CN108754203A - A kind of Alar fining agent of degeneration and its preparation method and application - Google Patents
A kind of Alar fining agent of degeneration and its preparation method and application Download PDFInfo
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Abstract
本发明公开了一种抗退化的铝硅系合金细化剂,及其制备方法和其作为铝硅系合金细化剂的应用,该细化剂是由铝、钒和硼三种元素所形成的中间合金,其中各成分的质量百分数为:铝20~99.8%,钒0.1~40%,硼0.1~40%。制备方法是由铝、钒、硼、铝钒合金、铝硼合金、硼盐和钒盐中的两种或三种成分经过熔炼和凝固制备而成。本发明制备的铝硅系合金细化剂在三个小时内不会出现退化现象,显著推迟了退化时间,可以在工业上应用,具有非常重要的理论意义和实际应用价值,尤其适用于硅含量大于4wt.%Si的铝硅系合金;本发明所述铝硅系合金细化剂制备方法,工艺简单,原料易于获取;本发明制备的铝硅系合金细化剂具有良好的细化效果。The invention discloses an anti-degeneration aluminum-silicon alloy refiner, its preparation method and its application as an aluminum-silicon alloy refiner. The refiner is formed of three elements: aluminum, vanadium and boron The master alloy, wherein the mass percentage of each component is: aluminum 20-99.8%, vanadium 0.1-40%, boron 0.1-40%. The preparation method is prepared by melting and solidifying two or three components of aluminum, vanadium, boron, aluminum vanadium alloy, aluminum boron alloy, boron salt and vanadium salt. The aluminum-silicon alloy refiner prepared by the present invention will not degenerate within three hours, significantly delaying the degeneration time, and can be applied in industry. It has very important theoretical significance and practical application value, especially suitable for silicon content An aluminum-silicon-based alloy with Si greater than 4wt.%; the preparation method of the aluminum-silicon-based alloy refiner of the invention has a simple process and easy access to raw materials; the aluminum-silicon-based alloy refiner prepared by the invention has a good refiner effect.
Description
技术领域technical field
本发明公开了一种抗退化的铝硅系合金细化剂及其制备方法和应用,属于合金细化剂技术领域。The invention discloses an anti-degeneration aluminum-silicon alloy refiner, a preparation method and application thereof, and belongs to the technical field of alloy refiners.
背景技术Background technique
晶粒细化是目前唯一一种既能保证强度增大,同时不会使塑性性能降低的强化方法。由于几乎所有金属的制备都要经历至少一次凝固过程,且凝固过程作为金属加工前端工序,对金属的组织和性能起非常重要的作用。经过研究发现,凝固细晶不仅能够提高力学性能,而且可以减少凝固缺陷。因此,在金属的凝固过程中实现晶粒细化具有重要的实际意义。在金属液中添加细化剂因为操作简单、细化效果显著等原因得到广泛的研究和关注,尤其在铝合金和镁合金中已经实现工业化应用。例如,Al-Ti-B晶粒细化剂已经在某些铝合金得到广泛应用。Grain refinement is currently the only strengthening method that can guarantee an increase in strength without reducing plastic properties. Since the preparation of almost all metals undergoes at least one solidification process, and the solidification process, as the front-end process of metal processing, plays a very important role in the structure and properties of metals. After research, it is found that solidification fine grain can not only improve the mechanical properties, but also reduce solidification defects. Therefore, it is of great practical significance to achieve grain refinement during the solidification of metals. Adding a refiner to molten metal has been extensively researched and paid attention to because of its simple operation and remarkable refinement effect, especially in aluminum alloys and magnesium alloys. For example, Al-Ti-B grain refiner has been widely used in some aluminum alloys.
铝硅系合金作为用量最大的铸造铝合金,由于密度小、易回收、具有良好的力学性能和物理化学性能等优点,现已广泛的应用于航天航空、汽车等领域,例如用于制造汽车轮毂、发动机活塞等。然而,对铝硅系合金,尤其对于硅含量高于4%的铝硅系合金,目前却没有非常有效的晶粒细化剂。传统上使用的Al-Ti-B细化剂在铸造铝硅系合金时会出现严重的退化现象,根本原因在于Al-Ti-B细化剂会和硅元素反应,导致加入的细化剂失去细化作用。随后,有人开发出Al-B、Al-Nb-B等细化剂。但是,通过实践发现,这些细化剂在熔体中超过1小时后都存在严重的退化现象。而一个细化剂要在工业中进行应用,一般要求其有效时间能在2小时以上。As the cast aluminum alloy with the largest amount, aluminum-silicon series alloy has been widely used in aerospace, automobile and other fields due to its low density, easy recycling, good mechanical properties and physical and chemical properties, such as for the manufacture of automobile hubs , Engine pistons, etc. However, there is currently no very effective grain refiner for Al-Si alloys, especially for Al-Si alloys with a silicon content higher than 4%. The traditionally used Al-Ti-B refiner will cause serious degradation when casting aluminum-silicon alloys. The root cause is that the Al-Ti-B refiner will react with silicon, resulting in the loss of the added refiner. refinement. Subsequently, refiners such as Al-B and Al-Nb-B were developed. However, it has been found through practice that these refiners are severely degraded after being in the melt for more than 1 hour. However, if a refiner is to be applied in industry, its effective time is generally required to be more than 2 hours.
发明内容Contents of the invention
发明目的:为解决上述技术问题,本发明的目的是提供一种抗退化的铝硅系合金细化剂及其制备方法和应用,所得细化剂能够显著提高铝硅系合金的综合性能。Purpose of the invention: In order to solve the above technical problems, the purpose of the present invention is to provide an anti-degeneration aluminum-silicon alloy refiner and its preparation method and application. The obtained refiner can significantly improve the comprehensive performance of the aluminum-silicon alloy.
技术方案:为达到上述目的,本发明采用以下技术方案:Technical solution: In order to achieve the above object, the present invention adopts the following technical solutions:
一种抗退化的铝硅系合金细化剂,其是由铝、钒和硼三种元素所形成的中间合金,其中各成分的重量百分数为:铝20~99.8%,钒0.1~40%,硼0.1~40%。An anti-degeneration aluminum-silicon alloy refiner, which is an intermediate alloy formed of three elements: aluminum, vanadium and boron, wherein the weight percentage of each component is: aluminum 20-99.8%, vanadium 0.1-40%, Boron 0.1-40%.
所述的抗退化的铝硅系合金细化剂的制备方法,该细化剂是由铝、钒、硼、铝钒合金、铝硼合金、硼盐和钒盐中的两种或三种成分经过熔炼和凝固制备而成。The preparation method of the anti-degeneration aluminum-silicon alloy refiner, the refiner is composed of two or three components of aluminum, vanadium, boron, aluminum-vanadium alloy, aluminum-boron alloy, boron salt and vanadium salt Prepared by smelting and solidification.
作为优选:As preferred:
所述铝为棒状、片状、块状或粒状工业纯铝;所述钒为99.9%的颗粒状工业纯钒,粒度为50~1000目;所述硼为99.9%的颗粒状工业纯硼,粒度为50~1000目;所述铝钒合金为棒状、块状、片状或颗粒状工业铝钒中间合金,可由铝热法、两步法、真空法、电铝热法、熔盐法等工业常用方法制得;所述铝硼合金为棒状、块状、片状或颗粒状工业铝硼中间合金,可由熔盐法等工业常用方法制得。The aluminum is rod-shaped, flake-shaped, massive or granular industrially pure aluminum; the vanadium is 99.9% granular industrially pure vanadium with a particle size of 50-1000 mesh; the boron is 99.9% granular industrially pure boron, The particle size is 50-1000 mesh; the aluminum-vanadium alloy is a rod-shaped, block-shaped, flake-shaped or granular industrial aluminum-vanadium master alloy, which can be produced by thermite method, two-step method, vacuum method, electric thermite method, molten salt method, etc. The aluminum-boron alloy is produced by a common industrial method; the aluminum-boron alloy is an industrial aluminum-boron master alloy in the form of a rod, a block, a sheet or a particle, and can be produced by a common industrial method such as a molten salt method.
所述硼盐可以选自氟硼酸钾,所述钒盐可以选自偏钒酸铵、氟铝酸钠、氟铝酸钾、五氧化二钒、三氧化二钒中的一种或多种混合。The boron salt can be selected from potassium fluoroborate, and the vanadium salt can be selected from one or more of ammonium metavanadate, sodium fluoroaluminate, potassium fluoroaluminate, vanadium pentoxide, and vanadium trioxide. .
所述铝硅系合金细化剂可由工业纯铝、纯钒和纯硼加热熔炼制成;也可由铝钒合金和工业纯硼加热熔炼制成;也可由铝硼合金和工业纯钒加热熔炼制成;也可由铝钒合金和铝硼合金加热熔炼制成;也可由工业纯铝、铝钒合金和铝硼合金加热熔炼制成;也可由铝钒合金和硼盐加热熔炼反应制成;也可由工业纯铝、铝钒合金和硼盐加热熔炼反应制成;也可由工业纯铝、铝硼合金和钒盐加热熔炼反应制成;也可由铝硼合金和钒盐加热熔炼制成;也可由工业纯铝、硼盐和钒盐加热熔炼制成;也可由工业纯铝、纯钒和硼盐加热熔炼制成;也可由工业纯铝、纯硼和钒盐加热熔炼制成。The aluminum-silicon alloy refining agent can be made by heating and melting industrial pure aluminum, pure vanadium and pure boron; it can also be made by heating and melting aluminum-vanadium alloy and industrial pure boron; it can also be made by heating and melting aluminum-boron alloy and industrial pure vanadium It can also be made by heating and melting aluminum vanadium alloy and aluminum boron alloy; it can also be made by heating and melting industrial pure aluminum, aluminum vanadium alloy and aluminum boron alloy; it can also be made by heating and melting reaction of aluminum vanadium alloy and boron salt; it can also be made by It can also be made by heating and melting reaction of industrial pure aluminum, aluminum-vanadium alloy and boron salt; it can also be made by heating and melting reaction of industrial pure aluminum, aluminum-boron alloy and vanadium salt; it can also be made by heating and melting of aluminum-boron alloy and vanadium salt; it can also be made by industrial It can be made by heating and melting pure aluminum, boron salt and vanadium salt; it can also be made by heating and melting industrial pure aluminum, pure vanadium and boron salt; it can also be made by heating and melting industrial pure aluminum, pure boron and vanadium salt.
所述的抗退化的铝硅系合金细化剂的制备方法,包括以下步骤:The preparation method of the anti-degeneration aluminum-silicon alloy refiner comprises the following steps:
(1)配料:按照质量比例,计算和称量所述原料;(1) Ingredients: calculate and weigh the raw materials according to the mass ratio;
(2)熔炼:将步骤(1)配好的原料一起加热保温,或者先后加入,在不同温度下加热保温;(2) Smelting: heat and keep the raw materials prepared in step (1) together, or add them successively, and heat and keep them at different temperatures;
(3)凝固:待步骤(2)熔炼得到的中间合金冷却至室温后,即得到一种抗退化的铝硅系合金细化剂。(3) Solidification: After the master alloy obtained by smelting in step (2) is cooled to room temperature, an anti-degeneration aluminum-silicon alloy refiner is obtained.
步骤(2)中所述加热的温度范围为600℃~3000℃,保温时间为0.1h~24h。The heating temperature range in step (2) is 600° C. to 3000° C., and the holding time is 0.1 h to 24 h.
优选,所述的抗退化的铝硅系合金细化剂的制备方法,包括以下步骤(第一种):Preferably, the preparation method of the anti-degeneration aluminum-silicon alloy refiner comprises the following steps (the first):
(1)配料:按照质量比例,计算和称量所述原料铝、钒和硼;(1) Batching: calculate and weigh the raw materials aluminum, vanadium and boron according to the mass ratio;
(2)熔炼:将步骤(1)配好的铝、钒、硼均匀混合,然后将混合均匀的原料包裹在铝箔中,在真空条件下进行熔炼,熔炼温度为1500℃到2000℃,反复翻样熔炼,然后随炉冷却。(2) Melting: Evenly mix the aluminum, vanadium, and boron prepared in step (1), then wrap the evenly mixed raw materials in aluminum foil, and smelt under vacuum conditions. The smelting temperature is 1500°C to 2000°C. It is melted and then cooled in the furnace.
(3)凝固:待步骤(2)熔炼得到的中间合金冷却至室温后,即得到一种抗退化的铝硅系合金细化剂。(3) Solidification: After the master alloy obtained by smelting in step (2) is cooled to room temperature, an anti-degeneration aluminum-silicon alloy refiner is obtained.
所述的抗退化的铝硅系合金细化剂的制备方法,包括以下步骤(第二种):The preparation method of the anti-degeneration aluminum-silicon alloy refiner comprises the following steps (the second):
(1)配料:按照质量比例,计算和称量所述原料铝钒合金和硼盐;(1) Batching: calculate and weigh the raw material aluminum-vanadium alloy and boron salt according to the mass ratio;
(2)熔炼:将步骤(1)中配好的铝钒合金进行加热处理,待温度升至700~900℃后保温1~2h,然后加入配好的硼盐,将温度升至1000~1200℃保温2~5小时,搅拌均匀;(2) Smelting: Heat the aluminum-vanadium alloy prepared in step (1), keep it warm for 1-2 hours after the temperature rises to 700-900°C, then add the prepared boron salt, and raise the temperature to 1000-1200°C Keep warm at ℃ for 2-5 hours and stir evenly;
(3)浇铸凝固:将步骤(2)熔炼得到的合金液浇铸为铸锭,冷却至室温后去除氧化皮,即得到一种抗退化的铝硅系合金细化剂。(3) Casting and solidification: casting the alloy liquid obtained in the step (2) into an ingot, and removing the oxide skin after cooling to room temperature to obtain an anti-degeneration aluminum-silicon alloy refiner.
所述的抗退化的铝硅系合金细化剂的制备方法,包括以下步骤(第三种):The preparation method of the anti-degeneration aluminum-silicon alloy refiner comprises the following steps (the third):
(1)配料:按照质量比例,计算和称量所述原料铝硼合金和钒盐;(1) Ingredients: calculate and weigh the raw material aluminum-boron alloy and vanadium salt according to the mass ratio;
(2)熔炼:将步骤(1)中配好的铝硼合金进行加热处理,待温度升至700~900℃后保温1~2h,然后加入配好的钒盐,将温度升至1000~1200℃保温2~5小时,搅拌均匀;(2) Smelting: Heat the aluminum-boron alloy prepared in step (1), keep it warm for 1-2 hours after the temperature rises to 700-900°C, then add the prepared vanadium salt, and raise the temperature to 1000-1200°C Keep warm at ℃ for 2-5 hours and stir evenly;
(3)浇铸凝固:将步骤(2)熔炼得到的合金液浇铸为铸锭,冷却至室温后去除氧化皮,即得到一种抗退化的铝硅系合金细化剂。(3) Casting and solidification: casting the alloy liquid obtained in the step (2) into an ingot, and removing the oxide skin after cooling to room temperature to obtain an anti-degeneration aluminum-silicon alloy refiner.
所述的抗退化的铝硅系合金细化剂的制备方法,包括以下步骤(第四种):The preparation method of the anti-degeneration aluminum-silicon alloy refiner comprises the following steps (the fourth):
(1)配料:按照质量比例,计算和称量所述原料铝钒合金和铝硼合金;(1) Ingredients: calculate and weigh the raw material aluminum-vanadium alloy and aluminum-boron alloy according to the mass ratio;
(2)熔炼:将步骤(1)中配好的铝钒合金和铝硼合金进行加热处理,待温度升至700~900℃后保温1~3h,搅拌均匀;(2) Smelting: heat-treat the aluminum-vanadium alloy and aluminum-boron alloy prepared in step (1), keep warm for 1-3 hours after the temperature rises to 700-900°C, and stir evenly;
(3)浇铸凝固:将步骤(2)熔炼得到的合金液浇铸为铸锭,冷却至室温后去除氧化皮,即得到一种抗退化的铝硅系合金细化剂。(3) Casting and solidification: casting the alloy liquid obtained in the step (2) into an ingot, and removing the oxide skin after cooling to room temperature to obtain an anti-degeneration aluminum-silicon alloy refiner.
所述的抗退化的铝硅系合金细化剂的制备方法,包括以下步骤(第五种):The preparation method of the anti-degeneration aluminum-silicon alloy refiner comprises the following steps (the fifth):
(1)配料:按照质量比例,计算和称量所述原料铝、硼盐和钒盐;(1) Batching: calculate and weigh the raw material aluminum, boron salt and vanadium salt according to the mass ratio;
(2)熔炼:将步骤(1)中配好的工业纯铝进行加热处理,待温度升至700~900℃后保温1~3h,然后加入配好的硼盐和钒盐,然后将炉温升至1000~1200℃保温2~5小时,搅拌均匀;(2) Smelting: Heat the industrial pure aluminum prepared in step (1), keep it warm for 1-3 hours after the temperature rises to 700-900°C, then add the prepared boron salt and vanadium salt, and then lower the furnace temperature Rise to 1000-1200°C and keep warm for 2-5 hours, stirring evenly;
(3)浇铸凝固:将步骤(2)熔炼得到的合金液浇铸为铸锭,冷却至室温后去除氧化皮,即得到一种抗退化的铝硅系合金细化剂。(3) Casting and solidification: casting the alloy liquid obtained in the step (2) into an ingot, and removing the oxide skin after cooling to room temperature to obtain an anti-degeneration aluminum-silicon alloy refiner.
上述五种制备方法的原料选择和制备过程,更具体地如下:The raw material selection and preparation process of above-mentioned five kinds of preparation methods, more specifically are as follows:
1、第一种制备方法的工艺步骤:1. The process steps of the first preparation method:
(1)配料(1) Ingredients
原料为工业纯铝、工业纯钒和工业纯硼,按照上述铝硅合金细化剂所述的铝、钒、硼的质量百分数,计算和称量所述原料;The raw materials are industrial pure aluminum, industrial pure vanadium and industrial pure boron, and the raw materials are calculated and weighed according to the mass percentages of aluminum, vanadium and boron described in the aluminum-silicon alloy refiner;
(2)熔炼(2) Melting
将步骤(1)配好的铝、钒、硼均匀混合,然后将混合均匀的原料包裹在铝箔中。然后将包装好的原料置于电弧熔炼炉的坩埚中,在真空条件下进行熔炼,熔炼温度为1500℃到2000℃。反复翻样熔炼3~5次,每次熔炼时间为5~10分钟。然后随炉冷却。The aluminum, vanadium and boron prepared in step (1) are uniformly mixed, and then the uniformly mixed raw materials are wrapped in aluminum foil. Then put the packaged raw materials in the crucible of the electric arc melting furnace, and melt them under vacuum condition at a melting temperature of 1500°C to 2000°C. Repeat the sample melting for 3 to 5 times, and the melting time for each time is 5 to 10 minutes. Then cool down with the furnace.
(3)凝固(3) Solidification
待步骤(2)熔炼得到的中间合金冷却至室温后,即得到一种抗退化的铝硅系合金细化剂。After the master alloy obtained by smelting in step (2) is cooled to room temperature, an anti-degeneration aluminum-silicon alloy refiner is obtained.
上述制备步骤中,所述用于制备铝硅系合金细化剂的铝为99.99%的片状工业纯铝。厚度为0.1~50mm,长为50~300mm,宽为50~300mm。优选厚度为1mm,长为150mm,宽为150mm。In the above preparation steps, the aluminum used to prepare the aluminum-silicon alloy refiner is 99.99% flaky industrial pure aluminum. The thickness is 0.1-50mm, the length is 50-300mm, and the width is 50-300mm. The preferred thickness is 1 mm, the length is 150 mm, and the width is 150 mm.
所述用于制备铝硅系合金细化剂的钒为99.9%的颗粒状工业纯钒。粒度为50~1000目,优选目数为300目。The vanadium used to prepare the aluminum-silicon alloy refiner is 99.9% granular industrial pure vanadium. The particle size is 50-1000 mesh, preferably 300 mesh.
所述用于制备铝硅系合金细化剂的硼为99.9%的颗粒状工业纯硼。粒度为50~1000目,优选目数为300目。The boron used to prepare the aluminum-silicon alloy refiner is 99.9% granular industrial pure boron. The particle size is 50-1000 mesh, preferably 300 mesh.
2、第二种制备方法的工艺步骤:2. The process steps of the second preparation method:
(1)配料(1) Ingredients
原料为铝钒合金和硼盐,按照上述铝硅合金细化剂所述的铝、钒、硼的质量百分数,计算和称量所述原料;The raw materials are aluminum-vanadium alloy and boron salt, and the raw materials are calculated and weighed according to the mass percentages of aluminum, vanadium and boron described in the above-mentioned aluminum-silicon alloy refiner;
(2)熔炼(2) Melting
将步骤(1)中配好的铝钒合金置于刚玉坩埚中,然后将刚玉坩埚放到热处理炉中加热,待炉温升至700~900℃后保温1~2h后加入配好的硼盐,然后将炉温升至1000~1200℃保温2~5小时,搅拌均匀。Put the aluminum-vanadium alloy prepared in step (1) in a corundum crucible, then put the corundum crucible in a heat treatment furnace to heat, wait for the temperature of the furnace to rise to 700-900°C, keep it warm for 1-2 hours, and then add the prepared boron salt , and then raise the temperature of the furnace to 1000-1200°C for 2-5 hours, and stir evenly.
(3)浇铸凝固(3) casting and solidification
将步骤(2)熔炼得到的合金液除渣后浇铸为铸锭,冷却至室温后去除氧化皮,即得到一种抗退化的铝硅系合金细化剂。Deslagging the alloy liquid obtained in step (2) and casting it into an ingot, and removing the scale after cooling to room temperature to obtain an anti-degeneration aluminum-silicon alloy refiner.
上述制备步骤中,所述用于制备铝硅系合金细化剂的铝钒合金为棒状、块状、片状或颗粒状的工业铝钒中间合金,可由铝热法、两步法、真空法、电铝热法、熔盐法等工业常用方法制得。In the above preparation steps, the aluminum-vanadium alloy used to prepare the aluminum-silicon alloy refiner is a rod-shaped, block-shaped, flake-shaped or granular industrial aluminum-vanadium master alloy, which can be prepared by the aluminothermic method, two-step method, or vacuum method. , Electric thermite method, molten salt method and other common industrial methods.
所述用于制备铝硅系合金细化剂的硼盐优选为氟硼酸钾。The boron salt used to prepare the aluminum-silicon alloy refiner is preferably potassium fluoroborate.
3、第三种制备方法的工艺步骤:3. The process steps of the third preparation method:
(1)配料(1) Ingredients
原料为铝硼合金和钒盐,按照上述铝硅系合金细化剂所述的铝、钒、硼的质量百分数,计算和称量所述原料;The raw materials are aluminum-boron alloy and vanadium salt, and the raw materials are calculated and weighed according to the mass percentages of aluminum, vanadium and boron described in the above-mentioned aluminum-silicon alloy refiner;
(2)熔炼(2) Melting
将步骤(1)中配好的铝硼合金置于刚玉坩埚中,然后将刚玉坩埚放到热处理炉中加热,待炉温度升至700~900℃后保温1~2h,然后加入配好的钒盐,将温度升至1000~1200℃保温2~5小时,搅拌均匀;Put the aluminum-boron alloy prepared in step (1) into a corundum crucible, then put the corundum crucible into a heat treatment furnace to heat, wait for the temperature of the furnace to rise to 700-900°C, keep it warm for 1-2 hours, and then add the prepared vanadium salt, raise the temperature to 1000-1200°C for 2-5 hours, and stir evenly;
(3)浇铸凝固(3) casting and solidification
将步骤(2)熔炼得到的合金液除渣后浇铸为铸锭,冷却至室温后去除氧化皮,即得到一种抗退化的铝硅系合金细化剂。Deslagging the alloy liquid obtained in step (2) and casting it into an ingot, and removing the scale after cooling to room temperature to obtain an anti-degeneration aluminum-silicon alloy refiner.
上述制备步骤中,所述用于制备铝硅合金细化剂的铝硼合金为棒状、块状、片状或颗粒状的工业铝硼中间合金。In the above preparation steps, the aluminum-boron alloy used to prepare the aluminum-silicon alloy refiner is an industrial aluminum-boron master alloy in the form of rods, blocks, flakes or granules.
所述用于制备铝硅系合金细化剂的钒盐可选自偏钒酸铵、氟铝酸钠、氟铝酸钾、五氧化二钒和三氧化二钒的一种或多种混合,优选为偏钒酸铵。The vanadium salt used to prepare the aluminum-silicon alloy refiner can be selected from one or more mixtures of ammonium metavanadate, sodium fluoroaluminate, potassium fluoroaluminate, vanadium pentoxide and vanadium trioxide, Ammonium metavanadate is preferred.
4、第四种制备方法的工艺步骤:4. The process steps of the fourth preparation method:
(1)配料(1) Ingredients
原料为铝钒合金和铝硼合金,按照上述铝硅合金细化剂所述的铝、钒、硼的质量百分数,计算和称量所述原料;The raw materials are aluminum-vanadium alloy and aluminum-boron alloy, and the raw materials are calculated and weighed according to the mass percentages of aluminum, vanadium and boron described in the above-mentioned aluminum-silicon alloy refiner;
(2)熔炼(2) Melting
将步骤(1)中配好的铝硼合金和铝钒合金置于刚玉坩埚中,然后将刚玉坩埚放到热处理炉中加热,待炉温度升至700~900℃后保温1~3h,搅拌均匀;Put the aluminum-boron alloy and aluminum-vanadium alloy prepared in step (1) in a corundum crucible, then put the corundum crucible into a heat treatment furnace for heating, and keep it warm for 1-3 hours after the furnace temperature rises to 700-900°C, and stir evenly ;
(3)浇铸凝固(3) casting and solidification
将步骤(2)熔炼得到的合金液除渣后浇铸为铸锭,冷却至室温后去除氧化皮,即得到一种抗退化的铝硅系合金细化剂。Deslagging the alloy liquid obtained in step (2) and casting it into an ingot, and removing the scale after cooling to room temperature to obtain an anti-degeneration aluminum-silicon alloy refiner.
上述制备步骤中,所述用于制备铝硅系合金细化剂的铝硼合金为棒状、块状、片状或颗粒状的工业铝硼中间合金。In the above preparation steps, the aluminum-boron alloy used to prepare the aluminum-silicon alloy refiner is an industrial aluminum-boron master alloy in the form of rods, blocks, flakes or granules.
所述用于制备铝硅系合金细化剂的铝钒合金为棒状、块状、片状或颗粒状的工业铝钒中间合金,可由铝热法、两步法、真空法、电铝热法、熔盐法等工业常用方法制得。The aluminum-vanadium alloy used to prepare the aluminum-silicon alloy refiner is a rod-shaped, block-shaped, flake-shaped or granular industrial aluminum-vanadium master alloy, which can be prepared by the aluminothermic method, two-step method, vacuum method, electric aluminothermic method , Molten salt method and other common industrial methods.
5、第五种制备方法的工艺步骤:5. Process steps of the fifth preparation method:
(1)配料(1) Ingredients
原料为工业纯铝、硼盐和钒盐,按照上述铝硅合金细化剂所述的铝、钒、硼的重质量百分数,计算和称量所述原料;The raw materials are industrial pure aluminum, boron salt and vanadium salt, and the raw materials are calculated and weighed according to the weight percentages of aluminum, vanadium and boron described in the above-mentioned aluminum-silicon alloy refiner;
(2)熔炼(2) Melting
将步骤(1)中配好的工业纯铝置于刚玉坩埚中,待温度升至700~900℃后保温1~3h,然后加入配好的硼盐和钒盐,然后将炉温升至1000~1200℃保温2~5小时,搅拌均匀;Put the industrially pure aluminum prepared in step (1) in a corundum crucible, keep it warm for 1-3 hours after the temperature rises to 700-900°C, then add the prepared boron salt and vanadium salt, and then raise the furnace temperature to 1000 ~1200℃ heat preservation for 2~5 hours, stirring evenly;
(3)浇铸凝固(3) casting and solidification
将步骤(2)熔炼得到的合金液除渣后浇铸为铸锭,冷却至室温后去除氧化皮,即得到一种抗退化的铝硅系合金细化剂。Deslagging the alloy liquid obtained in step (2) and casting it into an ingot, and removing the scale after cooling to room temperature to obtain an anti-degeneration aluminum-silicon alloy refiner.
上述制备步骤中,所述用于制备铝硅系合金细化剂的工业纯铝为棒状、块状、片状或颗粒状。In the above preparation steps, the industrially pure aluminum used to prepare the aluminum-silicon alloy refiner is in the form of rods, blocks, flakes or granules.
所述用于制备铝硅系合金细化剂的硼盐优选为氟硼酸钾。The boron salt used to prepare the aluminum-silicon alloy refiner is preferably potassium fluoroborate.
所述用于制备铝硅合金细化剂的钒盐可选自偏钒酸铵、氟铝酸钠、氟铝酸钾、五氧化二钒和三氧化二钒中的一种或多种混合,优选为偏钒酸铵。The vanadium salt used to prepare the aluminum-silicon alloy refiner can be selected from one or more mixtures of ammonium metavanadate, sodium fluoroaluminate, potassium fluoroaluminate, vanadium pentoxide and vanadium trioxide, Ammonium metavanadate is preferred.
所述的细化剂(可称作Al-V-B细化剂)作为铝硅系合金细化剂的应用,可用于细化铝硅系合金铸锭、铸件等The application of the refiner (may be referred to as Al-V-B refiner) as an aluminum-silicon alloy refiner can be used to refine aluminum-silicon alloy ingots, castings, etc.
应用时,所述细化剂可以在成品铝硅系合金熔化后加入,或者也可以在铝硅系合金的制备过程中加入。In application, the refiner can be added after the finished aluminum-silicon alloy is melted, or can also be added during the preparation of the aluminum-silicon alloy.
所述加入的方法为:将制备的细化剂以成品形式加入,或者以原料形式加入。The adding method is: adding the prepared refining agent in the form of finished product or in the form of raw material.
钒在所述铝硅系合金中的含量控制在10~2000ppm,硼在所述铝硅系合金中的含量控制在在10~2000ppm。The content of vanadium in the aluminum-silicon alloy is controlled at 10-2000 ppm, and the content of boron in the aluminum-silicon alloy is controlled at 10-2000 ppm.
优选地,应用方法包括以下四种:Preferably, the application methods include the following four types:
第一种应用方法,包括以下步骤:The first application method includes the following steps:
(1)配料:按质量比例取工业纯铝、工业纯硅和所述铝硅系合金细化剂,其中工业纯硅:1%~25%,铝硅系合金细化剂:0.001%~5%,余量为工业纯铝;(1) Ingredients: take industrial pure aluminum, industrial pure silicon and the aluminum-silicon alloy refiner according to the mass ratio, wherein industrial pure silicon: 1% to 25%, aluminum-silicon alloy refiner: 0.001% to 5% %, the balance is industrial pure aluminum;
(2)熔炼:将配置好的纯铝加热,待温度升至700~800℃后保温0.5~1小时,接着加入配置好的工业纯硅,700~800℃保温1~2小时,最后加入所述铝硅系合金细化剂,保温1~4小时;(2) Smelting: heat the prepared pure aluminum, keep it warm for 0.5-1 hour after the temperature rises to 700-800°C, then add the prepared industrial pure silicon, keep it at 700-800°C for 1-2 hours, and finally add the Aluminum-silicon alloy refiner, heat preservation for 1 to 4 hours;
(3)浇铸凝固:将步骤(2)得到的合金液浇铸为铸锭,冷却至室温即可得到铝硅系合金细化后的铸锭。(3) Casting and solidification: casting the alloy liquid obtained in step (2) into an ingot, and cooling to room temperature to obtain a refined ingot of the aluminum-silicon alloy.
第二种应用方法,包括以下步骤:The second application method includes the following steps:
(1)配料:按质量比例取已经配置好的铝硅系合金和所述铝硅系合金细化剂,其中铝硅系合金百分含量为:90%~99.999%,铝硅系合金细化剂百分含量为:0.001%~10%;(1) Ingredients: take the prepared aluminum-silicon alloy and the aluminum-silicon alloy refiner according to the mass ratio, wherein the percentage content of the aluminum-silicon alloy is: 90% to 99.999%, and the aluminum-silicon alloy refiner The percentage content of the agent is: 0.001% ~ 10%;
(2)熔炼:将工业铝硅系合金加热,待温度升至700~800℃后保温0.5~1小时,接着加入所述铝硅系合金细化剂,保温1~4小时;(2) Melting: heat the industrial aluminum-silicon alloy, and keep it warm for 0.5-1 hour after the temperature rises to 700-800°C, then add the aluminum-silicon alloy refiner and keep it warm for 1-4 hours;
(3)浇铸凝固:将步骤(2)得到的合金液浇铸或压铸为铸件,冷却至室温即可得到铝硅系合金细化后的铸件。(3) Casting and solidification: casting or die-casting the alloy solution obtained in step (2) into a casting, and cooling to room temperature to obtain a refined aluminum-silicon alloy casting.
第三种应用方法,包括以下步骤:The third application method includes the following steps:
(1)配料:按质量比例取工业纯铝、工业纯硅、铝钒合金和铝硼合金,其中工业纯硅:1%~25%,铝钒合金:0.001%~5%,铝硼合金:0.001%~5%,余量为工业纯铝;(1) Ingredients: Industrial pure aluminum, industrial pure silicon, aluminum vanadium alloy and aluminum boron alloy are taken according to the mass ratio, of which industrial pure silicon: 1% ~ 25%, aluminum vanadium alloy: 0.001% ~ 5%, aluminum boron alloy: 0.001%~5%, the balance is industrial pure aluminum;
(2)熔炼:将配置好的纯铝加热,待温度升至700~800℃后保温0.5~1小时,接着加入配置好的工业纯硅,700~800℃保温1~2小时,最后加入所述一定比例的铝钒合金和铝硼合金,保温1~4小时;(2) Smelting: heat the prepared pure aluminum, keep it warm for 0.5-1 hour after the temperature rises to 700-800°C, then add the prepared industrial pure silicon, keep it at 700-800°C for 1-2 hours, and finally add the A certain proportion of aluminum-vanadium alloy and aluminum-boron alloy, heat preservation for 1 to 4 hours;
(3)浇铸凝固:将步骤(2)得到的合金液浇铸或压铸为铸件,冷却至室温即可得到铝硅系合金细化后的铸件。(3) Casting and solidification: casting or die-casting the alloy solution obtained in step (2) into a casting, and cooling to room temperature to obtain a refined aluminum-silicon alloy casting.
第四种应用方法,包括以下步骤:The fourth application method includes the following steps:
(1)配料:按质量比例取工业纯铝、工业纯硅、所述铝硅系合金细化剂,其中工业纯硅:1%~25%,铝钒硼合金细化剂:0.001%~5%,余量为工业纯铝;(1) Ingredients: take industrial pure aluminum, industrial pure silicon, and the aluminum-silicon alloy refiner according to the mass ratio, wherein industrial pure silicon: 1% to 25%, aluminum vanadium boron alloy refiner: 0.001% to 5% %, the balance is industrial pure aluminum;
(2)熔炼:将配置好的纯铝加热,待温度升至700~800℃后保温0.5~1小时,接着加入所述一定比例的铝硅系合金细化剂,700~800℃保温1~2小时,最后加入配置好的工业纯硅,保温1~4小时;(2) Smelting: heat the prepared pure aluminum, keep it warm for 0.5-1 hour after the temperature rises to 700-800°C, then add a certain proportion of the aluminum-silicon alloy refiner, keep it at 700-800°C for 1-2 hours 2 hours, finally add the prepared industrial pure silicon, keep warm for 1 to 4 hours;
(3)浇铸凝固:将步骤(2)得到的合金液浇铸或压铸为铸件,冷却至室温即可得到铝硅系合金细化后的铸件。(3) Casting and solidification: casting or die-casting the alloy solution obtained in step (2) into a casting, and cooling to room temperature to obtain a refined aluminum-silicon alloy casting.
上述四种应用方法的原料选择和制备过程,更具体地如下:The raw material selection and preparation process of the above four application methods are more specifically as follows:
1、第一种应用方法:1. The first application method:
(1)配料(1) Ingredients
原料为工业纯铝、工业纯硅和配置好的Al-V-B细化剂,按照一定比例计算和称量所述原料,其中工业纯硅:1%~25%,Al-V-B细化剂:0.001%~5%,余量为工业纯铝。The raw materials are industrial pure aluminum, industrial pure silicon and prepared Al-V-B refiner, and the raw materials are calculated and weighed according to a certain ratio, among which industrial pure silicon: 1% to 25%, Al-V-B refiner: 0.001 % to 5%, and the balance is industrial pure aluminum.
(2)熔炼(2) Melting
将配置好的纯铝置于坩埚中,然后将坩埚置于马弗炉中加热,待炉内温度升至700~800℃后保温0.5~1小时,接着将配置好的工业纯硅加入坩埚中,700~800℃小保温1~2小时,最后将一定比例的细化剂加入坩埚中保温1~4小时。Put the prepared pure aluminum in the crucible, then place the crucible in a muffle furnace to heat, wait for the temperature in the furnace to rise to 700-800°C and keep it warm for 0.5-1 hour, then add the prepared industrial pure silicon into the crucible , 700 ~ 800 ℃ small heat preservation for 1 to 2 hours, and finally add a certain proportion of refiner into the crucible heat preservation for 1 to 4 hours.
(3)浇铸凝固(3) casting and solidification
将步骤(2)得到的合金液浇铸为铸锭,冷却至室温即可得到铝硅系合金细化后的铸锭。The alloy liquid obtained in step (2) is cast into an ingot, and cooled to room temperature to obtain an aluminum-silicon alloy refined ingot.
上述步骤中,所述用于制备铝硅系合金的铝为棒状、块状、片状或粒状的工业纯铝。In the above steps, the aluminum used to prepare the aluminum-silicon alloy is industrially pure aluminum in the form of rods, blocks, flakes or granules.
所述用于制备铝硅系合金的硅为工业纯硅。The silicon used to prepare the aluminum-silicon alloy is industrial pure silicon.
所述用于制备铝硅系合金的钒源和硼源为上述含钒、硼的Al-V-B细化剂。The vanadium source and boron source used to prepare the aluminum-silicon alloy are the above-mentioned Al-V-B refiner containing vanadium and boron.
所述用于盛装合金液的坩埚为石墨坩埚或刚玉坩埚。The crucible for containing the alloy liquid is a graphite crucible or a corundum crucible.
最终所得铝硅系合金各成分百分含量控制为:硅:1%~25%,钒:0.001%~0.2%(10~2000ppm),硼:0.001%~0.2%(10~2000ppm)。The percentage content of each component of the finally obtained aluminum-silicon alloy is controlled as follows: silicon: 1%-25%, vanadium: 0.001%-0.2% (10-2000ppm), boron: 0.001%-0.2% (10-2000ppm).
2、第二种应用方法:2. The second application method:
(1)配料(1) Ingredients
原料为已经配置好工业铝硅系合金、Al-V-B细化剂,按照一定比例计算和称量所述原料,其中铝硅合金百分含量为:90%~99.999%,Al-V-B细化剂百分含量为:0.001%~10%。The raw materials are prepared industrial aluminum-silicon alloys and Al-V-B refiner, and the raw materials are calculated and weighed according to a certain ratio. The percentage content is: 0.001% to 10%.
(2)熔炼(2) Melting
将配置好的铝硅系合金置于坩埚中,然后将坩埚置于马弗炉中加热,待炉内温度升至700~800℃后保温0.5~1小时,接着一定比例的Al-V-B细化剂加入坩埚中保温1~4小时。Put the prepared aluminum-silicon alloy in the crucible, and then place the crucible in the muffle furnace to heat it. After the temperature in the furnace rises to 700-800°C, keep it warm for 0.5-1 hour, and then refine it with a certain proportion of Al-V-B Add the agent to the crucible and keep it warm for 1 to 4 hours.
(3)浇铸凝固(3) casting and solidification
将步骤(2)得到的合金液浇铸或压铸为铸件,冷却至室温即可得到铝硅系合金细化后的铸件。Casting or die-casting the alloy solution obtained in step (2) into a casting, and cooling to room temperature to obtain a refined aluminum-silicon alloy casting.
上述步骤中,所述用工业铝硅系合金为棒状、块状、片状或粒状。In the above steps, the industrial aluminum-silicon alloy is in the shape of rods, blocks, flakes or granules.
所述用于制备铝硅系合金的钒源和硼源为上述含钒、硼的Al-V-B细化剂。The vanadium source and boron source used to prepare the aluminum-silicon alloy are the above-mentioned Al-V-B refiner containing vanadium and boron.
所述用于盛装合金液的坩埚为石墨坩埚或刚玉坩埚。The crucible for containing the alloy liquid is a graphite crucible or a corundum crucible.
最终所得铝硅系合金各成分百分含量控制为:硅:1%~25%,钒:0.001%~0.2%(10~2000ppm),硼:0.001%~0.2%(10~2000ppm)。The percentage content of each component of the finally obtained aluminum-silicon alloy is controlled as follows: silicon: 1%-25%, vanadium: 0.001%-0.2% (10-2000ppm), boron: 0.001%-0.2% (10-2000ppm).
3、第三种应用方法:3. The third application method:
(1)配料(1) Ingredients
原料为工业纯铝、工业纯硅、铝钒合金和铝硼合金,按照一定比例计算和称量所述原料,其中工业纯硅:1%~25%,铝钒合金:0.001%~5%,铝硼合金:0.001%~5%,余量为工业纯铝。The raw materials are industrial pure aluminum, industrial pure silicon, aluminum-vanadium alloy and aluminum-boron alloy. The raw materials are calculated and weighed according to a certain ratio, of which industrial pure silicon: 1%-25%, aluminum-vanadium alloy: 0.001%-5%, Aluminum-boron alloy: 0.001% to 5%, and the balance is industrial pure aluminum.
(2)熔炼(2) Melting
将配置好的纯铝置于坩埚中,然后将坩埚置于马弗炉中加热,待炉内温度升至700~800℃后保温0.5~1小时,接着将配置好的工业纯硅加入坩埚中,700~800℃小保温1~2小时,最后将一定比例的铝钒合金和铝硼合金同时加入坩埚中保温1~4小时。Put the prepared pure aluminum in the crucible, then place the crucible in a muffle furnace to heat, wait for the temperature in the furnace to rise to 700-800°C and keep it warm for 0.5-1 hour, then add the prepared industrial pure silicon into the crucible , 700-800 ℃ small heat preservation for 1-2 hours, and finally a certain proportion of aluminum-vanadium alloy and aluminum-boron alloy are added to the crucible at the same time and heat preservation for 1-4 hours.
(3)浇铸凝固(3) casting and solidification
将步骤(2)得到的合金液浇铸或压铸为铸件,冷却至室温即可得到铝硅系合金细化后的铸件。Casting or die-casting the alloy solution obtained in step (2) into a casting, and cooling to room temperature to obtain a refined aluminum-silicon alloy casting.
上述步骤中,所述用于制备铝硅系合金的铝为棒状、块状、片状或粒状的工业纯铝。In the above steps, the aluminum used to prepare the aluminum-silicon alloy is industrially pure aluminum in the form of rods, blocks, flakes or granules.
所述用于制备铝硅系合金的硅为工业纯硅。The silicon used to prepare the aluminum-silicon alloy is industrial pure silicon.
所述用于盛装合金液的坩埚为石墨坩埚或刚玉坩埚。The crucible for containing the alloy liquid is a graphite crucible or a corundum crucible.
最终所得铝硅系合金各成分百分含量控制为:硅:1%~25%,钒:0.001%~0.2%The percentage content of each component of the final aluminum-silicon alloy is controlled as follows: silicon: 1% to 25%, vanadium: 0.001% to 0.2%
(10~2000ppm),硼:0.001%~0.2%(10~2000ppm)。(10-2000ppm), boron: 0.001%-0.2% (10-2000ppm).
4、第四种应用方法:4. The fourth application method:
(1)配料(1) Ingredients
原料为工业纯铝、工业纯硅和配置好的Al-V-B细化剂,按照一定比例计算和称量所述原料,其中工业纯硅:1%~25%,Al-V-B细化剂:0.001%~5%,余量为工业纯铝。The raw materials are industrial pure aluminum, industrial pure silicon and prepared Al-V-B refiner, and the raw materials are calculated and weighed according to a certain ratio, among which industrial pure silicon: 1% to 25%, Al-V-B refiner: 0.001 % to 5%, and the balance is industrial pure aluminum.
(2)熔炼(2) Melting
将配置好的纯铝置于坩埚中,然后将坩埚置于马弗炉中加热,待炉内温度升至700~800℃后保温0.5~1小时,接着将一定比例的细化剂加入坩埚中,700~800℃小保温1~2小时,最后将配置好的工业纯硅加入坩埚中保温1~4小时。Put the prepared pure aluminum in the crucible, then place the crucible in a muffle furnace to heat, wait for the temperature in the furnace to rise to 700-800°C and keep it warm for 0.5-1 hour, then add a certain proportion of refiner into the crucible , 700 ~ 800 ℃ small heat preservation for 1 to 2 hours, and finally put the prepared industrial pure silicon into the crucible and heat preservation for 1 to 4 hours.
(3)浇铸凝固(3) casting and solidification
将步骤(2)得到的合金液浇铸为铸锭,冷却至室温即可得到铝硅系合金细化后的铸锭。The alloy liquid obtained in step (2) is cast into an ingot, and cooled to room temperature to obtain an aluminum-silicon alloy refined ingot.
上述步骤中,所述用于制备铝硅系合金的铝为棒状、块状、片状或粒状的工业纯铝。In the above steps, the aluminum used to prepare the aluminum-silicon alloy is industrially pure aluminum in the form of rods, blocks, flakes or granules.
所述用于制备铝硅系合金的硅为工业纯硅。The silicon used to prepare the aluminum-silicon alloy is industrial pure silicon.
所述用于制备铝硅系合金的钒源和硼源为上述含钒、硼的Al-V-B细化剂。The vanadium source and boron source used to prepare the aluminum-silicon alloy are the above-mentioned Al-V-B refiner containing vanadium and boron.
所述用于盛装合金液的坩埚为石墨坩埚或刚玉坩埚。The crucible for containing the alloy liquid is a graphite crucible or a corundum crucible.
最终所得铝硅系合金各成分百分含量控制为:硅:1%~25%,钒:0.001%~0.2%(10~2000ppm),硼:0.001%~0.2%(10~2000ppm)。The percentage content of each component of the finally obtained aluminum-silicon alloy is controlled as follows: silicon: 1%-25%, vanadium: 0.001%-0.2% (10-2000ppm), boron: 0.001%-0.2% (10-2000ppm).
技术效果:相对于现有技术,本发明具有以下技术优势:Technical effect: Compared with the prior art, the present invention has the following technical advantages:
(1)相较于其他铝硅合金细化剂一个小时内就会出现退化现象,本发明制备的铝硅合金细化剂在三个小时内不会出现退化现象(见图2),显著推迟了退化时间,可以在工业上应用,具有非常重要的理论意义和实际应用价值,尤其适用于硅含量大于4wt.%Si的铝硅系合金;(1) Compared with other aluminum-silicon alloy refiners, degradation will occur within one hour, the aluminum-silicon alloy refiner prepared by the present invention will not degrade within three hours (see Figure 2), significantly delaying It can be applied in industry and has very important theoretical significance and practical application value, especially suitable for aluminum-silicon alloys with a silicon content greater than 4wt.% Si;
(2)本发明所述铝硅系合金细化剂制备方法,工艺简单,原料易于获取;(2) The preparation method of the aluminum-silicon alloy refiner of the present invention has a simple process and easy access to raw materials;
(3)本发明制备的铝硅系合金细化剂具有良好的细化效果。(3) The aluminum-silicon alloy refiner prepared by the present invention has a good refinement effect.
附图说明Description of drawings
图1是不加细化剂的Al-7wt.%Si合金凝固组织的宏观腐蚀图片。Figure 1 is a macroscopic corrosion picture of the solidified structure of Al-7wt.% Si alloy without refiner.
图2是加入本发明Al-V-B细化剂保温1小时的Al-7wt.%Si合金凝固组织的宏观腐蚀图片。Fig. 2 is a macroscopic corrosion picture of the Al-7wt.% Si alloy solidified structure added with the Al-V-B refiner of the present invention and kept for 1 hour.
图3是加入本发明Al-V-B细化剂保温3小时的Al-7wt.%Si合金凝固组织的宏观腐蚀图片。Fig. 3 is a macroscopic corrosion picture of the Al-7wt.% Si alloy solidified structure added with the Al-V-B refiner of the present invention and kept for 3 hours.
具体实施方式Detailed ways
下面结合具体实施方式对本发明进行详细描述,所述的实施例有助于对本发明的理解和实施,并非构成对本发明的限制。The present invention will be described in detail below in conjunction with specific embodiments, and the described embodiments are helpful to the understanding and implementation of the present invention, but are not intended to limit the present invention.
实施例1Example 1
(1)一种用于铝硅合金的Al-V-B细化剂,以99.99%的工业纯铝、99.9%的工业纯钒和99.9%的工业纯硼为原料制备而成,其中纯钒的重量百分数为2%,纯硼的重量百分数为2%,余量为工业纯铝。首先,按照上述铝硅系合金细化剂所述的铝、钒、硼的重量百分数计算和称量所述原料。接着将配好的铝、钒、硼均匀混合,然后将混合均匀的原料包裹在铝箔中。然后将混合包装好的原料置于电弧熔炼炉的坩埚中,在真空条件下进行熔炼,熔炼温度为1800℃。反复翻样熔炼3次,每次熔炼时间为5分钟。熔炼的Al-2%V-2%B合金冷却后取出放入刚玉坩埚中,将刚玉坩埚置于电阻炉中加热熔炼。当电阻炉温度升至800℃时保温两小时,将电阻炉温度升温至900℃,再保温两小时。最后,取出刚玉坩埚,置于空气中冷却至室温。取出刚玉坩埚中的Al-2%V-2%B合金,去除表面氧化皮,铝硅系合金细化剂制备完成。(1) An Al-V-B refiner for aluminum-silicon alloy, prepared from 99.99% industrial pure aluminum, 99.9% industrial pure vanadium and 99.9% industrial pure boron, wherein the weight of pure vanadium The percentage is 2%, the percentage by weight of pure boron is 2%, and the balance is industrial pure aluminum. First, calculate and weigh the raw materials according to the weight percentages of aluminum, vanadium and boron described in the aluminum-silicon alloy refiner. Next, the prepared aluminum, vanadium and boron are evenly mixed, and then the evenly mixed raw materials are wrapped in aluminum foil. Then the mixed and packaged raw materials are placed in the crucible of the arc melting furnace, and melted under vacuum conditions at a melting temperature of 1800°C. The sample was repeatedly smelted 3 times, and the smelting time was 5 minutes each time. After the melted Al-2%V-2%B alloy is cooled, it is taken out and put into a corundum crucible, and the corundum crucible is placed in a resistance furnace for heating and melting. When the temperature of the resistance furnace rises to 800°C, it is kept warm for two hours, and the temperature of the resistance furnace is raised to 900°C, and then kept for two hours. Finally, the corundum crucible was taken out and cooled to room temperature in air. Take out the Al-2%V-2%B alloy in the corundum crucible, remove the surface scale, and prepare the aluminum-silicon alloy refiner.
(2)、取出编号为1、2的两个刚玉坩埚放置于干燥箱中干燥一个小时后,将两个刚玉坩埚置于电阻炉中,分别向两个刚玉坩埚中加入184g纯度为99.9%工业纯铝,加热到800℃保温一个小时后,然后分别向两个刚玉坩埚中加入纯度为99.9999%的工业纯硅14g,接着再保温一个小时后,向2号刚玉坩埚中加入上述制备好的Al-2%V-2%B细化剂2g,再800℃保温一个小时后,取出两个刚玉坩埚,置于空气中冷却至室温。(2) Take out two corundum crucibles numbered 1 and 2 and place them in a drying oven for one hour to dry, then place the two corundum crucibles in a resistance furnace, and add 184g of industrial corundum with a purity of 99.9% to the two corundum crucibles respectively. For pure aluminum, heat it to 800°C for one hour, then add 14g of industrial pure silicon with a purity of 99.9999% to two corundum crucibles, and then add the above-prepared Al to No. 2 corundum crucible after another hour -2% V-2% B refiner 2g, after another hour of heat preservation at 800°C, take out two corundum crucibles and place them in air to cool to room temperature.
(3)待试样凝固后,对试样进行切割、打磨、腐蚀、拍照,试样1结果参见图1,试样2结果参见图2。由此可见加入Al-V-B细化剂的铝硅合金凝固组织有着明显的差别,后者的凝固组织更加的细小。使用IPP软件统计后发现,不加入细化剂的试样1的晶粒尺寸为3200μm,加入Al-V-B铝硅合金细化剂的试样2晶粒尺寸为450μm,细化效果得到显著提高。(3) After the sample is solidified, cut, polish, corrode, and take pictures of the sample. The results of sample 1 are shown in Figure 1, and the results of sample 2 are shown in Figure 2. It can be seen that the solidification structure of the aluminum-silicon alloy added with the Al-V-B refiner has obvious differences, and the solidification structure of the latter is finer. After statistics using IPP software, it is found that the grain size of sample 1 without adding refiner is 3200 μm, and the grain size of sample 2 with Al-V-B aluminum-silicon alloy refiner is 450 μm, and the refinement effect is significantly improved.
实施例2Example 2
(1)配料(1) Ingredients
原料为工业纯铝、工业纯钒和工业纯硼,按照铝硅合金细化剂所述的铝、钒、硼的质量百分数,计算和称量所述原料,其中铝20%,钒40%,硼40%;The raw materials are industrial pure aluminum, industrial pure vanadium and industrial pure boron. According to the mass percentages of aluminum, vanadium and boron described in the aluminum-silicon alloy refiner, the raw materials are calculated and weighed, wherein aluminum is 20%, vanadium is 40%, Boron 40%;
(2)熔炼(2) Melting
将步骤(1)配好的铝、钒、硼均匀混合,然后将混合均匀的原料包裹在铝箔中。然后将包装好的原料置于电弧熔炼炉的坩埚中,在真空条件下进行熔炼,熔炼温度为1800℃。反复翻样熔炼3次,每次熔炼时间为5分钟。然后随炉冷却。The aluminum, vanadium and boron prepared in step (1) are uniformly mixed, and then the uniformly mixed raw materials are wrapped in aluminum foil. Then put the packaged raw materials in the crucible of the electric arc melting furnace, and melt them under vacuum conditions at a melting temperature of 1800°C. The sample was repeatedly smelted 3 times, and the smelting time was 5 minutes each time. Then cool down with the furnace.
(3)凝固(3) Solidification
待步骤(2)熔炼得到的中间合金冷却至室温后去掉表面的氧化皮,即得到一种抗退化的铝硅系合金细化剂。After the master alloy obtained in the step (2) is cooled to room temperature, the oxide skin on the surface is removed, and an anti-degeneration aluminum-silicon alloy refiner is obtained.
上述制备步骤中,所述用于制备铝硅系合金细化剂的铝为99.99%的片状工业纯铝,厚度为0.3mm,长为150mm,宽为150mm。In the above preparation steps, the aluminum used to prepare the aluminum-silicon alloy refiner is 99.99% flaky industrial pure aluminum with a thickness of 0.3 mm, a length of 150 mm, and a width of 150 mm.
所述用于制备铝硅系合金细化剂的钒为99.9%的颗粒状工业纯钒,粒度为300目。The vanadium used to prepare the aluminum-silicon alloy refiner is 99.9% granular industrial pure vanadium with a particle size of 300 mesh.
所述用于制备铝硅系合金细化剂的硼为99.9%的颗粒状工业纯硼,粒度为300目。The boron used to prepare the aluminum-silicon alloy refiner is 99.9% granular industrial pure boron with a particle size of 300 mesh.
实施例3Example 3
(1)配料(1) Ingredients
原料为工业纯铝、工业纯钒和工业纯硼,按照铝硅合金细化剂所述的铝、钒、硼的质量百分数,计算和称量所述原料,其中铝99.8%,钒0.1%,硼0.1%;The raw materials are industrial pure aluminum, industrial pure vanadium and industrial pure boron. According to the mass percentages of aluminum, vanadium and boron described in the aluminum-silicon alloy refiner, the raw materials are calculated and weighed, wherein aluminum is 99.8%, vanadium is 0.1%, Boron 0.1%;
(2)熔炼(2) Melting
将步骤(1)配好的铝、钒、硼均匀混合,然后将混合均匀的原料包裹在铝箔中。然后将包装好的原料置于电弧熔炼炉的坩埚中,在真空条件下进行熔炼,熔炼温度为1500℃。反复翻样熔炼3次,每次熔炼时间为5分钟。然后随炉冷却。The aluminum, vanadium and boron prepared in step (1) are uniformly mixed, and then the uniformly mixed raw materials are wrapped in aluminum foil. Then put the packaged raw materials in the crucible of the electric arc melting furnace, and melt them under vacuum conditions at a melting temperature of 1500°C. The sample was repeatedly smelted 3 times, and the smelting time was 5 minutes each time. Then cool down with the furnace.
(3)凝固(3) Solidification
待步骤(2)熔炼得到的中间合金冷却至室温后去掉表面的氧化皮,即得到一种抗退化的铝硅系合金细化剂。After the master alloy obtained in the step (2) is cooled to room temperature, the oxide skin on the surface is removed, and an anti-degeneration aluminum-silicon alloy refiner is obtained.
上述制备步骤中,所述用于制备铝硅系合金细化剂的铝为99.99%的片状工业纯铝,厚度为0.3mm,长为150mm,宽为150mm。In the above preparation steps, the aluminum used to prepare the aluminum-silicon alloy refiner is 99.99% flaky industrial pure aluminum with a thickness of 0.3 mm, a length of 150 mm, and a width of 150 mm.
所述用于制备铝硅系合金细化剂的钒为99.9%的颗粒状工业纯钒,粒度为200目。The vanadium used to prepare the aluminum-silicon alloy refiner is 99.9% granular industrial pure vanadium with a particle size of 200 mesh.
所述用于制备铝硅系合金细化剂的硼为99.9%的颗粒状工业纯硼,粒度为200目。The boron used to prepare the aluminum-silicon alloy refiner is 99.9% granular industrial pure boron with a particle size of 200 mesh.
实施例4Example 4
(1)配料(1) Ingredients
原料为工业纯铝、工业纯钒和工业纯硼,按照铝硅合金细化剂所述的铝、钒、硼的质量百分数,计算和称量所述原料,其中铝60%,钒20%,硼20%;The raw materials are industrial pure aluminum, industrial pure vanadium and industrial pure boron. According to the mass percentages of aluminum, vanadium and boron described in the aluminum-silicon alloy refiner, the raw materials are calculated and weighed, wherein aluminum is 60%, vanadium is 20%, Boron 20%;
(2)熔炼(2) Melting
将步骤(1)配好的铝、钒、硼均匀混合,然后将混合均匀的原料包裹在铝箔中。然后将包装好的原料置于电弧熔炼炉的坩埚中,在真空条件下进行熔炼,熔炼温度为2000℃。反复翻样熔炼3次,每次熔炼时间为5分钟。然后随炉冷却。The aluminum, vanadium and boron prepared in step (1) are uniformly mixed, and then the uniformly mixed raw materials are wrapped in aluminum foil. Then put the packaged raw materials in the crucible of the electric arc melting furnace, and melt them under vacuum conditions at a melting temperature of 2000°C. The sample was repeatedly smelted 3 times, and the smelting time was 5 minutes each time. Then cool down with the furnace.
(3)凝固(3) Solidification
待步骤(2)熔炼得到的中间合金冷却至室温后去掉表面的氧化皮,即得到一种抗退化的铝硅系合金细化剂。After the master alloy obtained in the step (2) is cooled to room temperature, the oxide skin on the surface is removed, and an anti-degeneration aluminum-silicon alloy refiner is obtained.
上述制备步骤中,所述用于制备铝硅系合金细化剂的铝为99.99%的片状工业纯铝,厚度为0.3mm,长为150mm,宽为150mm。In the above preparation steps, the aluminum used to prepare the aluminum-silicon alloy refiner is 99.99% flaky industrial pure aluminum with a thickness of 0.3 mm, a length of 150 mm, and a width of 150 mm.
所述用于制备铝硅系合金细化剂的钒为99.9%的颗粒状工业纯钒,粒度为500目。The vanadium used to prepare the aluminum-silicon alloy refiner is 99.9% granular industrial pure vanadium with a particle size of 500 mesh.
所述用于制备铝硅系合金细化剂的硼为99.9%的颗粒状工业纯硼,粒度为500目。The boron used to prepare the aluminum-silicon alloy refiner is 99.9% granular industrial pure boron with a particle size of 500 mesh.
实施例5Example 5
(1)配料(1) Ingredients
原料为铝钒合金和氟硼酸钾,按照铝硅系合金细化剂所述的铝、钒、硼的质量百分数,计算和称量所述原料,其中铝99.8%,钒0.1%,硼0.1%;The raw materials are aluminum-vanadium alloy and potassium fluoroborate. Calculate and weigh the raw materials according to the mass percentages of aluminum, vanadium, and boron described in the aluminum-silicon alloy refiner, wherein aluminum is 99.8%, vanadium is 0.1%, and boron is 0.1%. ;
(2)熔炼(2) Melting
将步骤(1)中配好的铝钒合金置于刚玉坩埚中,然后将刚玉坩埚放到热处理炉中加热,待炉温升至700℃后保温2h后加入配好的氟硼酸钾,然后将炉温升至1000℃保温5小时,搅拌均匀。Put the aluminum-vanadium alloy prepared in step (1) in a corundum crucible, then put the corundum crucible in a heat treatment furnace to heat, wait for the temperature of the furnace to rise to 700°C and keep it warm for 2 hours, then add the prepared potassium fluoroborate, and then put The temperature of the furnace was raised to 1000° C. for 5 hours, and the mixture was evenly stirred.
(3)浇铸凝固(3) casting and solidification
将步骤(2)熔炼得到的合金液除渣后浇铸为铸锭,冷却至室温后去除氧化皮,即得到一种抗退化的铝硅系合金细化剂。Deslagging the alloy liquid obtained in step (2) and casting it into an ingot, and removing the scale after cooling to room temperature to obtain an anti-degeneration aluminum-silicon alloy refiner.
上述制备步骤中,所述用于制备铝硅系合金细化剂的铝钒合金为块状。In the above preparation steps, the aluminum-vanadium alloy used to prepare the aluminum-silicon alloy refiner is in block shape.
所述用于制备铝硅合金细化剂的氟硼酸钾分子式为KBF4。The molecular formula of the potassium fluoroborate used to prepare the aluminum-silicon alloy refiner is KBF 4 .
实施例6Example 6
(1)配料(1) Ingredients
原料为铝钒合金和氟硼酸钾,按照铝硅系合金细化剂所述的铝、钒、硼的质量百分数,计算和称量所述原料,其中铝20%,钒40%,硼40%;The raw materials are aluminum-vanadium alloy and potassium fluoroborate. Calculate and weigh the raw materials according to the mass percentages of aluminum, vanadium, and boron described in the aluminum-silicon alloy refiner, including 20% aluminum, 40% vanadium, and 40% boron ;
(2)熔炼(2) Melting
将步骤(1)中配好的铝钒合金置于刚玉坩埚中,然后将刚玉坩埚放到热处理炉中加热,待炉温升至900℃后保温1h后加入配好的氟硼酸钾,然后将炉温升至1200℃保温2小时,搅拌均匀。Put the aluminum vanadium alloy prepared in step (1) in a corundum crucible, then put the corundum crucible in a heat treatment furnace to heat, wait for the temperature of the furnace to rise to 900°C and keep it warm for 1 hour, then add the prepared potassium fluoroborate, and then put The temperature of the furnace was raised to 1200° C. for 2 hours, and the mixture was evenly stirred.
(3)浇铸凝固(3) casting and solidification
将步骤(2)熔炼得到的合金液除渣后浇铸为铸锭,冷却至室温后去除氧化皮,即得到一种抗退化的铝硅系合金细化剂。Deslagging the alloy liquid obtained in step (2) and casting it into an ingot, and removing the scale after cooling to room temperature to obtain an anti-degeneration aluminum-silicon alloy refiner.
上述制备步骤中,所述用于制备铝硅系合金细化剂的铝钒合金为块状。In the above preparation steps, the aluminum-vanadium alloy used for preparing the aluminum-silicon alloy refiner is in block shape.
所述用于制备铝硅系合金细化剂的氟硼酸钾分子式为KBF4。The molecular formula of the potassium fluoroborate used to prepare the aluminum-silicon alloy refiner is KBF 4 .
实施例7Example 7
(1)配料(1) Ingredients
原料为铝钒合金和氟硼酸钾,按照铝硅合金细化剂所述的铝、钒、硼的质量百分数,计算和称量所述原料,其中铝60%,钒20%,硼20%;The raw materials are aluminum-vanadium alloy and potassium fluoroborate, and the raw materials are calculated and weighed according to the mass percentages of aluminum, vanadium and boron described in the aluminum-silicon alloy refiner, wherein aluminum is 60%, vanadium is 20%, and boron is 20%;
(2)熔炼(2) Melting
将步骤(1)中配好的铝钒合金置于刚玉坩埚中,然后将刚玉坩埚放到热处理炉中加热,待炉温升至800℃后保温1.5h后加入配好的氟硼酸钾,然后将炉温升至1100℃保温3.5小时,搅拌均匀。Put the aluminum-vanadium alloy prepared in step (1) in a corundum crucible, then put the corundum crucible in a heat treatment furnace to heat, wait for the temperature of the furnace to rise to 800°C and keep it warm for 1.5h, then add the prepared potassium fluoroborate, and then The temperature of the furnace was raised to 1100°C for 3.5 hours, and the mixture was evenly stirred.
(3)浇铸凝固(3) casting and solidification
将步骤(2)熔炼得到的合金液除渣后浇铸为铸锭,冷却至室温后去除氧化皮,即得到一种抗退化的铝硅系合金细化剂。Deslagging the alloy liquid obtained in step (2) and casting it into an ingot, and removing the scale after cooling to room temperature to obtain an anti-degeneration aluminum-silicon alloy refiner.
上述制备步骤中,所述用于制备铝硅系合金细化剂的铝钒合金为块状。In the above preparation steps, the aluminum-vanadium alloy used to prepare the aluminum-silicon alloy refiner is in block shape.
所述用于制备铝硅系合金细化剂的氟硼酸钾分子式为KBF4。The molecular formula of the potassium fluoroborate used to prepare the aluminum-silicon alloy refiner is KBF 4 .
实施例8Example 8
(1)配料(1) Ingredients
原料为铝硼合金和偏钒酸铵,按照上述铝硅合金细化剂所述的铝、钒、硼的重量百分数,计算和称量所述原料,其中铝99.8%,钒0.1%,硼0.1%;The raw materials are aluminum-boron alloy and ammonium metavanadate. According to the weight percentages of aluminum, vanadium and boron described in the above-mentioned aluminum-silicon alloy refiner, calculate and weigh the raw materials, wherein aluminum is 99.8%, vanadium is 0.1%, and boron is 0.1%. %;
(2)熔炼(2) Melting
将步骤(1)中配好的铝硼合金置于刚玉坩埚中,然后将刚玉坩埚放到热处理炉中加热,待炉温度升至700℃后保温2h,然后加入配好的偏钒酸铵,将温度升至1000℃保温5小时,搅拌均匀;Put the aluminum-boron alloy prepared in step (1) in a corundum crucible, then put the corundum crucible in a heat treatment furnace to heat, wait for the temperature of the furnace to rise to 700°C and keep it warm for 2 hours, then add the prepared ammonium metavanadate, Raise the temperature to 1000°C and keep it warm for 5 hours, stirring evenly;
(3)浇铸凝固(3) casting and solidification
将步骤(2)熔炼得到的合金液除渣后浇铸为铸锭,冷却至室温后去除氧化皮,即得到一种抗退化的铝硅系合金细化剂。Deslagging the alloy liquid obtained in step (2) and casting it into an ingot, and removing scale after cooling to room temperature to obtain an anti-degeneration aluminum-silicon alloy refiner.
上述制备步骤中,所述用于制备铝硅系合金细化剂的铝硼合金为块状。In the above preparation steps, the aluminum-boron alloy used to prepare the aluminum-silicon alloy refiner is in block shape.
所述用于制备铝硅系合金细化剂的偏钒酸铵分子式为NH4VO3。The molecular formula of the ammonium metavanadate used for preparing the aluminum-silicon alloy refiner is NH 4 VO 3 .
实施例9Example 9
(1)配料(1) Ingredients
原料为铝硼合金和偏钒酸铵,按照上述铝硅系合金细化剂所述的铝、钒、硼的质量百分数,计算和称量所述原料,其中铝20%,钒40%,硼40%;The raw materials are aluminum-boron alloy and ammonium metavanadate. Calculate and weigh the raw materials according to the mass percentages of aluminum, vanadium and boron described in the above-mentioned aluminum-silicon alloy refiner, wherein aluminum is 20%, vanadium is 40%, boron 40%;
(2)熔炼(2) Melting
将步骤(1)中配好的铝硼合金置于刚玉坩埚中,然后将刚玉坩埚放到热处理炉中加热,待炉温度升至900℃后保温1h,然后加入配好的偏钒酸铵,将温度升至1200℃保温5小时,搅拌均匀;Put the aluminum-boron alloy prepared in step (1) in a corundum crucible, then put the corundum crucible in a heat treatment furnace to heat, wait for the temperature of the furnace to rise to 900°C and keep it warm for 1 hour, then add the prepared ammonium metavanadate, Raise the temperature to 1200°C for 5 hours and stir evenly;
(3)浇铸凝固(3) casting and solidification
将步骤(2)熔炼得到的合金液除渣后浇铸为铸锭,冷却至室温后去除氧化皮,即得到一种抗退化的铝硅系合金细化剂。Deslagging the alloy liquid obtained in step (2) and casting it into an ingot, and removing scale after cooling to room temperature to obtain an anti-degeneration aluminum-silicon alloy refiner.
上述制备步骤中,所述用于制备铝硅系合金细化剂的铝硼合金为块状。In the above preparation steps, the aluminum-boron alloy used to prepare the aluminum-silicon alloy refiner is in block shape.
所述用于制备铝硅系合金细化剂的偏钒酸铵分子式为NH4VO3。The molecular formula of the ammonium metavanadate used for preparing the aluminum-silicon alloy refiner is NH 4 VO 3 .
实施例10Example 10
(1)配料(1) Ingredients
原料为铝硼合金和偏钒酸铵,按照上述铝硅系合金细化剂所述的铝、钒、硼的质量百分数,计算和称量所述原料,其中铝60%,钒20%,硼20%;The raw materials are aluminum-boron alloy and ammonium metavanadate. Calculate and weigh the raw materials according to the mass percentages of aluminum, vanadium and boron described in the above-mentioned aluminum-silicon alloy refiner, wherein aluminum is 60%, vanadium is 20%, boron 20%;
(2)熔炼(2) Melting
将步骤(1)中配好的铝硼合金置于刚玉坩埚中,然后将刚玉坩埚放到热处理炉中加热,待炉温度升至900℃后保温1h,然后加入配好的偏钒酸铵,将温度升至1200℃保温5小时,搅拌均匀;Put the aluminum-boron alloy prepared in step (1) in a corundum crucible, then put the corundum crucible in a heat treatment furnace to heat, wait for the temperature of the furnace to rise to 900°C and keep it warm for 1 hour, then add the prepared ammonium metavanadate, Raise the temperature to 1200°C for 5 hours and stir evenly;
(3)浇铸凝固(3) casting and solidification
将步骤(2)熔炼得到的合金液除渣后浇铸为铸锭,冷却至室温后去除氧化皮,即得到一种抗退化的铝硅系合金细化剂。Deslagging the alloy liquid obtained in step (2) and casting it into an ingot, and removing scale after cooling to room temperature to obtain an anti-degeneration aluminum-silicon alloy refiner.
上述制备步骤中,所述用于制备铝硅系合金细化剂的铝硼合金为块状。In the above preparation steps, the aluminum-boron alloy used to prepare the aluminum-silicon alloy refiner is in block shape.
所述用于制备铝硅系合金细化剂的偏钒酸铵分子式为NH4VO3。The molecular formula of the ammonium metavanadate used for preparing the aluminum-silicon alloy refiner is NH 4 VO 3 .
实施例11Example 11
(1)配料(1) Ingredients
原料为铝钒合金和铝硼合金,按照上述铝硅系合金细化剂所述的铝、钒、硼的质量百分数,计算和称量所述原料,其中铝20%,钒40%,硼40%;The raw materials are aluminum-vanadium alloy and aluminum-boron alloy. Calculate and weigh the raw materials according to the mass percentages of aluminum, vanadium and boron described in the above-mentioned aluminum-silicon alloy refiner, wherein aluminum is 20%, vanadium is 40%, and boron is 40%. %;
(2)熔炼(2) Melting
将步骤(1)中配好的铝硼合金和铝钒合金置于刚玉坩埚中,然后将刚玉坩埚放到热处理炉中加热,待炉温度升至700℃后保温3h,搅拌均匀;Put the aluminum-boron alloy and aluminum-vanadium alloy prepared in step (1) in a corundum crucible, then put the corundum crucible into a heat treatment furnace for heating, keep the temperature for 3 hours after the temperature of the furnace rises to 700°C, and stir evenly;
(3)浇铸凝固(3) casting and solidification
将步骤(2)熔炼得到的合金液除渣后浇铸为铸锭,冷却至室温后去除氧化皮,即得到一种抗退化的铝硅系合金细化剂。Deslagging the alloy liquid obtained in step (2) and casting it into an ingot, and removing the scale after cooling to room temperature to obtain an anti-degeneration aluminum-silicon alloy refiner.
上述制备步骤中,所述用于制备铝硅系合金细化剂的铝硼合金为片状。In the above preparation steps, the aluminum-boron alloy used to prepare the aluminum-silicon alloy refiner is in the form of flakes.
所述用于制备铝硅系合金细化剂的铝钒合金为块状。The aluminum-vanadium alloy used for preparing the aluminum-silicon alloy refiner is in block shape.
实施例12Example 12
(1)配料(1) Ingredients
原料为铝钒合金和铝硼合金,按照上述铝硅系合金细化剂所述的铝、钒、硼的质量百分数,计算和称量所述原料,其中铝99.8%,钒0.1%,硼0.1%;The raw materials are aluminum-vanadium alloy and aluminum-boron alloy. According to the mass percentages of aluminum, vanadium and boron described in the above-mentioned aluminum-silicon alloy refiner, calculate and weigh the raw materials, wherein aluminum is 99.8%, vanadium is 0.1%, and boron is 0.1% %;
(2)熔炼(2) Melting
将步骤(1)中配好的铝硼合金和铝钒合金置于刚玉坩埚中,然后将刚玉坩埚放到热处理炉中加热,待炉温度升至900℃后保温1h,搅拌均匀;Put the aluminum-boron alloy and aluminum-vanadium alloy prepared in step (1) in a corundum crucible, then put the corundum crucible into a heat treatment furnace to heat, keep the temperature for 1 hour after the furnace temperature rises to 900°C, and stir evenly;
(3)浇铸凝固(3) casting and solidification
将步骤(2)熔炼得到的合金液除渣后浇铸为铸锭,冷却至室温后去除氧化皮,即得到一种抗退化的铝硅系合金细化剂。Deslagging the alloy liquid obtained in step (2) and casting it into an ingot, and removing the scale after cooling to room temperature to obtain an anti-degeneration aluminum-silicon alloy refiner.
上述制备步骤中,所述用于制备铝硅系合金细化剂的铝硼合金为块状。In the above preparation steps, the aluminum-boron alloy used to prepare the aluminum-silicon alloy refiner is in block shape.
所述用于制备铝硅系合金细化剂的铝钒合金为片状。The aluminum-vanadium alloy used for preparing the aluminum-silicon alloy refiner is in the form of flakes.
实施例13Example 13
(1)配料(1) Ingredients
原料为铝钒合金和铝硼合金,按照上述铝硅系合金细化剂所述的铝、钒、硼的质量百分数,计算和称量所述原料,其中铝60%,钒20%,硼20%;The raw materials are aluminum-vanadium alloy and aluminum-boron alloy. According to the mass percentages of aluminum, vanadium and boron described in the above-mentioned aluminum-silicon alloy refiner, calculate and weigh the raw materials, wherein aluminum is 60%, vanadium is 20%, and boron is 20%. %;
(2)熔炼(2) Melting
将步骤(1)中配好的铝硼合金和铝钒合金置于刚玉坩埚中,然后将刚玉坩埚放到热处理炉中加热,待炉温度升至800℃后保温2h,搅拌均匀;Put the aluminum-boron alloy and aluminum-vanadium alloy prepared in step (1) in a corundum crucible, then put the corundum crucible into a heat treatment furnace for heating, keep the temperature for 2 hours after the temperature of the furnace rises to 800°C, and stir evenly;
(3)浇铸凝固(3) casting and solidification
将步骤(2)熔炼得到的合金液除渣后浇铸为铸锭,冷却至室温后去除氧化皮,即得到一种抗退化的铝硅系合金细化剂。Deslagging the alloy liquid obtained in step (2) and casting it into an ingot, and removing the scale after cooling to room temperature to obtain an anti-degeneration aluminum-silicon alloy refiner.
上述制备步骤中,所述用于制备铝硅系合金细化剂的铝硼合金为颗粒状。In the above preparation steps, the aluminum-boron alloy used to prepare the aluminum-silicon alloy refiner is in granular form.
所述用于制备铝硅系合金细化剂的铝钒合金为块状。The aluminum-vanadium alloy used for preparing the aluminum-silicon alloy refiner is in block shape.
实施例14Example 14
(1)配料(1) Ingredients
原料为工业纯铝、氟硼酸钾和偏钒酸铵,按照上述铝硅系合金细化剂所述的铝、钒、硼的质量百分数,计算和称量所述原料,其中铝99.8%,钒0.1%,硼0.1%;The raw materials are industrial pure aluminum, potassium fluoroborate and ammonium metavanadate, and the raw materials are calculated and weighed according to the mass percentages of aluminum, vanadium and boron described in the above-mentioned aluminum-silicon alloy refiner, wherein aluminum is 99.8%, vanadium 0.1%, boron 0.1%;
(2)熔炼(2) Melting
将步骤(1)中配好的工业纯铝置于刚玉坩埚中,待温度升至700℃后保温3h,然后加入一定配比的氟硼酸钾和偏钒酸铵,然后将炉温升至1000℃保温5小时,搅拌均匀;Put the industrially pure aluminum prepared in step (1) in a corundum crucible, keep it warm for 3 hours after the temperature rises to 700°C, then add a certain proportion of potassium fluoroborate and ammonium metavanadate, and then raise the furnace temperature to 1000°C ℃ for 5 hours, stirring evenly;
(3)浇铸凝固(3) casting and solidification
将步骤(2)熔炼得到的合金液除渣后浇铸为铸锭,冷却至室温后去除氧化皮,即得到一种抗退化的铝硅系合金细化剂。Deslagging the alloy liquid obtained in step (2) and casting it into an ingot, and removing the scale after cooling to room temperature to obtain an anti-degeneration aluminum-silicon alloy refiner.
上述制备步骤中,所述用于制备铝硅系合金细化剂的工业纯铝为片状。In the above preparation steps, the industrially pure aluminum used to prepare the aluminum-silicon alloy refiner is in the form of flakes.
所述用于制备铝硅系合金细化剂的偏钒酸铵分子式为NH4VO3。The molecular formula of the ammonium metavanadate used for preparing the aluminum-silicon alloy refiner is NH 4 VO 3 .
所述用于制备铝硅系合金细化剂的氟硼酸钾分子式为KBF4。The molecular formula of the potassium fluoroborate used to prepare the aluminum-silicon alloy refiner is KBF 4 .
实施例15Example 15
(1)配料(1) Ingredients
原料为工业纯铝、氟硼酸钾和偏钒酸铵,按照上述铝硅系合金细化剂所述的铝、钒、硼的质量百分数,计算和称量所述原料,其中铝20%,钒40%,硼40%;The raw materials are industrial pure aluminum, potassium fluoroborate and ammonium metavanadate, and the raw materials are calculated and weighed according to the mass percentages of aluminum, vanadium and boron described in the above-mentioned aluminum-silicon alloy refiner, wherein aluminum is 20%, vanadium 40%, boron 40%;
(2)熔炼(2) Melting
将步骤(1)中配好的工业纯铝置于刚玉坩埚中,待温度升至900℃后保温1h,然后加入一定配比的氟硼酸钾和偏钒酸铵,然后将炉温升至1200℃保温2小时,搅拌均匀;Put the industrially pure aluminum prepared in step (1) in a corundum crucible, keep it warm for 1 hour after the temperature rises to 900°C, then add a certain proportion of potassium fluoroborate and ammonium metavanadate, and then raise the furnace temperature to 1200°C ℃ for 2 hours, stirring evenly;
(3)浇铸凝固(3) casting and solidification
将步骤(2)熔炼得到的合金液除渣后浇铸为铸锭,冷却至室温后去除氧化皮,即得到一种抗退化的铝硅系合金细化剂。Deslagging the alloy liquid obtained in step (2) and casting it into an ingot, and removing the scale after cooling to room temperature to obtain an anti-degeneration aluminum-silicon alloy refiner.
上述制备步骤中,所述用于制备铝硅系合金细化剂的工业纯铝为块状。In the above preparation steps, the industrially pure aluminum used to prepare the aluminum-silicon alloy refiner is in block form.
所述用于制备铝硅系合金细化剂的偏钒酸铵分子式为NH4VO3。The molecular formula of the ammonium metavanadate used for preparing the aluminum-silicon alloy refiner is NH 4 VO 3 .
所述用于制备铝硅系合金细化剂的氟硼酸钾分子式为KBF4。The molecular formula of the potassium fluoroborate used to prepare the aluminum-silicon alloy refiner is KBF 4 .
实施例16Example 16
(1)配料(1) Ingredients
原料为工业纯铝、氟硼酸钾和偏钒酸铵,按照上述铝硅系合金细化剂所述的铝、钒、硼的质量百分数,计算和称量所述原料,其中铝60%,钒20%,硼20%;The raw materials are industrial pure aluminum, potassium fluoroborate and ammonium metavanadate, and the raw materials are calculated and weighed according to the mass percentages of aluminum, vanadium and boron described in the above-mentioned aluminum-silicon alloy refiner, wherein aluminum is 60%, vanadium 20%, boron 20%;
(2)熔炼(2) Melting
将步骤(1)中配好的工业纯铝置于刚玉坩埚中,待温度升至800℃后保温2h,然后加入一定配比的氟硼酸钾和偏钒酸铵,然后将炉温升至1100℃保温3.5小时,搅拌均匀;Put the industrially pure aluminum prepared in step (1) in a corundum crucible, keep it warm for 2 hours after the temperature rises to 800°C, then add a certain proportion of potassium fluoroborate and ammonium metavanadate, and then raise the furnace temperature to 1100°C ℃ for 3.5 hours, stirring evenly;
(3)浇铸凝固(3) casting and solidification
将步骤(2)熔炼得到的合金液除渣后浇铸为铸锭,冷却至室温后去除氧化皮,即得到一种抗退化的铝硅系合金细化剂。Deslagging the alloy liquid obtained in step (2) and casting it into an ingot, and removing the scale after cooling to room temperature to obtain an anti-degeneration aluminum-silicon alloy refiner.
上述制备步骤中,所述用于制备铝硅系合金细化剂的工业纯铝为颗粒状,工业纯度为99.99%,目数为300目。In the above preparation steps, the industrially pure aluminum used to prepare the aluminum-silicon alloy refiner is granular, with an industrial purity of 99.99% and a mesh size of 300 mesh.
所述用于制备铝硅系合金细化剂的偏钒酸铵分子式为NH4VO3。The molecular formula of the ammonium metavanadate used for preparing the aluminum-silicon alloy refiner is NH 4 VO 3 .
所述用于制备铝硅系合金细化剂的氟硼酸钾分子式为KBF4。The molecular formula of the potassium fluoroborate used to prepare the aluminum-silicon alloy refiner is KBF 4 .
实施例17Example 17
(1)配料(1) Ingredients
原料为工业纯铝、工业纯硅和配置好的Al-V-B细化剂,按照一定比例计算和称量所述原料,其中工业纯硅:13%,Al-V-B细化剂:2.5%,余量为工业纯铝。The raw materials are industrial pure aluminum, industrial pure silicon and prepared Al-V-B refiner, and the raw materials are calculated and weighed according to a certain ratio, wherein industrial pure silicon: 13%, Al-V-B refiner: 2.5%, and the rest The quantity is industrial pure aluminum.
(2)熔炼(2) Melting
将配置好的纯铝置于坩埚中,然后将坩埚置于马弗炉中加热,待炉内温度升至750℃后保温0.8小时,接着将配置好的工业纯硅加入坩埚中,750℃小保温1.5小时,最后将一定比例的细化剂加入坩埚中保温2.5小时。Put the prepared pure aluminum in the crucible, then place the crucible in a muffle furnace to heat, wait for the temperature in the furnace to rise to 750°C and keep it warm for 0.8 hours, then add the prepared industrial pure silicon into the crucible, and heat it at 750°C Keep warm for 1.5 hours, and finally add a certain proportion of refiner into the crucible and keep warm for 2.5 hours.
(3)浇铸凝固(3) casting and solidification
将步骤(2)得到的合金液浇铸为铸锭,冷却至室温即可得到铝硅系合金细化后的铸锭。The alloy liquid obtained in step (2) is cast into an ingot, and cooled to room temperature to obtain an aluminum-silicon alloy refined ingot.
上述步骤中,所述用于制备铝硅系合金的铝为块状的工业纯铝。In the above steps, the aluminum used to prepare the aluminum-silicon alloy is block industrial pure aluminum.
所述用于制备铝硅系合金的硅为工业纯硅。The silicon used to prepare the aluminum-silicon alloy is industrial pure silicon.
所述用于盛装合金液的坩埚为石墨坩埚或刚玉坩埚。The crucible for containing the alloy liquid is a graphite crucible or a corundum crucible.
将实施例2-16所得Al-V-B细化剂,分别用上述方法制备硅铝系合金,所得合金按实施例1方法进行检测,效果与实施例1基本相同。The Al-V-B refining agents obtained in Examples 2-16 were used to prepare silicon-aluminum alloys by the above method, and the obtained alloys were tested according to the method of Example 1, and the effect was basically the same as that of Example 1.
实施例18Example 18
(1)配料(1) Ingredients
原料为购买的工业铝硅系合金(A356)、Al-V-B细化剂,按照一定比例计算和称量所述原料,其中铝硅系合金百分含量为:95%,Al-V-B细化剂百分含量为:5%。The raw materials are purchased industrial aluminum-silicon alloy (A356), Al-V-B refiner, and the raw materials are calculated and weighed according to a certain ratio, wherein the percentage content of aluminum-silicon alloy is: 95%, Al-V-B refiner The percentage content is: 5%.
(2)熔炼(2) Melting
将工业铝硅系合金置于坩埚中,然后将坩埚置于马弗炉中加热,待炉内温度升至750℃后保温0.8小时,接着一定比例的Al-V-B细化剂加入坩埚中保温2.5小时。Put the industrial aluminum-silicon alloy in the crucible, then place the crucible in a muffle furnace to heat, wait for the temperature in the furnace to rise to 750°C and keep it warm for 0.8 hours, then add a certain proportion of Al-V-B refiner to the crucible and keep it warm for 2.5 Hour.
(3)浇铸凝固(3) casting and solidification
将步骤(2)得到的合金液浇铸为铸锭或铸件,冷却至室温即可得到细化后的铝硅系合金铸锭或铸件。The alloy liquid obtained in step (2) is cast into an ingot or a casting, and cooled to room temperature to obtain a refined aluminum-silicon alloy ingot or casting.
上述步骤中,所述工业铝硅系合金为块状。In the above steps, the industrial aluminum-silicon alloy is in block shape.
所述用于盛装合金液的坩埚为石墨坩埚或刚玉坩埚。The crucible for containing the alloy liquid is a graphite crucible or a corundum crucible.
将实施例2‐16所得Al‐V‐B细化剂,分别用上述方法制备硅铝系合金,所得合金按实施例1方法进行检测,效果与实施例1基本相同。The Al-V-B refining agent obtained in Example 2-16 was used to prepare silicon-aluminum alloys by the above method, and the obtained alloy was tested according to the method of Example 1, and the effect was basically the same as that of Example 1.
实施例19Example 19
(1)配料(1) Ingredients
原料为工业纯铝、工业纯硅、铝钒合金和铝硼合金,按照一定比例计算和称量所述原料,其中工业纯硅:13%,铝钒合金:2.5%,铝硼合金:2.5%,余量为工业纯铝。The raw materials are industrial pure aluminum, industrial pure silicon, aluminum-vanadium alloy and aluminum-boron alloy. The raw materials are calculated and weighed according to a certain proportion, of which industrial pure silicon: 13%, aluminum-vanadium alloy: 2.5%, aluminum-boron alloy: 2.5% , and the balance is industrial pure aluminum.
(2)熔炼(2) Melting
将配置好的纯铝置于坩埚中,然后将坩埚置于马弗炉中加热,待炉内温度升至750℃后保温0.8小时,接着将配置好的工业纯硅加入坩埚中,750℃小保温1.5小时,最后将一定比例的铝钒合金和铝硼合金同时加入坩埚中保温2.5小时。Put the prepared pure aluminum in the crucible, then place the crucible in a muffle furnace to heat, wait for the temperature in the furnace to rise to 750°C and keep it warm for 0.8 hours, then add the prepared industrial pure silicon into the crucible, and heat it at 750°C Keep warm for 1.5 hours, and finally add a certain proportion of aluminum-vanadium alloy and aluminum-boron alloy into the crucible and keep warm for 2.5 hours.
(3)浇铸凝固(3) casting and solidification
将步骤(2)得到的合金液浇铸为铸锭或压铸为铸件,冷却至室温即可得到细化后的铝硅合金铸锭或铸件。The alloy liquid obtained in step (2) is cast into an ingot or die-cast into a casting, and cooled to room temperature to obtain a refined aluminum-silicon alloy ingot or casting.
上述步骤中,所述用于制备铝硅合金的铝为块状的工业纯铝。In the above steps, the aluminum used to prepare the aluminum-silicon alloy is block industrial pure aluminum.
所述用于盛装合金液的坩埚为石墨坩埚或刚玉坩埚。The crucible for containing the alloy liquid is a graphite crucible or a corundum crucible.
上述所得硅铝系合金按实施例1方法进行检测,效果与实施例1基本相同。The silicon-aluminum alloy obtained above is tested according to the method of Example 1, and the effect is basically the same as that of Example 1.
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CN110157935A (en) * | 2019-06-28 | 2019-08-23 | 上海大学 | Al-V-B refining agent for casting aluminum-silicon alloy, its preparation method and application |
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