CN110205652B - A kind of preparation method and application of copper-scandium master alloy - Google Patents

A kind of preparation method and application of copper-scandium master alloy Download PDF

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CN110205652B
CN110205652B CN201910407398.3A CN201910407398A CN110205652B CN 110205652 B CN110205652 B CN 110205652B CN 201910407398 A CN201910407398 A CN 201910407398A CN 110205652 B CN110205652 B CN 110205652B
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scandium
copper
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李斌川
马成贵
陈建设
韩庆
孔亚鹏
刘奎仁
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Northeastern University China
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Abstract

本发明公开了一种铜钪中间合金的制备方法,在含有钪的熔盐电解质中,以金属铜电极为可消耗阴极,以石墨为阳极,通过熔盐电解制备铜钪中间合金;上述方法制备的铜钪中间合金用于制备含钪铝合金或其它含钪合金。本发明提供的制备方法,工艺简单、无污染、生产成本低,制备的铜钪中间合金钪的含量可达10~75%,可用于多种含钪合金的制备。The invention discloses a preparation method of a copper-scandium intermediate alloy. In a molten salt electrolyte containing scandium, a metal copper electrode is used as a consumable cathode, and graphite is used as an anode, and the copper-scandium intermediate alloy is prepared by molten salt electrolysis; the above method prepares The copper-scandium master alloy is used to prepare scandium-containing aluminum alloys or other scandium-containing alloys. The preparation method provided by the invention has the advantages of simple process, no pollution and low production cost, the content of scandium in the prepared copper-scandium intermediate alloy can reach 10-75%, and can be used for the preparation of various scandium-containing alloys.

Description

一种铜钪中间合金的制备方法和应用A kind of preparation method and application of copper-scandium master alloy

技术领域technical field

本发明涉及合金制备技术领域,具体涉及一种铜钪中间合金的制备方法和应用。The invention relates to the technical field of alloy preparation, in particular to a preparation method and application of a copper-scandium master alloy.

背景技术Background technique

钪的原子序数为21,在周期表中与镧系稀土金属同属于Ⅲ副族,与钛、钒、铬等同属于3d型过渡金属。金属钪是铸造铝合金的优良变质剂,也是铁的优良改化剂。目前金属钪大量应用于制备铝钪合金,在铝合金中添加微量的金属钪(0.1~0.4%),可使合金晶粒细化,显著提高铝合金的强度、塑韧性、耐高温性能、耐腐蚀性能等。含钪铝合金综合性能明显优于传统铝合金,广泛应用于航天、军事工业等尖端科技领域。The atomic number of scandium is 21. In the periodic table, it belongs to the III subgroup with the lanthanide rare earth metals, and belongs to the 3d-type transition metal with titanium, vanadium, and chromium. Scandium metal is an excellent modifier for cast aluminum alloys and an excellent modifier for iron. At present, metal scandium is widely used in the preparation of aluminum-scandium alloys. Adding a small amount of metal scandium (0.1-0.4%) to the aluminum alloy can refine the grains of the alloy and significantly improve the strength, plasticity, toughness, high temperature resistance and resistance of the aluminum alloy. Corrosion properties, etc. The comprehensive performance of scandium-containing aluminum alloy is obviously better than that of traditional aluminum alloy, and it is widely used in cutting-edge scientific and technological fields such as aerospace and military industry.

由于单质钪化学性质活泼,且熔点高(1541℃),与铝熔点(660℃)相差较大,难以通过直接熔铸的方法制备含钪铝合金。在工业中铝钪合金的生产过程中,通常以中间合金的形式向合金中加入钪。目前,铝钪中间合金的制备方法主要有对掺法、金属热还原法和熔盐电解法。Due to the active chemical properties of elemental scandium and its high melting point (1541°C), which is quite different from the melting point of aluminum (660°C), it is difficult to prepare scandium-containing aluminum alloys by direct melting and casting. During the production of aluminum-scandium alloys in the industry, scandium is usually added to the alloy in the form of a master alloy. At present, the preparation methods of Al-scandium master alloy mainly include counter-doping method, metallothermic reduction method and molten salt electrolysis method.

对掺法是以高纯金属钪和纯铝为原料,在氩气保护气氛中,将特定比例的金属钪用铝箔包裹后加入铝熔体中,充分搅拌,保温足够时间后进行浇铸,即可制得铝钪中间合金。采用对掺法可以制得钪含量在2~4%的铝钪中间合金,工艺简单,但是对掺法需要采用高纯金属钪为原料,成本较高;合金损失多,回收率低;且钪、铝熔点相差大,合金中成分分布不均匀,品质较差。The counter-doping method uses high-purity metal scandium and pure aluminum as raw materials. In an argon protective atmosphere, a specific proportion of metal scandium is wrapped with aluminum foil and added to the aluminum melt, fully stirred, and kept for a sufficient time before casting. An aluminum-scandium master alloy was prepared. The Al-scandium master alloy with scandium content of 2-4% can be prepared by the counter-doping method, and the process is simple, but the counter-doping method needs to use high-purity metal scandium as the raw material, and the cost is high; the alloy loses a lot and the recovery rate is low; and the scandium , The melting point of aluminum has a large difference, the distribution of components in the alloy is uneven, and the quality is poor.

金属热还原法以氟化钪真空铝热还原法为主,采用氟化钪为原料,以金属铝为还原剂,在真空下进行还原制备铝钪中间合金。该法制得的中间合金中钪含量可达30%,但氟化钪原料制备过程复杂,且该工艺无法连续生产,产率较低。The metallothermic reduction method is mainly based on the vacuum aluminothermic reduction method of scandium fluoride. Scandium fluoride is used as raw material, and metal aluminum is used as reducing agent, and the aluminum-scandium master alloy is prepared by reduction under vacuum. The content of scandium in the master alloy prepared by this method can reach 30%, but the preparation process of the scandium fluoride raw material is complicated, the process cannot be continuously produced, and the yield is low.

熔盐电解法主要以氧化钪或氯化钪为原料,在氯盐体系或氟盐体系中进行电解。其中以氯化钪为原料时,多采用NaCl–KCl–ScCl3和LiCl–KCl–ScCl3为电解质,以液态金属铝作阴极,通过采用适宜的电解参数,钪离子在液态铝阴极上沉积并与其形成合金,在阳极上Cl-被氧化生成氯气。需要指出的是氯化钪易吸潮,难以运输和存储,并且电解过程中有氯气产生对环境有污染,故工业生产中较少采用。而以氧化钪为原料时,采用的电解质为NaF·AlF3–Sc2O3–ScF3–NaCl,NaF–Sc2O3–ScF3、CaCl2–Sc2O3或LiF–Sc2O3–ScF3,多采用液态金属铝作阴极或在熔盐中添加Al2O3从而电解时在阴极生成液态铝,电解过程中钪离子在阴极沉积并与铝形成中间合金。与对掺法和金属热还原法相比,熔盐电解法制备的铝钪中间合金具有成分均匀、生产成本低、易于连续化生产、不需用还原剂等优势。在关于熔盐电解法制备钪中间合金的研究中,基本都是以铝钪合金为目标产物,用液态铝来捕收钪,但是铝、钪熔点相差很大,电解制备铝钪合金的过程中,铝熔体需要很高的过热度,并且钪在铝中的扩散较慢,很难形成成分均匀的高浓度含钪合金成分,中间合金中钪的含量较低。The molten salt electrolysis method mainly uses scandium oxide or scandium chloride as raw materials, and conducts electrolysis in a chloride salt system or a fluoride salt system. Among them, when scandium chloride is used as raw material, NaCl–KCl–ScCl 3 and LiCl–KCl–ScCl 3 are mostly used as electrolytes, and liquid metal aluminum is used as cathode. Instead of alloying, Cl- is oxidized at the anode to form chlorine. It should be pointed out that scandium chloride is easy to absorb moisture, difficult to transport and store, and the production of chlorine in the electrolysis process pollutes the environment, so it is less used in industrial production. When scandium oxide is used as raw material, the electrolyte used is NaF·AlF 3 -Sc 2 O 3 -ScF 3 -NaCl, NaF-Sc 2 O 3 -ScF 3 , CaCl 2 -Sc 2 O 3 or LiF-Sc 2 O 3 -ScF 3 , mostly using liquid metal aluminum as the cathode or adding Al 2 O 3 to the molten salt to generate liquid aluminum at the cathode during electrolysis. During the electrolysis process, scandium ions are deposited at the cathode and form an intermediate alloy with aluminum. Compared with the counter-doping method and the metallothermic reduction method, the aluminum-scandium master alloy prepared by the molten salt electrolysis method has the advantages of uniform composition, low production cost, easy continuous production, and no reducing agent. In the research on the preparation of scandium master alloy by molten salt electrolysis, the aluminum-scandium alloy is basically the target product, and liquid aluminum is used to capture scandium, but the melting points of aluminum and scandium are very different. , the aluminum melt requires a high degree of superheat, and the diffusion of scandium in aluminum is slow, it is difficult to form a high-concentration scandium-containing alloy composition with uniform composition, and the content of scandium in the master alloy is low.

发明内容SUMMARY OF THE INVENTION

本发明要解决的技术问题是熔盐电解制备钪中间合金时存在钪含量低的问题,提供一种使用铜可消耗阴极进行电解制备高钪含量的铜钪中间合金的方法。The technical problem to be solved by the present invention is the problem of low scandium content during the preparation of scandium master alloy by molten salt electrolysis, and provides a method for preparing a copper-scandium master alloy with high scandium content by electrolysis using a copper consumable cathode.

为解决上述技术问题,本发明采用的技术方案为:In order to solve the above-mentioned technical problems, the technical scheme adopted in the present invention is:

一种铜钪中间合金的制备方法,在含有钪的熔盐电解质中,以金属铜电极为可消耗阴极,以石墨为阳极,通过熔盐电解制备铜钪中间合金。A method for preparing a copper-scandium intermediate alloy. In a molten salt electrolyte containing scandium, a metal copper electrode is used as a consumable cathode, and graphite is used as an anode, and the copper-scandium intermediate alloy is prepared by molten salt electrolysis.

进一步地,所述熔盐电解质按质量份数包括:20~70份LiF,5~60份ScF3,0~55份MCl或/和MF,其中M为碱金属元素和碱土金属元素中的一种或者多种。Further, the molten salt electrolyte includes, in parts by mass: 20-70 parts of LiF, 5-60 parts of ScF 3 , 0-55 parts of MCl or/and MF, wherein M is one of alkali metal elements and alkaline earth metal elements species or multiple species.

进一步地,在所述熔盐电解质中加入原料Sc2O3,Sc2O3的加入质量为熔盐质量的0~30%。Further, raw material Sc 2 O 3 is added to the molten salt electrolyte, and the added mass of Sc 2 O 3 is 0-30% of the mass of the molten salt.

进一步地,所述熔盐电解温度为875~1100℃。Further, the molten salt electrolysis temperature is 875-1100°C.

进一步地,所述熔盐电解,控制阴极电流密度为0.5~40A/cm2Further, in the molten salt electrolysis, the cathode current density is controlled to be 0.5-40 A/cm 2 .

进一步地,铜阴极下方放置盛接坩埚用以收集铜钪中间合金产物,所述盛接坩埚为钼坩埚、钨坩埚、钽坩埚或石墨坩埚。Further, a receiving crucible is placed under the copper cathode to collect the copper-scandium intermediate alloy product, and the receiving crucible is a molybdenum crucible, a tungsten crucible, a tantalum crucible or a graphite crucible.

上述方法制备的铜钪中间合金用于制备其它金属的含钪合金。The copper-scandium master alloy prepared by the above method is used to prepare scandium-containing alloys of other metals.

本发明提供的一种铜钪中间合金的制备方法,工艺简单、无污染,原料来源广、生产成本低;制备的铜钪中间合金中,杂质含量较低,钪的含量按物质的量比可达10~75%,可用于多种含钪合金的制备,可显著提高合金的机械性能、强度、塑韧性、耐高温、耐腐蚀等性能。The preparation method of the copper-scandium master alloy provided by the invention has the advantages of simple process, no pollution, wide source of raw materials and low production cost; in the prepared copper-scandium master alloy, the impurity content is relatively low, and the content of scandium can be adjusted according to the amount of the substance. It can be used in the preparation of various scandium-containing alloys, and can significantly improve the mechanical properties, strength, plastic toughness, high temperature resistance, corrosion resistance and other properties of the alloy.

具体实施方式Detailed ways

一种铜钪中间合金的制备方法,在含有钪的熔盐电解质中,以金属铜电极为可消耗阴极,以石墨为阳极,通过熔盐电解制备铜钪中间合金。A method for preparing a copper-scandium intermediate alloy. In a molten salt electrolyte containing scandium, a metal copper electrode is used as a consumable cathode, and graphite is used as an anode, and the copper-scandium intermediate alloy is prepared by molten salt electrolysis.

其中,熔盐电解质成分为LiF–ScF3–MCl/MF,M为碱金属元素和碱土金属元素中的一种或者多种,所述熔盐电解质按质量份数包括:20~70份LiF,5~60份ScF3,0~55份MCl或/和MF。在所述熔盐电解质中加入原料Sc2O3,Sc2O3的加入质量为熔盐质量的0~30%。The composition of the molten salt electrolyte is LiF-ScF 3 -MCl/MF, M is one or more of alkali metal elements and alkaline earth metal elements, and the molten salt electrolyte includes 20-70 parts by mass of LiF, 5-60 parts of ScF 3 , 0-55 parts of MCl or/and MF. The raw material Sc 2 O 3 is added to the molten salt electrolyte, and the added mass of Sc 2 O 3 is 0-30% of the mass of the molten salt.

具体地,一种铜钪中间合金的制备方法,将Sc2O3与熔盐电解质混合均匀,用石墨坩埚盛装,并以石墨坩埚为阳极,将铜棒插入熔化的熔盐中作为阴极,铜棒下方放置有盛接坩埚用以收集阴极产物产物,盛接坩埚与石墨坩埚绝缘隔开,熔盐电解制备铜钪中间合金。Specifically, a method for preparing a copper-scandium master alloy is to mix Sc 2 O 3 and a molten salt electrolyte evenly, use a graphite crucible as an anode, insert a copper rod into the molten molten salt as a cathode, and use the graphite crucible as an anode. A receiving crucible is placed under the rod for collecting cathode products, the receiving crucible is insulated from the graphite crucible, and the copper-scandium intermediate alloy is prepared by molten salt electrolysis.

所述熔盐电解温度为875~1100℃,控制阴极电流密度为0.5~40A/cm2 The molten salt electrolysis temperature is 875-1100°C, and the cathode current density is controlled to be 0.5-40A/cm 2

所述盛接坩埚为钼坩埚、钨坩埚、钽坩埚或石墨坩埚。。The receiving crucible is a molybdenum crucible, a tungsten crucible, a tantalum crucible or a graphite crucible. .

上述方法制备的铜钪中间合金用于制备含钪合金。以中间合金的形式添加到其它金属里面制备含钪合金。The copper-scandium master alloy prepared by the above method is used to prepare a scandium-containing alloy. It is added to other metals in the form of master alloys to prepare scandium-containing alloys.

铜、钪的熔点相差相对铝、钪较小,根据Cu–Sc相图可知,液相线较为平缓,钪与铜分别可在865℃形成含钪13%(物质的量比),875℃形成含钪30%或71%(物质的量比),890℃形成含钪36.5%(物质的量比)的Cu–Sc合金。因此本发明提出以氟化钪或氧化钪为原料,在氟化物或氯化物熔盐电解质中采用铜可消耗阴极,以石墨为阳极进行电解制备高钪含量的铜钪中间合金产品。电解过程中,钪离子Sc3+向阴极迁移并在铜阴极上还原为金属钪,金属钪与铜形成Cu-Sc合金,电解温度低于铜的熔点,但高于Cu-Sc合金的熔点,得到的液态合金与铜阴极分离下沉进入阴极下方的盛接坩埚中,而铜阴极又露出新的表面继续电解。随着电解的进行,铜阴极不断消耗形成合金。通过调整电解温度和电流密度,可得到不同钪含量的铜钪中间合金,盛接坩埚中的Cu-Sc合金经浇铸冷却后得到Cu-Sc合金锭。The melting point difference between copper and scandium is smaller than that of aluminum and scandium. According to the Cu–Sc phase diagram, the liquidus is relatively flat. Scandium and copper can form 13% scandium (the ratio of substances) at 865 °C, respectively, and form at 875 °C. A Cu-Sc alloy containing scandium 30% or 71% (in substance ratio) was formed at 890° C. with scandium content of 36.5% (in substance ratio). Therefore, the present invention proposes to use scandium fluoride or scandium oxide as raw material, use copper consumable cathode in fluoride or chloride molten salt electrolyte, and use graphite as anode for electrolysis to prepare copper-scandium master alloy products with high scandium content. During the electrolysis process, the scandium ion Sc 3+ migrates to the cathode and is reduced to metal scandium on the copper cathode. The metal scandium and copper form a Cu-Sc alloy. The electrolysis temperature is lower than the melting point of copper, but higher than the melting point of the Cu-Sc alloy. The obtained liquid alloy is separated from the copper cathode and sinks into the receiving crucible below the cathode, and the copper cathode exposes a new surface to continue electrolysis. As electrolysis progresses, the copper cathode is continuously consumed to form an alloy. By adjusting the electrolysis temperature and current density, copper-scandium intermediate alloys with different scandium contents can be obtained, and the Cu-Sc alloy in the crucible is poured and cooled to obtain a Cu-Sc alloy ingot.

本发明的创造性总结如下:The inventive step of the present invention is summarized as follows:

1、本发明阴极为可消耗阴极,阴极产物为液态,相对于固态产物,杂质含量低,后续加工便利;1. The cathode of the present invention is a consumable cathode, and the cathode product is liquid, with respect to the solid product, the impurity content is low, and the subsequent processing is convenient;

2、相对于采用液体阴极铝熔盐电解生产铝钪合金,本发明的钪含量显著增加,作为铝钪合金调配的中间合金,不仅应用方便,而且可大幅降低钪合金生产规模,节省设备投资及钪合金生产成本;2. Compared with the use of liquid cathode aluminum molten salt electrolysis to produce aluminum-scandium alloy, the scandium content of the present invention is significantly increased, and as the intermediate alloy prepared by aluminum-scandium alloy, it is not only convenient to use, but also can greatly reduce the production scale of scandium alloy, saving equipment investment and cost. Scandium alloy production cost;

3、可借鉴镝铁、铽铁等稀土-铁合金生产装备及模式,不用开发专门钪合金电解设备,技术成熟度高。3. The production equipment and models of rare earth-ferroalloys such as dysprosium iron and terbium iron can be used for reference, and there is no need to develop special scandium alloy electrolysis equipment, and the technology is highly mature.

实施例1一种铜钪中间合金的制备方法Embodiment 1 A kind of preparation method of copper-scandium master alloy

将500g熔盐与150g Sc2O3混合均匀后放入直径为80mm的石墨坩埚中,其中,按照质量百分比,熔盐电解质体系为60份的ScF3,20份的LiF和10份的NaF;石墨坩埚底部中心放置有与石墨绝缘处理过的直径为50mm的钼坩埚作为盛接坩埚;然后将石墨坩埚放入炉子内加热到875℃,待熔盐溶化后,将一根直径20mm的铜棒插入熔盐,浸入深度为30mm;以石墨坩埚为阳极,以铜棒为阴极进行电解,电流密度为40A/cm2;电解2h后用坩埚钳取出盛接的钼坩埚,将其中收集到的铜钪中间合金液浇铸到模具中,制成铜钪中间合金锭。经检测,合金成分按物质的量比为:铜25%、钪75%。Mix 500g of molten salt and 150g of Sc 2 O 3 evenly and put it into a graphite crucible with a diameter of 80 mm, wherein, according to the mass percentage, the molten salt electrolyte system is 60 parts of ScF 3 , 20 parts of LiF and 10 parts of NaF; A molybdenum crucible with a diameter of 50mm that has been insulated from graphite is placed in the center of the bottom of the graphite crucible as a receiving crucible; then the graphite crucible is placed in a furnace and heated to 875°C. After the molten salt is melted, a copper rod with a diameter of 20mm is placed. Insert molten salt, the immersion depth is 30mm; take graphite crucible as anode, copper rod as cathode for electrolysis, current density is 40A /cm The scandium master alloy liquid is poured into the mold to make a copper scandium master alloy ingot. After testing, the alloy composition according to the material ratio is: copper 25%, scandium 75%.

实施例2一种铜钪中间合金的制备方法Embodiment 2 A kind of preparation method of copper-scandium master alloy

将500g熔盐与100g Sc2O3混合均匀后放入直径为80mm的石墨坩埚中,其中,按照质量百分比,熔盐电解质体系为5份的ScF3和70份的LiF;石墨坩埚底部中心放置有与石墨绝缘处理过的直径为50mm的钼坩埚作为盛接坩埚;然后将石墨坩埚放入炉子内加热到1100℃,待熔盐溶化后,将一根直径20mm的铜棒插入熔盐,浸入深度为30mm;以石墨坩埚为阳极,以铜棒为阴极进行电解,电流密度为10A/cm2;电解2h后用坩埚钳取出盛接的钼坩埚,将其中收集到的铜钪中间合金液浇铸到模具中,制成铜钪中间合金锭。经检测,合金成分按物质的量比为:铜80%、钪20%。Mix 500g of molten salt and 100g of Sc 2 O 3 evenly and put it into a graphite crucible with a diameter of 80mm, wherein, according to the mass percentage, the molten salt electrolyte system is 5 parts of ScF 3 and 70 parts of LiF; the center of the bottom of the graphite crucible is placed There is a molybdenum crucible with a diameter of 50mm that has been insulated with graphite as the receiving crucible; then put the graphite crucible into the furnace and heat it to 1100 ° C. After the molten salt is melted, insert a copper rod with a diameter of 20mm into the molten salt and immerse it in the molten salt. The depth is 30mm; the graphite crucible is used as the anode, and the copper rod is used as the cathode for electrolysis, and the current density is 10A/cm 2 ; after the electrolysis for 2h, the molybdenum crucible is taken out with the crucible tongs, and the copper-scandium intermediate alloy liquid collected therein is cast. into a mold to make a copper-scandium master alloy ingot. After testing, the alloy composition according to the material ratio is: copper 80%, scandium 20%.

实施例3一种铜钪中间合金的制备方法Embodiment 3 A kind of preparation method of copper-scandium master alloy

将500g熔盐放入直径为80mm的石墨坩埚中,其中,按照质量百分比,熔盐电解质体系为5份的ScF3,70份的LiF和55份的MgCl;石墨坩埚底部中心放置有与石墨绝缘处理过的直径为50mm的钼坩埚作为盛接坩埚;然后将石墨坩埚放入炉子内加热到1000℃,待熔盐溶化后,将一根直径20mm的铜棒插入熔盐,浸入深度为30mm;以石墨坩埚为阳极,以铜棒为阴极进行电解,电流密度为0.5A/cm2;电解2h后用坩埚钳取出盛接的钼坩埚,将其中收集到的铜钪中间合金液浇铸到模具中,制成铜钪中间合金锭。经检测,合金成分按物质的量比为:铜90%、钪10%。Put 500g of molten salt into a graphite crucible with a diameter of 80mm, wherein, according to the mass percentage, the molten salt electrolyte system is 5 parts of ScF 3 , 70 parts of LiF and 55 parts of MgCl; the center of the bottom of the graphite crucible is placed with graphite insulation. The treated molybdenum crucible with a diameter of 50mm is used as the receiving crucible; then the graphite crucible is put into the furnace and heated to 1000°C. After the molten salt is melted, a copper rod with a diameter of 20mm is inserted into the molten salt, and the immersion depth is 30mm; The graphite crucible was used as the anode, and the copper rod was used as the cathode for electrolysis, and the current density was 0.5A/cm 2 ; after 2 hours of electrolysis, the molybdenum crucible was taken out with crucible tongs, and the copper-scandium intermediate alloy liquid collected therein was cast into the mold , made into copper-scandium master alloy ingots. After testing, the alloy composition according to the material ratio is: copper 90%, scandium 10%.

最后所应说明的是,以上具体实施方式仅用以说明本发明的技术方案而非限制,尽管参照实例对本发明进行了详细说明,本领域的普通技术人员应当理解,可以对本发明的技术方案进行修改或者等同替换,而不脱离本发明技术方案的精神和范围,其均应涵盖在本发明的权利要求范围当中。Finally, it should be noted that the above specific embodiments are only used to illustrate the technical solutions of the present invention and not to limit them. Although the present invention has been described in detail with reference to examples, those of ordinary skill in the art should understand that the technical solutions of the present invention can be Modifications or equivalent substitutions without departing from the spirit and scope of the technical solutions of the present invention should be included in the scope of the claims of the present invention.

Claims (4)

1.一种铜钪中间合金的制备方法,其特征在于:在含有钪的熔盐电解质中,以金属铜电极为可消耗阴极,以石墨为阳极,通过熔盐电解制备铜钪中间合金;所述熔盐电解质按质量份数包括:20~70份LiF,5~60份ScF3,0~55份MCl或/和MF,其中M为碱金属元素和碱土金属元素中的一种或者多种;所述熔盐电解温度为875℃,所述熔盐电解阴极电流密度为40 A/cm2,制备钪含量物质的量比为75%的铜钪中间合金;或:所述熔盐电解温度为1100℃,所述熔盐电解阴极电流密度为10 A/cm2,制备钪含量物质的量比为20%的铜钪中间合金;或:所述熔盐电解温度为1000℃,所述熔盐电解阴极电流密度为0.5A/cm2,制备钪含量物质的量比为10%的铜钪中间合金。1. a preparation method of copper-scandium master alloy, it is characterized in that: in the molten salt electrolyte containing scandium, take metal copper electrode as consumable cathode, take graphite as anode, prepare copper-scandium master alloy by molten salt electrolysis; Described molten salt electrolyte comprises by mass fraction: 20~70 parts of LiF, 5~60 parts of ScF 3 , 0~55 parts of MCl or/and MF, wherein M is one or more of alkali metal elements and alkaline earth metal elements The temperature of the molten salt electrolysis is 875°C, the cathode current density of the molten salt electrolysis is 40 A/cm 2 , and the copper-scandium master alloy with a scandium content material ratio of 75% is prepared; or: the molten salt electrolysis temperature is 1100 ℃, the cathode current density of the molten salt electrolysis is 10 A/cm 2 , and the copper-scandium master alloy with a scandium content material ratio of 20% is prepared; or: the molten salt electrolysis temperature is 1000 ℃, the molten salt The salt electrolysis cathode current density was 0.5A/cm 2 , and the copper-scandium master alloy was prepared with a scandium content-substance ratio of 10%. 2.如权利要求1所述的制备方法,其特征在于:在所述熔盐电解质中加入原料Sc2O3,Sc2O3的加入质量为熔盐质量的0~30%。2 . The preparation method according to claim 1 , wherein the raw material Sc 2 O 3 is added to the molten salt electrolyte, and the added mass of Sc 2 O 3 is 0-30% of the mass of the molten salt. 3 . 3.如权利要求1所述的制备方法,其特征在于:铜阴极下方放置盛接坩埚用以收集铜钪中间合金产物,所述盛接坩埚为钼坩埚、钨坩埚、钽坩埚或石墨坩埚。3. The preparation method as claimed in claim 1, characterized in that: a receiving crucible is placed below the copper cathode to collect the copper-scandium intermediate alloy product, and the receiving crucible is a molybdenum crucible, a tungsten crucible, a tantalum crucible or a graphite crucible. 4.权利要求1~3任一制备的铜钪中间合金用于制备其它金属的含钪合金。4. The copper-scandium master alloy prepared by any one of claims 1 to 3 is used to prepare the scandium-containing alloy of other metals.
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