CN106756149B - A kind of aluminium titanium boron carbon zirconium rare earth fining agent, its preparation method and its application - Google Patents

A kind of aluminium titanium boron carbon zirconium rare earth fining agent, its preparation method and its application Download PDF

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CN106756149B
CN106756149B CN201611141124.7A CN201611141124A CN106756149B CN 106756149 B CN106756149 B CN 106756149B CN 201611141124 A CN201611141124 A CN 201611141124A CN 106756149 B CN106756149 B CN 106756149B
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aluminium
rare earth
fining agent
impurity
potassium
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CN106756149A (en
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徐正祥
葛庆琪
葛红星
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Nanjing Yunhai Aluminum Industry Co.,Ltd.
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Nanjing Yunkai Alloys Co Ltd
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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
    • C22C1/03—Making non-ferrous alloys by melting using master alloys
    • 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

Abstract

The invention discloses a kind of aluminium titanium boron carbon zirconium rare earth fining agent, its preparation method and its applications.Aluminium titanium boron carbon zirconium rare earth fining agent, it is composed of the following components：Titanium 3 5%, boron 0.3 0.5%, carbon 0.08 0.15%, zirconium 0.08 0.22%, rare earth 0.8 1.2%, impurity F e≤0.10%, impurity V≤0.03%, impurity Si≤0.08%, the aluminium of other impurity summation≤0.15% and surplus, other single impurity contents are respectively less than 0.03%, and the percentage is mass percent.The present invention is by the reasonable addition of zr element and prepares the control of condition, effectively reduces the column of TiAl3 and spicule, reduces TiB2 aggregations, reduces and lead to the problem of harmful Al4C3 phases, reduce TiAl3 phases granular size, be distributed and reduce alloy inside air content；The gained fining agent refinement time is fast (10s), refinement duration length (being more than 12h).

Description

A kind of aluminium titanium boron carbon zirconium rare earth fining agent, its preparation method and its application
Technical field
The present invention relates to a kind of aluminium titanium boron carbon zirconium rare earth fining agent, its preparation method and its applications, belong to alloy field.
Background technology
With the development of society, market proposes higher requirement to the metallurgy, composition and performance of Al-alloy products, Aluminium processing industry needs to produce the Al-alloy products of qualified metallurgical quality, uniform ingredients and function admirable.
Conventionally produced aluminium intermediate alloy grain refiner kind has：Aluminium titanium boron, aluminium titanium carbon, aluminium titanium boron carbon rare earth etc.. At present, the preparation of aluminium intermediate alloy grain refiner be susceptible to TiB2 particles it is bigger than normal reunite, TiAl3 it is coarse be unevenly distributed, The problems such as time is long, the timeliness time is short, alloy inner clamps sundries is on the high side is refined, causes the later stage that cannot fully meet to internal group It knits and the crystal grain refinement of high aluminium and aluminium alloy is required to require.
The content of the invention
During in order to solve uneven aluminium intermediate alloy grain refiner structure in the prior art, refinement time length, timeliness Between it is short, alloy inner clamps sundries is on the high side the defects of, the present invention provide a kind of aluminium titanium boron carbon zirconium rare earth fining agent, its preparation method and It is applied.
In order to solve the above technical problems, the technical solution adopted in the present invention is as follows：
A kind of aluminium titanium boron carbon zirconium rare earth fining agent, it is composed of the following components：Titanium 3-5%, boron 0.3-0.5%, carbon 0.08- 0.15%th, zirconium 0.08-0.22%, rare earth 0.8-1.2%, impurity F e≤0.10%, impurity V≤0.03%, impurity Si≤ 0.08%th, other impurity summation≤0.15% and the aluminium of surplus, other single impurity contents are respectively less than 0.03%, described hundred Divide than being mass percent.
The fining agent refinement time of the present invention is fast (10s), and it is comprehensive to enhance alloy for refinement duration length (being more than 12h) Energy (intensity, fracture toughness etc.) and grain refining efficiency, suitable for the various refinement feed postitions such as refinement in online refinement and stove.
In current aluminium intermediate alloy grain refiner, there are no the hexa-atomic alloy refinement agent of aluminium base, applicant's warps Research is found：Zirconium is preferable getter, it can consumingly absorbed nitrogen, hydrogen, carrier of oxygen, more effectively control containing inside alloy Tolerance, and zirconium has an impact the recrystallization of aluminium, and zr element has significant stabilization to the Deformation structure of alloy, can be effectively It reduces TiAl3 particles, the column of Ti2Al20RE particles and spicule, TiB2 aggregations and leads to the problem of harmful Al4C3 phases, Simultaneously applicant further found that Trace Zr adds in, have clear improvement to the corrosion resistance of alloy.
The raw material of above-mentioned aluminium titanium boron carbon zirconium rare earth fining agent includes：Mass ratio is 1000：(200-320)：(40-50)： (0.8-6)：(3-20)：Aluminium ingot, potassium fluotitanate, potassium fluoborate, graphite carburant, potassium fluorozirconate and the mischmetal of (8-12), Wherein, the purity of aluminium ingot is not less than 99.7%, and carbon content is 65-99% in graphite carburant.
In order to further improve the uniformity of product, while shorten the refinement time, extend refinement timeliness, titanium in potassium fluotitanate Content >=19.2%, Boron contents are 8.0-8.7% in potassium fluoborate.
Above-mentioned preparation method used tool can be automatic stirring main frequency furnace and batch mixer.
In the application rpm be rpm the meaning.
In order to be further reduced impurity, uniformity is improved, shortens the refinement time, extend refinement timeliness, above-mentioned aluminium titanium boron carbon The preparation method of zirconium rare earth fining agent, including following steps connected in order：
1) time is mixed with the speed of 50 ± 5rpm in potassium fluotitanate, potassium fluoborate, potassium fluorozirconate, graphite carburant 10-20min；
2) aluminium ingot is melted；
3) after aluminium ingot is completely melt, under conditions of temperature is 750-850 DEG C, the material obtained by step 1) is added in into aluminium It is reacted in liquid, reaction time 20-30min；
4) slag after reaction, is scooped；
5) solvent for adding in quality of ingot aluminum 2% is stirred degassing refining, and solvent is blown into argon gas in aluminium alloy and is carried out Refining degassing, refining time are 20-25 minutes, argon pressure 0.1-0.3Mpa, mixing speed 300-400rpm, stirring temperature 800-850 DEG C of degree；
6) slag hitting, fishing slag being carried out with Fluorspar Powder after stirring degassing refining, cleaning is completed, and cooling stands 10-20min, Cool the temperature to 720-750 DEG C；
7) rare earth will be added in step 6) resulting material, rare earth is added in bell jar, and adition process middle bell jar is in aluminium alloy It is moved with the speed of 10 ± 2cm/min, until rare earth is all dissolved into aluminium alloy；
8) aluminium alloy obtained by step 7) is warming up to 800 ± 20 DEG C, is then imported by chute equipped with 30-40pp i oxygen In the filter box for changing aluminium ceramic filter, on-line filtration processing is carried out to aluminium alloy, the aluminium alloy after filtering connects by continuous casting Milling train is rolled into aluminium titanium boron carbon zirconium rare earth fining agent.
In order to further improve the uniformity of product, impurity content is reduced, solvent for use is potassium chloride, nitric acid in step 5) Magnesium, sodium chloride and calcium nitrate mass ratio are (5-15)：(10-15)：(1-3)：The mixture of (0.2-0.3).
This technological process simple possible, impurity content is extremely low, effectively prevents iron loss, so as to ensure in alloy Portion's cleannes reduce oxidation impurities.
The present invention is more significant compared with other fining agents by the reasonable addition of Zr elements and the control of preparation condition Ground reduces the column of TiAl3 and spicule, reduces TiB2 aggregations, reduce the harmful Al4C3 phases of generation, reduce TiAl3 phases granular size is distributed and reduces air content inside alloy.
The application of above-mentioned aluminium titanium boron carbon zirconium rare earth fining agent is aluminium 0.5-0.8kg per ton.
The unmentioned technology of the present invention is with reference to the prior art.
The present invention is by the reasonable addition of zr element and prepares the control of condition, compared with other fining agents relatively efficiently Reduce the column of TiAl3 and spicule, reduce TiB2 aggregations, reduce the harmful Al4C3 phases of generation, reduce TiAl3 Phase granular size, the problem of being distributed and reducing air content inside alloy；Gained aluminium titanium boron carbon zirconium rare earth fining agent of the invention is thin It is fast (10s) to change the time, refinement duration length (being more than 12h), enhances alloy comprehensive performance (intensity, fracture toughness etc.) and thin Change ability, suitable for the various refinement feed postitions such as refinement in online refinement and stove；It is detected by metallographic, arbitrary 1cm2Vertical cut TiAl in face3、Ti2Al20RE is substantially evenly distributed disperse, average-size<20 μm, single particle full-size<120 μm, Al3Zr ≤ 20 μm are substantially evenly distributed, and TiB2, TiC are distributed generally uniform disperse, average-size≤2 μm, Al2O3And salt attachment Length summation<800 μm, while hydrogen content can be controlled in 0.2-0.3ml/100gAl, better meets later stage aluminium and aluminium alloy is thin The requirement of change.
Description of the drawings
Fig. 1 is the schematic diagram before fine aluminium refinement in embodiment 1；
Fig. 2 is the schematic diagram of (20s) after fine aluminium refinement in embodiment 1.
Specific embodiment
For a better understanding of the present invention, with reference to the embodiment content that the present invention is furture elucidated, but the present invention Content is not limited solely to the following examples.
Embodiment 1
The manufacturing method of aluminium titanium boron carbon zirconium rare earth grain refiner (Al-Ti5-B0.2-C0.1-Zr0.1-Re1) includes suitable The following steps that sequence connects：
1) time is mixed with the speed of 50rpm in potassium fluotitanate, potassium fluoborate, potassium fluorozirconate, graphite carburant 15min；
2) aluminium ingot is melted；
3) after aluminium ingot is completely melt, under conditions of temperature is 800 DEG C, the material obtained by step 1) is added in molten aluminum It is reacted, reaction time 25min；
4) slag after reaction, is scooped；
5) solvent for adding in quality of ingot aluminum 2% is stirred degassing refining, and solvent is blown into argon gas in aluminium alloy and is carried out Refining degassing, refining time are 22 minutes, argon pressure 0.2Mpa, mixing speed 350rpm, and 820 DEG C of whipping temp is molten Agent is that potassium chloride, magnesium nitrate, sodium chloride and calcium nitrate mass ratio are 8：12：2：0.3 mixture；
6) slag hitting, fishing slag are carried out with Fluorspar Powder after stirring degassing refining, cleaning is completed, and cooling stands 15min, by temperature Degree is down to 740 DEG C；
7) mischmetal will be added in step 6) resulting material, rare earth is added in bell jar, and adition process middle bell jar is in alloy It is moved in liquid with the speed of 10cm/min, until rare earth is all dissolved into aluminium alloy；
8) aluminium alloy obtained by step 7) is warming up to 800 DEG C, is then imported by chute and made pottery equipped with 35pp i aluminium oxide In the filter box of porcelain filter, on-line filtration processing is carried out to aluminium alloy, the aluminium alloy after filtering is rolled by continuous casting and continuous rolling mill Aluminium titanium boron carbon zirconium rare earth fining agent is made.
It is raw materials used to be：1000kg99.7% aluminium ingots, 230kg potassium fluotitanates (Ti >=20%), 45kg potassium fluoborates (B： 8.5%), 8kg potassium fluorozirconates (Zr：31%), 2.5kg graphite carburant (three energy carbon Co., Ltd of Linzhang County, phosphorus content 99%), 10kg mischmetals (Zhengzhou Zhi Yi chemical products Co., Ltd, content of rare earth >=99%).
Products obtained therefrom is detected by microscope high power：Arbitrary 1cm2Longitudinal section in TiAl3、Ti2Al20RE is substantially distributed Even disperse, average-size<20 μm, single particle full-size<120 μm, Al3Zr≤20 μm are substantially evenly distributed, TiB2, TiC It is distributed generally uniform disperse, average-size≤2 μm, Al2O3And the length summation of salt attachment<800μm；It is examined by hydrogen meter It surveys：Hydrogen content is controlled in 0.2ml/100gAl.
The said goods refine fine aluminium (20000 μm), addition is fine aluminium 0.5kg per ton, and 5s is just refined, 12 it is small when refinement start to disappear, after 10s, more than 99% crystal grain reaches 1 grade (180 μm).
Embodiment 2
The manufacturing method of aluminium titanium boron carbon zirconium rare earth grain refiner includes following steps connected in order：
1) time is mixed with the speed of 55rpm in potassium fluotitanate, potassium fluoborate, potassium fluorozirconate, graphite carburant 20min；
2) aluminium ingot is melted；
3) after aluminium ingot is completely melt, under conditions of temperature is 850 DEG C, the material obtained by step 1) is added in molten aluminum It is reacted, reaction time 30min；
4) slag after reaction, is scooped；
5) solvent for adding in quality of ingot aluminum 2% is stirred degassing refining, and solvent is blown into argon gas in aluminium alloy and is carried out Refining degassing, refining time are 25 minutes, argon pressure 0.3Mpa, mixing speed 400rpm, and 850 DEG C of whipping temp is molten Agent is that potassium chloride, magnesium nitrate, sodium chloride and calcium nitrate mass ratio are 15：15：3：0.3 mixture；
6) slag hitting, fishing slag being carried out with Fluorspar Powder after stirring degassing refining, cleaning is completed, and cooling stands 10-20min, Cool the temperature to 750 DEG C；
7) rare earth will be added in step 6) resulting material, rare earth is added in bell jar, and adition process middle bell jar is in aluminium alloy It is moved with the speed of 10cm/min, until rare earth is all dissolved into aluminium alloy；
8) aluminium alloy obtained by step 7) is warming up to 800 DEG C, is then imported by chute and made pottery equipped with 40pp i aluminium oxide In the filter box of porcelain filter, on-line filtration processing is carried out to aluminium alloy, the aluminium alloy after filtering is rolled by continuous casting and continuous rolling mill Aluminium titanium boron carbon zirconium rare earth fining agent is made.
It is raw materials used to be：1000kg99.7% aluminium ingots, 260kg potassium fluotitanates (Ti >=20%), 50kg potassium fluoborates (B： 8.5%), 10kg potassium fluorozirconates (Zr：31%), 2kg graphite carburant (three energy carbon Co., Ltd of Linzhang County, phosphorus content 99%), 12kg mischmetals (Zhengzhou Zhi Yi chemical products Co., Ltd, content of rare earth >=99%)
Products obtained therefrom is detected by microscope high power：Arbitrary 1cm2Longitudinal section in TiAl3、Ti2Al20RE is substantially distributed Even disperse, average-size<20 μm, single particle full-size<120 μm, Al3Zr≤20 μm are substantially evenly distributed, TiB2, TiC It is distributed generally uniform disperse, average-size≤2 μm, Al2O3And the length summation of salt attachment<800μm；It is examined by hydrogen meter It surveys：Hydrogen content is controlled in 0.2ml/100gAl.
The said goods refine fine aluminium (20000 μm), addition is fine aluminium 0.5kg per ton, and 10s just occurs carefully Change, 12 it is small when refinement start to disappear, after 20s, more than 99% crystal grain reaches 1 grade (180 μm).
Embodiment 3
The manufacturing method of aluminium titanium boron carbon zirconium rare earth grain refiner includes following steps connected in order：
1) time is mixed with the speed of 50rpm in potassium fluotitanate, potassium fluoborate, potassium fluorozirconate, graphite carburant 10min；
2) aluminium ingot is melted；
3) after aluminium ingot is completely melt, under conditions of temperature is 750 DEG C, the material obtained by step 1) is added in molten aluminum It is reacted, reaction time 20min；
4) slag after reaction, is scooped；
5) solvent for adding in quality of ingot aluminum 2% is stirred degassing refining, and solvent is blown into argon gas in aluminium alloy and is carried out Refining degassing, refining time are 20 minutes, argon pressure 0.1Mpa, mixing speed 300rpm, and 800 DEG C of whipping temp is molten Agent is that potassium chloride, magnesium nitrate, sodium chloride and calcium nitrate mass ratio are 5：10：1：0.2 mixture；
6) slag hitting, fishing slag are carried out with Fluorspar Powder after stirring degassing refining, cleaning is completed, and cooling stands 10min, by temperature Degree is down to 720 DEG C；
7) rare earth will be added in step 6) resulting material, rare earth is added in bell jar, and adition process middle bell jar is in aluminium alloy It is moved with the speed of 10cm/min, until rare earth is all dissolved into aluminium alloy；
8) aluminium alloy obtained by step 7) is warming up to 800 DEG C, is then imported by chute equipped with 30ppi aluminium oxide ceramics In the filter box of filter, on-line filtration processing is carried out to aluminium alloy, the aluminium alloy after filtering is by continuous casting and continuous rolling mill, rolling Into aluminium titanium boron carbon zirconium rare earth fining agent.
It is raw materials used to be：1000kg99.7% aluminium ingots, 250kg potassium fluotitanates (Ti >=20%), 48kg potassium fluoborates (B： 8.5%), 6kg potassium fluorozirconates (Zr：31%), 1.2kg graphite carburant potassium, 10kg potassium fluorozirconates, 2kg graphite carburants (Linzhang County three can carbon Co., Ltd, phosphorus content 99%), 11kg mischmetals (Zhengzhou Zhi Yi chemical products Co., Ltd, content of rare earth >=99%)；
Products obtained therefrom is detected by microscope high power：Arbitrary 1cm2Longitudinal section in TiAl3、Ti2Al20RE is substantially distributed Even disperse, average-size<20 μm, single particle full-size<120 μm, Al3Zr≤20 μm are substantially evenly distributed, TiB2, TiC It is distributed generally uniform disperse, average-size≤2 μm, Al2O3And the length summation of salt attachment<800μm；It is examined by hydrogen meter It surveys：Hydrogen content is controlled in 0.2ml/100gAl.
The said goods refine fine aluminium (20000 μm), addition is fine aluminium 0.5kg per ton, and 5s is just refined, 12 it is small when refinement start to disappear, after 10s, more than 99% crystal grain reaches 1 grade (180 μm).

Claims (5)

1. a kind of preparation method of aluminium titanium boron carbon zirconium rare earth fining agent, it is characterised in that：Aluminium titanium boron carbon zirconium rare earth fining agent by with The following group is grouped into：Titanium 3-5%, boron 0.3-0.5%, carbon 0.08-0.15%, zirconium 0.08-0.22%, rare earth 0.8-1.2%, impurity Fe≤0.10%, impurity V≤0.03%, impurity Si≤0.08%, the aluminium of other impurity summation≤0.15% and surplus, Qi Tadan A impurity content is respectively less than 0.03%, and the percentage is mass percent；
The preparation method of above-mentioned aluminium titanium boron carbon zirconium rare earth fining agent, raw material include：Mass ratio is 1000：(200-320)：(40- 50)：(0.8-6)：(3-20)：The aluminium ingot of (8-12), potassium fluotitanate, potassium fluoborate, graphite carburant, potassium fluorozirconate and mixing are dilute Soil, wherein, the purity of aluminium ingot is not less than 99.7%, and carbon content is 65-99% in graphite carburant.
2. preparation method as described in claim 1, it is characterised in that：Ti content >=19.2% in potassium fluotitanate, potassium fluoborate Middle Boron contents are 8.0-8.7%.
3. preparation method as claimed in claim 1 or 2, it is characterised in that：Including following steps connected in order：
1) time 10- is mixed with the speed of 50 ± 5rpm in potassium fluotitanate, potassium fluoborate, potassium fluorozirconate, graphite carburant 20min；
2) aluminium ingot is melted；
3) after aluminium ingot is completely melt, under conditions of temperature is 750-850 DEG C, the material obtained by step 1) is added in molten aluminum It is reacted, reaction time 20-30min；
4) slag after reaction, is scooped；
5) solvent for adding in quality of ingot aluminum 2% is stirred degassing refining：Solvent is blown into argon gas in aluminium alloy and is refined Degassing, refining time are 20-25 minutes, argon pressure 0.1-0.3MPa, mixing speed 300-400rpm, whipping temp 800-850℃；
6) slag hitting, fishing slag are carried out with Fluorspar Powder after stirring degassing refining, cleaning is completed, and cooling stands 10-20min, by temperature Degree is down to 720-750 DEG C；
7) rare earth will be added in step 6) resulting material, rare earth is added in bell jar, and adition process middle bell jar is in aluminium alloy with 10 The speed movement of ± 2cm/min, until rare earth is all dissolved into aluminium alloy；
8) aluminium alloy obtained by step 7) is warming up to 800 ± 20 DEG C, is then imported by chute equipped with 30-40ppi aluminium oxide In the filter box of ceramic filter, on-line filtration processing is carried out to aluminium alloy, the aluminium alloy after filtering passes through continuous casting and continuous rolling mill, It is rolled into aluminium titanium boron carbon zirconium rare earth fining agent.
4. preparation method as claimed in claim 1 or 2, it is characterised in that：Solvent for use is potassium chloride, nitric acid in step 5) Magnesium, sodium chloride and calcium nitrate mass ratio are (5-15)：(10-15)：(1-3)：The mixture of (0.2-0.3).
5. the aluminium titanium boron carbon prepared by the preparation method of the aluminium titanium boron carbon zirconium rare earth fining agent described in claim 1-4 any one The application of zirconium rare earth fining agent, it is characterised in that：For aluminium 0.5-0.8kg per ton.
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CN108130444A (en) * 2017-11-21 2018-06-08 包头稀土研究院 The preparation method of Al-Ti-B-RE Grain Refiner
CN108130443A (en) * 2017-11-21 2018-06-08 包头稀土研究院 Rare earth Al-Ti-B alloy and preparation method thereof
CN108517428A (en) * 2018-03-30 2018-09-11 北京工业大学 A kind of grain refiner for aluminum or aluminum alloy
CN108251696A (en) * 2018-04-09 2018-07-06 林恒 Titanium niobium zirconium superelastic alloy material with high intensity high-flexibility and preparation method thereof
CN110157935B (en) * 2019-06-28 2021-05-07 上海大学 Al-V-B refiner for casting aluminum-silicon alloy, preparation method and application thereof
CN110551910B (en) * 2019-08-30 2022-03-22 江苏大学 Aluminum alloy composite refining and strengthening agent and preparation method and device thereof
CN110835697B (en) * 2019-11-29 2023-08-01 中北大学 Method for directly preparing aluminum alloy refiner by recycling waste aluminum
CN112410591B (en) * 2020-10-30 2022-03-04 滨州渤海活塞有限公司 Super-long-effect double-modification method for hypereutectic aluminum-silicon alloy

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