CN100386455C - Method for preparing aluminum-titanium-carbon intermediate alloy - Google Patents
Method for preparing aluminum-titanium-carbon intermediate alloy Download PDFInfo
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- CN100386455C CN100386455C CNB2006100469965A CN200610046996A CN100386455C CN 100386455 C CN100386455 C CN 100386455C CN B2006100469965 A CNB2006100469965 A CN B2006100469965A CN 200610046996 A CN200610046996 A CN 200610046996A CN 100386455 C CN100386455 C CN 100386455C
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Abstract
The present invention relates to a method for preparing an aluminum-titanium-carbon intermediate alloy. In the method, a cryolite is taken as a covering agent, and oxide of titanium, a high purity carbon source and metallic aluminium are used as raw materials; the proportioned electrolyte containing the cryolite, the oxide of titanium and the high purity carbon source is added to a crucible, and heated until complete melting, cryolite melt is stirred for 5 to 10 minutes, the metallic aluminium is added after a preset temperature is reached, thermal reduction reaction is carried out at a constant temperature of 960 to 1500 DEG C, the reduction time is 15 to 90 minutes, and the cryolite melt can be completely covered on the surface of the metallic aluminium liquid so as to prevent the alloy liquid from being polluted by air; the electrolyte and the aluminum liquid are poured out together after the reduction is completed, and cooled so as to obtain the aluminum-titanium-carbon intermediate alloy. In the present invention, the cryolite is used as a reaction carrier and a protective layer, is the reaction carrier, and can prevent the aluminium liquid from being polluted; the metallic aluminium, TiO2 and C have large dissolvability in the cryolite, and can react in the cryolite melt to generate TiC particles, which solves the problem that graphite can not be wet in aluminum liquids.
Description
One, technical field:
The present invention relates to a kind of preparation method of alloy, especially a kind of method for preparing the Al-Ti-C master alloy.
Two, background technology:
It is little that aluminium and aluminium alloy have density, and the cost performance height is handsome in appearance, and advantages such as good combination property are able to widespread use in fields such as machinery, automobile, aviation and military affairs.If contain large-sized crystal grain its mechanical property is worsened in aluminium and the alloy thereof, obtain the aluminium alloy of excellent comprehensive performance, optimal method is to obtain tiny equiax crystal, so crystal grain thinning is one of important means of improving aluminium and alloy mass thereof.
The Al-Ti-B master alloy is aluminium and the aluminum grain refiner that generally uses at present, but has more and more serious problem in production application, as TiB
2Aggregation of particles causes aluminium to roll the downgrade of plate and aluminium foil, when containing the aluminium alloy of elements such as Zr, Cr, Nb in refinement, and TiB
2Intoxicating phenomenon takes place in particle easily, has seriously reduced the thinning effect of Al-Ti-B master alloy.
Studies show that not have TiB based on the fining agent of TiC particle
2The shortcoming of particle, the immunizing power that demonstrates less size (0.5～1.5 μ m), lower gathering tendency and Zr and Cr are poisoned, and the wide material sources of C and can the realizing greenization of producing.The development and application of Al-Ti-C master alloy in recent years also more and more causes people's attention.
The method of at present synthetic Al-Ti-C master alloy adds particle composite algorithm and reaction in composite algorithm, because add the wettability extreme difference between particle and matrix, physical compatibility and chemical compatibility between them are relatively poor, are difficult to prepare the compound good matrix material in interface; The original position synthetic technology has been avoided above-mentioned many shortcomings, is widely adopted at present.Relatively more habitual at present in-situ reaction has solid-liquid reaction method, SHS casting, XD method, VLS method, contact reaction method etc.
These methods adopt expensive metal titanium or potassium fluotitanate as the raw material of titanium in the Al-Ti-C master alloy, have increased raw-material cost, the use of restriction Al-Ti-C master alloy.
Three, summary of the invention:
1, goal of the invention: the method that the invention provides a kind of Al-Ti-C of preparation master alloy, its objective is solve existing preparation Al-Ti-C master alloy add particle composite algorithm and reaction in composite algorithm, adopt expensive metal titanium or potassium fluotitanate raw material as titanium in the Al-Ti-C master alloy, increased raw-material cost, power consumption at high temperature is big, and titanium recovery rate is low; C is to in-problem problems in aspect such as aluminium liquid wettability differences.
2, technical scheme: the present invention is achieved through the following technical solutions:
A kind of method for preparing the Al-Ti-C master alloy is characterized in that: described method is that to get sodium aluminum fluoride be insulating covering agent, and titanyl compound, high pure carbon sources and metallic aluminium are raw material; The ionogen that contains sodium aluminum fluoride, titanyl compound and high pure carbon sources that proportioning is good is put into crucible, be warming up to after ionogen melts fully, stirred cryolite melts 5～10 minutes, after reaching preset temperature, add metallic aluminium, under 960～1500 ℃ constant temperature, carry out thermal reduction reaction, recovery time is 15～90 minutes, make cryolite melts cover the surface of metal aluminium liquid fully, in order to avoid atmospheric pollution alloy liquid, reduction is together poured out ionogen and aluminium liquid after finishing, and promptly gets the Al-Ti-C master alloy after the cooling.
Above-mentioned sodium aluminum fluoride insulating covering agent is that molecular ratio is a stage cryolite of 2.2.
Above-mentioned titanyl compound is the TiO of environment-friendly type
2
Above-mentioned high pure carbon sources is selected one or more in refinery coke, metallurgical coke, Graphite Powder 99, Graphite Electrodes bits, strengthening powder or the carbon black for use.
Above-mentioned crucible adopts plumbago crucible, alumina crucible, titanium oxide crucible, silicon carbide crucible or magnesia crucible.
Adopt graphite rod to stir cryolite melts.
3, advantage and effect: by the enforcement of technical solution of the present invention, what can solve existing preparation Al-Ti-C master alloy well adds particle composite algorithm and reaction in composite algorithm, adopt expensive metal titanium or potassium fluotitanate raw material as titanium in the Al-Ti-C master alloy, increased raw-material cost, power consumption at high temperature is big, and titanium recovery rate is low; C is to in-problem problems in aspect such as aluminium liquid wettability differences.The present invention adopts thermit reduction, and it possesses most of advantage of electrolytic process, and is not subjected to the restriction of temperature, and the present invention adds TiO in 960～1500 ℃ cryolite melts
2And the high purity graphite powder, be reductive agent with aluminium, preparing Ti quality percentage composition is 7.83～11.80%, C quality percentage composition is 0.10～2.30% Al-Ti-C master alloy.Make the back after testing every index of alloy and all meet the requirements of the result.
The present invention adopts carrier and the protective layer of sodium aluminum fluoride as reaction, covers above the aluminium liquid, and it is a thick protective layer of aluminium liquid, and it makes aluminium liquid avoid the pollution of airborne oxygen, hydrogen, nitrogen, is again a huge reaction carriers, and metallic aluminium, TiO
2Bigger with the solubleness of C in sodium aluminum fluoride, can react in cryolite melts generates the TiC particle, has solved aluminium liquid to the non-wetted problem of graphite.
Four, description of drawings:
Fig. 1 is a reaction unit structural representation of the present invention;
Fig. 2 composes for the XRD figure of the Al-Ti-C master alloy that the present invention makes;
The metallographic structure photo of the Al-Ti-C master alloy that Fig. 3 makes for the present invention;
The metallographic structure of TiC in the Al-Ti-C master alloy that Fig. 4 makes for the present invention.
Five, embodiment:
The present invention a kind ofly prepares the method for Al-Ti-C master alloy with thermit reduction, and described method is that to get sodium aluminum fluoride be insulating covering agent, and titanyl compound, high pure carbon sources and metallic aluminium are raw material; The ionogen that contains sodium aluminum fluoride, titanyl compound and high pure carbon sources that proportioning is good is put into crucible, be warming up to after ionogen melts fully, stirred cryolite melts 5～10 minutes, after reaching preset temperature, add metallic aluminium, under 960～1500 ℃ constant temperature, carry out thermal reduction reaction, recovery time is 15～90 minutes, make cryolite melts cover the surface of metal aluminium liquid fully, in order to avoid atmospheric pollution alloy liquid, reduction is together poured out ionogen and aluminium liquid after finishing, and promptly gets the Al-Ti-C master alloy after the cooling.The alloy that makes reaches the requirement of expection after testing.
Above-mentioned sodium aluminum fluoride insulating covering agent is that molecular ratio is a stage cryolite of 2.2, and the titanyl compound that is adopted is the TiO of environment-friendly type
2Or other titanyl compound.Above-mentioned carbon source is selected one or more in refinery coke, metallurgical coke, Graphite Powder 99, Graphite Electrodes bits, the strengthening powder for use.Above-mentioned crucible adopts plumbago crucible, alumina crucible, titanium oxide crucible, silicon carbide crucible or magnesia crucible.Adopt graphite rod to stir cryolite melts.
Embodiment 1:
(1). get starting material: 1. .A00 aluminium ingot; 2.. ionogen is a stage cryolite (Na
3AlF
6), molecular ratio is 2.2; 3. .TiO
2Be analytical reagent; 4.. high pure carbon powder; 5.. the high-density graphite crucible.
(2). experimental installation: Fig. 1 prepares Al-Ti-C master alloy device for the present invention, adopts accurate temperature controller of DWK-702 and Pt/Pt-10%Rh thermopair temperature control, makes vertical globars electric furnace heating by oneself, wherein: 1.. Stainless Steel Crucible; 2.. resistance furnace; 3.. plumbago crucible; 4.. cryolite melts; 5. .Al-Ti-C master alloy.
(3). the preparation method: the ionogen that proportioning is good is put into crucible, be warming up to after ionogen melts fully, stirred cryolite melts 5～10 minutes, after reaching preset temperature, add metallic aluminium, under 960～1500 ℃ constant temperature, carry out thermal reduction, recovery time is 15～60 minutes, should note making cryolite melts to cover the surface of metal aluminium liquid fully, in order to avoid atmospheric pollution alloy liquid, reduction is together poured out ionogen and aluminium liquid after finishing, and after the cooling alloy taking-up is promptly got the Al-Ti-C master alloy.The XRD figure spectrum that makes the Al-Ti-C master alloy is seen Fig. 2, and the metallographic structure photo of the Al-Ti-C master alloy that makes is seen Fig. 3, and Fig. 4 is seen in the metallographic structure of TiC in the Al-Ti-C master alloy that makes.
Embodiment 2:
(1). get starting material: 1. .A00 aluminium ingot; 2.. ionogen is a stage cryolite (Na
3AlF
6), molecular ratio is 2.2; 3. .TiO
2Be analytical reagent; 4.. high purity graphite powder or Graphite Electrodes bits; 5.. the high-density graphite crucible.
(2). experimental installation: Fig. 1 prepares Al-Ti-C master alloy device for the present invention, adopts accurate temperature controller of DWK-702 and Pt/Pt-10%Rh thermopair temperature control, makes vertical globars electric furnace heating by oneself, wherein: 1.. Stainless Steel Crucible; 2.. resistance furnace; 3.. plumbago crucible; 4.. cryolite melts; 5. .Al-Ti-C master alloy.Wherein Fan Ying crucible also can adopt alumina crucible, titanium oxide crucible, silicon carbide crucible or magnesia crucible.
(3). the preparation method: the ionogen that proportioning is good is put into crucible, be warming up to after ionogen melts fully, stirred cryolite melts 5～10 minutes, after reaching preset temperature, add metallic aluminium, under 960～1500 ℃ constant temperature, carry out thermal reduction, recovery time is 15～60 minutes, should note making cryolite melts to cover the surface of metal aluminium liquid fully, in order to avoid atmospheric pollution alloy liquid, reduction is together poured out ionogen and aluminium liquid after finishing, and after the cooling alloy taking-up is promptly got the Al-Ti-C master alloy.
Embodiment 3:
(1). get starting material: 1. .A00 aluminium ingot; 2.. ionogen is a stage cryolite (Na
3AlF
6), molecular ratio is 2.2; 3. .TiO
2Be analytical reagent; 4.. high-purity refinery coke or metallurgical coke or strengthening powder or carbon black; 5.. the high-density graphite crucible.
(2). experimental installation: Fig. 1 prepares Al-Ti-C master alloy device for the present invention, adopts accurate temperature controller of DWK-702 and Pt/Pt-10%Rh thermopair temperature control, makes vertical globars electric furnace heating by oneself, wherein: 1.. Stainless Steel Crucible; 2.. resistance furnace; 3.. plumbago crucible; 4.. cryolite melts; 5. .Al-Ti-C master alloy.
(3). the preparation method: the ionogen that proportioning is good is put into crucible, be warming up to after ionogen melts fully, stirred cryolite melts 5～10 minutes, after reaching preset temperature, add metallic aluminium, under 960～1500 ℃ constant temperature, carry out thermal reduction, recovery time is 15～60 minutes, should note making cryolite melts to cover the surface of metal aluminium liquid fully, in order to avoid atmospheric pollution alloy liquid, reduction is together poured out ionogen and aluminium liquid after finishing, and after the cooling alloy taking-up is promptly got the Al-Ti-C master alloy.
Claims (6)
1. method for preparing the Al-Ti-C master alloy is characterized in that: described method is that to get sodium aluminum fluoride be insulating covering agent, TiO
2, high pure carbon sources and metallic aluminium be raw material; With proportioning good contain sodium aluminum fluoride, TiO
2And the ionogen of high pure carbon sources is put into crucible, be warming up to after ionogen melts fully, stirred cryolite melts 5～10 minutes, reach preset temperature after, add metallic aluminium, carry out thermal reduction reaction under 960～1500 ℃ constant temperature, the recovery time is 15～90 minutes, makes cryolite melts cover the surface of metal aluminium liquid fully, in order to avoid atmospheric pollution alloy liquid, reduction is together poured out ionogen and aluminium liquid after finishing, and promptly gets the Al-Ti-C master alloy after the cooling.
2. the method for preparing the Al-Ti-C master alloy according to claim 1 is characterized in that: above-mentioned sodium aluminum fluoride insulating covering agent is that molecular ratio is a stage cryolite of 2.2.
3. the method for preparing the Al-Ti-C master alloy according to claim 1 is characterized in that: above-mentioned TiO
2TiO for environment-friendly type
2
4. the method for preparing the Al-Ti-C master alloy according to claim 1 is characterized in that: above-mentioned high pure carbon sources is selected one or more in refinery coke, metallurgical coke, Graphite Powder 99, Graphite Electrodes bits, strengthening powder or the carbon black for use.
5. the method for preparing the Al-Ti-C master alloy according to claim 1 is characterized in that: above-mentioned crucible adopts plumbago crucible, alumina crucible, titanium oxide crucible, silicon carbide crucible or magnesia crucible.
6. the method for preparing the Al-Ti-C master alloy according to claim 1 is characterized in that: adopt graphite rod to stir cryolite melts.
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| CNB2006100469965A CN100386455C (en) | 2006-06-22 | 2006-06-22 | Method for preparing aluminum-titanium-carbon intermediate alloy |
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| CN100386455C true CN100386455C (en) | 2008-05-07 |
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| CN105158237A (en) * | 2015-08-25 | 2015-12-16 | 常州大学 | Sulfur detector with room temperature cooling function |
| CN111498849B (en) * | 2020-06-08 | 2021-11-02 | 长江师范学院 | Aluminothermic reduction preparation of Ti2Method for preparing AlC ceramic powder |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1215087A (en) * | 1998-09-25 | 1999-04-28 | 清华大学 | Process for preparation of titanium- and carbon-contained aluminium-base intermediate alloy |
| CN1240833A (en) * | 1998-07-01 | 2000-01-12 | 山东工业大学 | Method for producing Al-Ti-B interalloy |
| CN1290760A (en) * | 2000-10-20 | 2001-04-11 | 山东大学 | Method for preparing aluminium-titanium-carbon intermediate alloy |
| CN1603435A (en) * | 2004-09-13 | 2005-04-06 | 中国铝业股份有限公司 | Method for preparing aluminum-titanium-carbon intermediate alloy |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1240833A (en) * | 1998-07-01 | 2000-01-12 | 山东工业大学 | Method for producing Al-Ti-B interalloy |
| CN1215087A (en) * | 1998-09-25 | 1999-04-28 | 清华大学 | Process for preparation of titanium- and carbon-contained aluminium-base intermediate alloy |
| CN1290760A (en) * | 2000-10-20 | 2001-04-11 | 山东大学 | Method for preparing aluminium-titanium-carbon intermediate alloy |
| CN1603435A (en) * | 2004-09-13 | 2005-04-06 | 中国铝业股份有限公司 | Method for preparing aluminum-titanium-carbon intermediate alloy |
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