CN1418973A - Refining agent for crystalline grain of aluminium titanium carbon intermediate alloy - Google Patents
Refining agent for crystalline grain of aluminium titanium carbon intermediate alloy Download PDFInfo
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Abstract
The aluminium titanium carbon intermediate alloy grain thinning agent relates to a AlTiC grain thining agent containing TiC granules for thinning aluminium and aluminium alloy and its preparation method. It is characterized by that said alloy composition contains (wt%) 3%-6% of Ti anjd 0.02%-0.5% of C, the reset is aluminium and inevitable impurity, in which the ratio of Ti:C is 25:1. Its preparation method is characterized by that the carbon powder prepared by using one selected from industrial graphite, natural graphite, amorphous graphite, active carbon and carbon black carbon is introduced into aluminium melt by means of graphite rotor of rotary refining equipment and stirred until the aluminium melt contains no monomer carbon.
Description
Technical field
A kind of aluminium titanium carbon master alloy grain-refining agent relates to a kind of preparation method who contains TiC particulate AlTiC grain-refining agent and this alloy grain fining agent thereof who is used for refinement aluminium and aluminium alloy.
Background technology
From the end of the sixties Al-Ti-B master alloy grain-refining agent be the preferential fining agent that adopts of aluminium industry member always, especially in recent ten years because supply of material factory constantly takes the extremely long-pending quality of improving of technical measures, obtaining bigger improvement aspect raising resultant metal cleanliness and the grain refining effect.The Al-Ti-B mass ratio of the nineties improves in the past greatly, as grain-size nineties of 99.7% commercial-purity aluminium be about 150 μ m, and be more than the 200 μ m in the past.However, existing TiB
2Particle aggregation defective, aluminium industry member wish just that for a long time a kind of acceptable Al-Ti-B substitute can be arranged.
Verified, contain less existence of grain-refining agent and the TiB of TiC
2The defective that particle aggregation is relevant, the tendency of TiC particle aggregation is little and Zr, Cr are poisoned immune.AlTiC is the most potential aluminium grain-refining agent.
At the end of the forties, Cibula fundamental research just proof removes TiB
2Outer TiC is the effective nucleating agent of aluminium, so far had half a century (Cibula A, J.Inst., 76,1949-50,321-360), and set up the carbide theory: (specially not adding) carbon reaction that exists usually in titanium and the molten aluminium generates TiC, the latter the molten aluminium solidificating period titanium concentration be significantly less than make under the peritectoid composition (0.15%Ti) α-Al forming core cause grain refining (with the periodical 80,1951-52,1-6).But,, do not make the AlTiC alloy realize producing and using owing to do not find actual effectively alloyage process.Major cause is the nonwetting aluminium of carbon, and difficulty contacts closely with melt aluminium.
The mid-80, Banerji and Reif reported a kind of Al-6%-1.2%C the AlTiC master alloy (metallurgial trans., Vol.16A 1985,2065-2068 and English Patent GB2171723,1986 and United States Patent (USP) 4748001,1988), but industrial application is realized at the end.
The Boone of U.S. KB Alloys company etc. (Light Metals 1990,845-850), experimental development KBX-22 AlTiC alloy by name (Al-5%Ti-(0.01%-0.1%) C).Studies have shown that compare with the Al-6%Ti of no boron and the Al-5%Ti-0.2%B of low boron, the KBX-22 grain refining effect has obtained very big improvement, and show and increase the purpose that carbon content (0.01%-0.1%C) does not reach increases validity.
Wide industrial experiment showed, that titanium can produce good grain refining effect in aluminium.Learn that further the grain refining effect of titanium improves greatly when adding boron again in aluminum titanium alloy.The AlTiB grain-refining agent is the industrial widely used effective grain-refining agent of aluminium so far always.But, the TiB in the existing AlTiB grain-refining agent
2Particle aggregation defective, for example foil pin hole and fracture, light are modified and surface imperfection and the aircraft application high strength alumin ium alloy slab and the forging crack of the strip defective of anodic oxidation thin plate, metal printing board, contain TiB in zirconium or the Ohmax
2Zr or Cr are poisoned cause uneven grain structure etc. still to have quality problems, be stranded surplus the aluminium industry member 30 year.For avoiding these defectives, Aluminum circle just wishes to find a kind of acceptable AlTiB substitute for a long time.
With TiB
2Particle is compared, less existence of TiC and TiB
2Relevant defective.TiC particle aggregation tendency is little and poison immune to Zr or Cr.AlTiC is the most potential aluminium grain-refining agent.
It is the alloy of Al-6%Ti-0.02%C that Britain Anglo-Blackwells company produced standard analysis in 1986, is used for controlling the grain structure of ingot casting in light and the production of anodic oxidation thin plate.The main drawback of this kind composition master alloy is Ti: C is than high (300: 1), in order to improve required TiC nucleus, titanium add-on height.Alcoa (Alcoa) uses Al6Ti0.02C for many years, but result of use is not exclusively satisfactory.The titanium add-on is generally 0.015%Ti, occurs thick intermetallic compound particle and twin column crystal and column crystal sometimes.
Still doing the new effective AlTiC grain-refining agent of various effort exploitations in the world now.For example India Hadia etc. (Light Metals 1996,729-736) laboratory scale has been developed a series of medium Ti: the AlTiC of C ratio (Al3.5Ti0.5C, Al3.5Ti0.7C and Al5Ti1C), obtained some successful experience.It is said that it produces the smallest grain size under the 0.5g/kg-2g/kg add-on in Al5Ti1C grain-refining agent thinning effect the best of overheated 1300 ℃ of temperature production, effective during the maintenance in 4 hours.
U.S. SMC company successfully developed Al-3%Ti-0.15%C master alloy grain-refining agent and 1996 Alcoa begin industrial production use and its factory of a few family assess use (Light Metals 1997,785-793).It is reported that the TiC average diameter of particles is 0.59 μ m among the Al3Ti0.15C.At 1974 μ m
2The TiC granule number is 199 in the area, is three times of Al6Ti0.02C in the equal area (67).The Ti amount of using Al3Ti0.15C to add Al6Ti0.02C alloy 1/3rd has been controlled grain structure with flying colors, twin column crystal do not occur.
Grain-refining agent (the Light Metals 1997 of the Al-5%Ti-0.25%C of a kind of improvement of five unit consolidation exploitations such as Europe academia and industry member Hoefs and Green etc., 777-784), carry out production-scale grain refining experiment, obtained good result.The typical composition of technic metal is 3%-6%Ti, 0.1%-0.3%C, i.e. 3%Ti-0.25%C, 6%Ti-0.2%C and 5%Ti-0.25%C.The latter has obtained optimum.(the whole cross section of ingot casting has obtained thin equiax crystal to Al5Ti0.25C alloy newly developed for 1750mm * 600mm) industrial scale test, the grain-refining agent of adding 0.6kg/t, and grain-size is 140 μ m to 220 μ m to 1050 slab ingots.
In sum, with AlTiC series master alloy grain-refining agent by Ti: the C ratio can be divided into low, high, in three types.
1) low Ti: the AlTiC of C ratio
The typical Ti of this type of AlTiC: the C ratio is 5: 1.As Al5Ti1C or Al6Ti1.2C, the experimental alloy of inventing by fritz Banerji and Reif80 mid-nineties 90.
2) high Ti: the AlTiC of C ratio
The typical Ti of this type of AlTiC: the C ratio is 300: 1.As Al6Ti0.02C, its shortcoming is that grain refining effect is not high.
3) medium Ti: the AlTiC of C ratio
This type of AlTiC is the new A lTiC master alloy grain-refining agent of the mid-90 exploitation, and typical Ti: the C ratio is 20: 1.As Al3Ti0.15C and Al5Ti0.25C, grain refining effect the best.
At present the research of AlTiC is also further being carried out.
Summary of the invention
Purpose of the present invention is further improved existing AlTiC exactly, and the better AlTiC master alloy of a kind of performance grain-refining agent and preparation method thereof is provided.
The objective of the invention is to be achieved through the following technical solutions.
A kind of aluminium titanium carbon master alloy grain-refining agent, the weight percent that it is characterized in that this alloy consists of and contains 3%-6%Ti and 0.02%-0.5%C, and all the other are aluminium and unavoidable impurities, wherein Ti: the C ratio is 25: 1.
A kind of preparation method of aluminium titanium carbon master alloy grain-refining agent, it is characterized in that it being at first in molten aluminium, to add titanium sponge to prepare the Al-Ti alloy, Al-Ti alloy melt with preparation, to be selected from the carbon dust introducing melt of a kind of preparation of industrial graphite, natural graphite, amorphous graphite, activated carbon and carbon black carbon with the graphite rotator of rotation a refining unit, the graphite rotator speed of rotation is 100rpm-400rpm, 200rpm-300rpm, when being stirred to monomer-free carbon and existing till.
Be distributed in purpose in the melt in order to reach the carbon dust grain, carbon dust dried under 200 ℃ of-300 ℃ of temperature removed moisture content in 1 hour-5 hours, improve wettability.
The alloy method that production provided by the invention contains TiC comprises that the carbon dust grain thoroughly is distributed in the metal melt neutralization reacts the titanium in scattered carbon dust grain and this metal melt, generates the particle of fine dispersive TiC in melt.
Compare with Al3Ti0.15C, it is significant that the present invention adopts Al5Ti0.2C to contain more superfluous titanium.As everyone knows, grain refining comprises crystal forming core and two aspects of limiting growth speed.Ti can limit crystalline growth velocity consumingly can improve constitutional supercooling, creates favorable conditions for new crystal forming core.Be dissolved in Ti in the aluminium and disobey rule in mixture, Ti is orderly at low temperatures.In the alloy of superfluous Ti, these ordered regions can exist before fining agent adds, and they may be near AlTi
3Concentration, this will be to working on the grain refining effect: because the surface tension of ordered region is low, then may exist to attract each other between the district of TiC particle and these rising sequences, help the crystal forming core.
On refinement mechanism, what AlTiC was different from AlTiB is that TiC can make α-Al forming core separately, and it has the face-centerd cubic structure identical with aluminium and lattice parameter is similar to aluminium very much; And TiB
2Be hexagonal lattice, do not play the effect of aluminium forming core, must be at TiB
2On could play the forming core effect when surperficial aluminium compound layer is arranged.In addition, the TiC fusing point is very high, is more stable under proper temperature, 750 ℃ of-1000 ℃ of maintenances for a long time, may cause TiC nucleus intoxicating phenomenon, may reduce the grain refining effect of final cast article.This is because keeping causing undesirable chemical reaction and surface active element for a long time gathers around the TiC partially, weakens or destroys the ability that makes the effective forming core of aluminium crystal.Learn that further this poisonous effect is because the Al that grows around TiC
4C
3And Ti
3Due to the AlC compound coats.This situation appears, if just melt is kept can removing in 5 to 10 minutes in 1300 ℃ to 1400 ℃ temperature before casting.
Proving aspect the aluminium foil production test, because of the TiC gathering is inclined to little little with size of particles, to reducing pinhole number in the thin foil production, for example adopt Al5Ti0.2C of the present invention and Al5TiB in 1235 the book paper tinsel of 0.0062mm, pinhole number is respectively 31 and 102; Reduced 3/4ths.
In addition, with Al5Ti0.2C of the present invention and Al5Ti1B the grain refining that A356 casting alloy Al-Si carries out in the production of aluminium wheel hub is tested, the fining agent add-on is similarly 2kg/t, grain-size is kept to for 1/5th when adding AlTiB when adding AlTiC of the present invention, and grain structure is very tiny and even.The improvement such as the table 1 of the mechanical property that obtains.
The table 1 A356 mechanical property of AlTiC grain refining
| Specimen coding | ??σ 0.2(MPa) | ????σ b | δ % unit elongation | ????HB |
| ????1 | ????172 | ????269 | ????11.0 | ????78.8 |
| ????2 | ????167 | ????267 | ????10.5 | ?????- |
| ????3 | ????163 | ????261 | ????9.9 | ?????- |
| ????4 | ????167 | ????266 | ????10.5 |
As can be seen from Table 1, average anti-grain intensity σ
bBe 266MPa, average unit elongation δ is 10.5% (criterion of acceptability: σ
b＞214MPa, δ are 8%).And the σ during Al5Ti1B
b=240MPa, δ are 8%.The result shows, uses the mechanical property of AlTiC of the present invention to be higher than criterion of acceptability and AlTiB far away.
In order to understand the present invention fully, introduce several examples of implementation now and illustrated by figure.
The production method of AlTiC grain-refining agent and this alloy grain fining agent thereof and this grain-refining agent is used for the crystal grain of refinement aluminium and aluminium alloy, comprise make carbon dust thoroughly be scattered in the aluminum titanium alloy melt and make the carbon dust grain and this metal melt in titanium be reflected at and generate the TiC dispersoid particle in the melt.The grain-refining agent that the present invention produces is suitable for carrying out the grain refining of aluminium based metal, especially to containing the alloy of zirconium, chromium or manganese, because these several elements easily cause TiB in the AlTiB grain-refining agent
2Poison.AlTiC grain-refining agent of the present invention also has good grain refining effect to the A356 casting Al-Si alloy.
Description of drawings
Fig. 1 is that the X-ray phase composite of AlTiC alloy of the present invention is analyzed, and wherein carbon (C) 100% has formed TiC, does not find uncombined carbon.Scanning electronic microscope (ESM) check shows that the TiC particle is less than 1 μ m.
Fig. 2 is the macrograph of casting sample, and magnification is 0.75: 1.They are with grain-refining agent of the present invention 99.7%Al to be added 2kg/t, and 725 ± 5 ℃ of melt temperatures are poured into the processing sample that U.S. Reynolds golf T standard mold makes, and the grain-size of acquisition is less than 100 μ m.Adopting ASTM E-112 straight line intercept method quantitative assay average grain size is 92 μ m.Do not fail at hold-time 120min thinning effect.We once tested 330 minute hold-time and did not find obvious decline.
Embodiment
A kind of aluminium titanium carbon master alloy grain-refining agent, the weight percent that it is characterized in that this alloy consists of and contains 3%-6%Ti and 0.02%-0.5%C, and all the other are aluminium and unavoidable impurities, wherein Ti: the C ratio is 25: 1.
A kind of preparation method of aluminium titanium carbon master alloy grain-refining agent, it is characterized in that it being at first in molten aluminium, to add titanium sponge to prepare the Al-Ti alloy, Al-Ti alloy melt with preparation, to be selected from the carbon dust introducing melt of a kind of preparation of industrial graphite, natural graphite, amorphous graphite, activated carbon and carbon black carbon with the graphite rotator of rotation a refining unit, the graphite rotator speed of rotation is 100rpm-400rpm, 200rpm-300rpm, when being stirred to monomer-free carbon and existing till.
Example 1
20kg99.7%Al and 1.1kg titanium sponge melted aluminium with plumbago crucible add titanium sponge in 800 ℃ of-900 ℃ of temperature and make the Al5Ti alloy melt, rotor feeding nitrogen or argon gas with the rotation a refining unit are introduced 80 gram graphite powders at 200rpm, make the titanium reaction in carbon and the melt generate TiC.Graphite Powder 99 keeps removing moisture content more than 2 hours, granularity average out to 20 μ m in 200 ℃ of temperature before use.Melt is superheated to before casting more than 1300 ℃ and keeps 5-10min, removes Al
4C
3And Ti
3AlC avoids weaken or destroy the effective nucleation ability of α-Al at the coating layer that TiC forms on every side, with the thorough descum of AlTiC melt that makes, is cast into desired ingot casting then.The AlTiC master alloy that makes is like this carried out carbon content fractional analysis result be 0.35%C, the grain-size of sample mean as a result of carrying out grain refining is 85 μ m.
Example 2
According to example 1, use 99.7%Al20kg, in adding 5.6kgKTF6 (potassium fluotitanate) under 750 ℃ of-800 ℃ of temperature and 85 gram activated carbon reactions were taken off removing dross after 20-30 minute, 0.16% the AlTiC master alloy that has been warming up to 1100 ℃, the average grain size of grain refinement sample is 97m.
Example 3
According to example 1, in the plumbago crucible of 5kg capacity, add the 2kgAl-5%Ti melt 850 ℃ of temperature, on the bath surface of cleaning, add 30 gram carbon inks, stirred gently 10-15 minute with graphite rod, made the AlTiC alloy that contains 0.05%C 1200 ℃ of temperature of reaction, the casting sample average grain size is 145 μ m.Melt keeps thinning effect obviously decline not yet in 330 minutes in 725 ℃ ± 5 ℃ in mold.
Example 4
Al5Ti0.2C grain-refining agent with the present invention's production, 99.7% commercial-purity aluminium is added 2kg/t, 750 ± 5 ℃ of melt temperatures, carry out grain refining in different duration of contact with golf T mold, sample macrostructure is shown in Fig. 2, grain-size the effect decline do not occur yet less than 100 μ m when hold-time 120min.The 0min sample is represented with grain-refining agent.
Claims (4)
1. aluminium titanium carbon master alloy grain-refining agent, the weight percent that it is characterized in that this alloy consists of and contains 3%-6%Ti and 0.02%-0.5%C, and all the other are aluminium and unavoidable impurities, wherein Ti: the C ratio is 25: 1.
2. the preparation method of an aluminium titanium carbon master alloy grain-refining agent, it is characterized in that at first adding titanium sponge in molten aluminium prepares the Al-Ti alloy, Al-Ti alloy melt with preparation, to be selected from the carbon dust introducing melt of a kind of preparation of industrial graphite, natural graphite, amorphous graphite, activated carbon and carbon black carbon with the graphite rotator of rotation a refining unit, the graphite rotator speed of rotation is 100rpm-400rpm, 200rpm-300rpm, when being stirred to monomer-free carbon and existing till.
3. the preparation method of a kind of aluminium titanium carbon master alloy grain-refining agent according to claim 2, it is characterized in that being distributed in purpose in the melt in order to reach the carbon dust grain, carbon dust dried under 200 ℃ of-300 ℃ of temperature removed moisture content in 1 hour-5 hours, improve wettability.
4. the preparation method of a kind of aluminium titanium carbon master alloy grain-refining agent according to claim 2, it is characterized in that alloy method that the production that provides contains TiC comprises that the carbon dust grain thoroughly is distributed in the metal melt neutralization makes titanium reaction in scattered carbon dust grain and this metal melt, the particle of the fine dispersive TiC of generation in melt.
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Cited By (18)
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|---|---|---|---|---|
| CN1298463C (en) * | 2004-12-31 | 2007-02-07 | 清华大学 | Preparation of aluminium titanium carbide intermediate alloy grain refiner in the ultrasonic field |
| CN101027419B (en) * | 2004-09-24 | 2010-06-16 | 爱尔康何纳吕公司 | High-strength aluminium alloy products and method for the production thereof |
| CN102181754A (en) * | 2011-03-30 | 2011-09-14 | 江阴新仁科技有限公司 | Light gauge aluminum foil woolen produced with AL-Ti-C wire refiner and preparation method |
| CN102268576A (en) * | 2011-08-05 | 2011-12-07 | 中信戴卡轮毂制造股份有限公司 | Smelting process for improving mechanical properties of aluminum wheel |
| WO2012065453A1 (en) * | 2011-06-10 | 2012-05-24 | 新星化工冶金材料(深圳)有限公司 | Preparation method for aluminum-zirconium-titanium-carbon intermediate alloy |
| CN102676892A (en) * | 2012-04-25 | 2012-09-19 | 宁波信泰机械有限公司 | 6410 aluminium alloy and preparation method and application of 6410 aluminium alloy |
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| CN106480331A (en) * | 2015-08-28 | 2017-03-08 | 中国科学院金属研究所 | A kind of Al-Ti-C intermediate alloy and preparation method thereof |
| CN106755702A (en) * | 2017-02-07 | 2017-05-31 | 吉林大学 | A kind of titanium aluminum carbide intermediate alloy as gray cast iron inovulant application |
| CN107541619A (en) * | 2016-06-27 | 2018-01-05 | 天津明源机械设备有限公司 | A kind of Al-Ti-C master alloy grain refiner |
| CN107739866A (en) * | 2017-11-28 | 2018-02-27 | 广西南宁桂启科技发展有限公司 | Grain refiner and its application in rare earth aluminum alloy material is prepared |
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| CN115341115A (en) * | 2021-05-12 | 2022-11-15 | 中国科学院过程工程研究所 | Aluminum-titanium-carbon intermediate alloy refiner and preparation method thereof |
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| CN101027419B (en) * | 2004-09-24 | 2010-06-16 | 爱尔康何纳吕公司 | High-strength aluminium alloy products and method for the production thereof |
| CN1298463C (en) * | 2004-12-31 | 2007-02-07 | 清华大学 | Preparation of aluminium titanium carbide intermediate alloy grain refiner in the ultrasonic field |
| CN102181754A (en) * | 2011-03-30 | 2011-09-14 | 江阴新仁科技有限公司 | Light gauge aluminum foil woolen produced with AL-Ti-C wire refiner and preparation method |
| CN102181754B (en) * | 2011-03-30 | 2012-11-14 | 江阴新仁科技有限公司 | Light gauge aluminum foil woolen produced with AL-Ti-C wire refiner and preparation method |
| WO2012065453A1 (en) * | 2011-06-10 | 2012-05-24 | 新星化工冶金材料(深圳)有限公司 | Preparation method for aluminum-zirconium-titanium-carbon intermediate alloy |
| CN102268576A (en) * | 2011-08-05 | 2011-12-07 | 中信戴卡轮毂制造股份有限公司 | Smelting process for improving mechanical properties of aluminum wheel |
| CN102676892A (en) * | 2012-04-25 | 2012-09-19 | 宁波信泰机械有限公司 | 6410 aluminium alloy and preparation method and application of 6410 aluminium alloy |
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| CN106480331B (en) * | 2015-08-28 | 2018-06-19 | 中国科学院金属研究所 | A kind of Al-Ti-C intermediate alloys and preparation method thereof |
| CN106480331A (en) * | 2015-08-28 | 2017-03-08 | 中国科学院金属研究所 | A kind of Al-Ti-C intermediate alloy and preparation method thereof |
| CN107541619A (en) * | 2016-06-27 | 2018-01-05 | 天津明源机械设备有限公司 | A kind of Al-Ti-C master alloy grain refiner |
| CN106244838B (en) * | 2016-09-21 | 2017-12-15 | 燕山大学 | Niobium titanium carbon Al-alloy alterant and preparation method thereof |
| CN106244838A (en) * | 2016-09-21 | 2016-12-21 | 燕山大学 | Niobium titanium carbon Al-alloy alterant and preparation method thereof |
| CN106755702A (en) * | 2017-02-07 | 2017-05-31 | 吉林大学 | A kind of titanium aluminum carbide intermediate alloy as gray cast iron inovulant application |
| CN106755702B (en) * | 2017-02-07 | 2019-01-25 | 吉林大学 | A kind of application of titanium carbide-aluminium intermediate alloy as gray cast iron inovulant |
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| CN110396614A (en) * | 2019-07-25 | 2019-11-01 | 江苏大学 | A kind of Al-V (C, N) intermediate alloy and preparation method thereof |
| CN112921203A (en) * | 2021-01-25 | 2021-06-08 | 广东工程职业技术学院 | Grain refiner for regenerated aluminum alloy and preparation method and application thereof |
| CN115341115A (en) * | 2021-05-12 | 2022-11-15 | 中国科学院过程工程研究所 | Aluminum-titanium-carbon intermediate alloy refiner and preparation method thereof |
| CN115341115B (en) * | 2021-05-12 | 2023-06-02 | 中国科学院过程工程研究所 | Aluminum-titanium-carbon intermediate alloy refiner and preparation method thereof |
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