CN117987673A - Preparation method of large-diameter high-cleanliness fine-grain homogeneous aluminum alloy casting rod - Google Patents
Preparation method of large-diameter high-cleanliness fine-grain homogeneous aluminum alloy casting rod Download PDFInfo
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- 238000007670 refining Methods 0.000 claims abstract description 96
- 239000007789 gas Substances 0.000 claims abstract description 38
- 238000001914 filtration Methods 0.000 claims abstract description 23
- 238000007872 degassing Methods 0.000 claims abstract description 22
- 239000011449 brick Substances 0.000 claims abstract description 13
- 238000007664 blowing Methods 0.000 claims abstract description 12
- 238000000265 homogenisation Methods 0.000 claims abstract description 12
- 238000003723 Smelting Methods 0.000 claims abstract description 9
- 238000009749 continuous casting Methods 0.000 claims abstract description 9
- 239000003795 chemical substances by application Substances 0.000 claims description 69
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 56
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 41
- INHCSSUBVCNVSK-UHFFFAOYSA-L lithium sulfate Inorganic materials [Li+].[Li+].[O-]S([O-])(=O)=O INHCSSUBVCNVSK-UHFFFAOYSA-L 0.000 claims description 31
- 238000002844 melting Methods 0.000 claims description 29
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- 238000006356 dehydrogenation reaction Methods 0.000 claims description 23
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 claims description 22
- 229910052757 nitrogen Inorganic materials 0.000 claims description 20
- 238000010438 heat treatment Methods 0.000 claims description 19
- 239000011261 inert gas Substances 0.000 claims description 17
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 16
- 238000000034 method Methods 0.000 claims description 15
- 239000002994 raw material Substances 0.000 claims description 15
- 229910002804 graphite Inorganic materials 0.000 claims description 14
- 239000010439 graphite Substances 0.000 claims description 14
- OTYBMLCTZGSZBG-UHFFFAOYSA-L potassium sulfate Chemical compound [K+].[K+].[O-]S([O-])(=O)=O OTYBMLCTZGSZBG-UHFFFAOYSA-L 0.000 claims description 14
- 229910052939 potassium sulfate Inorganic materials 0.000 claims description 14
- 229910000027 potassium carbonate Inorganic materials 0.000 claims description 13
- 238000001816 cooling Methods 0.000 claims description 12
- 239000002245 particle Substances 0.000 claims description 12
- 239000000460 chlorine Substances 0.000 claims description 11
- 239000000203 mixture Substances 0.000 claims description 11
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims description 9
- 229910052801 chlorine Inorganic materials 0.000 claims description 9
- 239000000843 powder Substances 0.000 claims description 9
- -1 aluminum titanium boron Chemical group 0.000 claims description 8
- 238000004519 manufacturing process Methods 0.000 claims description 8
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- 239000000498 cooling water Substances 0.000 claims description 6
- 239000003595 mist Substances 0.000 claims description 6
- 239000011592 zinc chloride Substances 0.000 claims description 6
- 229910000521 B alloy Inorganic materials 0.000 claims description 5
- 229910001339 C alloy Inorganic materials 0.000 claims description 3
- 238000005273 aeration Methods 0.000 claims description 2
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- 239000002893 slag Substances 0.000 abstract description 21
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 abstract description 19
- 239000001257 hydrogen Substances 0.000 abstract description 19
- 229910052739 hydrogen Inorganic materials 0.000 abstract description 19
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- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 27
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- 239000012535 impurity Substances 0.000 description 16
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- 229910001094 6061 aluminium alloy Inorganic materials 0.000 description 5
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- JIAARYAFYJHUJI-UHFFFAOYSA-L zinc dichloride Chemical compound [Cl-].[Cl-].[Zn+2] JIAARYAFYJHUJI-UHFFFAOYSA-L 0.000 description 4
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- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 2
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- VHHHONWQHHHLTI-UHFFFAOYSA-N hexachloroethane Chemical compound ClC(Cl)(Cl)C(Cl)(Cl)Cl VHHHONWQHHHLTI-UHFFFAOYSA-N 0.000 description 2
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- 159000000000 sodium salts Chemical class 0.000 description 2
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- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 1
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Abstract
The invention discloses a preparation method of a large-diameter high-cleanliness fine-grain homogeneous aluminum alloy casting rod, which sequentially comprises the following steps: smelting to prepare aluminum alloy liquid, blowing refining slag in a furnace, refining and removing hydrogen from an air brick at the bottom of the furnace, refining grains on line, removing hydrogen on line by a degassing box, filtering slag on line by a deep bed filter box or a tubular filter box, semi-continuous casting by oil gas sliding and homogenizing at high temperature. According to the invention, through scientifically designing the smelting and casting process of the aluminum alloy, the gas slag content of the aluminum alloy liquid is reduced, the cleanliness of the aluminum alloy casting rod is improved, the crystal grains of the aluminum alloy casting rod are thinned, coarse intermetallic compounds are melted through high-temperature homogenization treatment, component segregation is eliminated, the structural component uniformity and extrusion performance of the large-diameter aluminum alloy casting rod are improved, and the requirements of the fields of new energy automobiles, rail transit, photovoltaic power generation, electronic communication, ultra-high voltage transmission and the like on high-clean and high-performance aluminum alloy extrusion materials are met.
Description
Technical Field
The invention belongs to the technical field of aluminum alloy preparation, and particularly relates to a preparation method of a large-diameter high-cleanliness fine-grain homogeneous aluminum alloy casting rod.
Background
The aluminum alloy has the advantages of low density, high specific strength, corrosion resistance, anodic oxidation, easy processing and forming, recycling and the like, and is widely applied to the fields of building, electric power, electronic communication, transportation, mechanical equipment, aerospace, weaponry and the like. In recent years, with the rapid development of new energy sources such as new energy automobiles, photovoltaic power generation, 5G communication, ultra-high voltage transmission, high-speed rail transit and the like and new infrastructure industry in China, the requirements on the performances such as mechanics, oxidation coloring, electric conduction and heat conduction, corrosion resistance and fatigue resistance of aluminum products are higher and higher.
Hydrogen pores and inclusions are common defects in the aluminum alloy casting rod and finally remain in the aluminum product, so that the mechanical, electric and heat conduction, oxidation coloring, corrosion resistance, fatigue resistance and the like of the aluminum product are reduced. The grain structure of the aluminum alloy casting rod is thinned, the uniformity of the structural components is improved, the performance of the aluminum product is improved, and the extrusion speed and the surface quality of the aluminum product are improved. Therefore, the high-purity fine-grain homogeneous aluminum alloy casting rod is the basis and key for producing high-performance aluminum products.
The patent application with publication number CN112605352A discloses a casting method of an aluminum alloy casting rod, by optimizing the chemical composition elements of the aluminum alloy casting rod and the structure of a crystallizer, when the aluminum alloy casting rod is cast, the temperature, the stirring speed and the stirring time can be controlled more accurately through a controller, the uniformity of the internal temperature of an aluminum alloy melt can be ensured while the formability of the aluminum alloy melt is ensured, the non-uniform nucleation is increased, the effect of grain refinement is generated, the tendency of cracking of the casting rod is further reduced, the casting quality and the yield are improved, and the problem that the internal cracking of the casting rod is caused due to the non-uniform temperature of the melt when the large-diameter aluminum alloy casting rod is cast is solved.
The patent application with publication number CN110923526A discloses a preparation method of an oversized aluminum alloy round bar, which comprises the following ingredients: preparing soft starting materials and formal materials, and casting: and (3) filling the soft starting materials into a filter box, discharging the soft starting materials from the outlet end of the filter box, guiding the soft starting materials into a round bar crystallizer, guiding the main materials into the inlet end of the filter box, filling the aluminum melt to the height of 120-180mm, starting casting to obtain aluminum alloy round bars, and carrying out stress relief treatment. The patent solves the problems of uneven components, increased bottom cracks and gate cracks, high hydrogen content and slag content, coarse grains and the like in casting large-specification round bars.
The patent application with publication number CN109055786A discloses a production process of a 6-series aluminum alloy casting rod, which mainly comprises smelting, deslagging, refining, filtering, degassing and casting, wherein the refining agent adopted in the refining process is CaCO 3 and SrCO 3 powder which are uniformly mixed according to the mass ratio of 1-19:1, and then are ground into powder with the particle size of 30-40 mu m, an Al-Ti-B wire refiner is added in the refining process for carrying out online refining, a graphite rotor is adopted in the degassing process for degassing aluminum liquid, the hydrogen content of the aluminum liquid is basically controlled within 0.2ml/100gAl, and the problem that the refining effect is poor when the existing refining agent is applicable to the preparation of the 6-series aluminum alloy casting rod is solved.
From the results of production practice and document data retrieval, the aluminum alloy casting rod prepared by the prior art still has the problems of low cleanliness, coarse grains, excessively thick segregation phase, uneven structure components and the like, so that the aluminum product has low performance, poor surface quality, low extrusion speed, low yield and the like, and severely restricts the high-quality development of the aluminum processing industry. Thus, the existing aluminum alloy casting bar preparation technology still needs to be improved and developed.
Disclosure of Invention
The invention aims to solve the problems and the shortcomings, and provides a preparation method of a large-diameter high-cleanliness fine-grain homogeneous aluminum alloy casting rod.
The technical scheme of the invention is realized as follows:
the preparation method of the large-diameter high-cleanliness fine-grain homogeneous aluminum alloy casting rod is characterized by comprising the following steps in sequence:
(1) Smelting to prepare aluminum alloy liquid according to the component composition and mass percentage of the aluminum alloy casting rod;
(2) Adopting inert gas and a refining agent to carry out blowing refining deslagging treatment on aluminum alloy liquid in a furnace, then removing scum on the surface of the aluminum alloy liquid, and scattering a covering agent on the surface of the aluminum alloy liquid;
(3) Introducing inert gas into the aluminum alloy liquid in the furnace through the air brick arranged at the bottom of the furnace to carry out refining and dehydrogenation treatment;
(4) Introducing aluminum alloy liquid into a launder, and then adding a grain refiner into the aluminum alloy liquid in the launder to carry out grain refining treatment;
(5) The aluminum alloy liquid subjected to grain refinement treatment flows through a degassing tank arranged on a launder to carry out deep dehydrogenation treatment;
(6) Allowing the aluminum alloy liquid subjected to deep dehydrogenation treatment to flow through a deep bed filter box or a tubular filter box arranged on a launder for filtration treatment;
(7) The aluminum alloy liquid is semicontinuously cast into an aluminum alloy casting rod by adopting an oil-gas sliding semicontinuous casting machine;
(8) And carrying out high-temperature homogenization treatment on the aluminum alloy casting rod, and cooling by spraying water mist to obtain the large-diameter high-cleanliness fine-grain homogenized aluminum alloy casting rod.
Preferably, the inert gas in the step (2) is argon with the purity of more than or equal to 99.9% or nitrogen with the purity of more than or equal to 99.9%.
The higher the purity of the inert gas, the less water vapor is contained, which is beneficial to reducing the gas content of the aluminum alloy liquid in the furnace. Thus, the higher the grade of aluminum material produced, the higher the purity of the inert gas selected should be. However, the higher the purity of the inert gas, the higher the price and the corresponding increase in production costs.
Preferably, the amount of the refining agent in the step (2) is 0.2-0.4% by weight of the aluminum alloy liquid, and the blowing refining time is 20-30 minutes.
The blowing refining adopts a powder spraying tank and a stainless steel pipe, takes inert gas as a carrier, blows a powdery refining agent into the aluminum alloy liquid, enables the refining agent to fully contact and react with the aluminum alloy liquid, brings impurities in the aluminum alloy liquid to float up to the liquid level, achieves the deslagging effect, and has a certain dehydrogenation effect. The amount and refining time of the refining agent are closely related to the quality of the refining agent, and the higher the quality of the refining agent is, the smaller the amount and the smaller the refining time can be.
Preferably, the refining agent in the step (2) is composed of the following components in percentage by mass ：ZnCl2 40-50％,K2CO3 20-30％,NaNO3 5-10％,KF 8-13％,K2SO4 5-8％,Li2SO4 3-5％.
Preferably, the preparation method of the refining agent in the step (2) sequentially comprises the following steps: (1) ZnCl 2、K2CO3、NaNO3、KF、K2SO4、Li2SO4 with the purity more than or equal to 99.8 percent is selected as a raw material for batching; (2) Heating and melting raw materials at 1150-1200 ℃ under the protection of argon with purity more than or equal to 99.99%, and then cooling and solidifying the block refining agent; (3) And (3) crushing the block refining agent into powder with the particle size less than or equal to 2 mm to obtain the refining agent.
The cleanliness of the aluminum alloy liquid in the furnace affects the cleanliness of the final aluminum alloy cast rod, and the cleanliness of the aluminum alloy liquid in the furnace is closely related to the quality of the refining agent. The existing refining agent is mainly prepared by directly crushing and mixing raw materials such as sodium salt, fluoride salt, chloride salt, hexachloroethane and the like, and does not exert interaction among the raw materials, so that the refining agent has high melting point, low slag removal efficiency and slag removal rate of 30-40 percent. In order to improve the cleanliness of aluminum alloy liquid in a furnace, the inventor develops a more efficient and environment-friendly refining agent through a large number of experimental researches, the refining agent takes ZnCl 2 as a main component, a small amount of K 2CO3、NaNO3、KF、K2SO4、Li2SO4 is matched, raw materials are heated and melted at 1150-1200 ℃ under the protection of high-purity argon, then are cooled, solidified and crushed into a powdery refining agent, the melting point of ZnCl 2 in the refining agent is 290 ℃, and the melting point of NaNO 3 is 306.8 ℃, so that the refining agent is very easy to melt in the aluminum alloy liquid. The melting point of K 2CO3 is 891 ℃, the melting point of KF is 858 ℃, the melting point of K 2SO4 is 1069 ℃, the melting point of Li 2SO4 is 859 ℃, and although the melting point of K 2CO3、KF、K2SO4、Li2SO4 is higher, KF 2CO3 and KF can form KF-K 2CO3 eutectic with the melting point of only 688 ℃, K 2 SO4 and Li 2SO4 can form K 2SO4·Li2SO4 eutectic with the melting point of only 716 ℃, SO that the melting point of the refining agent is further greatly reduced, the refining agent is easier to melt in an aluminum alloy liquid, wherein ZnCl 2 is decomposed into Cl 2,K2CO3 and CO 2,NaNO3 is decomposed into N 2、CO2 and NO gas, and a large number of bubbles capture impurities in the aluminum alloy liquid in the floating process, thereby achieving the effect of efficient slag removal. The K 2SO4·Li2SO4 eutectic is melted into liquid molten salt, which has good wetting spheroidization effect on inclusions such as alumina, promotes the separation of the inclusions and aluminum liquid, can further improve the deslagging efficiency, and has the deslagging rate of 50 percent. In addition, the refining agent does not contain sodium salt and hexachloroethane, only contains a small amount of fluoride salt, and is more environment-friendly to use.
Preferably, the inert gas in step (3) is argon with a purity of 99.99% or more or nitrogen with a purity of 99.99% or more.
Preferably, the inert gas flow rate in step (3) is 0.3-0.6 cubic meters per minute and the aeration time is 10-20 minutes.
The degassing of the furnace bottom air brick is to install a plurality of air bricks with a large number of holes at the bottom of an aluminum melting furnace, then to introduce inert gas into the aluminum alloy liquid in the furnace through the air bricks, the inert gas is decomposed into tiny and uniform small bubbles after passing through the porous air bricks, the small bubbles capture hydrogen in the aluminum alloy liquid in the floating process, and then the aluminum alloy liquid is floated up to play a role in removing hydrogen. Because the bottom of the aluminum melting furnace is uniformly provided with a plurality of air bricks, the air bubbles are uniformly distributed in the aluminum alloy liquid, and the inert gas bubbles have stirring effect on the aluminum alloy liquid when floating upwards, so that the dehydrogenation efficiency is improved, and dead angles are avoided. The hydrogen content of the aluminum alloy liquid in the furnace can be reduced to below 0.2ml/100gAl by refining and removing hydrogen in the furnace through the air brick, so that the cleanliness of the aluminum alloy liquid in the furnace is greatly improved.
Preferably, in the step (4), the grain refiner is an aluminum titanium boron alloy wire or an aluminum titanium carbon alloy wire, and the adding amount of the grain refiner is 0.1-0.3% of the weight of the aluminum alloy liquid.
The grain refiner is slowly added into the aluminum alloy liquid according to the flow of the aluminum alloy liquid in the launder by adopting a wire feeder, so that the grain refining effect of the grain refiner can be exerted to the greatest extent, the grain structure of the aluminum alloy casting rod is obviously refined, and the structure uniformity of the aluminum alloy casting rod is improved. Generally, the larger the addition amount of the grain refiner is, the better the grain refining effect is, but too much grain refiner is added, the refining effect is not increased proportionally, but the production cost is increased. Thus, the addition amount of the grain refiner should be reasonably selected according to the characteristics of the aluminum alloy and the grade of the aluminum product.
Preferably, in the step (5), the rotating speed of the graphite rotor in the degassing tank is 300-500 rpm, the gas flow rate on the graphite rotor is 1-5 cubic meters per hour, and the gas pressure is 0.3-0.9MPa.
Preferably, the gas introduced into the degassing tank in the step (5) is argon with the purity of more than or equal to 99.99%, or nitrogen with the purity of more than or equal to 99.99%, or mixed gas composed of argon with the purity of more than or equal to 99.99%, or nitrogen with the purity of more than or equal to 99.99% and chlorine with the purity of more than or equal to 99.99%, and the volume percentage of the chlorine in the mixed gas is 1-5%.
The dehydrogenation of the degassing tank is that a graphite rotor rotating at high speed in the degassing tank breaks mixed gas consisting of argon, nitrogen or chlorine-containing gas into tiny bubbles and enters the aluminum alloy liquid, and hydrogen atoms in the aluminum alloy liquid are continuously diffused into the bubbles by utilizing partial pressure difference of hydrogen between the aluminum alloy liquid and the bubbles and then float upwards along with the bubbles to escape from the aluminum alloy liquid, so that the dehydrogenation effect is achieved. After the dehydrogenation of the degassing tank, the hydrogen content of the aluminum alloy liquid can be reduced to below 0.1ml/100gAl, thereby greatly improving the cleanliness of the aluminum alloy liquid.
The filter medium of the deep-bed filter box in the step (6) is formed by stacking alumina balls or particles with different particle diameters layer by layer according to a certain proportion, and the removal rate of impurities with the particle diameter of more than 5 mu m in the filtered aluminum alloy liquid can reach more than 95 percent. The filter medium of the tubular filter box is a ceramic tube formed by sintering silicon nitride ceramic particles with the particle size of 2-6mm and a binder at high temperature, a large number of zigzag pores are formed in the ceramic tube, and when aluminum alloy liquid flows through the ceramic filter tube, impurities are adsorbed or blocked on the surface of the ceramic filter tube and the inner walls of the pores, so that the filtering and deslagging effects are achieved. The removal rate of the impurities above 5 mu m in the aluminum alloy liquid after filtration can reach above 98 percent. The deep-bed filtration and the tubular filtration belong to high-precision filtration, and the deep-bed filtration or the tubular filtration is selected according to the specific requirements of aluminum products, but the filtering effect of the deep-bed filtration or the tubular filtration is far better than that of a foam ceramic plate, so that the cleanliness of the aluminum alloy casting rod can be greatly improved.
Preferably, the temperature of the aluminum alloy liquid in the step (7) is 680-720 ℃, the semi-continuous casting speed is 50-200 mm/min, and the cooling water temperature is less than or equal to 40 ℃.
The oil gas is introduced into the graphite ring in the casting crystallizer to form a layer of oil gas film between the graphite ring and the aluminum alloy liquid, and the thickness of a segregation layer on the surface of the casting rod is greatly reduced by reducing the chilling of the aluminum alloy liquid, so that the aluminum alloy casting rod with a smooth surface is obtained. In order to obtain high quality aluminum alloy cast bars, strict adherence to the operating regulations of semi-continuous casting and strict control of the process parameters of semi-continuous casting are required in order to prevent accidents of aluminum leakage.
Preferably, the high temperature homogenization in step (8) is conducted at a heating temperature of 560 to 590 ℃ for a heating time of 5 to 10 hours.
The high-temperature homogenization treatment is carried out on the aluminum alloy casting rod, so that coarse intermetallic compounds in the casting rod are melted, macro-micro component segregation and internal stress in the casting rod are eliminated, the uniformity of the structural components of the aluminum alloy casting rod is further improved, the deformation resistance of the aluminum alloy casting rod is reduced, the extrusion speed of the aluminum material is improved, and the performance and quality of the aluminum material are further improved. The heating temperature is low or the heating time is short, resulting in insufficient homogenization. Too high a heating temperature may cause excessive firing of the aluminum alloy cast rod, which may adversely reduce the extrusion performance of the cast rod and the performance of the aluminum product.
Compared with the prior art, the invention has the following beneficial effects: according to the invention, through scientifically designing the preparation process flow and process parameters of the aluminum alloy casting rod, the hydrogen content and the slag content of the aluminum alloy liquid are greatly reduced, the cleanliness of the aluminum alloy casting rod is improved, the grains of the aluminum alloy casting rod are refined, the uniformity of the structural components of the large-diameter aluminum alloy casting rod is improved, the high-purity fine-grained and homogeneous aluminum alloy casting rod is obtained, the hydrogen content of the aluminum alloy casting rod is as low as below 0.1ml/100gAl, and the slag content is as low as 0.05mm 2/kgAl.
Drawings
FIG. 1 shows a metallographic microstructure of an aluminum alloy casting rod according to example 1.
Fig. 2 is a metallographic microstructure of the aluminum alloy casting bar of comparative example 1.
Fig. 3 is a metallographic microstructure of the aluminum alloy casting bar of comparative example 2.
FIG. 4 is a metallographic microstructure of the casting bar of comparative example 3.
FIG. 5 is a metallographic microstructure of the casting bar of comparative example 4.
Detailed Description
The technical solution of the present invention will be further described with reference to the specific embodiments, comparative examples and drawings, but the present invention is not limited thereto, and other variations of the disclosed embodiments, as will be apparent to those skilled in the art, should fall within the scope of the present invention as defined in the appended claims.
Example 1
The 6063 aluminum alloy casting rod with the diameter of 229mm comprises the following components in percentage by mass: 0.42% of Si, 0.14% of Fe, 0.53% of Mg, the balance of Al and unavoidable impurity elements, wherein the single impurity is less than or equal to 0.05%, the total impurity amount is less than or equal to 0.15%, and the preparation method sequentially comprises the following steps:
(1) Smelting and preparing 6063 aluminum alloy liquid according to the component composition and mass percent of the 6063 aluminum alloy casting rod;
(2) And (3) adopting argon with the purity of 99.95% and a refining agent with the weight of 0.3% of the aluminum alloy liquid to carry out slag removal treatment on the aluminum alloy liquid in the furnace by blowing refining for 25 minutes, then removing scum on the surface of the aluminum alloy liquid, and scattering a covering agent on the surface of the aluminum alloy liquid.
(3) Introducing argon with the purity of 99.99% into the aluminum alloy liquid in the furnace through the air brick arranged at the furnace bottom for refining and dehydrogenation treatment, wherein the flow rate of the argon is 0.5 cubic meter/min, and the time for introducing the argon is 15 min;
(4) Introducing aluminum alloy liquid into a launder, and then adding aluminum titanium boron alloy wires accounting for 0.2% of the weight of the aluminum alloy liquid into the aluminum alloy liquid in the launder to carry out grain refinement treatment;
(5) The aluminum alloy liquid subjected to grain refinement treatment flows through a degassing tank arranged on a launder to be subjected to deep dehydrogenation treatment, the rotating speed of a graphite rotor in the degassing tank is 400 revolutions per minute, the flow rate of argon on the graphite rotor is 2.5 cubic meters per hour, the pressure of the argon is 0.6MPa, and the purity of the argon is 99.99%;
(6) Allowing the aluminum alloy liquid subjected to deep dehydrogenation treatment to flow through a deep bed filter box arranged on a launder for filtration treatment;
(7) Adopting an oil-gas sliding semi-continuous casting machine to semi-continuously cast aluminum alloy liquid at 700 ℃ into 6063 aluminum alloy casting bars with diameter of 229mm at the speed of 110 mm/min and the cooling water temperature of 30 ℃;
(8) Heating the aluminum alloy casting rod at 585 ℃ for 6 hours to carry out high-temperature homogenization treatment, and cooling by spraying water mist to obtain the 6063 aluminum alloy casting rod with the diameter of 229 mm.
The refining agent of the embodiment comprises ：ZnCl2 45.6％,K2CO324.3％,NaNO3 8.2％,KF 10.9％,K2SO4 7.3％,Li2SO4 3.7％, of the following components in percentage by mass: (1) ZnCl 2、K2CO3、NaNO3、KF、K2SO4、Li2SO4 with the purity more than or equal to 99.8 percent is selected as a raw material for batching; (2) Heating and melting raw materials at 1180 ℃ under the protection of argon with the purity of more than or equal to 99.99%, and then cooling and solidifying the block refining agent; (3) And (3) crushing the block refining agent into powder with the particle size less than or equal to 2 mm to obtain the refining agent.
Example 2
The 6061 aluminum alloy casting rod with the diameter of 292mm comprises the following components in percentage by mass: 0.54% of Si, 0.12% of Fe, 0.85% of Mg, 0.19% of Cu, the balance of Al and unavoidable impurity elements, wherein the total amount of single impurities is less than or equal to 0.05%, and the preparation method sequentially comprises the following steps:
(1) Smelting and preparing 6061 aluminum alloy liquid according to the component composition and mass percentage of the 6061 aluminum alloy casting rod;
(2) And (3) adopting nitrogen with the purity of 99.9% and a refining agent with the weight of 0.4% of the aluminum alloy liquid to carry out slag removal treatment on the aluminum alloy liquid in the furnace by blowing refining for 30 minutes, then removing scum on the surface of the aluminum alloy liquid, and scattering a covering agent on the surface of the aluminum alloy liquid.
(3) Introducing nitrogen with the purity of 99.99% into the aluminum alloy liquid in the furnace through the air brick arranged at the furnace bottom for refining and dehydrogenation treatment, wherein the nitrogen flow is 0.3 cubic meter/min, and the nitrogen introducing time is 20min;
(4) Introducing aluminum alloy liquid into a launder, and then adding aluminum titanium carbon alloy wires accounting for 0.3% of the weight of the aluminum alloy liquid into the aluminum alloy liquid in the launder to carry out grain refinement treatment;
(5) The aluminum alloy liquid subjected to grain refinement treatment flows through a degassing tank arranged on a launder to be subjected to deep dehydrogenation treatment, the rotating speed of a graphite rotor in the degassing tank is 500 revolutions per minute, the nitrogen flow rate on the graphite rotor is 1 cubic meter per hour, the nitrogen pressure is 0.3MPa, and the nitrogen purity is 99.99%;
(6) Allowing the aluminum alloy liquid subjected to deep dehydrogenation treatment to flow through a deep bed filter box arranged on a launder for filtration treatment;
(7) Adopting an oil-gas sliding semi-continuous casting machine to semi-continuously cast aluminum alloy liquid at 720 ℃ into 6061 aluminum alloy casting bars with the diameter of 292mm under the conditions that the speed is 50 mm/min and the cooling water temperature is 20 ℃;
(8) And heating the aluminum alloy casting rod at 590 ℃ for 5 hours to carry out high-temperature homogenization treatment, and cooling by spraying water mist to obtain the 6061 aluminum alloy casting rod with the diameter of 292 mm.
The refining agent of the embodiment comprises ：ZnCl2 49.5％,K2CO324.3％,NaNO3 5.1％,KF 8.3％,K2SO4 7.9％,Li2SO4 4.9％, of the following components in percentage by mass: (1) ZnCl 2、K2CO3、NaNO3、KF、K2SO4、Li2SO4 with the purity more than or equal to 99.8 percent is selected as a raw material for batching; (2) Heating and melting raw materials at 1150 ℃ under the protection of argon with purity more than or equal to 99.99%, and then cooling and solidifying the block refining agent; (3) And (3) crushing the block refining agent into powder with the particle size less than or equal to 2 mm to obtain the refining agent.
Example 3
The 7003 aluminum alloy cast rod with the diameter of 380mm comprises the following components in percentage by mass: 0.12% of Si, 0.15% of Fe, 0.92% of Mg, 5.43% of Zn, 0.11% of Zr, the balance of Al and unavoidable impurity elements, wherein the single impurity is less than or equal to 0.05%, the total impurity amount is less than or equal to 0.15%, and the preparation method sequentially comprises the following steps:
(1) Smelting to prepare 7003 aluminum alloy liquid according to the component composition and mass percentage of the 7003 aluminum alloy cast rod;
(2) And (3) adopting argon with the purity of 99.9% and a refining agent with the weight of 0.2% of the aluminum alloy liquid to carry out slag removal treatment on the aluminum alloy liquid in the furnace by blowing and refining for 20 minutes, then removing scum on the surface of the aluminum alloy liquid, and scattering a covering agent on the surface of the aluminum alloy liquid.
(3) Introducing argon with the purity of 99.99% into the aluminum alloy liquid in the furnace through the air brick arranged at the furnace bottom for refining and dehydrogenation treatment, wherein the flow rate of the argon is 0.6 cubic meter/min, and the time of introducing the argon is 10min;
(4) Introducing aluminum alloy liquid into a launder, and then adding aluminum titanium boron alloy wires accounting for 0.1% of the weight of the aluminum alloy liquid into the aluminum alloy liquid in the launder to carry out grain refinement treatment;
(5) The aluminum alloy liquid subjected to grain refinement treatment flows through a degassing tank arranged on a launder to be subjected to deep dehydrogenation treatment, the rotating speed of a graphite rotor in the degassing tank is 300 revolutions per minute, the gas flow rate on the graphite rotor is 5 cubic meters per hour, the gas pressure is 0.9MPa, the gas is mixed gas consisting of argon with the purity of 99.99% and chlorine with the purity of 99.99%, and the volume percentage of the chlorine in the mixed gas is 1%.
(6) The aluminum alloy liquid subjected to the deep dehydrogenation treatment flows through a tubular filter box arranged on a launder to be filtered;
(7) Semi-continuously casting the aluminum alloy liquid with 680 ℃ into a 7003 aluminum alloy casting rod with the diameter of 380mm by adopting an oil-gas sliding semi-continuous casting machine under the condition that the speed is 200 mm/min and the cooling water temperature is 40 ℃;
(8) And heating the aluminum alloy casting rod at 560 ℃ for 10 hours to carry out high-temperature homogenization treatment, and cooling by spraying water mist to obtain the 7003 aluminum alloy casting rod with the diameter of 380 mm.
The refining agent of the embodiment comprises ：ZnCl240％,K2CO329％,NaNO310％,KF 13％,K2SO4 5％,Li2SO4 3％, of the following components in percentage by mass: (1) ZnCl 2、K2CO3、NaNO3、KF、K2SO4、Li2SO4 with the purity more than or equal to 99.8 percent is selected as a raw material for batching; (2) Heating and melting raw materials at 1200 ℃ under the protection of argon with purity more than or equal to 99.99%, and then cooling and solidifying the block refining agent; (3) And (3) crushing the block refining agent into powder with the particle size less than or equal to 2 mm to obtain the refining agent.
Example 4
The 1060 aluminum alloy casting rod with the diameter of 430mm comprises the following components in percentage by mass: 0.11% of Si, 0.13% of Fe, 0.03% of Mg, the balance of Al and unavoidable impurity elements, wherein the single impurity is less than or equal to 0.05%, the total impurity amount is less than or equal to 0.15%, and the preparation method sequentially comprises the following steps:
(1) Smelting and preparing 1060 aluminum alloy liquid according to the component composition and mass percent of the 1060 aluminum alloy casting rod;
(2) And (3) adopting nitrogen with the purity of 99.9% and a refining agent with the weight of 0.3% of the aluminum alloy liquid to carry out slag removal treatment on the aluminum alloy liquid in the furnace by blowing refining for 25 minutes, then removing scum on the surface of the aluminum alloy liquid, and sprinkling a covering agent on the surface of the aluminum alloy liquid.
(3) Introducing nitrogen with the purity of 99.99% into the aluminum alloy liquid in the furnace through the air brick arranged at the furnace bottom for refining and dehydrogenation treatment, wherein the nitrogen flow is 0.4 cubic meter/min, and the nitrogen introducing time is 12 min;
(4) Introducing aluminum alloy liquid into a launder, and then adding aluminum titanium boron alloy wires accounting for 0.2% of the weight of the aluminum alloy liquid into the aluminum alloy liquid in the launder to carry out grain refinement treatment;
(5) The aluminum alloy liquid subjected to grain refinement treatment flows through a degassing tank arranged on a launder to be subjected to deep dehydrogenation treatment, the rotating speed of a graphite rotor in the degassing tank is 350 r/min, the gas flow rate on the graphite rotor is 3 cubic meters/h, the gas pressure is 0.5MPa, the gas is mixed gas composed of nitrogen with purity of 99.99% and chlorine with purity of 99.99%, and the volume percentage of the chlorine in the mixed gas is 5%.
(6) The aluminum alloy liquid subjected to the deep dehydrogenation treatment flows through a tubular filter box arranged on a launder to be filtered;
(7) Adopting an oil-gas sliding semi-continuous casting machine to semi-continuously cast aluminum alloy liquid at 710 ℃ into 1060 aluminum alloy casting bars with the diameter of 430mm at the speed of 80 mm/min and the cooling water temperature of 30 ℃;
(8) Heating the aluminum alloy casting rod at 570 ℃ for 8 hours to carry out high-temperature homogenization treatment, and cooling by spraying water mist to obtain the 1060 aluminum alloy casting rod with the diameter of 430 mm.
The refining agent of the embodiment comprises ：ZnCl2 43％,K2CO330％,NaNO3 7％,KF 10％,K2SO4 6％,Li2SO4 4％, of the following components in percentage by mass: (1) ZnCl 2、K2CO3、NaNO3、KF、K2SO4、Li2SO4 with the purity more than or equal to 99.8 percent is selected as a raw material for batching; (2) Heating and melting raw materials at 1180 ℃ under the protection of argon with the purity of more than or equal to 99.99%, and then cooling and solidifying the block refining agent; (3) And (3) crushing the block refining agent into powder with the particle size less than or equal to 2 mm to obtain the refining agent.
Comparative example 1
The components and the preparation process of the aluminum alloy casting rod in the comparative example are the same as those of the example 1, except that the refining agent used in the step (2) is a commercially available refining agent commonly used at present, and the refining agent consists of the following components in percentage by mass: 26.1% of NaCl,10.6% of Na 2SiF6, 17.1% of Na 2SO4, 6.9% of CaF 2, 9.3% of C 6Cl6, 14.3% of Na 2S2O3 and 15.7% of NaF.
Comparative example 2
The composition and preparation process of the aluminum alloy cast bar in this comparative example were the same as in example 2, except that the deep-bed filtration tank or the tube filtration tank was not used in step (6) but filtration was performed using a common foam ceramic plate.
Comparative example 3
The composition and preparation process of the aluminum alloy cast bar in this comparative example were the same as in example 3, except that the oil and gas slip semicontinuous casting was not employed in step (7) but the ordinary water-cooled semicontinuous casting of the aluminum alloy cast bar was employed.
Comparative example 4
The composition and preparation process of the aluminum alloy cast bar in this comparative example were the same as in example 4, except that the homogenizing process of the aluminum alloy cast bar in step (8) was heating at 550℃for 6 hours.
Verification example 1
Melting points of the refining agents used in example 1 and comparative example 1 were measured by an OXFORD-DSC500 type differential scanning calorimeter, respectively, and the results are shown in table 1, and table 1 shows a comparison of melting points of the refining agents of example 1 and comparative example 1. As can be seen from Table 1, the refining agent of example 1 had a melting start temperature of 290℃and a melting end temperature of 716℃only. The refining agent of comparative example 1 had a melting start temperature of 564℃and a melting end temperature of 1249 ℃. As can be seen by comparison, the refining agent developed by the invention has lower melting initial temperature and melting end temperature, which shows that the refining agent developed by the invention is easier to be melted in aluminum alloy liquid, thereby being beneficial to improving the deslagging effect.
| Example 1 | Comparative example 1 | |
| Melting initiation temperature/. Degree.C | 290 | 564 |
| Melting end temperature/. Degree.C | 716 | 1249 |
TABLE 1
Verification example 2
The hydrogen content and the slag content of the aluminum alloy liquids before casting of examples 1 to 4 and comparative examples 1 to 4 were measured on site by using an HDA-V hydrogen meter and an Analyze PoDFA slag meter, and the results are shown in Table 2, and Table 2 shows the comparison of the hydrogen content and the slag content of the aluminum alloy liquids before casting. As can be seen from Table 2, the aluminum alloys of examples 1 to 4 had a hydrogen content of less than 0.12ml/100gAl and a slag content of less than 0.08mm2/kg. In comparative example 1, the conventional commercial refining agent was used for in-furnace blowing refining, so that the hydrogen content of the aluminum alloy liquid before casting was 0.135ml/100gAl, and the slag content was 0.094mm 2/kg. Comparative example 2 the slag content of the aluminum alloy liquid before casting was as high as 0.108mm 2/kg because the deep-bed filtration or the tube filtration was not employed but the common foam ceramic plate filtration was employed. As can be seen by comparison, the method can greatly reduce the gas slag content of the aluminum alloy liquid, thereby improving the cleanliness of the aluminum alloy casting rod.
| Hydrogen content/(ml/100 gAl) | Slag content/(mm 2/kgAl) | |
| Example 1 | 0.118 | 0.078 |
| Example 2 | 0.107 | 0.072 |
| Example 3 | 0.086 | 0.065 |
| Example 4 | 0.092 | 0.069 |
| Comparative example 1 | 0.135 | 0.094 |
| Comparative example 2 | 0.105 | 0.108 |
| Comparative example 3 | 0.088 | 0.066 |
| Comparative example 4 | 0.091 | 0.068 |
TABLE 2
Verification example 3
Samples were taken on the aluminum alloy cast bars obtained in example 1 and comparative examples 1 to 4, and then observed under a metallographic microscope after grinding, polishing and etching, and the metallographic structures of the aluminum alloy cast bars are shown in FIGS. 1 to 5, respectively. As can be seen from FIG. 1, the aluminum alloy cast rod of example 1 had fine and uniform grains, and no pores and inclusions were found to exist. As can be seen from fig. 2 and 3, comparative example 1, which was an in-furnace blowing refining using a conventional commercial refining agent, and comparative example 2, which was an aluminum alloy ingot, was a large number of air holes and inclusions due to no filtering using a deep-bed filter box or a tube filter box. As can be seen from fig. 4, since comparative example 3 did not employ oil and gas slip semicontinuous casting but ordinary water-cooled semicontinuous casting, the grains of the aluminum alloy cast bar were coarse. As can be seen from fig. 5, since the homogenization temperature of the comparative example 4 aluminum alloy ingot was too low, the aluminum alloy ingot was insufficiently homogenized, and a large amount of coarse intermetallic compounds remained inside.
Verification example 4
The aluminum alloy cast bars of examples 1 to 4 and comparative examples 1 to 4 were heated to 500℃and then extruded into aluminum materials on the same die and extruder, room temperature stretching was performed on an electronic tensile tester after heat treatment at a stretching rate of 2mm/min, and the tensile strength, yield strength and elongation after break of the aluminum materials were examined, and the results are shown in Table 3, table 3 being a comparison of room temperature tensile mechanical properties of aluminum alloy cast bars extruded aluminum materials. It can be seen from Table 3 that the tensile mechanical properties of the extruded aluminum material of the example aluminum alloy cast bars were significantly higher than those of the extruded aluminum material of the comparative example aluminum alloy cast bars with the same composition of the aluminum alloy cast bars. As can be seen by comparison, the invention can improve the cleanliness of the aluminum alloy casting rod, refine the crystal grains of the aluminum alloy casting rod and improve the structural component uniformity of the aluminum alloy casting rod, and finally can obviously improve the mechanical property of the aluminum material.
| Tensile strength/MPa | Yield strength/MPa | Elongation after break/% | |
| Example 1 | 249.1 | 217.6 | 15.2 |
| Example 2 | 294.6 | 276.8 | 13.9 |
| Example 3 | 398.6 | 362.4 | 15.6 |
| Example 4 | 108.5 | 82.6 | 25.6 |
| Comparative example 1 | 220.5 | 195.5 | 12.8 |
| Comparative example 2 | 281.4 | 259.6 | 11.3 |
| Comparative example 3 | 375.6 | 343.1 | 13.8 |
| Comparative example 4 | 95.1 | 73.5 | 18.4 |
Table 3.
Claims (10)
1. The preparation method of the large-diameter high-cleanliness fine-grain homogeneous aluminum alloy casting rod is characterized by comprising the following steps in sequence:
(1) Smelting to prepare aluminum alloy liquid according to the component composition and mass percentage of the aluminum alloy casting rod;
(2) Adopting inert gas and a refining agent to carry out blowing refining deslagging treatment on aluminum alloy liquid in a furnace, then removing scum on the surface of the aluminum alloy liquid, and scattering a covering agent on the surface of the aluminum alloy liquid;
(3) Introducing inert gas into the aluminum alloy liquid in the furnace through the air brick arranged at the bottom of the furnace to carry out refining and dehydrogenation treatment;
(4) Introducing aluminum alloy liquid into a launder, and then adding a grain refiner into the aluminum alloy liquid in the launder to carry out grain refining treatment;
(5) The aluminum alloy liquid subjected to grain refinement treatment flows through a degassing tank arranged on a launder to carry out deep dehydrogenation treatment;
(6) Allowing the aluminum alloy liquid subjected to deep dehydrogenation treatment to flow through a deep bed filter box or a tubular filter box arranged on a launder for filtration treatment;
(7) The aluminum alloy liquid is semicontinuously cast into an aluminum alloy casting rod by adopting an oil-gas sliding semicontinuous casting machine;
(8) And carrying out high-temperature homogenization treatment on the aluminum alloy casting rod, and cooling by spraying water mist to obtain the large-diameter high-cleanliness fine-grain homogenized aluminum alloy casting rod.
2. The method for preparing a large-diameter high-cleanliness fine-grain homogeneous aluminum alloy casting rod according to claim 1, wherein in the step (2), the inert gas is argon with the purity of more than or equal to 99.9% or nitrogen with the purity of more than or equal to 99.9%, the consumption of the refining agent is 0.2-0.4% of the weight of the aluminum alloy liquid, and the blowing refining time is 20-30 minutes.
3. The method for producing a large-diameter high-purity fine-grain homogeneous aluminum alloy cast rod according to claim 1, wherein the refining agent in the step (2) consists of the following components in mass percent ：ZnCl240-50％,K2CO3 20-30％,NaNO35-10％,KF 8-13％,K2SO4 5-8％,Li2SO43-5％.
4. The method for preparing a large-diameter high-cleanliness fine-grain homogeneous aluminum alloy casting rod according to claim 1, wherein the method for preparing the refining agent in the step (2) comprises the following steps in sequence: (1) ZnCl 2、K2CO3、NaNO3、KF、K2SO4、Li2SO4 with the purity more than or equal to 99.8 percent is selected as a raw material for batching; (2) Heating and melting raw materials at 1150-1200 ℃ under the protection of argon with purity more than or equal to 99.99%, and then cooling and solidifying the block refining agent; (3) And (3) crushing the block refining agent into powder with the particle size less than or equal to 2mm to obtain the refining agent.
5. The method for producing a large-diameter high-purity fine-grain homogeneous aluminum alloy cast rod according to claim 1, wherein the inert gas in the step (3) is argon gas with a purity of 99.99% or more or nitrogen gas with a purity of 99.99% or more, the flow rate of the inert gas is 0.3-0.6 cubic meters per minute, and the aeration time is 10-20 minutes.
6. The method for preparing a large-diameter high-cleanliness fine-grain homogeneous aluminum alloy casting rod according to claim 1, wherein in the step (4), the grain refiner is an aluminum titanium boron alloy wire or an aluminum titanium carbon alloy wire, and the adding amount of the grain refiner is 0.1-0.3% of the weight of the aluminum alloy liquid.
7. The method for preparing a large-diameter high-cleanliness fine-grain homogeneous aluminum alloy casting rod according to claim 1, wherein in the step (5), the rotation speed of a graphite rotor in the degassing tank is 300-500 rpm, the gas flow rate on the graphite rotor is 1-5 cubic meters per hour, and the gas pressure is 0.3-0.9MPa.
8. The method for preparing the large-diameter high-cleanliness fine-grain homogeneous aluminum alloy casting rod according to claim 1, wherein the gas introduced into the degassing tank in the step (5) is argon with the purity of more than or equal to 99.99%, or nitrogen with the purity of more than or equal to 99.99%, or mixed gas composed of argon with the purity of more than or equal to 99.99%, or nitrogen with the purity of more than or equal to 99.99% and chlorine with the purity of more than or equal to 99.99%, and the volume percentage of the chlorine in the mixed gas is 1-5%.
9. The method for producing a large diameter, high purity fine grain homogeneous aluminum alloy cast rod as defined in claim 1, wherein the aluminum alloy liquid in step (7) has a temperature of 680-720 ℃, a semi-continuous casting speed of 50-200 mm/min, and a cooling water temperature of 40 ℃ or less.
10. The method for producing a large-diameter high-purity fine-grain homogeneous aluminum alloy cast rod according to claim 1, wherein the high-temperature homogenization in step (8) is carried out at a heating temperature of 560 to 590 ℃ for a heating time of 5 to 10 hours.
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