WO2021007893A1 - Process for preparing aluminum-titanium-boron refiner plate and strip - Google Patents

Process for preparing aluminum-titanium-boron refiner plate and strip Download PDF

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WO2021007893A1
WO2021007893A1 PCT/CN2019/099563 CN2019099563W WO2021007893A1 WO 2021007893 A1 WO2021007893 A1 WO 2021007893A1 CN 2019099563 W CN2019099563 W CN 2019099563W WO 2021007893 A1 WO2021007893 A1 WO 2021007893A1
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aluminum
titanium
boron
master alloy
casting
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PCT/CN2019/099563
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French (fr)
Chinese (zh)
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许光明
赵凯
李勇
王昭东
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东北大学
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
    • B22D11/00—Continuous casting of metals, i.e. casting in indefinite lengths
    • B22D11/001—Continuous casting of metals, i.e. casting in indefinite lengths of specific alloys
    • B22D11/003—Aluminium alloys
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
    • B22D11/00—Continuous casting of metals, i.e. casting in indefinite lengths
    • B22D11/06—Continuous casting of metals, i.e. casting in indefinite lengths into moulds with travelling walls, e.g. with rolls, plates, belts, caterpillars
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys
    • C22C1/10—Alloys containing non-metals
    • C22C1/1036—Alloys containing non-metals starting from a melt
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C21/00—Alloys based on aluminium
    • C22C21/003—Alloys based on aluminium containing at least 2.6% of one or more of the elements: tin, lead, antimony, bismuth, cadmium, and titanium
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C32/00—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ
    • C22C32/0047—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with carbides, nitrides, borides or silicides as the main non-metallic constituents
    • C22C32/0073—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with carbides, nitrides, borides or silicides as the main non-metallic constituents only borides

Definitions

  • the invention relates to the field of alloy smelting, in particular to a preparation process of an aluminum-titanium-boron refiner strip.
  • the most commonly used and effective method of structure refinement is to add a refiner to the aluminum alloy melt.
  • the heterogeneous nucleation of the refiner is used to make The organization is refined.
  • Aluminum-titanium-B master alloy is currently the most widely used aluminum alloy refiner. 75% of the world's aluminum industry uses aluminum-titanium-boron refiner. There are more than 20 manufacturers in my country, with an annual output of 2000 Tons, but still cannot meet the rapidly growing demand of the domestic market, and it is still necessary to import more than 3000 tons from abroad every year.
  • TiAl 3 particles have three morphologies: massive, needle-like and petal-like. Among them, massive TiAl 3 particles are most beneficial to the refinement effect; TiB 2 particles are generally granular, and the more uniform and finer the particles, the better the refinement effect.
  • the existing production processes of aluminum-titanium-boron refiner mainly include fluoride salt method, element mixing method and self-propagating high-temperature synthesis method, etc. These preparation processes have many defects, such as: aluminum-titanium-prepared by fluoride salt method
  • the TiAl 3 particles in the boron alloy coexist in the form of agglomerates and needles, and the TiB 2 particles are present in agglomerates; there are fewer TiB 2 particles in the aluminum-titanium-boron refiner prepared by the element mixing method; however, self-propagating
  • the SHS reaction temperature is difficult to control.
  • the aluminum processing industry has increasingly higher requirements for aluminum-titanium-boron refining agents.
  • the aluminum-titanium-boron refining agents prepared by the existing process The level of transformation is far from meeting the demand for high-quality aluminum.
  • the present invention proposes a production method for preparing the aluminum titanium boron refiner strip by stepwise liquid preparation, control of the reaction temperature and time, and the casting and rolling process.
  • the technical solution adopted by the present invention to solve its technical problems is: a preparation process of aluminum-titanium-boron thinner strip, and the process is: preparation of thinner alloy melt-casting-rolling, wherein thinning
  • the preparation method of the agent alloy melt includes the following steps: prepare aluminum-titanium and aluminum-boron master alloy melts respectively, and control the temperature of the master alloy melt to be 750 ⁇ 900°C; and process the aluminum-titanium and aluminum-boron master alloy melts. Mix the reaction and keep it at 750-900°C for 10-60 minutes, and then reduce the temperature of the mixed melt to 710-750°C.
  • the titanium content in the aluminum-titanium master alloy is 8% to 20%
  • the boron content in the aluminum-titanium master alloy is 1% to 5%.
  • -Boron master alloy ratio is mixed according to the required ratio of titanium and boron.
  • the preparation method of the refiner alloy melt specifically includes the following steps:
  • the intermediate alloy batching is carried out according to the above-mentioned ratio. Among them, industrial pure aluminum ingot is used for aluminum, and titanium salt or metal titanium and boron salt can be used for titanium and boron;
  • Preparation of aluminum-titanium master alloy melt use a smelting furnace to heat the aluminum ingot to melt it. When the temperature reaches 850 to 950°C, add the prepared metal titanium or titanium salt to the aluminum melt, and stir to make the metal The titanium or titanium salt fully contacts and reacts with the aluminum, and the metal titanium or titanium salt is completely dissolved in the aluminum melt, and the temperature is kept for 30-60 minutes, then the slag is removed, and the temperature is reduced to 750-900°C for use;
  • Preparation of aluminum-boron master alloy melt use aluminum-boron master alloy raw materials, and the other preparation methods are the same as those of aluminum-titanium master alloy melt;
  • Reaction control Transfer the spare aluminum-titanium and aluminum-boron master alloy melts into the reaction furnace, and fully stir them, control the temperature and holding time of the mixed solution, and transfer to the tundish or static furnace after cooling. Waiting for casting and rolling into plate.
  • the casting-rolling process method is: using a vertical or horizontal casting-rolling mill for casting, the diameter of the casting roll is 500-1050mm, the thickness of the cast-rolled plate is 2-10mm, and the casting-rolling temperature is 680-715°C, The casting-rolling speed is controlled at 0.5-5m/min; the crimping process is to wind the plate-shaped aluminum-titanium-boron refining agent through a crimping machine into a standardized coil.
  • the yield of titanium and boron needs to be considered during the compounding process.
  • Another aspect of the present invention provides an aluminum-titanium-boron refiner strip prepared based on the above process.
  • the use of the present invention first prepares aluminum-titanium and aluminum-boron intermediate alloy melts, then controls the temperature of the aluminum-titanium and aluminum-boron melts to a suitable temperature, and then mixes the aluminum-titanium and aluminum-boron melts
  • the way of reaction is to control the size of TiB 2 particles by controlling the melt temperature and mixing reaction time, and use the rapid solidification of the casting-rolling process to achieve a uniform distribution of active particles in the refiner to avoid aggregation and agglomeration;
  • the present invention has simple process and convenient operation, and solves the problems of uneven distribution, small quantity and large size of TiAl 3 and TiB 2 particles in the aluminum-titanium-boron refiner prepared by the traditional process method, and improves the refinement effectiveness.
  • Figure 1 is a flow chart of the preparation process of the present invention
  • the reference signs are: 1. Aluminum-titanium master alloy melting furnace; 2. Aluminum-boron master alloy melting furnace; 3. Reaction furnace; 4. Standing furnace; 5. Casting nozzle; 6. Casting rolling mill; 7. Coiler ;
  • Figure 2 is a microstructure diagram (metallographic diagram) of the Al-Ti-B master alloy in Example 1;
  • Figure 3 is a microstructure diagram (metallographic diagram) of the Al-Ti-B master alloy in Example 2;
  • Figure 4 is a microstructure diagram (metallographic diagram) of the Al-Ti-B master alloy in Example 3;
  • Figure 5 is a microstructure diagram (metallographic diagram) of the Al-Ti-B master alloy in Example 4.
  • Figure 6 is a microstructure diagram (metallographic diagram) of the Al-Ti-B refiner master alloy prepared by the traditional process.
  • the process of the present invention is as follows: first prepare aluminum-titanium and aluminum-boron master alloy melts in the smelting furnace (1, 2), control the temperature of the master alloy melt, and then in the reaction furnace (3) In the process, the aluminum-titanium and aluminum-boron master alloy melts are mixed and reacted, the temperature of the mixed melt and the mixing reaction time are controlled, and then the mixed melt is transferred to the static furnace (4), and cast-rolled into a plate by the casting-rolling machine (6). Finally, it is wound into a standard coil by a crimper (7).
  • the aluminum-titanium master alloy and the aluminum-boron master alloy are batched and weighed.
  • the aluminum-titanium master alloy has a titanium content of 10%; aluminum- Boron master alloy with a boron content of 2%; raw materials are industrial pure aluminum ingots, sponge titanium and potassium borate, among which the purity of industrial pure aluminum ingots Al is 99.85%;
  • Casting and rolling Pour the heat-preserved mixed melt into a tundish or a static furnace for casting and rolling into a plate.
  • the casting-rolling machine adopts a horizontal casting-rolling mill, the casting temperature is 700°C, the casting roll diameter is 1000mm, and the casting thickness is 7mm.
  • the casting-rolling speed is 1m/min. After the mixed melt passes through the casting-rolling machine, a plate-shaped aluminum titanium boron refiner with a thickness of 7 mm is obtained.
  • Casting and rolling Pour the heat-preserved mixed melt into a tundish or a static furnace for casting and rolling into a plate.
  • the casting-rolling machine adopts a horizontal casting-rolling machine with a casting temperature of 690°C, a casting roll diameter of 820mm, and a casting thickness of 6mm.
  • the casting-rolling speed is 1.2m/min. After the mixed melt passes through the casting-rolling machine, a plate-shaped aluminum titanium boron refiner with a thickness of 6 mm is obtained.
  • the aluminum-titanium master alloy and the aluminum-boron master alloy are batched and weighed.
  • the aluminum-titanium master alloy has a titanium content of 16%; aluminum- Boron master alloy with a boron content of 2%; raw materials are industrial pure aluminum ingots, potassium titanate and potassium borate, and the purity of industrial pure aluminum ingots Al is 99.85%;
  • Casting and rolling Pour the heat-preserved mixed melt into a tundish or a static furnace for casting and rolling into a plate.
  • the casting-rolling machine adopts a horizontal casting-rolling machine, the casting temperature is 695°C, the casting roll diameter is 920mm, and the casting thickness is 8mm.
  • the casting-rolling speed is 0.8m/min. After the mixed melt passes through the casting-rolling machine, a plate-shaped aluminum titanium boron refiner with a thickness of 8 mm is obtained.
  • Casting and rolling Pour the heat-preserved mixed melt into a tundish or a static furnace for casting and rolling into a plate.
  • the casting-rolling machine adopts a vertical casting-rolling machine with a casting temperature of 705°C, a casting roll diameter of 500mm, and a casting thickness of 2mm.
  • the casting-rolling speed is 5m/min. After the mixed melt passes through the casting-rolling mill, a plate-shaped aluminum titanium boron refiner with a thickness of 2 mm is obtained.

Abstract

Disclosed is a process for preparing an aluminum-titanium-boron refiner plate and strip, comprising the preparation-cast rolling-crimping of a refiner alloy melt, wherein a method for preparing the refiner alloy melt comprises the following steps: respectively preparing aluminum-titanium and aluminum-boron intermediate alloy melts, and controlling the temperature of the intermediate alloy melts at 750-900ºC; and mixing and reacting the aluminum-titanium and aluminum-boron intermediate alloy melts, and keeping the temperature at 750-900ºC for 10-60 minutes, and then reducing the temperature of the mixed melt to 710-750ºC. The process solves the problem of the uneven distribution, small quantity, and larger size of TiAl3 and TiB2 particles in the aluminum-titanium-boron refiner, and improves the refining efficiency thereof.

Description

一种铝-钛-硼细化剂板带的制备工艺Preparation process of aluminum-titanium-boron thinning agent strip 技术领域Technical field
本发明涉及合金冶炼领域，具体为一种铝-钛-硼细化剂板带的制备工艺。The invention relates to the field of alloy smelting, in particular to a preparation process of an aluminum-titanium-boron refiner strip.
背景技术Background technique
在制造和生产铝及铝合金产品时最常用和有效的组织细化方法是在铝合金熔体中加入细化剂，在铝及铝合金的凝固过程中通过细化剂的异质形核使组织得到细化。铝-钛-B中间合金是目前使用的最为广泛的铝合金细化剂，世界上75％的铝工业使用铝-钛-硼细化剂，我国生产厂家已达20多家，产量每年达2000吨，但仍不能满足国内市场快速增长的需求，每年仍需从国外进口3000吨以上。与国外的铝钛硼细化剂产品相比，我国生产的铝-钛-硼细化剂的质量存在一定差距，主要包括铝-钛-硼细化剂线杆中TiAl 3分布不够均匀，TiB 2颗粒较为粗大且分布不均，偏聚现象严重，细化效果欠佳。 In the manufacture and production of aluminum and aluminum alloy products, the most commonly used and effective method of structure refinement is to add a refiner to the aluminum alloy melt. During the solidification process of aluminum and aluminum alloy, the heterogeneous nucleation of the refiner is used to make The organization is refined. Aluminum-titanium-B master alloy is currently the most widely used aluminum alloy refiner. 75% of the world's aluminum industry uses aluminum-titanium-boron refiner. There are more than 20 manufacturers in my country, with an annual output of 2000 Tons, but still cannot meet the rapidly growing demand of the domestic market, and it is still necessary to import more than 3000 tons from abroad every year. Compared with foreign aluminum-titanium-boron refiner products, there is a certain gap in the quality of aluminum-titanium-boron refiner produced in China, mainly including the insufficient distribution of TiAl 3 in the aluminum-titanium-boron refiner wire rod and TiB 2 The particles are relatively coarse and unevenly distributed, the segregation phenomenon is serious, and the refinement effect is not good.
大量的研究工作表明，铝-钛-硼细化剂对铝及铝合金的细化效果主要与TiAl 3、TiB 2活性质点的形状、大小、分布和数量有关，活性质点尺寸越细小、分布越均匀，数量越多，其细化效果越好。TiAl 3粒子有块状、针状和花瓣状三种形貌，其中块状的TiAl 3粒子对细化效果最有利；TiB 2粒子一般为颗粒状，粒子越均匀细小，细化效果越好。 A lot of research work has shown that the refining effect of aluminum-titanium-boron refining agent on aluminum and aluminum alloys is mainly related to the shape, size, distribution and quantity of TiAl 3 and TiB 2 active particles. The smaller the size of the active particles, the more the distribution. Even, the more the quantity, the better the refinement effect. TiAl 3 particles have three morphologies: massive, needle-like and petal-like. Among them, massive TiAl 3 particles are most beneficial to the refinement effect; TiB 2 particles are generally granular, and the more uniform and finer the particles, the better the refinement effect.
现有的铝-钛-硼细化剂的生产工艺主要有氟盐法、元素混合法和自蔓延高温合成法等，这些制备工艺存在诸多缺陷，如：在氟盐法制备的铝-钛-硼合金中TiAl 3粒子为团块状与针片状共存，TiB 2粒子呈聚集团状存在；在元素混合法制备的铝-钛-硼细化剂中TiB 2粒子较少；而使用自蔓延高温合成法在制备铝-钛-硼合金时，SHS反应温度很难控制。随着高质量、高性能铝材的广泛应用，铝加工业对铝-钛-硼细化剂的要求也越来越高，显然使用现有工艺制备的铝-钛-硼细化剂的细化水平远不能满足高质量铝材的需求。 The existing production processes of aluminum-titanium-boron refiner mainly include fluoride salt method, element mixing method and self-propagating high-temperature synthesis method, etc. These preparation processes have many defects, such as: aluminum-titanium-prepared by fluoride salt method The TiAl 3 particles in the boron alloy coexist in the form of agglomerates and needles, and the TiB 2 particles are present in agglomerates; there are fewer TiB 2 particles in the aluminum-titanium-boron refiner prepared by the element mixing method; however, self-propagating When preparing aluminum-titanium-boron alloys by high-temperature synthesis, the SHS reaction temperature is difficult to control. With the wide application of high-quality and high-performance aluminum materials, the aluminum processing industry has increasingly higher requirements for aluminum-titanium-boron refining agents. Obviously, the aluminum-titanium-boron refining agents prepared by the existing process The level of transformation is far from meeting the demand for high-quality aluminum.
发明概述Summary of the invention
技术问题technical problem
问题的解决方案The solution to the problem
技术解决方案Technical solutions
本发明针对目前铝钛硼细化剂制备中存在的问题提出了一种通过分步制液、控制反应温度和时间及采用铸轧工艺制备铝钛硼细化剂板带的生产方法。Aiming at the problems existing in the preparation of the current aluminum titanium boron refiner, the present invention proposes a production method for preparing the aluminum titanium boron refiner strip by stepwise liquid preparation, control of the reaction temperature and time, and the casting and rolling process.
本发明解决其技术问题所采用的技术方案是：一种铝-钛-硼细化剂板带的制备工艺，其流程为：细化剂合金熔体的制备-铸轧-卷曲，其中细化剂合金熔体的制备方法包括如下步骤：分别制备铝-钛和铝-硼中间合金熔体，控制中间合金熔体温度为750～900℃；将铝-钛和铝-硼中间合金熔体进行混合反应，并在750～900℃下保温10～60分钟，然后把混合熔体温度降低至710～750℃。The technical solution adopted by the present invention to solve its technical problems is: a preparation process of aluminum-titanium-boron thinner strip, and the process is: preparation of thinner alloy melt-casting-rolling, wherein thinning The preparation method of the agent alloy melt includes the following steps: prepare aluminum-titanium and aluminum-boron master alloy melts respectively, and control the temperature of the master alloy melt to be 750～900℃; and process the aluminum-titanium and aluminum-boron master alloy melts. Mix the reaction and keep it at 750-900°C for 10-60 minutes, and then reduce the temperature of the mixed melt to 710-750°C.
进一步地，以质量分数计，所述铝-钛中间合金中，钛含量为8％～20％，所述铝-钛中间合金中，硼含量为1％～5％，其中铝-钛、铝-硼中间合金配比根据所需钛与硼的比例配入。Further, in terms of mass fraction, the titanium content in the aluminum-titanium master alloy is 8% to 20%, and the boron content in the aluminum-titanium master alloy is 1% to 5%. -Boron master alloy ratio is mixed according to the required ratio of titanium and boron.
进一步地，所述细化剂合金熔体的制备方法具体包括如下步骤：Further, the preparation method of the refiner alloy melt specifically includes the following steps:
(1)配料：按上述配比进行中间合金配料，其中，铝采用工业纯铝锭，钛和硼可以采用钛盐或金属钛和硼盐；(1) Batching: The intermediate alloy batching is carried out according to the above-mentioned ratio. Among them, industrial pure aluminum ingot is used for aluminum, and titanium salt or metal titanium and boron salt can be used for titanium and boron;
(2)中间合金熔体的制备：(2) Preparation of master alloy melt:
铝-钛中间合金熔体的制备：采用熔炼炉加热铝锭使其熔化，当温度达到850～950℃，向铝熔体中加入配好料的金属钛或钛盐，并进行搅拌，使金属钛或钛盐与铝进行充分接触、反应，并使金属钛或钛盐完全溶解到铝熔体中，保温30～60分钟，然后进行扒渣，降温至750～900℃，备用；Preparation of aluminum-titanium master alloy melt: use a smelting furnace to heat the aluminum ingot to melt it. When the temperature reaches 850 to 950°C, add the prepared metal titanium or titanium salt to the aluminum melt, and stir to make the metal The titanium or titanium salt fully contacts and reacts with the aluminum, and the metal titanium or titanium salt is completely dissolved in the aluminum melt, and the temperature is kept for 30-60 minutes, then the slag is removed, and the temperature is reduced to 750-900°C for use;
铝-硼中间合金熔体的制备：采用铝-硼中间合金原料，其余制备方法与铝-钛中间合金熔体的制备方法相同；Preparation of aluminum-boron master alloy melt: use aluminum-boron master alloy raw materials, and the other preparation methods are the same as those of aluminum-titanium master alloy melt;
(3)反应控制：将备用的铝-钛、铝-硼中间合金熔体转入反应炉内，并进行充分搅拌，控制混合溶体的温度和保温时间，降温后转移至中间包或静置炉，等待铸轧成板。(3) Reaction control: Transfer the spare aluminum-titanium and aluminum-boron master alloy melts into the reaction furnace, and fully stir them, control the temperature and holding time of the mixed solution, and transfer to the tundish or static furnace after cooling. Waiting for casting and rolling into plate.
进一步地，所述铸轧工艺方法为：采用立式或卧式铸轧机进行铸轧，铸轧辊的直径在500～1050mm，铸轧板厚度在2～10mm，铸轧温度在680～715℃，铸轧速度控制在0.5～5m/min；所述卷曲工艺为将板状铝-钛-硼细化剂通过卷曲机绕制 成规范的盘卷。Further, the casting-rolling process method is: using a vertical or horizontal casting-rolling mill for casting, the diameter of the casting roll is 500-1050mm, the thickness of the cast-rolled plate is 2-10mm, and the casting-rolling temperature is 680-715°C, The casting-rolling speed is controlled at 0.5-5m/min; the crimping process is to wind the plate-shaped aluminum-titanium-boron refining agent through a crimping machine into a standardized coil.
进一步地，所述配料过程中需要考虑钛和硼的收得率。Further, the yield of titanium and boron needs to be considered during the compounding process.
本发明另一方面提供一种基于上述工艺制备的铝-钛-硼细化剂板带。Another aspect of the present invention provides an aluminum-titanium-boron refiner strip prepared based on the above process.
发明的有益效果The beneficial effects of the invention
有益效果Beneficial effect
本发明的有益效果为：The beneficial effects of the present invention are:
1.本发明的采用先制备铝钛和铝硼中间合金熔体，再把铝-钛和铝-硼熔体的温度控制到合适的温度，然后把铝-钛和铝-硼熔体进行混合反应的方式，通过控制熔体温度和混合反应时间，来控制TiB 2颗粒的大小，并利用铸轧工艺的快速凝固实现细化剂中活性质点的均匀分布，避免聚集和成团； 1. The use of the present invention first prepares aluminum-titanium and aluminum-boron intermediate alloy melts, then controls the temperature of the aluminum-titanium and aluminum-boron melts to a suitable temperature, and then mixes the aluminum-titanium and aluminum-boron melts The way of reaction is to control the size of TiB 2 particles by controlling the melt temperature and mixing reaction time, and use the rapid solidification of the casting-rolling process to achieve a uniform distribution of active particles in the refiner to avoid aggregation and agglomeration;
2.本发明工艺简单，操作方便，解决了传统工艺方法制备的铝-钛-硼细化剂中的TiAl 3、TiB 2粒子分布不均，数量少，尺寸较大的问题，提高了细化效率。 2. The present invention has simple process and convenient operation, and solves the problems of uneven distribution, small quantity and large size of TiAl 3 and TiB 2 particles in the aluminum-titanium-boron refiner prepared by the traditional process method, and improves the refinement effectiveness.
对附图的简要说明Brief description of the drawings
附图说明Description of the drawings
图1为本发明制备工艺流程图；Figure 1 is a flow chart of the preparation process of the present invention;
附图标记为：1、铝-钛中间合金熔炼炉；2、铝-硼中间合金熔炼炉；3、反应炉；4、静置炉；5、铸咀；6、铸轧机；7、卷取机；The reference signs are: 1. Aluminum-titanium master alloy melting furnace; 2. Aluminum-boron master alloy melting furnace; 3. Reaction furnace; 4. Standing furnace; 5. Casting nozzle; 6. Casting rolling mill; 7. Coiler ；
图2为实施例1中Al-Ti-B中间合金微观组织结构图(金相图)；Figure 2 is a microstructure diagram (metallographic diagram) of the Al-Ti-B master alloy in Example 1;
图3为实施例2中Al-Ti-B中间合金微观组织结构图(金相图)；Figure 3 is a microstructure diagram (metallographic diagram) of the Al-Ti-B master alloy in Example 2;
图4为实施例3中Al-Ti-B中间合金微观组织结构图(金相图)；Figure 4 is a microstructure diagram (metallographic diagram) of the Al-Ti-B master alloy in Example 3;
图5为实施例4中Al-Ti-B中间合金微观组织结构图(金相图)；Figure 5 is a microstructure diagram (metallographic diagram) of the Al-Ti-B master alloy in Example 4;
图6为传统工艺制备的Al-Ti-B细化剂中间合金微观组织结构图(金相图)。Figure 6 is a microstructure diagram (metallographic diagram) of the Al-Ti-B refiner master alloy prepared by the traditional process.
发明实施例Invention embodiment
本发明的实施方式Embodiments of the invention
为了使本发明的目的、技术方案及优点更加清楚明白，以下结合附图及实施例，对本发明进行进一步详细说明。应当理解，此处所描述的具体实施例仅用以解释本发明，并不用于限定本发明。In order to make the objectives, technical solutions, and advantages of the present invention clearer, the following further describes the present invention in detail with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described here are only used to explain the present invention, but not to limit the present invention.
如图1所示，本发明的流程为：先分别在熔炼炉(1、2)中制备铝-钛和铝-硼中间合金熔体，控制中间合金熔体温度，然后在反应炉(3)中进行铝-钛和铝-硼中间合金熔体混合反应，控制混合熔体温度和混合反应时间，然后将混合熔体转移至静置炉(4)，通过铸轧机(6)铸轧成板，最后通过卷曲机(7)绕制成规范的盘卷。As shown in Figure 1, the process of the present invention is as follows: first prepare aluminum-titanium and aluminum-boron master alloy melts in the smelting furnace (1, 2), control the temperature of the master alloy melt, and then in the reaction furnace (3) In the process, the aluminum-titanium and aluminum-boron master alloy melts are mixed and reacted, the temperature of the mixed melt and the mixing reaction time are controlled, and then the mixed melt is transferred to the static furnace (4), and cast-rolled into a plate by the casting-rolling machine (6). Finally, it is wound into a standard coil by a crimper (7).
实施例1Example 1
1.配料：按照Ti∶B＝10∶1的成分比例对铝-钛中间合金、铝-硼中间合金进行配料并称重，其中，铝-钛中间合金，钛的含量为10％；铝-硼中间合金，硼含量为2％；原料采用工业纯铝锭、海绵钛和硼酸钾，其中工业纯铝锭Al的纯度为99.85％；1. Batching: According to the composition ratio of Ti:B=10:1, the aluminum-titanium master alloy and the aluminum-boron master alloy are batched and weighed. Among them, the aluminum-titanium master alloy has a titanium content of 10%; aluminum- Boron master alloy with a boron content of 2%; raw materials are industrial pure aluminum ingots, sponge titanium and potassium borate, among which the purity of industrial pure aluminum ingots Al is 99.85%;
2.熔炼：将铝锭分别放入铝-钛、铝-硼中间合金熔炼炉内，两个熔炼炉型号相同，加热，使铝锭完全熔化，当加热温度达到950℃时，向铝-钛中间合金熔炼炉中加入海绵钛，向铝-硼中间合金熔炼炉中加入硼酸钾，并对两熔体进行充分搅拌，然后保温30分钟，随后对两熔体进行扒渣，并把熔体温度降低到850℃时，等待进行混合反应；2. Melting: Put the aluminum ingots into the aluminum-titanium and aluminum-boron intermediate alloy smelting furnaces. The two smelting furnaces are of the same model. Heat them to completely melt the aluminum ingots. When the heating temperature reaches 950℃, Sponge titanium is added to the master alloy smelting furnace, potassium borate is added to the aluminum-boron master alloy smelting furnace, and the two melts are fully stirred, and then kept for 30 minutes. Then the two melts are slag off and the melt temperature When it is lowered to 850℃, wait for the mixing reaction;
3.把熔炼好的铝-钛和铝-硼中间合金熔体转入到反应炉中，并进行搅拌，使两熔体充分接触、反应，然后在850℃的温度下保温30分钟，然后在把熔体温度降低到720℃，等待转入中间包或静置炉进行铸轧；3. Transfer the smelted aluminum-titanium and aluminum-boron master alloy melts into the reaction furnace, and stir to make the two melts fully contact and react, and then keep the temperature at 850℃ for 30 minutes, and then Reduce the melt temperature to 720℃, and wait for transfer to the tundish or static furnace for casting and rolling;
4.铸轧：把保温后的混合熔体倒入中间包或静置炉，进行铸轧成板，铸轧机采用卧式铸轧机，铸轧温度700℃，铸轧辊直径1000mm，铸轧厚度7mm，铸轧速度1m/min，混合熔体经过铸轧机后获得厚度为7mm的板状铝钛硼细化剂。4. Casting and rolling: Pour the heat-preserved mixed melt into a tundish or a static furnace for casting and rolling into a plate. The casting-rolling machine adopts a horizontal casting-rolling mill, the casting temperature is 700℃, the casting roll diameter is 1000mm, and the casting thickness is 7mm. The casting-rolling speed is 1m/min. After the mixed melt passes through the casting-rolling machine, a plate-shaped aluminum titanium boron refiner with a thickness of 7 mm is obtained.
实施例2Example 2
1.配料：按照Ti∶B＝5∶1的成分比例对铝-钛中间合金、铝-硼中间合金进行配料并称重，其中，铝-钛中间合金，钛的含量为20％；铝-硼中间合金，硼含量为4％；原料采用工业纯铝锭、钛酸钾和硼酸钾，其中工业纯铝锭Al的纯度为99.85％；1. Batching: According to the composition ratio of Ti:B=5:1, the aluminum-titanium master alloy and the aluminum-boron master alloy are batched and weighed. Among them, the content of titanium in the aluminum-titanium master alloy is 20%; Boron master alloy with a boron content of 4%; raw materials are industrial pure aluminum ingots, potassium titanate and potassium borate, of which the purity of industrial pure aluminum ingots Al is 99.85%;
2.熔炼：将铝锭分别放入铝-钛、铝-硼中间合金熔炼炉内，两个熔炼炉型号相同，加热，使铝锭完全熔化，当加热温度达到900℃时，向铝-钛中间合金熔炼 炉中加入钛酸钾，向铝-硼中间合金熔炼炉中加入硼酸钾，并对两熔体进行充分搅拌，然后保温30分钟，随后对两熔体进行扒渣，并把熔体温度降低到800℃时，等待进行混合反应；2. Melting: Put the aluminum ingots into the aluminum-titanium and aluminum-boron intermediate alloy melting furnaces. The two melting furnaces are of the same model. Heat to completely melt the aluminum ingots. When the heating temperature reaches 900℃, the aluminum-titanium Potassium titanate is added to the master alloy smelting furnace, potassium borate is added to the aluminum-boron master alloy smelting furnace, and the two melts are fully stirred, and then kept for 30 minutes, then the two melts are slagging off and the melt When the temperature drops to 800℃, wait for the mixing reaction;
3.把熔炼好的铝-钛和铝-硼中间合金熔体转入到反应炉中，并进行搅拌，使两熔体充分接触、反应，然后在800℃的温度下保温45分钟，然后在把熔体温度降低到720℃，等待转入中间包或静置炉进行铸轧；3. Transfer the smelted aluminum-titanium and aluminum-boron master alloy melts into the reaction furnace and stir to make the two melts fully contact and react, and then keep them at 800℃ for 45 minutes, and then Reduce the melt temperature to 720℃, and wait for transfer to the tundish or static furnace for casting and rolling;
4.铸轧：把保温后的混合熔体倒入中间包或静置炉，进行铸轧成板，铸轧机采用卧式铸轧机，铸轧温度690℃，铸轧辊直径820mm，铸轧厚度6mm，铸轧速度1.2m/min，混合熔体经过铸轧机后获得厚度为6mm的板状铝钛硼细化剂。4. Casting and rolling: Pour the heat-preserved mixed melt into a tundish or a static furnace for casting and rolling into a plate. The casting-rolling machine adopts a horizontal casting-rolling machine with a casting temperature of 690°C, a casting roll diameter of 820mm, and a casting thickness of 6mm. The casting-rolling speed is 1.2m/min. After the mixed melt passes through the casting-rolling machine, a plate-shaped aluminum titanium boron refiner with a thickness of 6 mm is obtained.
实施例3Example 3
1.配料：按照Ti∶B＝4∶1的成分比例对铝-钛中间合金、铝-硼中间合金进行配料并称重，其中，铝-钛中间合金，钛的含量为16％；铝-硼中间合金，硼含量为2％；原料采用工业纯铝锭、钛酸钾和硼酸钾，其中工业纯铝锭Al的纯度为99.85％；1. Batching: According to the composition ratio of Ti:B=4:1, the aluminum-titanium master alloy and the aluminum-boron master alloy are batched and weighed. Among them, the aluminum-titanium master alloy has a titanium content of 16%; aluminum- Boron master alloy with a boron content of 2%; raw materials are industrial pure aluminum ingots, potassium titanate and potassium borate, and the purity of industrial pure aluminum ingots Al is 99.85%;
2.熔炼：将铝锭分别放入铝-钛、铝-硼中间合金熔炼炉内，两个熔炼炉型号相同，加热，使铝锭完全熔化，当加热温度达到950℃时，向铝-钛中间合金熔炼炉中加入钛酸钾，向铝-硼中间合金熔炼炉中加入硼酸钾，并对两熔体进行充分搅拌，然后保温30分钟，随后对两熔体进行扒渣，并把熔体温度降低到750℃时，等待进行混合反应；2. Melting: Put the aluminum ingots into the aluminum-titanium and aluminum-boron intermediate alloy smelting furnaces. The two smelting furnaces are of the same model. Heat them to completely melt the aluminum ingots. When the heating temperature reaches 950℃, Potassium titanate is added to the master alloy smelting furnace, potassium borate is added to the aluminum-boron master alloy smelting furnace, and the two melts are fully stirred, and then kept for 30 minutes, then the two melts are slagging off and the melt When the temperature drops to 750℃, wait for the mixing reaction;
3.把熔炼好的铝-钛和铝-硼中间合金熔体转入到反应炉中，并进行搅拌，使两熔体充分接触、反应，然后在750℃的温度下保温60分钟，然后在把熔体温度降低到720℃，等待转入中间包或静置炉进行铸轧；3. Transfer the smelted aluminum-titanium and aluminum-boron master alloy melts into the reaction furnace and stir to make the two melts fully contact and react, and then keep them at 750℃ for 60 minutes, and then Reduce the melt temperature to 720℃, and wait for transfer to the tundish or static furnace for casting and rolling;
4.铸轧：把保温后的混合熔体倒入中间包或静置炉，进行铸轧成板，铸轧机采用卧式铸轧机，铸轧温度695℃，铸轧辊直径920mm，铸轧厚度8mm，铸轧速度0.8m/min，混合熔体经过铸轧机后获得厚度为8mm的板状铝钛硼细化剂。4. Casting and rolling: Pour the heat-preserved mixed melt into a tundish or a static furnace for casting and rolling into a plate. The casting-rolling machine adopts a horizontal casting-rolling machine, the casting temperature is 695℃, the casting roll diameter is 920mm, and the casting thickness is 8mm. The casting-rolling speed is 0.8m/min. After the mixed melt passes through the casting-rolling machine, a plate-shaped aluminum titanium boron refiner with a thickness of 8 mm is obtained.
实施例4Example 4
1.配料：按照Ti∶B＝3∶1的成分比例对铝-钛中间合金、铝-硼中间合金进行配料并称重，其中，铝-钛中间合金，钛含量为9％；铝-硼中间合金，硼含量为3％； 原料采用工业纯铝锭、钛酸钾和硼酸钾，其中工业纯铝锭Al的纯度为99.85％；1. Batching: According to the composition ratio of Ti:B=3:1, the aluminum-titanium master alloy and the aluminum-boron master alloy are batched and weighed. Among them, the aluminum-titanium master alloy has a titanium content of 9%; aluminum-boron The intermediate alloy has a boron content of 3%; the raw materials are industrial pure aluminum ingots, potassium titanate and potassium borate, and the purity of the industrial pure aluminum ingots Al is 99.85%;
2.熔炼：将铝锭分别放入铝-钛、铝-硼中间合金熔炼炉内，两个熔炼炉型号相同，加热，使铝锭完全熔化，当加热温度达到950℃时，向铝-钛中间合金熔炼炉中加入钛酸钾，向铝-硼中间合金熔炼炉中加入硼酸钾，并对两熔体进行充分搅拌，然后保温50分钟，随后对两熔体进行扒渣，并把熔体温度降低到900℃时，等待进行混合反应；2. Melting: Put the aluminum ingots into the aluminum-titanium and aluminum-boron intermediate alloy smelting furnaces. The two smelting furnaces are of the same model. Heat them to completely melt the aluminum ingots. When the heating temperature reaches 950℃, Potassium titanate is added to the master alloy smelting furnace, potassium borate is added to the aluminum-boron master alloy smelting furnace, and the two melts are fully stirred, and then kept for 50 minutes, and then the two melts are slag off and the melt When the temperature drops to 900℃, wait for the mixing reaction;
3.把熔炼好的铝-钛和铝-硼中间合金熔体转入到反应炉中，并进行搅拌，使两熔体充分接触、反应，然后在900℃的温度下保温10分钟，然后在把熔体温度快速降低到720℃，等待转入中间包或静置炉进行铸轧；3. Transfer the smelted aluminum-titanium and aluminum-boron master alloy melts into the reaction furnace and stir to make the two melts fully contact and react, and then keep the temperature at 900℃ for 10 minutes, and then Reduce the melt temperature to 720℃ quickly, and wait for transfer to the tundish or static furnace for casting and rolling;
4.铸轧：把保温后的混合熔体倒入中间包或静置炉，进行铸轧成板，铸轧机采用立式铸轧机，铸轧温度705℃，铸轧辊直径500mm，铸轧厚度2mm，铸轧速度5m/min，混合熔体经过铸轧机后获得厚度为2mm的板状铝钛硼细化剂。4. Casting and rolling: Pour the heat-preserved mixed melt into a tundish or a static furnace for casting and rolling into a plate. The casting-rolling machine adopts a vertical casting-rolling machine with a casting temperature of 705°C, a casting roll diameter of 500mm, and a casting thickness of 2mm. The casting-rolling speed is 5m/min. After the mixed melt passes through the casting-rolling mill, a plate-shaped aluminum titanium boron refiner with a thickness of 2 mm is obtained.
实施例1～4制备的Al-Ti-B细化剂微观组织结构图如图2～5所示，通过传统工艺制备的Al-Ti-B细化剂如图6所示，明显看出，本发明所述工艺制备的Al-Ti-B细化剂的TiAl 3、TiB 2活性质点数量明显增多，尺寸明显减小，并且弥散分布，达到理想效果，能满足高质量铝材的需求。 The microstructure of the Al-Ti-B refiner prepared in Examples 1 to 4 is shown in Figures 2 to 5, and the Al-Ti-B refiner prepared by the traditional process is shown in Figure 6, which clearly shows that The TiAl 3 and TiB 2 active particles of the Al-Ti-B refining agent prepared by the process of the present invention are obviously increased, the size is obviously reduced, and the dispersed distribution achieves the ideal effect and can meet the demand for high-quality aluminum materials.
以上技术方案阐述了本发明的技术思路，不能以此限定本发明的保护范围，凡是未脱离本发明技术方案的内容，依据本发明的技术实质对以上技术方案所作的任何改动及修饰，均属于本发明技术方案的保护范围。The above technical solutions illustrate the technical ideas of the present invention and cannot be used to limit the scope of protection of the present invention. Any changes and modifications made to the above technical solutions based on the technical essence of the present invention without departing from the technical solutions of the present invention belong to The protection scope of the technical solution of the present invention.

Claims (6)

  1. 一种铝-钛-硼细化剂板带的制备工艺，其流程为：细化剂合金熔体的制备-铸轧-卷曲，其特征在于，其中细化剂合金熔体的制备方法包括如下步骤：分别制备铝-钛和铝-硼中间合金熔体，控制中间合金熔体温度为750～900℃；将铝-钛和铝-硼中间合金熔体进行混合反应，并在750～900℃下保温10～60分钟，然后把混合熔体温度降低至710～750℃。A process for preparing aluminum-titanium-boron refiner strips. The process is: preparation of refiner alloy melt-casting-rolling, characterized in that the preparation method of refiner alloy melt includes the following Steps: Prepare aluminum-titanium and aluminum-boron master alloy melts respectively, and control the temperature of the master alloy melt to be 750～900℃; mix and react the aluminum-titanium and aluminum-boron master alloy melts at 750～900℃ Keep the temperature for 10-60 minutes, and then lower the temperature of the mixed melt to 710-750°C.
  2. 根据权利要求1所述的一种铝-钛-硼细化剂板带的制备工艺，其特征在于，以质量分数计，所述铝-钛中间合金中，钛含量为8％～20％，所述铝-硼中间合金中，硼含量为1％～5％，其中铝-钛、铝-硼中间合金配比根据所需钛与硼的比例配入。The preparation process of an aluminum-titanium-boron refiner strip according to claim 1, wherein the content of titanium in the aluminum-titanium master alloy is 8-20% in terms of mass fraction. In the aluminum-boron master alloy, the boron content is 1% to 5%, and the ratio of the aluminum-titanium and aluminum-boron master alloy is mixed according to the required ratio of titanium to boron.
  3. 根据权利要求2所述的一种铝-钛-硼细化剂板带的制备工艺，其特征在于，所述细化剂合金熔体的制备方法具体包括如下步骤：The process for preparing aluminum-titanium-boron thinner strips according to claim 2, wherein the method for preparing the thinner alloy melt specifically comprises the following steps:
    (1)配料：按配比进行中间合金配料，其中，铝采用工业纯铝锭，钛和硼可以采用钛盐或金属钛和硼盐；(1) Batching: The batching of the intermediate alloy is carried out according to the proportioning. Among them, the aluminum uses industrial pure aluminum ingots, and the titanium and boron can use titanium salts or metallic titanium and boron salts;
    (2)中间合金熔体的制备：(2) Preparation of master alloy melt:
    铝-钛中间合金熔体的制备：采用熔炼炉加热铝锭使其熔化，当温度达到850～950℃，向铝熔体中加入配好料的金属钛或钛盐，并进行搅拌，使金属钛或钛盐与铝进行充分接触、反应，并使金属钛或钛盐完全溶解到铝熔体中，保温30～60分钟，然后进行扒渣，降温至750～900℃，备用；Preparation of aluminum-titanium master alloy melt: use a smelting furnace to heat the aluminum ingot to melt it. When the temperature reaches 850 to 950°C, add the prepared metal titanium or titanium salt to the aluminum melt, and stir to make the metal The titanium or titanium salt fully contacts and reacts with the aluminum, and the metal titanium or titanium salt is completely dissolved in the aluminum melt, and the temperature is kept for 30-60 minutes, then the slag is removed, and the temperature is reduced to 750-900°C for use;
    铝-硼中间合金熔体的制备：采用铝-硼中间合金原料，其余制备方法与铝-钛中间合金熔体的制备方法相同；Preparation of aluminum-boron master alloy melt: use aluminum-boron master alloy raw materials, and the other preparation methods are the same as those of aluminum-titanium master alloy melt;
    (3)反应控制：将备用的铝-钛、铝-硼中间合金熔体转入反应炉内，并进行充分搅拌，控制混合溶体的温度和保温时间，降温后转移至中间包或静置炉，等待铸轧成板。(3) Reaction control: Transfer the spare aluminum-titanium and aluminum-boron master alloy melts into the reaction furnace, and fully stir them, control the temperature and holding time of the mixed solution, and transfer to the tundish or static furnace after cooling. Waiting for casting and rolling into plate.
  4. 根据权利要求1所述的一种铝-钛-硼细化剂板带的制备工艺，其特征在于，所述铸轧工艺为：采用立式或卧式铸轧机进行铸轧，铸 轧辊的直径在500～1050mm，铸轧板厚度在2～10mm，铸轧温度在680～715℃，铸轧速度控制在0.5～5m/min。The preparation process of an aluminum-titanium-boron refiner strip according to claim 1, wherein the casting-rolling process is: using a vertical or horizontal casting-rolling mill for casting, and the diameter of the casting roll At 500～1050mm, the thickness of cast-rolled sheet is 2～10mm, the casting temperature is 680～715℃, and the casting speed is controlled at 0.5～5m/min.
  5. 根据权利要求3所述的一种铝-钛-硼细化剂板带的制备工艺，其特征在于，所述配料过程中需要考虑钛和硼的收得率。The preparation process of an aluminum-titanium-boron thinner strip according to claim 3, wherein the yield of titanium and boron needs to be considered in the batching process.
  6. 一种铝-钛-硼细化剂板带，其特征在于：所述铝-钛-硼细化剂板带基于权利要求1～5其中任意一项工艺制备而成。An aluminum-titanium-boron thinning agent strip, characterized in that: the aluminum-titanium-boron thinning agent strip is prepared based on any one of the processes of claims 1 to 5.
PCT/CN2019/099563 2019-07-12 2019-08-07 Process for preparing aluminum-titanium-boron refiner plate and strip WO2021007893A1 (en)

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