CN114703390B - Refining agent and refining and purifying method of aluminum alloy cast on line by combining refining agent with argon - Google Patents
Refining agent and refining and purifying method of aluminum alloy cast on line by combining refining agent with argon Download PDFInfo
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- C22C1/00—Making non-ferrous alloys
- C22C1/06—Making non-ferrous alloys with the use of special agents for refining or deoxidising
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C21/00—Alloys based on aluminium
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Abstract
The invention belongs to the field of metal materials and metallurgy, and particularly relates to a refining agent and a refining and purifying method of an aluminum alloy cast on line by combining the refining agent with argon. The refining agent is prepared from hexachloroethane, sodium carbonate and alumina nano-particles. Based on the total weight of the refining agent, the refining agent comprises 35-40 wt% of hexachloroethane, 20-40 wt% of sodium carbonate and 20-40 wt% of alumina nanoparticles. The refining agent is a granular refining agent with the grain diameter of 0.5-6 mm. According to the invention, the hydrogen content of the cast ingot molten aluminum is reduced by selecting the process of jointly pressing the refining agent and the high-grade argon gas and filtering and purifying, so that the adverse factors that the gas distribution is uniform, smaller impurities are reserved as a crystallization core and crystal grains are coarsened and the like cannot be completely achieved by manual blowing can be favorably solved, and the gas consumption can be greatly reduced.
Description
Technical Field
The invention belongs to the field of metal materials and metallurgy, and particularly relates to a refining agent and a refining and purifying method of an aluminum alloy cast on line by combining the refining agent with argon.
Background
In aluminum alloy castings, the reliability of the material and the properties of the casting face a great threat due to the presence of inclusions. The inclusions in the aluminum alloy melt can cause difficulty in removing hydrogen, and the degassing effect is influenced. Generally, the more the oxide inclusions in the molten aluminum are, the more hydrogen is adsorbed, the hydrogen content is increased, the formation of pores in the casting is promoted, and the performance is influenced. The continuity of the matrix can be damaged by the existence of the inclusions, a core for fatigue crack initiation is provided, stress concentration is caused, crack propagation is promoted, the anti-fatigue capability of the part is reduced, the mechanical properties of the part such as elongation, tensile strength and the like can be seriously deteriorated, and the early failure of the product is caused.
The refining agent used in the traditional aluminum alloy manufacturing process can cause the electric conductivity, the thermal conductivity and the corrosion resistance of a finished product to be not strong, the porosity of the produced alloy casting is high, seven holes are generated on the surface of the casting, the proportion of oxidized impurities is high, the performance of the alloy casting is influenced, the product in the refining process has pungent smell, and the harm to human bodies of workers is great. In conclusion, the refining agent has the problems of more slag inclusion, large oxidation burning loss, incomplete separation of alloy slag and poor degassing and deslagging effects.
In addition, the aluminum alloy melt degassing modes comprise in-furnace degassing and on-line degassing, the degassing method comprises inert gas degassing and flux degassing, the inert gas degassing utilizes the partial pressure diffusion of high-purity inert gas hydrogen to realize the dehydrogenation, and the flux and aluminum form a low-boiling-point compound to volatilize and remove the hydrogen. The small bubbles can adsorb impurities in the floating process, and can clamp the pressure difference between the argon bubbles and the contact surface of the alloy liquid, so that the hydrogen dissolved in the alloy liquid is absorbed into the bubbles. Although the inert gas overcomes the defect that the active gas corrodes equipment, the purification efficiency of the inert gas is far lower than that of the active gas, and the removal of alkali metals and alkaline earth metals cannot be realized.
Therefore, to develop the potential of the material and fully develop its own properties, the production and quality control of the cast slab must be solved first.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention provides a refining agent, a preparation method thereof and a refining and purifying method for casting aluminum alloy on line by using the refining agent and argon in a combined manner.
The invention is realized by the following technical scheme:
in a first aspect, the invention provides a refining agent comprising hexachloroethane, sodium carbonate and alumina nanoparticles.
According to the invention, the refining agent consists of hexachloroethane, sodium carbonate and alumina nanoparticles.
According to the invention, the particle size of the alumina nanoparticles is 30-50 nm, for example 30nm, 40nm or 50 nm.
According to the invention, based on the total weight of the refining agent, the refining agent comprises 35-40 wt% of hexachloroethane, 20-40 wt% of sodium carbonate and 20-40 wt% of alumina nanoparticles.
Preferably, wherein hexachloroethane 35wt%, 36wt%, 37wt%, 38wt%, 39wt%, 40wt%, based on the total weight of the refining agent; 20wt%, 22wt%, 25wt%, 28wt%, 30wt%, 32wt%, 34wt%, 35wt%, 36wt%, 38wt%, 40wt% of sodium carbonate; 20wt%, 22wt%, 25wt%, 28wt%, 30wt%, 32wt%, 34wt%, 35wt%, 36wt%, 38wt%, 40wt% of alumina nanoparticles.
According to the invention, the average grain diameter of the refining agent is 0.5mm-6 mm.
According to the invention, the alumina nanoparticles are alpha-Al 2 O 3 . Compared with alumina with other configuration, the research shows that the alpha-Al 2 O 3 The nano-particles can be rapidly filled into the gaps of the protective film on the surface of the melt.
The second aspect of the present invention provides a method for preparing the refining agent, the method comprising:
and uniformly mixing sodium carbonate, hexachloroethane and alumina nano particles, compacting, and crushing to obtain the refining agent.
According to the invention, the grain size of the refining agent is 0.5mm-6 mm.
The third aspect of the invention provides an on-line casting aluminum alloy refining and purifying method by using the refining agent and argon in combination.
According to the invention, the method comprises the following steps:
(1) putting the aluminum alloy ingot into a preheated aluminum alloy smelting furnace for smelting;
(2) after the smelted aluminum alloy melt is introduced into a standing furnace and the temperature of the smelted aluminum alloy melt is adjusted to 730-740 ℃, under the stirring condition, dry inert gas and the refining agent are sprayed into the aluminum alloy melt through a guide pipe to carry out degassing refining in the furnace;
(3) and (3) filtering the melt obtained in the step (2) by using a ceramic filter plate to obtain the aluminum alloy.
According to the present invention, in the step (1), the aluminum alloy is not particularly defined, and is, for example, a 2000 series aluminum alloy or a 7000 series aluminum alloy.
According to the invention, in the step (1), the preheating temperature is 620-650 ℃, and the preheating time is 10-20 min.
According to the invention, in the step (2), the rotation speed of the stirring is 20-40 rpm, such as 20rpm, 25rpm, 30rpm, 35rpm or 40 rpm.
According to the invention, in the step (2), the dry inert gas is dry high-purity argon gas with the purity level of 99.999 percent.
According to the invention, in step (2), the amount of the refining agent added is 1.5 to 3.0kg/t (melt mass), for example, 1.5kg/t, 1.6kg/t, 1.8kg/t, 2kg/t, 2.2kg/t, 2.5kg/t, 2.8kg/t, 3 kg/t.
According to the invention, in step (2), the pressure of the dry inert gas is 0.20-0.60 MPa, such as 0.20MPa, 0.30MPa, 0.40MPa, 0.50MPa, 0.60MPa, and the gas flow rate is 20-100L/min, such as 20L/min, 30L/min, 40L/min, 50L/min, 60L/min, 70L/min, 80L/min, 90L/min, 100L/min.
According to the invention, in the step (2), the conduit is a conduit provided with a plurality of openings.
According to the invention, in the step (2), the aperture of the conduit is 3-6mm, and the hole density is 1-5 holes/cm 2 。
According to the invention, in the step (2), the average size of gas bubbles obtained after the dry inert gas and the refining agent are sprayed into the aluminum alloy melt through the guide pipe is 0.5-20.0 mm.
According to the invention, in the step (2), the degassing time is 30-90 min.
According to the invention, in the step (3), the aperture of the filter plate is 30-70 meshes.
The technical scheme of the invention has the following beneficial effects:
according to the protection film strengthening concept, active alumina nano-particles and Na are used 2 CO 3 Refining agent with hexachloroethane, wherein the alumina nanoparticles are very compatibleIs easy to be filled into the gaps of the protective film on the surface of the melt and simultaneously carries Na 2 CO 3 With hexachloroethane, decomposition at high temperatures to CO X With Cl 2 Wetting and partially dissolving oxides, increasing the viscosity of the aluminum alloy melt to the oxides, blowing argon to adjust the balance state of the system, combining with H in the aluminum alloy melt to fix hydrogen in the oxides, gathering smaller particles to form larger oxide inclusions, and filtering to remove the oxide inclusions, thereby reducing the hydrogen content in the aluminum alloy melt. The components are compounded, and the hydrogen fixation effect and the condensation effect of oxide inclusions are utilized, so that deslagging and degassing are fully combined, the hydrogen content in the degassed aluminum alloy melt is 0.01-0.06 ml/100gAl, and the micro-porosity size of the aluminum alloy cast ingot is obviously reduced. In addition, the invention reduces the hydrogen content of the cast ingot molten aluminum by selecting the process of combined spraying and filtering purification of the refining agent and the high-grade argon, can favorably solve the problem that the manual blowing can not completely achieve the adverse factors of uniform gas distribution, smaller impurities remained as a crystallization core to coarsen crystal grains and the like, and can also greatly reduce the gas consumption. The aluminum alloy ingot obtained after refining and purification has excellent metallurgical quality, no slag inclusion and low hydrogen content, can also obviously reduce the micro-porosity size of the aluminum alloy ingot, improve the metallurgical quality of the ingot, and lay a good foundation for developing a new and high-performance aluminum alloy material for subsequent research.
Detailed Description
The present invention will be described in further detail with reference to specific examples. It is to be understood that the following examples are only illustrative and explanatory of the present invention and should not be construed as limiting the scope of the present invention. All the technologies realized based on the above-mentioned contents of the present invention are covered in the protection scope of the present invention.
The experimental methods used in the following examples are all conventional methods unless otherwise specified; reagents, materials and the like used in the following examples are commercially available unless otherwise specified.
Preparation example 1
Argon of grade 99.999% is selected.
Preparation example 2
Argon of 99.99% grade is selected.
TABLE 1 compositions of argon for preparation 1 and preparation 2
Example 1
The refining agent comprises, by weight, 35% of hexachloroethane, 35% of sodium carbonate and 30% of alumina nanoparticles. The refining agent has an average particle size of 3-6 mm.
The preparation method of the refining agent comprises the following steps: and uniformly mixing the sodium carbonate, hexachloroethane and alumina nano-particle solid powder according to the above dosage, compacting, and crushing to obtain the refining agent A1.
Example 2
A refining agent comprises, based on the total weight of the refining agent, 40% of hexachloroethane, 40% of sodium carbonate and 20% of alumina nanoparticles. The refining agent has an average particle size of 2-4 mm.
The preparation method of the refining agent comprises the following steps: and uniformly mixing sodium carbonate, hexachloroethane and aluminum oxide nano-particle solid powder according to the above dosage, compacting, and crushing to obtain the refining agent A2.
Example 3
The refining agent comprises 45% of hexachloroethane, 45% of sodium carbonate and 10% of alumina nano-particles by weight of the total refining agent. The refining agent has an average particle size of 3-6 mm.
The preparation method of the refining agent comprises the following steps: and uniformly mixing sodium carbonate, hexachloroethane and aluminum oxide nano-particle solid powder according to the above dosage, compacting, and crushing to obtain the refining agent A3.
Comparative example 1
The refining agent comprises 45% of hexachloroethane and 55% of sodium carbonate based on the total weight of the refining agent. The refining agent has an average particle size of 3-6 mm.
The preparation method of the refining agent comprises the following steps: and uniformly mixing the sodium carbonate and the hexachloroethane solid powder according to the above dosage, compacting, and crushing to obtain the refining agent B1.
Test example 1
The refining and purifying method of the aluminum alloy cast on line by using the refining agent and argon gas in a combined mode comprises the following steps:
(1) and putting the 7000 series aluminum alloy ingot into a preheated aluminum alloy smelting furnace, wherein the preheating temperature is 650 ℃, and the preheating time is 20 min.
(2) And (3) when the alloy melt is introduced into a standing furnace and the temperature of the alloy melt is adjusted to 740 ℃, degassing and refining the alloy melt in the furnace under the stirring condition. Wherein the degassing in the furnace is specifically to adopt a conduit to spray a refining agent and argon into the aluminum alloy melt for degassing, the conduit is provided with holes with the aperture of 3-4 mm and the hole density of 5 holes/cm 2 (ii) a The guide pipe sprays a refining agent and argon into the aluminum alloy melt, the gas pressure is controlled to be 0.40MPa, the gas flow is 80L/min, the average size of bubbles is 15-20.0 mm, the addition amount of the refining agent is 1.5kg/t, and the degassing time is 60 min;
(3) and filtering by using a ceramic filter plate with the aperture of 50 meshes to obtain the refined aluminum alloy.
The refining agents prepared in examples 1-2 and comparative examples 1-2 and the argon gas of preparation examples 1-2 were respectively injected under the above conditions, the refined alloy melt was directly cooled and semi-continuously cast, and hydrogen and the content of oxide inclusions were measured on line before casting.
The online liquid hydrogen content is obtained by testing an ABB online hydrogen measuring instrument, the removal rate of the oxide inclusion is obtained by testing a statistical method, specifically, samples are obtained by observing and preparing microstructures of samples taken before refining and after refining and filtering, 20 positions are randomly selected in a 200-time visual field for observation and calculation, and the removal rate of the oxide inclusion is = (the number of the oxide inclusion in the samples before refining is counted, the number of the oxide inclusion in the samples after refining is counted), and the number of the oxide inclusion in the samples before refining is multiplied by 100%. The specific test results are detailed in table 2.
TABLE 2 Performance test results for refined aluminum alloy melts and aluminum alloy ingots cast therefrom
In summary, the use of a catalyst comprising activated alumina nanoparticles, Na 2 CO 3 The technology of combined spraying and filtering purification with a refining agent of hexachloroethane and high-grade argon reduces the hydrogen content of cast ingot molten aluminum, can favorably solve the problem that manual blowing can not completely achieve the adverse factors of uniform gas distribution, smaller impurities remained as a crystallization core to coarsen crystal grains and the like, and can also greatly reduce the gas consumption. The aluminum alloy obtained after refining and purification in the invention has stable and lower hydrogen content, thereby obviously reducing the micro-porosity size of the aluminum alloy cast ingot, improving the metallurgical quality of the cast ingot, and laying a good foundation for developing a new and high-performance aluminum alloy material for subsequent research.
The embodiments of the present invention have been described above. However, the present invention is not limited to the above embodiment. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (8)
1. A refining agent, characterized in that the refining agent comprises hexachloroethane, sodium carbonate and alumina nanoparticles; based on the total weight of the refining agent, 35-40 wt% of hexachloroethane, 35-40 wt% of sodium carbonate and 20-30 wt% of alumina nano particles are used;
the refining agent is prepared by the following method:
uniformly mixing sodium carbonate, hexachloroethane and alumina nano-particles, compacting, and crushing to obtain the refining agent; the refining agent is a granular refining agent with the grain diameter of 0.5mm-6 mm.
2. A refining agent, wherein the weight of hexachloroethane is 35 percent, the weight of sodium carbonate is 35 percent, and the weight of alumina nano-particles is 30 percent; the refining agent is prepared by the following method:
uniformly mixing sodium carbonate, hexachloroethane and alumina nano-particles, compacting, and crushing to obtain the refining agent; the refining agent has an average particle size of 3-6 mm.
3. A refining agent, wherein the weight percentage of hexachloroethane is 40%, the weight percentage of sodium carbonate is 40%, and the weight percentage of alumina nano-particles is 20%; the refining agent is prepared by the following method:
uniformly mixing sodium carbonate, hexachloroethane and alumina nano-particles, compacting, and crushing to obtain the refining agent; the refining agent has an average particle size of 2-4 mm.
4. An in-line cast aluminum alloy refining purification process using the refining agent as claimed in any one of claims 1 to 3 in combination with argon gas.
5. The method of claim 4, wherein the method comprises the steps of:
(1) putting the aluminum alloy ingot into a preheated aluminum alloy smelting furnace for smelting;
(2) when the smelted aluminum alloy melt is introduced into a standing furnace and the temperature of the smelted aluminum alloy melt is adjusted to 730-740 ℃, under the condition of stirring, dry inert gas and the refining agent are sprayed into the aluminum alloy melt through a guide pipe to carry out degassing refining in the furnace;
(3) and (3) filtering the melt obtained in the step (2) by using a ceramic filter plate to obtain the aluminum alloy.
6. The method of claim 5, wherein in step (2), the dry inert gas is dry high purity argon gas having a purity level of 99.999%.
7. The method according to claim 5, wherein in the step (2), the refining agent is added in an amount of 1.5 to 3.0 kg/t.
8. The method according to claim 5, wherein in the step (2), the pressure of the dry inert gas is 0.20 to 0.60MPa, and the gas flow rate is 1 to 100L/min.
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| CN115679112A (en) * | 2022-09-29 | 2023-02-03 | 中信戴卡股份有限公司 | Purification method of recycled aluminum melt for automobile hub |
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