CN113106301B - Preparation process of aluminum-titanium-boron-carbon grain refiner and refiner prepared by same - Google Patents
Preparation process of aluminum-titanium-boron-carbon grain refiner and refiner prepared by same Download PDFInfo
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- CN113106301B CN113106301B CN202110275404.1A CN202110275404A CN113106301B CN 113106301 B CN113106301 B CN 113106301B CN 202110275404 A CN202110275404 A CN 202110275404A CN 113106301 B CN113106301 B CN 113106301B
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- 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
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- 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
- C22C1/02—Making non-ferrous alloys by melting
- C22C1/026—Alloys based on aluminium
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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
- C22C1/06—Making non-ferrous alloys with the use of special agents for refining or deoxidising
Abstract
The invention provides a preparation process of an aluminum titanium boron carbon grain refiner and the prepared aluminum titanium boron carbon grain refiner, which comprises the following steps: adding the aluminum ingot into an induction furnace, melting and heating to 800-850 ℃; adjusting an induction furnace to be in a stirring mode, adding the mixture of potassium fluotitanate and potassium fluoborate into the induction furnace, reacting for 15-20 min, adding a carbon agent, and continuing to react for 30 min; cleaning molten salt on the surface of the alloy after the reaction is finished; after molten salt on the surface of the alloy is cleaned, introducing argon into the induction furnace, rapidly heating the alloy to 1200-1300 ℃, preserving the temperature for 15-20 min, reducing the temperature of the alloy to 850-860 ℃, refining and degassing; and cleaning dross on the surface of the alloy, and continuously casting, continuously rolling or continuously casting, continuously rolling and continuously extruding the alloy to form the alloy. Through the technical scheme of the invention, TiAl in the prepared Al-Ti-B-C grain refiner3The shape is short rod shape, and is easy to dissolve in aluminum water.
Description
Technical Field
The invention relates to the technical field of alloys, in particular to a preparation process of an aluminum-titanium-boron-carbon grain refiner and the prepared aluminum-titanium-boron-carbon grain refiner.
Background
Grain refinement is one of the important methods for improving the quality of aluminum and aluminum alloy products, and the existing aluminum alloy grain refiner mainly comprises two types of Al-Ti-B and Al-Ti-C, namely TiB2The easy decline of the ion agglomeration and refining effects is a defect which is difficult to overcome by the Al-Ti-B grain refiner. During the preparation of the Al-Ti-C grain refiner, carbon element and aluminum melt are difficult to wet, alloyed TiC is difficult to form at low temperature, and in order to improve the wettability of carbon and aluminum, the temperature is generally required to be more than 1200 ℃ in the preparation process, so that the Al-Ti-C grain refiner has high energy consumption during the preparation, extremely high requirements on equipment and process, and cannot form industrialized products all the time.
Disclosure of Invention
The present invention is directed to solving at least one of the problems of the prior art or the related art.
Therefore, the invention aims to provide aluminumThe preparation process of the titanium boron carbon grain refiner has the advantages of low cost, low energy consumption, high efficiency and stable quality, and the prepared aluminum titanium boron carbon grain refiner has dispersed particle distribution and greatly reduced TiB2The agglomeration of the aluminum oxide is easy to dissolve in aluminum water when in use, and the refining effect is good.
In order to achieve the above object, a technical solution of a first aspect of the present invention provides a preparation process of an aluminum titanium boron carbon grain refiner, comprising the following steps:
adding the aluminum ingot into an induction furnace, melting and heating to 800-850 ℃;
adjusting the induction furnace to be in a stirring mode, adding the mixture of potassium fluotitanate and potassium fluoborate into the induction furnace, reacting for 15-20 min, adding a carbon agent, and continuing to react for 30 min;
pouring out the molten salt on the surface of the alloy after the reaction is finished, and adding calcium fluoride to clean the residual molten salt on the surface of the alloy;
after molten salt on the surface of the alloy is cleaned, introducing argon into the induction furnace, rapidly heating the alloy to 1200-1300 ℃, preserving the temperature for 15-20 min, reducing the temperature of the alloy to 850-860 ℃, refining and degassing;
and (4) cleaning dross on the surface of the alloy after refining and degassing, and continuously casting and rolling the alloy into a certain shape to prepare the aluminum-titanium-boron-carbon grain refiner.
Preferably, the carbon agent is prepared by pressing aluminum powder with the granularity of 50 meshes and carbon powder with the granularity of 300 meshes and the purity of more than 99.9 percent according to the mass ratio of 3: 2; the carbon agent is in a round cake shape with the diameter of 90mm-100mm and the thickness of 5mm-7 mm.
Preferably, the purity of the aluminum ingot is more than 99.7%, the purity of the potassium fluotitanate is more than 98%, the purity of the potassium fluoborate is more than 98%, and the preparation process comprises the following raw materials in parts by mass: 1000 parts of aluminum ingot, 208 parts of potassium fluotitanate 154-208 parts, 12-36 parts of potassium fluoborate, 2.5-7.5 parts of carbon agent and 3.0 parts of calcium fluoride.
Preferably, the stirring power in the stirring mode is 160KW to 200 KW.
Preferably, the specific steps of refining degassing include: after the alloy temperature is reduced to 850-860 ℃, a rotary degasser is used for introducing argon to carry out refining degassing for 10-15 min.
Preferably, the alloy is continuously cast and rolled into wire rods with a diameter of 9.5 mm.
The technical scheme of the second aspect of the invention provides an aluminum-titanium-boron-carbon grain refiner prepared by the preparation process of the aluminum-titanium-boron-carbon grain refiner provided by any one of the technical schemes, which comprises the following components in percentage by mass: 3.0-5.0% of titanium, 0.1-0.3% of boron, 0.1-0.3% of carbon and less than 0.02% of V, wherein the mass ratio of boron to carbon in the alloy is 1: 1.
Preferably, TiAl in the AlTiOB grain refiner3The appearance is short rod-shaped.
The preparation process of the aluminum titanium boron carbon grain refiner and the prepared aluminum titanium boron carbon grain refiner have the following beneficial technical effects:
(1) the aluminum-titanium-boron-carbon alloy grain refiner is directly produced by adding the potassium fluotitanate and potassium fluoborate mixture and the carbon agent into aluminum water by using an induction furnace, and has the advantages of low cost, low energy consumption, high efficiency and stable quality.
(2) TiAl in the Al-Ti-B-C grain refiner prepared by the preparation process of the Al-Ti-B-C grain refiner3The shape is short rod shape, the aluminum-titanium-boron-carbon grain refiner is very easy to melt in aluminum water when in use, a large amount of Ti-B-C composite ions are formed in the aluminum-titanium-boron-carbon grain refiner, the particles are distributed and dispersed, the size is less than 2um, and TiB is greatly reduced2And (3) agglomeration.
(3) The preparation process of the Al-Ti-B-C grain refiner adopts the addition of the carbon agent for reaction, thoroughly solves the problem of poor wettability of carbon powder and aluminum water during the preparation of the Al-Ti-C grain refiner in the prior art, and simultaneously solves the problem that Al is easily formed during the preparation of the Al-Ti-C grain refiner in the prior art4C3And (5) problems are solved. The invention provides a preparation process for producing the aluminum-titanium-boron-carbon grain refiner alloy by an in-situ generation method with low cost, low energy consumption, high efficiency and stable quality, the reliability is strong, and the prepared aluminum-titanium-boron-carbon grain refiner has excellent performance.
Additional aspects and advantages of the invention will be set forth in part in the description which follows and, in part, will be obvious from the description, or may be learned by practice of the invention.
Drawings
The above and/or additional aspects and advantages of the present invention will become apparent and readily appreciated from the following description of the embodiments, taken in conjunction with the accompanying drawings of which:
FIG. 1 shows Al-Ti produced by a process for preparing an AlTiB carbon grain refiner according to an embodiment of the invention3-B0.1-C0.1Grain refiner gold phase diagram;
FIG. 2 illustrates Al-Ti produced by a process for preparing an AlTiB carbon grain refiner according to an embodiment of the invention4-B0.15-C0.15Grain refiner gold phase diagram;
FIG. 3 illustrates Al-Ti produced by a process for preparing an AlTiB carbon grain refiner according to an embodiment of the invention5-B0.2-C0.2Grain refiner gold phase diagram;
FIG. 4 shows Al-Ti produced by the process for preparing the AlTiB carbon grain refiner according to one embodiment of the invention5-B0.3-C0.3Grain refiner gold phase diagram.
Detailed Description
The invention discloses a preparation process of an aluminum titanium boron carbon grain refiner and the prepared aluminum titanium boron carbon grain refiner, and the technical personnel in the field can use the content for reference and appropriately improve the process parameters for realization. It is expressly intended that all such similar substitutes and modifications which would be obvious to one skilled in the art are deemed to be included in the invention. While the methods and applications of this invention have been described in terms of preferred embodiments, it will be apparent to those of ordinary skill in the art that variations and modifications in the methods and applications described herein, as well as other suitable variations and combinations, may be made to implement and use the techniques of this invention without departing from the spirit and scope of the invention.
The invention is further illustrated by the following examples:
example 1
Adding 1000Kg of 99.7% aluminum ingot into an induction furnace, melting and heating to 800 ℃, converting the electric furnace into a stirring mode, stirring with 160KW, uniformly mixing 154Kg of potassium fluotitanate and 12Kg of potassium fluoborate, adding the mixture into the induction furnace by using an automatic feeder, and reacting for 15 minutes. Adding 2.5Kg of carbon agent into the furnace by using a bell jar, continuously reacting for 30 minutes, pouring out the molten salt on the surface of the alloy after the reaction is finished, and adding 3.0 Kg of calcium fluoride to clean the residual fluorine salt on the surface of the alloy after the pouring is finished; and after cleaning, introducing argon, quickly heating the alloy to 1200 ℃, keeping the temperature for 15 minutes, then cooling the alloy to 850 ℃, introducing argon by using a rotary degasser to carry out refining degassing for 10 minutes, cleaning dross on the surface of the alloy after refining degassing, and then continuously casting and rolling the alloy into a wire rod with the diameter of 9.5 mm.
Preparing to obtain Al-Ti3-B0.1-C0.1Grain refiner, titanium content 3%, boron content 0.1%, carbon content 0.1% in the alloy, through metallographic examination, as shown in figure 1, TiAl3The shape is short rod-shaped, a large amount of Ti-B-C composite ions are formed in the alloy, the particles are distributed and dispersed, the size is less than 2um, and no TiB exists2And (3) agglomeration. The Al-Ti3-B0.1-C0.1The grain refiner is easy to dissolve in aluminum water when in use, and has good refining effect.
Example 2
Adding 1000Kg of 99.7% aluminum ingot into an induction furnace, melting and heating to 820 ℃, converting the electric furnace into a stirring mode, stirring with 170KW, uniformly mixing 207Kg of potassium fluotitanate and 18Kg of potassium fluoborate, adding the mixture into the induction furnace by using an automatic feeder, and reacting for 20 minutes. Adding 3.75Kg of carbon agent into the furnace by using a bell jar, continuously reacting for 30 minutes, pouring out the molten salt on the surface of the alloy after the reaction is finished, and adding 3.0 Kg of calcium fluoride to clean the residual fluorine salt on the surface of the alloy after the pouring is finished; after cleaning, argon is introduced, the alloy is rapidly heated to 1250 ℃, after heat preservation is carried out for 17 minutes, the alloy is cooled to 850 ℃, a rotary degasser is used for introducing argon to carry out refining degassing for 12 minutes, after refining degassing, dross on the surface of the alloy is cleaned, and then the alloy is continuously cast and rolled into a wire rod with the diameter of 9.5 mm.
Preparing Al-Ti4-B0.15-C0.15The grain refiner contains 4% of titanium, 0.15% of boron and 0.15% of carbon. TiAl is shown in figure 2 by metallographic examination3The shape is short rod-shaped, a large amount of Ti-B-C composite ions are formed in the alloy, the particles are distributed and dispersed, the size is less than 2um, and no TiB exists2And (3) agglomeration. The Al-Ti4-B0.15-C0.15The grain refiner is easy to dissolve in aluminum water when in use, and has good refining effect.
Example 3
Adding 1000Kg of 99.7 percent aluminum ingot into an induction furnace, melting and heating to 830 ℃, converting the electric furnace into a stirring mode, stirring with 180KW of power, uniformly mixing 258Kg of potassium fluotitanate and 24Kg of potassium fluoborate, adding the mixture into the induction furnace by using an automatic feeder, and reacting for 18 minutes. Adding 5Kg of carbon agent into the furnace by using a bell jar, continuously reacting for 30 minutes, pouring out the molten salt on the surface of the alloy after the reaction is finished, and adding 3.0 Kg of calcium fluoride to clean the residual fluorine salt on the surface of the alloy after the pouring is finished; after cleaning, argon is introduced, the temperature of the alloy is rapidly raised to 1280 ℃, the alloy is cooled to 850 ℃ after heat preservation is carried out for 20 minutes, a rotary degasser is used for introducing argon to carry out refining degassing for 14 minutes, after refining degassing, dross on the surface of the alloy is cleaned, and then the alloy is continuously cast and rolled into a wire rod with the diameter of 9.5 mm.
Preparing Al-Ti5-B0.2-C0.2A grain refiner, wherein the content of titanium is 5%, the content of boron is 0.2%, and the content of carbon is 0.2%. TiAl is shown in figure 3 by metallographic examination3The shape is short rod-shaped, a large amount of Ti-B-C composite ions are formed in the alloy, the particles are distributed and dispersed, the size is less than 2um, and no TiB exists2And (3) agglomeration. The Al-Ti5-B0.2-C0.2The grain refiner is easy to dissolve in aluminum water when in use, and has good refining effect.
Example 4
Adding 1000Kg of 99.7 percent aluminum ingot into an induction furnace, melting and heating to 850 ℃, converting the electric furnace into a stirring mode, stirring with the power of 200KW, uniformly mixing 258Kg of potassium fluotitanate and 36Kg of potassium fluoborate, adding the mixture into the induction furnace by using an automatic feeder, and reacting for 20 minutes. Adding 7.5Kg of carbon agent into the furnace by using a bell jar, continuously reacting for 30 minutes, pouring out the molten salt on the surface of the alloy after the reaction is finished, and adding 3.0 Kg of calcium fluoride to clean the residual fluorine salt on the surface of the alloy after the pouring is finished; after cleaning, argon is introduced, the alloy is rapidly heated to 1300 ℃, after heat preservation is carried out for 20 minutes, the alloy is cooled to 860 ℃, a rotary degasser is used for introducing argon to carry out refining degassing for 15 minutes, after refining degassing, dross on the surface of the alloy is cleaned, and then the alloy is continuously cast and rolled into a wire rod with the diameter of 9.5 mm.
Preparing Al-Ti5-B0.3-C0.3A grain refiner, wherein the content of titanium is 5%, the content of boron is 0.3%, and the content of carbon is 0.3%. TiAl is shown in figure 4 by metallographic examination3The shape is short rod-shaped, a large amount of Ti-B-C composite ions are formed in the alloy, the particles are distributed and dispersed, the size is less than 2um, and no TiB exists2And (3) agglomeration. The Al-Ti5-B0.3-C0.3The grain refiner is easy to dissolve in aluminum water when in use, and has good refining effect.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (7)
1. A preparation process of an aluminum titanium boron carbon grain refiner is characterized by comprising the following steps:
adding the aluminum ingot into an induction furnace, melting and heating to 800-850 ℃;
adjusting the induction furnace to be in a stirring mode, adding the mixture of potassium fluotitanate and potassium fluoborate into the induction furnace, reacting for 15-20 min, adding a carbon agent, and continuing to react for 30 min;
pouring out the molten salt on the surface of the alloy after the reaction is finished, and adding calcium fluoride to clean the residual molten salt on the surface of the alloy;
after molten salt on the surface of the alloy is cleaned, introducing argon into the induction furnace, rapidly heating the alloy to 1200-1300 ℃, preserving the temperature for 15-20 min, reducing the temperature of the alloy to 850-860 ℃, refining and degassing;
after refining and degassing, cleaning dross on the surface of the alloy, continuously casting, continuously rolling and continuously extruding the alloy into a certain shape to prepare the aluminum-titanium-boron-carbon grain refiner,
the aluminum titanium boron carbon grain refiner comprises the following components in percentage by mass: 3.0 to 5.0 percent of titanium, 0.1 to 0.3 percent of boron, 0.1 to 0.3 percent of carbon, less than 0.02 percent of V, and the mass ratio of boron to carbon in the alloy is 1:1,
TiAl in the Al-Ti-B-C grain refiner3The appearance is short rod-shaped.
2. The process for preparing an Al-Ti-B-C grain refiner according to claim 1,
the carbon agent is formed by pressing aluminum powder with the granularity of 50 meshes and carbon powder with the granularity of 300 meshes and the purity of more than 99.9 percent according to the mass ratio of 3: 2;
the carbon agent is in a round cake shape with the diameter of 90mm-100mm and the thickness of 5mm-7 mm.
3. The process for preparing an Al-Ti-B-C grain refiner according to claim 2,
the purity of the aluminum ingot is more than 99.7 percent, the purity of the potassium fluotitanate is more than 98 percent, the purity of the potassium fluoborate is more than 98 percent,
the preparation process comprises the following raw materials in parts by mass:
1000 parts of aluminum ingot, 208 parts of potassium fluotitanate 154-208 parts, 12-36 parts of potassium fluoborate, 2.5-7.5 parts of carbon agent and 3.0 parts of calcium fluoride.
4. The process for preparing an Al-Ti-B-C grain refiner according to claim 1,
the stirring power in the stirring mode is 160kW-200 kW.
5. The process for preparing an Al-Ti-B-C grain refiner as defined in claim 1, wherein the refining degassing comprises:
after the alloy temperature is reduced to 850-860 ℃, a rotary degasser is used for introducing argon to carry out refining degassing for 10-15 min.
6. The process for preparing an Al-Ti-B-C grain refiner according to claim 1,
the alloy is continuously cast and rolled into a wire rod with the diameter of 9.5 mm.
7. An Al-Ti-B-C grain refiner prepared by the preparation process of the Al-Ti-B-C grain refiner according to any one of claims 1 to 6, which is characterized by comprising the following components in percentage by mass:
3.0 to 5.0 percent of titanium, 0.1 to 0.3 percent of boron, 0.1 to 0.3 percent of carbon, less than 0.02 percent of V, and the mass ratio of boron to carbon in the alloy is 1:1,
TiAl in the Al-Ti-B-C grain refiner3The appearance is short rod-shaped.
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Citations (4)
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|---|---|---|---|---|
| CN1046945A (en) * | 1990-04-18 | 1990-11-14 | 沈阳工业大学 | Quaternary grain refiner and manufacture method thereof |
| CN1088996A (en) * | 1993-11-18 | 1994-07-06 | 沈阳工业大学 | A kind of novel master alloy fining agent |
| CN106987735A (en) * | 2016-09-29 | 2017-07-28 | 山东滨州华创金属有限公司 | A kind of preparation technology of aluminium intermediate alloy |
| CN109355520A (en) * | 2018-11-27 | 2019-02-19 | 中国科学院金属研究所 | A kind of Al-Ti-C-B intermediate alloy and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| JPS54114411A (en) * | 1978-02-28 | 1979-09-06 | Nippon Keikinzoku Sougou Kenki | Production of aluminiumm titaniummboron alloy for finely dividing crystal |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1046945A (en) * | 1990-04-18 | 1990-11-14 | 沈阳工业大学 | Quaternary grain refiner and manufacture method thereof |
| CN1088996A (en) * | 1993-11-18 | 1994-07-06 | 沈阳工业大学 | A kind of novel master alloy fining agent |
| CN106987735A (en) * | 2016-09-29 | 2017-07-28 | 山东滨州华创金属有限公司 | A kind of preparation technology of aluminium intermediate alloy |
| CN109355520A (en) * | 2018-11-27 | 2019-02-19 | 中国科学院金属研究所 | A kind of Al-Ti-C-B intermediate alloy and preparation method thereof |
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