CN117107087A - Preparation method and application of four-step high-quality Al-Ti-B grain refiner - Google Patents
Preparation method and application of four-step high-quality Al-Ti-B grain refiner Download PDFInfo
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- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 77
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 77
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 45
- 239000000203 mixture Substances 0.000 claims abstract description 39
- 239000002893 slag Substances 0.000 claims abstract description 39
- 238000007872 degassing Methods 0.000 claims abstract description 31
- 238000005266 casting Methods 0.000 claims abstract description 30
- 238000006243 chemical reaction Methods 0.000 claims abstract description 29
- 238000005096 rolling process Methods 0.000 claims abstract description 22
- 238000009749 continuous casting Methods 0.000 claims abstract description 19
- 238000007670 refining Methods 0.000 claims abstract description 15
- 238000005275 alloying Methods 0.000 claims abstract description 14
- 229910020491 K2TiF6 Inorganic materials 0.000 claims abstract description 5
- 229910020261 KBF4 Inorganic materials 0.000 claims abstract description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 68
- 239000007788 liquid Substances 0.000 claims description 63
- 239000007789 gas Substances 0.000 claims description 52
- 238000003756 stirring Methods 0.000 claims description 38
- 229910052786 argon Inorganic materials 0.000 claims description 34
- 238000000034 method Methods 0.000 claims description 27
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 26
- 230000006698 induction Effects 0.000 claims description 26
- 150000003839 salts Chemical class 0.000 claims description 19
- 239000000956 alloy Substances 0.000 claims description 17
- 229910045601 alloy Inorganic materials 0.000 claims description 16
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 13
- 239000000463 material Substances 0.000 claims description 12
- 230000008569 process Effects 0.000 claims description 11
- 239000000155 melt Substances 0.000 claims description 8
- 238000012546 transfer Methods 0.000 claims description 8
- 229910000521 B alloy Inorganic materials 0.000 claims description 4
- 238000007667 floating Methods 0.000 claims description 2
- 238000010438 heat treatment Methods 0.000 abstract description 5
- 230000000694 effects Effects 0.000 abstract description 3
- 238000004519 manufacturing process Methods 0.000 abstract 1
- 239000002253 acid Substances 0.000 description 27
- 239000002245 particle Substances 0.000 description 21
- 229910000838 Al alloy Inorganic materials 0.000 description 7
- 229910010038 TiAl Inorganic materials 0.000 description 7
- 230000001590 oxidative effect Effects 0.000 description 4
- 238000012545 processing Methods 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 230000009467 reduction Effects 0.000 description 3
- 239000013078 crystal Substances 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- ASZZHBXPMOVHCU-UHFFFAOYSA-N 3,9-diazaspiro[5.5]undecane-2,4-dione Chemical compound C1C(=O)NC(=O)CC11CCNCC1 ASZZHBXPMOVHCU-UHFFFAOYSA-N 0.000 description 1
- QYEXBYZXHDUPRC-UHFFFAOYSA-N B#[Ti]#B Chemical compound B#[Ti]#B QYEXBYZXHDUPRC-UHFFFAOYSA-N 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 229910010039 TiAl3 Inorganic materials 0.000 description 1
- 229910033181 TiB2 Inorganic materials 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005034 decoration Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 230000005923 long-lasting effect Effects 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 230000008520 organization Effects 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 239000013612 plasmid Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000008719 thickening Effects 0.000 description 1
- 238000009827 uniform distribution Methods 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
Classifications
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- 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
- C22C1/02—Making non-ferrous alloys by melting
- C22C1/026—Alloys based on aluminium
-
- 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
- C22C1/06—Making non-ferrous alloys with the use of special agents for refining or deoxidising
-
- 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
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- Chemical & Material Sciences (AREA)
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- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
The application discloses a preparation method and application of a four-step high-quality Al-Ti-B grain refiner, wherein the preparation method of the refiner comprises the following steps: 1) Heating aluminum water to 700-800 deg.C, degassing, and then KBF-treating 4 And K 2 TiF 6 Adding the mixture into molten aluminum for four times to react; 2) A first time; adding 22-25 wt% KBF 4 And K 2 TiF 6 Pouring out water slag after the mixture is reacted, alloying for 3-5 min, and removing residual water slag; 3) Adding 24-27 wt% KBF for the second time 4 And K 2 TiF 6 Alloying the mixture for 5-10 min after the addition of the mixture is finished, and pouring out water slag after the reaction is finished; 4) Repeating the step 3) twice to respectively finish the third feeding reaction and the fourth feeding reaction; wherein 24 to 27 weight percent of KBF4 and K2TiF6 are added for the third time to be mixedMixing, adding the rest KBF for the fourth time 4 And K 2 TiF 6 A mixture; 5) Transferring into a casting furnace through a launder, degassing, standing, fishing out surface scum, and then directly casting a trapezoid bar ingot or rolling into a wire rod through a continuous casting and rolling machine. The application has simple operation, convenient industrialized production, high product quality, less consumption and good refining effect.
Description
Technical Field
The application relates to a preparation method and application of a four-step high-quality Al-Ti-B grain refiner, belonging to the technical field of preparation of Al-Ti-B grain refiners.
Background
Aluminum and its alloys have low density, high specific strength, excellent electric conductivity, heat conductivity and corrosion resistance, excellent cost performance, good shape and good comprehensive performance, and are widely applied to the fields of aviation, aerospace, ships, automobiles, machinery, construction, decoration, packaging, household appliances and the like. At present, the yield of aluminum is inferior to steel, and the aluminum is the first of various nonferrous metals.
With the wide application of aluminum profiles, particularly in the field of high and new technology, the subsequent deep processing technology puts strict requirements on the organization of aluminum ingot blanks. To obtain excellent mechanical properties and processing properties of aluminum and its alloys, it is first necessary to obtain aluminum and aluminum alloy ingots having acceptable chemical compositions, fine and uniform structure, and low gas content and nonmetallic inclusions. Grain size and morphology are the most important features of as-cast structure, with fine, uniform equiaxed crystals being the most preferred as-cast structure. The aluminum and aluminum alloy can be subjected to fine and uniform crystal grain ingot, and the aluminum and aluminum alloy subjected to fine treatment has good surface finish, so that the use value of aluminum products is greatly improved; in addition, the refined aluminum and the aluminum alloy can greatly improve the yield and reduce the rejection rate in the casting process.
The miniaturization treatment of aluminum and aluminum alloy structure is an important research branch in the aluminum processing industry, and plays an important role in improving aluminum materials, improving the yield of aluminum products, improving the mechanical properties and cold and hot processing technological properties of aluminum and aluminum alloy and the like.
Along with the development of society, the quality requirement of clients on the refiner is higher and higher, in order to meet the demands of clients, the inventor particularly develops a preparation method of a four-step high-quality Al-Ti-B grain refiner, and the prepared refiner can be used for refining demands of high-quality products.
Disclosure of Invention
The application provides a preparation method and application of a four-step high-quality Al-Ti-B grain refiner, which are used for meeting the requirements of high-quality products.
In order to solve the technical problems, the technical scheme adopted by the application is as follows:
a preparation method of a four-step high-quality Al-Ti-B grain refiner comprises the following steps:
1) After the aluminum water is heated to 700-800 ℃, starting up and down stirring function of the induction furnace, simultaneously introducing argon into the aluminum water for degassing, and then performing KBF 4 And K 2 TiF 6 The mixture is transferred into molten aluminum for reaction in four times through an integrated salt mixing gas conveying system, namely KBF 4 And K 2 TiF 6 The mixture is added in four times;
2) A first time; uniformly adding 22-25wt% KBF into molten aluminum by utilizing an integrated salt mixing gas conveying system 4 And K 2 TiF 6 Mixing materials, controlling the feeding time to be 10-15 min, pouring out water slag, alloying for 3-5 min at 700-800 ℃, uniformly scattering light calcium carbonate on the surface of molten liquid, and removing residual water slag;
3) Maintaining 700-800 deg.c, and adding 24-27 wt% KBF for the second time 4 And K 2 TiF 6 The mixture is added for 5-8 min, and KBF is added uniformly by utilizing an integrated gas conveying system 4 And K 2 TiF 6 Alloying the mixture for 5-10 min at 700-800 ℃ after the addition of the mixture, pouring out water slag after the reaction, uniformly scattering light calcium carbonate on the surface of the molten liquid, and removing residual water slag;
4) Repeating the step 3) twice to respectively finish the third feeding reaction and the fourth feeding reaction; wherein, 24 to 27 weight percent of KBF4 and K2TiF6 mixture is added for the third time, and the rest KBF is added for the fourth time 4 And K 2 TiF 6 A mixture;
5) And (3) after the temperature of the obtained melt is adjusted to 720-800 ℃, transferring the melt into a casting furnace through a launder, degassing and standing the melt in the casting furnace for 10-30 min, fishing out surface scum, and then directly casting a trapezoid bar ingot or rolling the trapezoid bar ingot into a bar through a continuous casting and rolling machine.
The stirring power in each step is 300KW, and the electromagnetic frequency is as follows: 75HZ. All the steps are in a stirring state until the reaction is finished, and the acid water slag is turned off when the acid water slag is poured.
The mixture of KBF4 and K2TiF6 is added into aluminum water in four times. The inventor finds that under the specific process conditions, the charging step of KBF4 and K2TiF6 mixtures can have a relatively large influence on the quality of the refiner, the excessive charging step can lead to the growth and thickening of plasmids, the insufficient charging step can lead to uneven distribution of TiAl3 and TiB2 particles in the interior, and the insufficient charging step can lead to the reduction of refining capability in the subsequent use.
The internal tissue TiB of the Al-Ti-B product produced by the application 2 Particle and TiAl 3 The particle size is fine, the distribution is uniform and dispersed, and the oxide and boride in the internal tissue are effectively controlled. Can meet the requirements of refining treatment of high-quality aluminum and aluminum alloy materials.
The light calcium carbonate can effectively adsorb acid residues and crust, and is convenient for complete cleaning.
To further ensure the quality of the refiner, KBF 4 And K 2 TiF 6 In the mixture, KBF 4 And K 2 TiF 6 The mass ratio of (3) is 3.9: (6.1±0.5); aluminum water and KBF 4 And K 2 TiF 6 The mass ratio of the mixture is 10: (4-6).
KBF 4 And K 2 TiF 6 Is completed on an integrated salt-mixing gas conveying device. First KBF is carried out 4 And K 2 TiF 6 Placing the mixed salt in a feeding bin, then setting the conveying coefficient of integrated mixed salt gas conveying equipment, starting the first-step automatic weighing mixed salt system of the integrated mixed salt gas conveying equipment, and carrying out KBF (potassium hydrogen fluoride) treatment 4 And K 2 TiF 6 According to the calculated weight ratio, then self-heatingMixing is dynamically carried out until the raw materials are uniformly mixed.
The feeding through the integrated gas conveying ensures that KBF is ensured in the reaction process 4 And K 2 TiF 6 The mixture is added uniformly, and the reaction is more complete and complete. Effective control of boride (TiB) 2 、TiB 3 ……TiB 12 Etc.).
The step 1) is to heat the clean aluminum water after refining and slag fishing to 700-800 ℃, transfer the aluminum water into an induction furnace through an aluminum water transfer system, start the up-down stirring function of the induction furnace, and simultaneously gas and remove the argon gas in the aluminum water. The pressure of argon in the induction furnace is 0.1-0.5Mpa.
Argon is introduced in the reaction process in the step 2-4), so that the gas pressure is maintained at 0.1-0.5Mpa.
In order to further improve the quality of the refiner, the step 5) is to adjust the temperature of the obtained melt to 720-800 ℃, transfer the melt into a casting furnace through a launder, and carry out degassing and refining according to the following method: starting up and down stirring function (stirring power 300KW, frequency 75 Hz) of the casting furnace, simultaneously starting a rotary degassing machine and an argon gas source, adjusting argon gas pressure to 0.1-0.5Mpa, continuously floating residues in a melt out of the liquid level, closing the up and down stirring function, closing the degassing machine and closing the argon gas source after 3-5 min, and fishing out the liquid level scum, wherein the process (from the process of starting up the up and down stirring function of the casting furnace to the process of fishing out the liquid level scum) is repeated for 3-4 times until the liquid level is clean; after degassing and refining are finished, the upper and lower stirring functions of the degassing machine and the induction furnace are closed, the air source is closed, surface scum is fished out until the liquid level is clean, and after the alloy liquid is kept stand for less than or equal to 10min, casting or continuous casting and rolling are prepared.
The total time of degassing and refining is controlled to be less than or equal to 40min.
Casting or continuous casting and rolling as described above: when the temperature of the alloy liquid is 720-750 ℃, casting or continuous casting and rolling are started, and the alloy liquid in the furnace flows into a casting machine through a launder to directly produce Al-Ti-B alloy trapezoidal long ingots or flows into a continuous casting and rolling machine to produce Al-Ti-B alloy wires.
The technology not mentioned in the present application refers to the prior art.
The preparation method of the four-step high-quality Al-Ti-B grain refiner is simple to operate and convenient for industrial production; can prepare high-quality Al-Ti-B grain refiner, and the prepared Al-Ti-B grain refiner is 1cm at random 2 TiB in the longitudinal section of (2) 2 Particle 95% < 0.5 μm, average size: about 0.11 microns, uniformly dispersed particles, high uniformity and no annular TiB 2 Inclusions in agglomerates and linear agglomerates, optionally 1cm 2 99.7% of TiAl in the longitudinal section of (C) 3 Particle < 6 mu m, tiAl 3 The average particle size is 2-4 mu m, can be used for preparing high-quality products, and has the advantages of small dosage, long-lasting effect and no reduction of conductivity.
Drawings
FIG. 1 is a diagram of a four-step process high quality Al-Ti-B grain refiner according to the present application;
FIG. 2 shows the metallographic structure of the four-step high quality Al-Ti-B grain refiner of the present application;
FIG. 3 shows TiB in the four-step high quality Al-Ti-B grain refiner of the present application 2 SEM morphology pictures of particles;
FIG. 4 is a graph showing the effect of refining the high-quality Al-Ti-B grain refiner by the four-step method of the application;
FIG. 5 is a state diagram of the microscope of FIG. 4;
Detailed Description
For a better understanding of the present application, the following examples are further illustrated, but are not limited to the following examples.
Example 1
A preparation method of a four-step high-quality Al-Ti-B grain refiner comprises the following steps:
heating clean 1 ton molten aluminum (purity 99.9 wt%) to 720 deg. C, transferring molten aluminum into induction furnace by molten aluminum transfer system, removing slag, starting up-down stirring function of induction furnace (stirring power 300KW, frequency 75 Hz), introducing argon into molten aluminum to remove gas, maintaining argon pressure in induction furnace at 0.3-0.4Mpa (all the pressure is required in charging process), then making KBF 4 And K 2 TiF 6 Mixed material(KBF 4 And K 2 TiF 6 The mass ratio of (3) is 3.9:6.1 Four times of conveying the mixed salt gas into molten aluminum for reaction through an integrated mixed salt gas conveying system, and the method specifically comprises the following steps:
1) A first time; 128kg KBF is uniformly added into molten aluminum by utilizing an integrated salt mixing gas conveying system 4 And K 2 TiF 6 Mixing, controlling the feeding time to be 10min, pouring acid water slag after the feeding, alloying for 3min at 720 ℃, uniformly scattering light calcium carbonate on the surface of molten liquid, and removing residual acid water slag;
2) Maintaining 720 deg.c for the second feeding reaction, adding 130kg KBF 4 And K 2 TiF 6 The mixed material is added for 6min, and KBF is added uniformly by utilizing an integrated gas conveying system 4 And K 2 TiF 6 After the mixture is added, alloying for 5min at 720 ℃, pouring acid water slag after the reaction is finished, uniformly scattering light calcium carbonate on the surface of the molten liquid, and removing residual acid water slag;
3) Repeating the step 2) twice to respectively finish the third feeding reaction and the fourth feeding reaction; adding KBF for the third time and the fourth time 4 And K 2 TiF 6 The amount of the mixture is 130kg;
4) The temperature of the obtained molten liquid is adjusted to 720 ℃, the molten liquid is transferred into a casting furnace through a launder, the up-and-down stirring function (stirring power 300KW, frequency 75 Hz) of the casting furnace is started, meanwhile, a rotary degassing machine and an argon gas source are started, the argon gas pressure is adjusted to 0.2-0.3Mpa, acid residues in the molten liquid continuously float out of the liquid surface, after 3min, the up-and-down stirring function is closed, the degassing machine is closed, the argon gas source is closed, the acid residues on the liquid surface are fished out, the process is repeated for 3 times, and the liquid surface is clean; and (3) closing the degassing machine, the induction furnace, the up-down stirring function and the air source, fishing out surface scum (oxidizing slag) until the liquid level is clean, standing the alloy liquid for 5min, and allowing the alloy liquid at 720 ℃ to flow into a continuous casting and rolling machine through a launder to perform continuous casting and rolling to obtain a phi 9.5mm wire rod, wherein the product is shown in figure 1.
Metallographic structure, as shown in FIG. 2, it can be seen that TiAl 3 The particles are fine and uniform and have no aggregation.
Arbitrary 1cm 2 99.7% of TiAl in the longitudinal section of (C) 3 Particle < 6 mu m, tiAl 3 The average diameter was 2.68 microns and the maximum diameter was 6.83 microns.
Arbitrary 1cm 2 TiB in the longitudinal section of (2) 2 Particle 98% < 0.4 μm, average size: 0.11 micron, maximum size of 0.48 micron, minimum size of 0.05 micron, dispersed and uniform distribution, and no ring TiB 2 Agglomerates and inclusions in linear agglomerates. Meets the industry standard 447.1-2011.
Refinement test: 500 g of industrial pure aluminum is heated and melted to 720 ℃, the prepared Al-Ti-B grain refiner is added according to the amount of 0.2 g/100 g of aluminum, the temperature is kept for 15 minutes, a Reynolds standard golf T-shaped die is poured, the refining effect is shown in figures 4-5, the grain size at the position 51mm away from the bottom surface of the sample is measured, the grain size of the refined industrial pure aluminum can reach about 60 mu m, and the conductivity is not reduced.
Comparative example 1
A preparation method of a five-step high-quality Al-Ti-B grain refiner comprises the following steps:
heating 1 ton of clean molten aluminum (purity 99.9 wt%) to 720 deg. C, transferring molten aluminum into induction furnace by molten aluminum transfer system, removing slag, starting up-down stirring function (stirring power 300KW, frequency 75 Hz) of induction furnace, introducing argon into molten aluminum to remove gas, maintaining argon pressure in induction furnace at 0.3-0.4Mpa, and then making KBF 4 And K 2 TiF 6 Mixed material (KBF) 4 And K 2 TiF 6 The mass ratio of (3) is 3.9:6.1 Four times of conveying the mixed salt gas into molten aluminum for reaction through an integrated mixed salt gas conveying system, and the method specifically comprises the following steps:
1) A first time; 128kg KBF is uniformly added into molten aluminum by utilizing an integrated salt mixing gas conveying system 4 And K 2 TiF 6 Mixing, controlling the feeding time to be 10min, pouring acid water slag after the feeding, alloying for 3min at 720 ℃, uniformly scattering light calcium carbonate on the surface of molten liquid, and removing residual acid water slag;
2) Maintaining the temperature at 720 deg.C, adding for the second timeReacting the materials, adding 97.5kg KBF for the second time 4 And K 2 TiF 6 The mixed material is added for 6min, and KBF is added uniformly by utilizing an integrated gas conveying system 4 And K 2 TiF 6 After the mixture is added, alloying for 5min at 720 ℃, pouring acid water slag after the reaction is finished, uniformly scattering light calcium carbonate on the surface of the molten liquid, and removing residual acid water slag;
3) Repeating the step 2) for three times to respectively finish the third, fourth and fifth feeding reactions; adding KBF for the third, fourth and fifth times 4 And K 2 TiF 6 The amount of the mixture is 97.5kg;
4) The temperature of the obtained molten liquid is adjusted to 720 ℃, the molten liquid is transferred into a casting furnace through a launder, the up-and-down stirring function (stirring power 300KW, frequency 75 Hz) of the casting furnace is started, meanwhile, a rotary degassing machine and an argon gas source are started, the argon gas pressure is adjusted to 0.2-0.3Mpa, acid residues in the molten liquid continuously float out of the liquid surface, after 3min, the up-and-down stirring function is closed, the degassing machine is closed, the argon gas source is closed, the acid residues on the liquid surface are fished out, the process is repeated for 3 times, and the liquid surface is clean; and (3) closing the degassing machine, the induction furnace, the up-down stirring function and the air source, fishing out surface scum (oxidizing slag) until the liquid level is clean, standing the alloy liquid for 5min, and allowing the alloy liquid at 720 ℃ to flow into a continuous casting and rolling machine through a launder to perform continuous casting and rolling to obtain a phi 9.5mm wire rod.
This example differs from example 1 in that KBF is used 4 And K 2 TiF 6 The mixture was added in 5 steps. Any 1cm of this example 2 99.7% of TiAl in the longitudinal section of (C) 3 Particle < 100 mu m, tiAl 3 The average diameter was 24.8 microns. Arbitrary 1cm 2 TiB in the longitudinal section of (2) 2 Particle 95% < 2 μm, average size: 2 microns.
Refinement test: 500 g of industrial pure aluminum is heated and melted to 720 ℃, the prepared Al-Ti-B grain refiner is added according to the amount of 0.2 g/100 g of aluminum, the temperature is kept for 15 minutes, the mixture is poured into a standard golf T-shaped die with Reynolds number, the grain size of the position 51mm away from the bottom surface of the sample is measured, the grain size of the refined industrial pure aluminum can reach about 100 mu m, and the conductivity is reduced by 1.01%.
It can be seen that after 5 steps of addition, the particles have a significant tendency to increase.
Comparative example 2
A preparation method of a three-step high-quality Al-Ti-B grain refiner comprises the following steps:
heating 1 ton of clean molten aluminum (purity 99.9 wt%) to 720 deg. C, transferring molten aluminum into induction furnace by molten aluminum transfer system, removing slag, starting up-down stirring function (stirring power 300KW, frequency 75 Hz) of induction furnace, introducing argon into molten aluminum to remove gas, maintaining argon pressure in induction furnace at 0.3-0.4Mpa, and then making KBF 4 And K 2 TiF 6 Mixed material (KBF) 4 And K 2 TiF 6 The mass ratio of (3) is 3.9:6.1 Four times of conveying the mixed salt gas into molten aluminum for reaction through an integrated mixed salt gas conveying system, and the method specifically comprises the following steps:
1) A first time; 128kg KBF is uniformly added into molten aluminum by utilizing an integrated salt mixing gas conveying system 4 And K 2 TiF 6 Mixing, controlling the feeding time to be 10min, pouring acid water slag after the feeding, alloying for 3min at 720 ℃, uniformly scattering light calcium carbonate on the surface of molten liquid, and removing residual acid water slag;
2) Maintaining 720 deg.c, and adding 195kg KBF for the second time 4 And K 2 TiF 6 The mixed material is added for 6min, and KBF is added uniformly by utilizing an integrated gas conveying system 4 And K 2 TiF 6 After the mixture is added, alloying for 5min at 720 ℃, pouring acid water slag after the reaction is finished, uniformly scattering light calcium carbonate on the surface of the molten liquid, and removing residual acid water slag;
3) Repeating the step 2) once to respectively finish the third feeding reaction; adding KBF for the third time 4 And K 2 TiF 6 The amount of the mixture is 195kg;
4) The temperature of the obtained molten liquid is adjusted to 720 ℃, the molten liquid is transferred into a casting furnace through a launder, the up-and-down stirring function (stirring power 300KW, frequency 75 Hz) of the casting furnace is started, meanwhile, a rotary degassing machine and an argon gas source are started, the argon gas pressure is adjusted to 0.2-0.3Mpa, acid residues in the molten liquid continuously float out of the liquid surface, after 3min, the up-and-down stirring function is closed, the degassing machine is closed, the argon gas source is closed, the acid residues on the liquid surface are fished out, the process is repeated for 3 times, and the liquid surface is clean; and (3) closing the degassing machine, the induction furnace, the up-down stirring function and the air source, fishing out surface scum (oxidizing slag) until the liquid level is clean, standing the alloy liquid for 5min, and allowing the alloy liquid at 720 ℃ to flow into a continuous casting and rolling machine through a launder to perform continuous casting and rolling to obtain a phi 9.5mm wire rod.
This example differs from example 1 in that KBF is used 4 And K 2 TiF 6 The mixture was added in 3 steps. Any 1cm of this example 2 91.2% of TiAl in the longitudinal section of (C) 3 Particle < 15 mu m, tiAl 3 The average diameter was 8.8 microns. Arbitrary 1cm 2 TiB in the longitudinal section of (2) 2 Particle 92.6% < 2 μm, average size: 1.86 microns, with a maximum dimension of 5.36 microns.
Refinement test: 500 g of industrial pure aluminum is heated and melted to 720 ℃, the prepared Al-Ti-B grain refiner is added according to the amount of 0.2 g/100 g of aluminum, the temperature is kept for 15 minutes, the mixture is poured into a standard golf T-shaped die with Reynolds number, the grain size at the position 51mm away from the bottom surface of a sample is measured, the grain size of the refined industrial pure aluminum can reach 86 mu m, and the conductivity is reduced by 0.86%.
It can be seen that after 3 steps, the particles have a significant tendency to increase, and the particles are too few and unevenly distributed.
Comparative example 3
The preparation method of the two-step high-quality Al-Ti-B grain refiner comprises the following steps:
heating 1 ton of clean molten aluminum (purity 99.9 wt%) to 720 deg. C, transferring molten aluminum into induction furnace by molten aluminum transfer system, removing slag, starting up-down stirring function (stirring power 300KW, frequency 75 Hz) of induction furnace, introducing argon into molten aluminum to remove gas, maintaining argon pressure in induction furnace at 0.3-0.4Mpa, and then making KBF 4 And K 2 TiF 6 Mixed material (KBF) 4 And K 2 TiF 6 The mass ratio of (3) is 3.9:6.1 Four times of conveying the molten aluminum into molten aluminum through an integrated salt mixing gas conveying system for reactionThe method is characterized by comprising the following steps:
1) A first time; 128kg KBF is uniformly added into molten aluminum by utilizing an integrated salt mixing gas conveying system 4 And K 2 TiF 6 Mixing, controlling the feeding time to be 10min, pouring acid water slag after the feeding, alloying for 3min at 720 ℃, uniformly scattering light calcium carbonate on the surface of molten liquid, and removing residual acid water slag;
2) Maintaining 720 deg.c for the second feeding reaction, adding 390kg KBF 4 And K 2 TiF 6 The mixed material is added for 6min, and KBF is added uniformly by utilizing an integrated gas conveying system 4 And K 2 TiF 6 After the mixture is added, alloying for 5min at 720 ℃, pouring acid water slag after the reaction is finished, uniformly scattering light calcium carbonate on the surface of the molten liquid, and removing residual acid water slag;
3) The temperature of the obtained molten liquid is adjusted to 720 ℃, the molten liquid is transferred into a casting furnace through a launder, the up-and-down stirring function (stirring power 300KW, frequency 75 Hz) of the casting furnace is started, meanwhile, a rotary degassing machine and an argon gas source are started, the argon gas pressure is adjusted to 0.2-0.3Mpa, acid residues in the molten liquid continuously float out of the liquid surface, after 3min, the up-and-down stirring function is closed, the degassing machine is closed, the argon gas source is closed, the acid residues on the liquid surface are fished out, the process is repeated for 3 times, and the liquid surface is clean; and (3) closing the degassing machine, the induction furnace, the up-down stirring function and the air source, fishing out surface scum (oxidizing slag) until the liquid level is clean, standing the alloy liquid for 5min, and allowing the alloy liquid at 720 ℃ to flow into a continuous casting and rolling machine through a launder to perform continuous casting and rolling to obtain a phi 9.5mm wire rod.
This example differs from example 1 in that KBF is used 4 And K 2 TiF 6 The mixture was added in 2 steps. Any 1cm of this example 2 91.2% of TiAl in the longitudinal section of (C) 3 Particle < 15 mu m, tiAl 3 The average diameter was 8.8 microns. Arbitrary 1cm 2 TiB in the longitudinal section of (2) 2 Particle 92.9% < 2 μm, average size: 1.83 microns, with a maximum dimension of 4.96 microns.
Refinement test: 500 g of industrial pure aluminum is heated and melted to 720 ℃, the prepared Al-Ti-B grain refiner is added according to the amount of 0.2 g/100 g of aluminum, the temperature is kept for 15 minutes, the mixture is poured into a standard golf T-shaped die with Reynolds number, the grain size of the position 51mm away from the bottom surface of the sample is measured, the grain size of the refined industrial pure aluminum can reach about 85 mu m, and the conductivity is reduced by 0.82%.
From this, it can be seen that the results after the reduction to 2 steps are closer to those of 3, but the results tend to be significantly larger than those of example 1, and the uniformity is poor due to too few particles.
Claims (9)
1. A preparation method of a four-step high-quality Al-Ti-B grain refiner is characterized by comprising the following steps of: the method comprises the following steps:
1) After the aluminum water is heated to 700-800 ℃, starting up and down stirring function of the induction furnace, simultaneously introducing argon into the aluminum water for degassing, and then performing KBF 4 And K 2 TiF 6 The mixture is transferred into molten aluminum for reaction in four times through an integrated salt mixing gas conveying system;
2) A first time; uniformly adding 22-25wt% KBF into molten aluminum by utilizing an integrated salt mixing gas conveying system 4 And K 2 TiF 6 Mixing materials, controlling the feeding time to be 10-15 min, pouring out water slag, alloying for 3-5 min at 700-800 ℃, uniformly scattering light calcium carbonate on the surface of molten liquid, and removing residual water slag;
3) Maintaining 700-800 deg.c, and adding 24-27 wt% KBF for the second time 4 And K 2 TiF 6 The mixture is added for 5-8 min, and KBF is added uniformly by utilizing an integrated gas conveying system 4 And K 2 TiF 6 Alloying the mixture for 5-10 min at 700-800 ℃ after the addition of the mixture, pouring out water slag after the reaction, uniformly scattering light calcium carbonate on the surface of the molten liquid, and removing residual water slag;
4) Repeating the step 3) twice to respectively finish the third feeding reaction and the fourth feeding reaction; wherein, 24 to 27 weight percent of KBF4 and K2TiF6 mixture is added for the third time, and the rest KBF is added for the fourth time 4 And K 2 TiF 6 A mixture;
5) And (3) after the temperature of the obtained melt is adjusted to 720-800 ℃, transferring the melt into a casting furnace through a launder, degassing and standing the melt in the casting furnace for 10-30 min, fishing out surface scum, and then directly casting a trapezoid bar ingot or rolling the trapezoid bar ingot into a bar through a continuous casting and rolling machine.
2. The method for preparing the four-step high-quality Al-Ti-B grain refiner according to claim 1, which is characterized in that: KBF (K-BF) 4 And K 2 TiF 6 In the mixture, KBF 4 And K 2 TiF 6 The mass ratio of (3) is 3.9: (6.1±0.5); aluminum water and KBF 4 And K 2 TiF 6 The mass ratio of the mixture is 10: (4-6).
3. The method for preparing the four-step high-quality Al-Ti-B grain refiner according to claim 1 or 2, which is characterized in that: step 1) after the clean aluminum water after refining and slag dragging is heated to 700-800 ℃, transferring the aluminum water into an induction furnace through an aluminum water transfer system, starting an up-down stirring function of the induction furnace, and simultaneously introducing argon gas into the aluminum water for degassing.
4. A method for preparing the four-step high quality Al-Ti-B grain refiner according to claim 3, wherein: the pressure of argon in the induction furnace is 0.1-0.5Mpa.
5. The method for preparing the four-step high-quality Al-Ti-B grain refiner according to claim 1 or 2, which is characterized in that: in the reaction process of the step 2-4), argon is introduced, so that the gas pressure is maintained at 0.1-0.5Mpa.
6. The method for preparing the four-step high-quality Al-Ti-B grain refiner according to claim 1 or 2, which is characterized in that: step 5) after the temperature of the obtained melt is adjusted to 720-800 ℃, the melt is transferred into a casting furnace through a launder, and degassing and refining are carried out according to the following method: starting up and down stirring functions of the casting furnace, starting a rotary degassing machine and an argon gas source, adjusting the argon pressure to 0.1-0.5Mpa, continuously floating residues in the melt out of the liquid level for 3-5 min, closing the up and down stirring functions, closing the degassing machine and closing the argon gas source, fishing out scum on the liquid level, and repeating the process for 3-4 times until the liquid level is clean; after degassing and refining are finished, the upper and lower stirring functions of the degassing machine and the induction furnace are closed, the air source is closed, surface scum is fished out until the liquid level is clean, and after the alloy liquid is kept stand for less than or equal to 10min, casting or continuous casting and rolling are prepared.
7. The method for preparing the four-step high-quality Al-Ti-B grain refiner according to claim 6, which is characterized in that: the total time of degassing and refining is controlled to be less than or equal to 40min.
8. The method for preparing the four-step high-quality Al-Ti-B grain refiner according to claim 1 or 2, which is characterized in that: casting or continuous casting and rolling: when the temperature of the alloy liquid is 720-750 ℃, casting or continuous casting and rolling are started, and the alloy liquid in the furnace flows into a casting machine through a launder to directly produce Al-Ti-B alloy trapezoidal long ingots or flows into a continuous casting and rolling machine to produce Al-Ti-B alloy wires.
9. Use of the four-step high quality Al-Ti-B grain refiner made by the method of any one of claims 1-8, characterized in that: for refining aluminum, the dosage is 0.1-0.3 g/100 g aluminum.
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