised with the uniform acceleration power of 50W/min;
(4) aluminothermic reduction: when the temperature is raised to 680 ℃, keeping the heating power constant, melting the mixed material of the aluminum ingot, the scandium oxide and the solvent, carrying out aluminothermic reduction reaction on the aluminum ingot and the scandium oxide in a molten state, and keeping the temperature at 665 ℃ for 30min to ensure that the reaction is complete;
(5) removing slag on the surface: sodium sulfite powder, sodium carbonate powder, vermiculite, primary octadecyl amine crystals and primary palmityl amine crystals are mixed according to the mass ratio of 1: 1.5: 1.5: 1.5: 0.5, and crushing the mixture into powder with the particle size of 40 meshes to prepare the slag removing agent; uniformly spreading a slag removing agent on the surface of the molten material for removing slag;
(6) and (3) heat preservation casting: keeping the temperature at 670 ℃, starting a stirring paddle of the non-vacuum intermediate frequency induction furnace to stir the molten material at the stirring speed of 180pm, simultaneously carrying out vertical casting on the molten material after the thermite reduction reaction, and after the casting is finished, rapidly cooling the molten material to the normal temperature at the speed of 190 ℃/min by using circulating water at 15 ℃ to obtain an aluminum-scandium intermediate alloy ingot;
(7) surface treatment: polishing the cooled aluminum-scandium intermediate alloy ingot by using a grinding wheel machine, and removing salt slag remaining on the surface to obtain an aluminum-scandium intermediate alloy;
(8) detecting and packaging: sampling and detecting the aluminum-scandium intermediate alloy, and packaging after the detection is qualified.
The Al-Sc master alloy with an average scandium content of 2.17% was analyzed by ICP-AES, and the scandium recovery rate was 92.56%.
Example 4:
(1) mixing materials: mixing silicon dioxide, magnesium oxide, aluminum oxide, polyethylene glycol 2000 and kerosene in a ratio of 5: 1: 2.5: 0.5: 0.02 mass ratio to prepare a solvent;
(2) weighing raw materials: scandium oxide with the purity of 80%, aluminum ingot and solvent are mixed according to the mass ratio of 3: 30: 0.07, putting the solvent and scandium oxide with the purity of 60% into a ball mill for ball milling and uniformly mixing, wherein the temperature is 190 ℃, the rotating speed is 550rpm, and the time is 15 min, and then taking out the mixed material of the scandium oxide and the solvent;
(3) charging and heating: the method comprises the following steps of (1) loading a mixed material of scandium oxide and a solvent into a non-vacuum medium-frequency induction furnace, inserting an aluminum ingot into the mixed material of scandium oxide and the solvent, and heating at a uniform acceleration power of 100W/min;
(4) aluminothermic reduction: when the temperature rises to 675 ℃, the heating power is kept constant, so that the mixed material of the aluminum ingot, the scandium oxide and the solvent is melted, the aluminum ingot and the scandium oxide are subjected to aluminothermic reduction reaction in a molten state, and the temperature is kept at 675 ℃ for 20 min to ensure that the reaction is complete;
(5) removing slag on the surface: sodium sulfite powder, sodium carbonate powder, vermiculite and soybean oil-based primary amine crystals are mixed according to the mass ratio of 1: 2: 1.5: 2.5, mixing, and crushing to obtain powder with the particle size of 60 meshes to prepare the slag removing agent; uniformly spreading a slag removing agent on the surface of the molten material for removing slag;
(6) and (3) heat preservation casting: continuing to keep the temperature at 660 ℃, starting a stirring paddle of the non-vacuum intermediate frequency induction furnace to stir the molten material at the stirring speed of 80rpm, simultaneously carrying out vertical casting on the molten material after the thermite reduction reaction, and after the casting is finished, rapidly cooling the molten material to normal temperature at the speed of 200 ℃/min by using circulating water at 4 ℃ to obtain an aluminum-scandium intermediate alloy ingot;
(7) surface treatment: polishing the cooled aluminum-scandium intermediate alloy ingot by using a grinding wheel machine, and removing salt slag remaining on the surface to obtain an aluminum-scandium intermediate alloy;
(8) detecting and packaging: sampling and detecting the aluminum-scandium intermediate alloy, and packaging after the detection is qualified.
The Al-Sc master alloy with an average scandium content of 1.84% was analyzed by ICP-AES, and the scandium recovery rate was 93.41%.
Claims (9)
1. A method for preparing an aluminum-scandium master alloy by using low-grade scandium oxide is characterized by comprising the following steps:
(1) mixing materials: mixing silicon dioxide, magnesium oxide, aluminum oxide, polyethylene glycol 2000 and kerosene to prepare a solvent;
(2) weighing raw materials: scandium oxide, aluminum ingot and solvent are mixed according to the mass ratio (2-4): (20-35): (0.01-0.1), weighing, putting the solvent and scandium oxide into a ball mill, performing ball milling and mixing uniformly, and taking out a mixed material of the scandium oxide and the solvent;
(3) charging and heating: the method comprises the following steps of (1) loading a mixed material of scandium oxide and a solvent into a non-vacuum medium-frequency induction furnace, inserting an aluminum ingot into the mixed material of scandium oxide and the solvent, and heating at a uniform acceleration power of 50-100W/min;
(4) aluminothermic reduction: when the temperature rises to 660-680 ℃, keeping the heating power constant, melting the mixed material of the aluminum ingot, the scandium oxide and the solvent, carrying out an aluminothermic reduction reaction on the aluminum ingot and the scandium oxide in a molten state, and keeping the temperature at 660-680 ℃ for 10-30 min to ensure that the reaction is complete;
(5) removing slag on the surface: sodium sulfite powder, sodium carbonate powder, vermiculite and primary amine crystals are mixed according to the mass ratio of 1: (1-2): (1-2): (2-3) mixing, and crushing to obtain powder with the particle size of 40-100 meshes to obtain a slag-removing agent; uniformly spreading a slag removing agent on the surface of the molten material for removing slag;
(6) and (3) heat preservation casting: continuing to keep the temperature of 660-680 ℃, starting a stirring paddle of the non-vacuum intermediate frequency induction furnace to stir the molten material, simultaneously vertically casting the molten material after the aluminothermic reduction reaction, and rapidly cooling the molten material to normal temperature by using circulating water after the casting is finished to obtain an aluminum-scandium intermediate alloy ingot;
(7) surface treatment: polishing the cooled aluminum-scandium intermediate alloy ingot by using a grinding wheel machine, and removing salt slag remaining on the surface to obtain an aluminum-scandium intermediate alloy;
(8) detecting and packaging: sampling and detecting the aluminum-scandium intermediate alloy, and packaging after the detection is qualified;
the solvent is prepared from (5-10) by mass: 1: (2-4): (0.1-0.5): (0.02-0.05) silicon dioxide, magnesium oxide, aluminum oxide, polyethylene glycol 2000 and kerosene.
2. The method for preparing the aluminum-scandium master alloy from the low-grade scandium oxide according to claim 1, wherein a purity of the scandium oxide is 60-95%.
3. The method for preparing the aluminum-scandium master alloy from the low-grade scandium oxide according to claim 2, wherein the purity of the scandium oxide is 60-70%.
4. The method for preparing the aluminum-scandium master alloy from the low-grade scandium oxide according to claim 1, wherein the solvent is a mixture of a solvent and a solvent, wherein the mass ratio of the solvent is 6: 1: 2: 0.2: 0.04 parts of silica, magnesia, alumina, polyethylene glycol 2000 and kerosene.
5. The method for preparing the aluminum-scandium master alloy from the low-grade scandium oxide according to any one of claims 1 to 4, wherein the weight ratio of scandium oxide to aluminum ingot to solvent is 3: 28: 0.03 weight.
6. The method for preparing the aluminum-scandium master alloy from the low-grade scandium oxide according to claim 1, wherein the primary amine crystal is one or a combination of several of decyl primary amine crystal, dodecyl primary amine crystal, coco primary amine crystal, tetradecyl primary amine crystal, hexadecyl primary amine crystal, octadecyl primary amine crystal, palmityl primary amine crystal and soybean oil-based primary amine crystal.
7. The method for preparing the aluminum-scandium master alloy from the low-grade scandium oxide according to claim 1, wherein the ball milling is performed under conditions of a temperature of 90-200 ℃, a rotation speed of 400-600 rpm, and a time of 10-30 min.
8. The method for preparing the aluminum-scandium master alloy from the low-grade scandium oxide according to claim 1, wherein a rotation speed of the stirring is 50-200 rpm.
9. The method for preparing the aluminum-scandium master alloy from the low-grade scandium oxide according to claim 1, wherein the temperature of the circulating water is 4-15 ℃, and the cooling speed is 150-200 ℃/min.
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| JP5094031B2 (en) * | 2006-03-23 | 2012-12-12 | 大平洋金属株式会社 | Method for producing scandium-containing alloy |
| CN102337406B (en) * | 2011-09-26 | 2014-12-17 | 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 |
| 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 |
| KR101724288B1 (en) * | 2015-07-17 | 2017-04-10 | 재단법인 포항산업과학연구원 | Method for producing aluminum-scandium alloy with high purity |
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