CN109518040B - Method for continuously preparing Al-Ti-B grain refiner by ultrasonic treatment - Google Patents

Method for continuously preparing Al-Ti-B grain refiner by ultrasonic treatment Download PDF

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CN109518040B
CN109518040B CN201910068755.8A CN201910068755A CN109518040B CN 109518040 B CN109518040 B CN 109518040B CN 201910068755 A CN201910068755 A CN 201910068755A CN 109518040 B CN109518040 B CN 109518040B
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grain refiner
launder
ultrasonic treatment
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melt
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CN109518040A (en
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韩延峰
陆树生
张佼
王俊
孙宝德
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Shanghai Jiaotong University
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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C21/00—Alloys based on aluminium
    • C22C21/003—Alloys based on aluminium containing at least 2.6% of one or more of the elements: tin, lead, antimony, bismuth, cadmium, and titanium
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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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
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys
    • C22C1/10—Alloys containing non-metals
    • C22C1/1036—Alloys containing non-metals starting from a melt
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys
    • C22C1/10—Alloys containing non-metals
    • C22C1/1036—Alloys containing non-metals starting from a melt
    • C22C1/1047—Alloys containing non-metals starting from a melt by mixing and casting liquid metal matrix composites
    • C22C1/1052—Alloys containing non-metals starting from a melt by mixing and casting liquid metal matrix composites by mixing and casting metal matrix composites with reaction
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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Abstract

The invention discloses a method for continuously preparing an Al-Ti-B grain refiner by ultrasonic treatment, which comprises the following steps: weighing potassium fluotitanate and potassium fluoborate; heating the launder and preserving heat, and introducing the ultrasonic probes distributed in a Z shape; injecting potassium fluotitanate and potassium fluoborate mixed salt into the launder, starting ultrasonic equipment when pure aluminum and mixed salt melt flow in the launder, and applying continuous ultrasonic treatment; and (3) allowing the mixed melt after ultrasonic treatment to enter a transfer ladle, separating reaction slag and Al-Ti-B melt, degassing and deslagging the Al-Ti-B melt flowing into the standing holding furnace, and then casting to obtain the grain refiner. The method can realize the large-scale continuous preparation of the grain refiner by the ultrasonic treatment of 500-8000 kg/h, breaks through the defect of serious limitation of the capacity in the preparation of the traditional ultrasonic treatment process, and the size of the cast grain of the industrial pure aluminum refined by the prepared Al-Ti-B grain refiner is obviously superior to the refining effect of the traditional grain refiner.

Description

Method for continuously preparing Al-Ti-B grain refiner by ultrasonic treatment
Technical Field
The invention relates to a preparation method of a grain refiner in the field of metal materials, in particular to a method for continuously preparing an Al-Ti-B grain refiner in a large scale by utilizing ultrasonic treatment.
Background
At present, a villiaumite reaction method is generally adopted at home and abroad to prepare the Al-Ti-B grain refiner widely used in the aluminum industry. Through the literature search of the prior art, the article 'gain refining of aluminum and its allogenic catalysis and alloying' published by B.S. Murty in journal of International Materials Reviews, volume 47, pages 1, 3-29, 2002 details the fluoride salt reaction preparation process of Al-Ti-B Grain refiner; the fluoride salt reaction preparation process generally comprises the step of reacting potassium fluotitanate (K)2TiF6) And potassium fluoroborate (KBF)4) Adding the mixed salt into an aluminum melt with the temperature of more than 750 ℃, and carrying out mechanical or electromagnetic stirring for more than one hour to obtain the Al-Ti-B grain refiner. The Al-Ti-B grain refiner prepared by the method has one to the industrial pure aluminum and the alloy thereofThe refining effect is definite, but in order to ensure the full reaction of the villiaumite and the aluminum melt, the reaction melt needs to be stirred mechanically or electromagnetically for more than one hour, the preparation period is long, the energy consumption is high, and the oxidation burning loss of metal is serious; even more disadvantageously, the long-term preparation leads to TiB being formed in different stages of the reaction2The particle size is greatly different and shows non-uniform aggregation and bulk distribution in the final tissue; meanwhile, TiAl in the refiner3The phase size is more than 80 mu m, and the melting response lags when the grains are refined; the refining capability of the Al-Ti-B grain refiner prepared by adopting the conventional fluorine salt reaction process has a limit, and only the industrial pure aluminum cast-state grains can be refined to about 150 mu m at the minimum.
Patent ZL200410084303.2 proposes that Al-Ti-B grain refiner is prepared by applying ultrasonic treatment in the fluoride salt reaction process, the preparation period is shortened to 2-10 minutes, and TiAl in the refiner tissue is simultaneously used3Phase size, TiB2The distribution state of the particles is beneficially improved, and the refinement capability of the Al-Ti-B grain refiner is improved. Due to the limited effective working space of the ultrasonic probe in the aluminum melt, the ultrasonic probe is usually 500cm3About, the Al-Ti-B grain refiner prepared by the process method has limited productivity which is usually lower than 10 kg/h, which can not meet the requirements of industrial production.
Disclosure of Invention
The invention aims to overcome the defects of the technology, and provides a method for continuously preparing the Al-Ti-B grain refiner on a large scale by ultrasonic treatment, so as to realize large-scale preparation of the Al-Ti-B grain refiner with excellent tissue morphology and refining performance at the level of 500-8000 kg/h.
In order to achieve the above object, the present invention provides a method for continuously preparing an Al-Ti-B grain refiner by ultrasonic treatment, comprising:
s1, weighing potassium fluotitanate K according to the target component of the Al-Ti-B grain refiner to be prepared2TiF6KBF of potassium fluoroborate4Is a reaction of K2TiF6、KBF4Mixing homogeneously to obtain K2TiF6And KBF4Mixed salt；
S2, heating the launder to 750-1200 ℃, preserving heat, and introducing cylindrical ultrasonic probes in Z-shaped distribution at the upper part of the launder in order to ensure that the action range of ultrasonic waves is distributed in the whole near-surface area of the aluminum liquid;
s3, continuously introducing industrial pure aluminum melt with the temperature of 750-1000 ℃ at the upper port of the launder, controlling the height of the aluminum liquid in the launder to be 8-10 cm and the flowing time of the aluminum liquid in the launder to be 3-10 minutes in order to ensure that ultrasonic waves can act on the bottom of the aluminum liquid and promote full reaction of villiaumite and the aluminum liquid; simultaneous continuous injection of K formulated in S12TiF6And KBF4Mixed salt, controlling K according to the target component of Al-Ti-B grain refiner to be prepared and the flow of aluminum liquid2TiF6And KBF4The addition amount of the mixed salt;
s4, when the pure aluminum and the mixed salt melt flow in the flow groove, starting ultrasonic equipment, and applying continuous ultrasonic treatment on the upper part of the flow groove;
and S5, allowing the ultrasonically treated mixed melt to enter a transfer ladle through the lower port of the runner, allowing reaction slag to flow out of the upper opening of the transfer ladle, allowing the Al-Ti-B melt to flow into a standing holding furnace through the lower opening of the transfer ladle, degassing and deslagging in the standing holding furnace, and casting to obtain the Al-Ti-B grain refiner.
Preferably, in S1, in the Al-Ti-B grain refiner, the weight percentage of Ti is 1.00-7.00%, and the weight percentage of B is 0.50-1.30%, under the condition, the refining performance of the grain refiner prepared by the invention can be better improved.
Preferably, in S2, the total length of the runner is 2-12 m, the cross section of the runner is U-shaped, and the cross-sectional dimension is: the lower bottom is 6-12 cm wide, the upper opening is 15-25 cm wide and the height is 15-25 cm, and the proportioning requirement of the aluminum liquid and the mixed villiaumite can be better ensured under the condition.
Preferably, in S2, the launder is heated to 800-1000 ℃, and the temperature is kept for 8-24 hours, under the condition, the temperature and the fluidity of the aluminum liquid can be fully ensured.
Preferably, in S2, the number of the ultrasonic probes is 10-50, the distance between adjacent probes of the probes is 15-30 cm, and the distance between the bottom end surface of each probe and the bottom of the launder is 8-12 cm, so that the ultrasonic action can be better realized in the whole area of the aluminum liquid.
Preferably, in S3, the temperature of the industrial pure aluminum melt is 800-900 ℃, under which the refining performance of the grain refiner prepared by the invention can be better improved.
Preferably, in S3, the aluminum liquid flows through the whole launder for 5-8 minutes, and under the condition, the refining performance of the grain refiner prepared by the invention can be better improved.
Preferably, in S4, the ultrasonic frequency is 20 + -1 kHz, and the power is 500-5000W, under which the refining performance of the grain refiner prepared by the invention can be better improved.
Compared with the prior art, the invention has the following beneficial effects:
the invention realizes the large-scale continuous preparation of the Al-Ti-B grain refiner by ultrasonic treatment, the yield of the Al-Ti-B grain refiner reaches the level of 500-8000 kg/h, and the defect of serious limitation of the productivity when the Al-Ti-B grain refiner is prepared by the traditional ultrasonic treatment process is broken through.
In the Al-Ti-B grain refiner prepared by the invention, TiB2Small size difference of particles, uniform dispersion distribution and TiAl3The phases are in the form of blocks of less than 30 μm (see FIG. 2); the grain size of the industrial pure aluminum as cast state refined by the Al-Ti-B grain refiner prepared by the invention is obviously superior to the refining effect of the traditional Al-Ti-B grain refiner (see the figure 3 and the figure 4)
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Other features, objects and advantages of the invention will become more apparent upon reading of the detailed description of non-limiting embodiments with reference to the following drawings:
FIG. 1a and FIG. 1B are schematic diagrams of core processing equipment for continuously preparing Al-Ti-B grain refiner by ultrasonic treatment according to an embodiment of the invention;
in fig. 1a and 1 b: 1-ultrasonic probe, 2-launder, 3-lining, 4-heating cover, 5-launder shell;
FIG. 2 is a scanning electron microscope topography of the microstructure of the Al-Ti-B grain refiner prepared in example 5 of the present invention;
FIG. 3 is a diagram of a metallurgical macroscopic grain structure of industrial pure aluminum added with 0.20 wt% of a traditional Al-5 Ti-1B refined;
FIG. 4 is a graph with addition of 0.20 wt% Al-5 Ti-1B refined industrial pure aluminum metallographic macroscopic grain structure prepared in example 5.
Detailed Description
The present invention will be described in detail with reference to specific examples. The following examples will assist those skilled in the art in further understanding the invention, but are not intended to limit the invention in any way. It should be noted that variations and modifications can be made by persons skilled in the art without departing from the spirit of the invention. All falling within the scope of the present invention.
Referring to fig. 1a and 1B, a schematic diagram of core process equipment for continuously preparing an Al-Ti-B grain refiner by ultrasonic treatment is shown, wherein: 1-ultrasonic probe, 2-launder, 3-lining, 4-heating cover, 5-launder shell; the Al-Ti-B grain refiner can be continuously prepared on a large scale by ultrasonic treatment through the process equipment.
The following examples 1-7 were carried out using the above equipment and can be carried out as follows:
(1) according to the target components of Al-Ti-B grain refiner to be prepared, the weight percentage of Ti is 1.00-7.00%, the weight percentage of B is 0.50-1.30%, according to the generated weight percentage, potassium fluotitanate (K) with corresponding proportion is weighed2TiF6) Potassium fluoroborate (KBF)4) And is combined with K2TiF6And KBF4Mixing uniformly, and charging into a hopper for later use.
(2) Heating a flow groove with a U-shaped section with the total length of 2-12 m to 750-1200 ℃, preserving heat for 8-24 hours, introducing 10-50 cylindrical ultrasonic probes in Z-shaped distribution at the upper part of the flow groove, wherein the distance between adjacent probes is 15-30 cm, and the distance between the bottom end surface of each probe and the bottom of the flow groove is 8-12 cm.
(3) At the upper port of the flow groove, the temperature is continuously introduced to 750-1000 DEG CControlling the height of the aluminum liquid in the launder to be 8-10 cm and the time for the aluminum liquid to flow through the whole launder to be 3-10 minutes; simultaneously and continuously injecting the K prepared in the step (1)2TiF6And KBF4And (3) mixed salt, wherein the adding amount of the mixed fluorine salt is controlled according to the target component of the Al-Ti-B grain refiner to be prepared and the flow rate of the aluminum liquid.
(4) When the aluminum melt and the mixed salt melt flow in the launder, the ultrasonic equipment is started, continuous ultrasonic treatment is introduced to the upper part of the launder, the ultrasonic frequency is 20 +/-1 kHz, and the power is 500-.
(5) And the ultrasonically treated mixed melt enters a transfer ladle through a lower port of the runner, reaction slag flows out from an upper opening of the transfer ladle, Al-Ti-B melt flows into a standing holding furnace through a lower opening of the transfer ladle, and the prepared Al-Ti-B melt enters a casting production line after being degassed and deslagged in the standing holding furnace to obtain the Al-Ti-B grain refiner.
Refining test: 500 g of industrial pure aluminum, heating and melting to 730 ℃, adding the prepared Al-Ti-B grain refiner according to the amount of 0.2 g/100 g of aluminum, preserving the temperature for 15 minutes, pouring into a Reynolds standard golf T-shaped die, and measuring the grain size at a position 51mm away from the bottom surface of a sample.
The parameters and the results of the specific examples 1 to 7 are shown in the following table:
Figure BDA0001956594550000051
in the embodiment of the invention, the process equipment shown in fig. 1a and 1B is used for realizing the continuous large-scale preparation of the Al-Ti-B grain refiner by ultrasonic treatment, and the defect that the yield is severely limited when the Al-Ti-B grain refiner is prepared by the traditional ultrasonic treatment process is overcome, for example, the yield of the Al-Ti-B grain refiner reaches 6800 kg/h level in the embodiment 6; in the Al-Ti-B grain refiner prepared in the embodiment 5 of the invention, TiB2Uniform dispersion distribution of particles, TiAl3The phases are in the form of blocks of less than 30 μm (see FIG. 2); the size of the cast-state crystal grain of the industrial pure aluminum refined by the Al-Ti-B grain refiner prepared by the embodiment of the invention is obviously superior to that of the traditional Al-Ti-oneThe grain size of the grain refiner B can reach 90 μm, for example, the grain size of the industrial pure aluminum refined in the embodiment 5.
FIG. 2 shows a scanning electron microscope morphology of the microstructure of the Al-Ti-B grain refiner prepared in example 5 of the present invention;
as shown in figure 3, the microstructure of the metallurgical macroscopic crystal grain of the industrial pure aluminum is refined by adding 0.20 weight percent of the traditional Al-5 Ti-1B, wherein the columnar crystal is obviously refined, and the refined crystal grain size is about 150 mu m.
As shown in figure 4, the 0.20 weight percent Al-5 Ti-1B refined industrial pure aluminum metallographic macroscopic grain structure prepared in example 5 is added, wherein compared with figure 3, the grain refining effect is better, the grain size after refining is about 90 μm, and the refining limit of the Al-Ti-B series grain refiner on the aluminum alloy is broken through.
In conclusion, the embodiment of the invention can realize the large-scale continuous preparation of the grain refiner by the ultrasonic treatment of 500-8000 kg/h level through the continuous matching of various parameters and operations, breaks through the defect that the yield is seriously limited when the Al-Ti-B grain refiner is prepared by the traditional ultrasonic treatment process, and the grain size of the cast-state industrial pure aluminum refined by the prepared Al-Ti-B grain refiner is obviously superior to the refining effect of the traditional Al-Ti-B grain refiner.
It should be understood that the above-described embodiments are only some of the embodiments of the present invention, and are provided only for the purpose of better understanding of the embodiments of the present invention, and not all of the embodiments of the present invention. In practical applications, by adjusting the contents of the above components and the combination manner of the components, different and countless embodiments can be obtained, which are all within the scope of the present invention.
While the present invention has been described in detail with reference to the preferred embodiments, it should be understood that the above description should not be taken as limiting the invention. Various modifications and alterations to this invention will become apparent to those skilled in the art upon reading the foregoing description. Accordingly, the scope of the invention should be determined from the following claims.

Claims (6)

1. A method for continuously preparing Al-Ti-B grain refiner by ultrasonic treatment is characterized by comprising the following steps:
s1, weighing potassium fluotitanate K according to the target component of the Al-Ti-B grain refiner to be prepared2TiF6KBF of potassium fluoroborate4Is a reaction of K2TiF6、KBF4Mixing homogeneously to obtain K2TiF6And KBF4Mixing salt;
s2, heating the launder to 750-1200 ℃, preserving heat, and introducing cylindrical ultrasonic probes in Z-shaped distribution at the upper part of the launder in order to ensure that the action range of ultrasonic waves is distributed in the whole near-surface area of the aluminum liquid; the total length of the launder is 2-12 m, the launder section is U-shaped, and the section size is: the lower bottom is 6-12 cm wide, the upper opening is 15-25 cm wide, and the height is 15-25 cm; the number of the ultrasonic probes is 10-50, the distance between every two adjacent probes is 15-30 cm, and the distance between the bottom end surface of each probe and the bottom of the launder is 8-12 cm;
s3, continuously introducing industrial pure aluminum melt with the temperature of 750-1000 ℃ at the upper port of the launder, controlling the height of the aluminum liquid in the launder to be 8-10 cm and the flowing time of the aluminum liquid in the launder to be 3-10 minutes in order to ensure that ultrasonic waves can act on the bottom of the aluminum liquid and promote full reaction of villiaumite and the aluminum liquid; simultaneous continuous injection of K formulated in S12TiF6And KBF4Mixed salt, controlling K according to the target component of Al-Ti-B grain refiner to be prepared and the flow of aluminum liquid2TiF6And KBF4The addition amount of the mixed salt; the ultrasonic frequency is 20 +/-1 kHz, and the power is 500-5000W;
s4, when the pure aluminum and the mixed salt melt flow in the flow groove, starting ultrasonic equipment, and applying continuous ultrasonic treatment on the upper part of the flow groove;
and S5, allowing the ultrasonically treated mixed melt to enter a transfer ladle through the lower port of the runner, allowing reaction slag to flow out of the upper opening of the transfer ladle, allowing the Al-Ti-B melt to flow into a standing holding furnace through the lower opening of the transfer ladle, degassing and deslagging in the standing holding furnace, and casting to obtain the Al-Ti-B grain refiner.
2. The method of claim 1, wherein in the step of S1, the grain refiner of Al-Ti-B comprises Ti in an amount of 1.00-7.00 wt% and B in an amount of 0.50-1.30 wt%.
3. The method for continuously preparing an Al-Ti-B grain refiner using ultrasonic treatment as claimed in claim 1, wherein in S2, the launder is heated to 800-1000 ℃ and is maintained for 8-24 hours.
4. The method for continuously preparing an Al-Ti-B grain refiner using ultrasonic treatment as claimed in claim 1, wherein the temperature of the industrial pure aluminum melt is 800-900 ℃ in S3.
5. The method for continuously preparing an Al-Ti-B grain refiner using ultrasonic treatment as claimed in claim 1, wherein in S3, the aluminum liquid flows through the whole launder for 5-8 minutes.
6. The method for continuously preparing Al-Ti-B grain refiner by ultrasonic treatment as claimed in any one of claims 1 to 5, wherein the method can realize the large-scale continuous preparation of Al-Ti-B grain refiner by ultrasonic treatment at the level of 500-8000 kg/h.
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