CN103627917A - Method for refining commercially pure aluminum with aluminum-titanium interalloy - Google Patents
Method for refining commercially pure aluminum with aluminum-titanium interalloy Download PDFInfo
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Abstract
The invention belongs to the field of preparation of metal materials, and particularly relates to a method for refining commercially pure aluminum with an aluminum-titanium interalloy. The principles of the method are as follows: uniformly mixed aluminum-titanium mixed powder is sintered at certain temperature to prepare an Al-10 wt.% Ti interalloy in which the particle size of the Al3Ti phase is 2-6, and the aluminum-titanium interalloy is added into commercial molten aluminum; and since the dispersed fine granular Al3Ti provides more effective nucleation cores, the addition amount of the modifier is reduced, the deterioration response time is shortened, the crystal nucleation ratio is effectively enhanced, and the deterioration temperature can be lowered, thereby further achieving the goal of refining the grain size of the commercially pure aluminum.
Description
Technical field
The invention belongs to metallic substance preparation field, be specifically related to a kind of method of aluminium titanium master alloy refinement commercial-purity aluminium.
Background technology
Aluminium and aluminium alloy are the widely used important materials of modern industry, and further improve its over-all properties is one of key content of material supply section scholar research always; Aluminium alloy due to light weight, the characteristic such as specific tenacity is high, corrosion-resistant, electrical and thermal conductivity performance is good, easy processing, be widely used in the fields such as machinery, aerospace, building, electric appliance and electronic and automobile, especially in the application of high-technology field, to aluminium ingot and aluminium base, organizing in follow-up deep processing technology also proposed strict requirement, and one of key of controlling its tissue and performance is founding, goes out best as-cast grain structure---tiny uniform equiax crystal; Yet aluminium and alloy thereof easily form thick grain structure under casting condition, realize its widespread use, must improve its as-cast structure; Grain refining has extremely important effect to improving aluminium and alloy product quality and yield rate, for example grain refining, Neng Shi cast structure is even, prevent ingot casting crackle, improve casting speed and qualified casting, thereby improve mechanical property, processing characteristics and inner and the surface quality etc. of converted products; Al-Ti be grain-refining agent in aluminium alloy, especially in semicontinuous or the Continuous casting process industrial production aluminium ingot casting to have obtained application early, facts have proved, use Al-Ti grain-refining agent, pass through Al
3the Peritectic Reaction of Ti phase is
(Al) nucleation, has promoted cast structure's refinement; The tissue of aluminium and aluminium alloy is carried out to grain refining processing, can significantly improve process industrial art performance and the mechanical property of material, thereby there is important effect to improving aluminium and alloy product quality and yield rate, for obtaining good as cast condition crystal grain thinning tissue, both can, by add fining agent in liquid aluminium and aluminium alloy, also can realize by control cooling rate or by refinement means such as external energies (as mechanical shock, induction stirring, convection current and ultrasonic wave); Studies show that for many years, in molten aluminium, adding fining agent is thinning processing method simple and effective and the most with low cost.
At present, the aluminum grain refiner extensively adopting in industrial production has the master alloys such as AlTi, AlTiB, compares with by adding the method for titanium salt, has that the gas of emitting is few, titanium recovery rate is high and the advantage such as easy control of components; AlTiC master alloy originates from 1949, and Cibula finds that the TiC that carbon generates in Al-Ti binary alloy has Grain Refinement Effect, thereby it is theoretical to have set up carbide; TiC is difficult for occurring aggregate and precipitate, to causing the element such as pick, chromium, manganese of AlTiB " poisoning " to there is " immunity " function, but, the grain refining efficiency of AlTiC is lower than AlTiB master alloy, and show obvious Decay Rate, add the complexity of preparation, never replace the industrial application of AlTiB, due to the Al in conventional aluminium titanium master alloy
3ti is still thicker mutually, so its metamorphism can not get fully playing.
At present, along with industrial, to the improving constantly of the physicals of fine aluminium and mechanical property requirements, require the better aluminium titanium of exploitation modification effect master alloy, require its add-on less on the one hand, reduce rotten cost; Require on the other hand the Al in aluminium titanium master alloy
3ti mutually more tiny and disperse distributes, and makes its rotten time of response to fine aluminium shorter, improves rotten treatment effect.
In order to improve the modification effect of aluminium titanium master alloy to fine aluminium, patent CN 102994788 A " a kind of method of Al-5%Ti master alloy refinement fine aluminium " employing waits channel deformation preparation to have tiny block Al
3the Al-5%Ti master alloy of Ti phase, goes bad after processing to fine aluminium, makes the grain-size of fine aluminium refine to 200
below, obtained good comprehensive physical mechanical property; But this patent is to aluminium titanium master alloy through the deformation process to multi-pass, and the production cost of alterant is too high, and due to Al in the aluminium titanium master alloy after extruding
3ti is still thicker mutually, therefore, the rotten processing of commercial-purity aluminium is also had to very large room for promotion.
Summary of the invention
Object of the present invention is mainly to prepare a kind of aluminium titanium master alloy by powder metallurgic method, and a kind of method of refinement commercial-purity aluminium is provided.
A method for aluminium titanium master alloy refinement commercial-purity aluminium, comprises the steps:
A: aluminium titanium master alloy preparation
By aluminium powder with through the nano titanium powder of modifying, take mass ratio as 9:1 ball milling mixing in medium-acetone, by aluminium titanium mixed powder compressing tablet, the vacuum sintering of drying, prepare Al
3the Al-10wt.%Ti master alloy that Ti phase small and dispersed distributes;
B: technical pure aluminium block and the conventional refining agent using are put into plumbago crucible 690 ~ 710
pit furnace in be heated to fusing, be incubated 10 ~ 15min, Al-10wt.%Ti master alloy is joined in the aluminium liquid of melting, by controlling add-on and the rotten treatment time of aluminium titanium master alloy, obtain modification effect good fine aluminium liquid;
C: the industrial aluminum liquid after rotten is poured into and is chilled to room temperature in punching block and obtains required commercial-purity aluminium foundry goods.
In steps A, aluminium powder mean particle size is below 300 orders, and the mean particle size of nano titanium powder is 800nm.
Described by aluminium powder with take mass ratio through the nano titanium powder of modifying and refer to as 9:1 ball milling in medium-acetone mixes: first with acetone and nano titanium powder, to be made into suspension liquid, the volume fraction of nano titanium powder is the 1vol% of acetone, the add-on of Tween 80 is the 1vol% of acetone, utilize formic acid and ammoniacal liquor to regulate the pH value to 7 of suspension liquid, then carry out the supersound process of 30min; Aluminium powder is joined in nano titanium powder suspension liquid, according to aluminium powder with through the nano titanium powder of modifying, take mass ratio as 9:1, configuration aluminium titanium mixed powder suspension liquid; By aluminium titanium mixed powder suspension liquid wet ball grinding, the rotating speed of ball milling is 150r/min, and Ball-milling Time is 2.5 hours.
The pressure of described compressing tablet is 11MPa, and compressing tablet diameter is 8mm, and thickness is 2mm; Sintering temperature is 625
, soaking time is 10 hours, vacuum tightness is less than 0.1pa; Al in aluminium titanium master alloy after sintering
3ti phase granular size is 2 ~ 6
.
The smelting temperature of the commercial-purity aluminium in step B is 690 ~ 710
, the smelting temperature while processing than the common alterant of employing is low by 30 ~ 50
; The corresponding time shorten of rotten processing, controlling stirring and time of repose is 30 ~ 300 seconds, when the time is only 30 ~ 120 seconds, just can obtain preferably modification effect.
In step B, the add-on of master alloy is 0.1 ~ 1.0% of commercial-purity aluminium weight, and the average grain size of the commercial-purity aluminium after going bad is at 100-165
between; Compare with common alterant, when agent add-on is on the turn identical, the alterant modification effect that the present invention adopts is better.
Principle of the present invention is: by by mixed uniformly aluminium titanium mixed powder sintering at a certain temperature, be prepared into Al
3ti phase particle size is 2 ~ 6
al-10wt.%Ti master alloy in scope, then by joining in industrial aluminum liquid in the middle of this aluminium titanium, due to the tiny particulate state Al of disperse
3ti provides more effective heterogeneous forming core cores, can reduce the rotten time of response of add-on, shortening of alterant, effectively improves the nucleation rate of crystal, meanwhile, can reduce deterroration, reaches the object of further refinement commercial-purity aluminium grain-size.
Embodiment
Embodiment 1
The particle diameter that adopts Changsha Tian Jiu metallic substance company limited to produce is less than 300 object aluminium powders, the nano titanium powder that the mean particle size that Shanghai Chao Wei nanosecond science and technology company limited produces is 800nm, two kinds of powder be take to mass ratio and divide another name sample as 9:1 proportioning, preparation Al-Ti mixed powder; In XQM-1 type planetary ball mill with the rotating speed ball milling 2.5h of 150r/min, again powder is shaped with 11MPa pressure compressing tablet on tabletting machine, compressing tablet diameter is 8mm, thickness is 2mm, then compressing tablet sample is put into corundum crucible, utilize and to assemble voluntarily vacuum unit and be sealed in silica tube, the vacuum tightness in silica tube is less than 0.1pa, by the sample of sealing in KBF1400 box-annealing furnace 625
lower sintering 10h; Commercial-purity aluminium and refining agent are put into plumbago crucible 690
pit furnace in be heated to melting, insulation 15min, joins the aluminium titanium master alloy of preparation in the aluminium liquid of melting, the add-on of master alloy is 0.1% of fine aluminium weight, at aluminium liquid surface coverage one deck through NaCl, KCl and the Na of processed
3alF
6with the composite salt insulating covering agent of 30:47:23 weight ratio preparation, melt is stirred and standing 30s respectively, aluminium liquid is poured in punching block, the demoulding, water-cooled is to room temperature.
By the aluminium ingot of having cast, at 20mm above bottom, cut at place, prepare metallographic specimen, observe microstructure, measure grain-size, utilize HXD-1000TMC micro Vickers to carry out hardness measurement to sample.
Embodiment 2
The particle diameter that adopts Changsha Tian Jiu metallic substance company limited to produce is less than 300 object aluminium powders, the nano titanium powder that the mean particle size that Shanghai Chao Wei nanosecond science and technology company limited produces is 800nm, two kinds of powder be take to mass ratio and divide another name sample as 9:1 proportioning, preparation Al-Ti mixed powder; In XQM-1 type planetary ball mill with the rotating speed ball milling 2.5h of 150r/min, again powder is shaped with 11MPa pressure compressing tablet on tabletting machine, compressing tablet diameter is 8mm, thickness is 2mm, then compressing tablet sample is put into corundum crucible, utilize and to assemble voluntarily vacuum unit and be sealed in silica tube, the vacuum tightness in silica tube is less than 0.1pa, by the sample of sealing in KBF1400 box-annealing furnace 625
lower sintering 10h; Commercial-purity aluminium and refining agent are put into plumbago crucible 700
pit furnace in be heated to melting, insulation 12min; The aluminium titanium master alloy of preparation is joined in the aluminium liquid of melting, and the add-on of master alloy is 0.1% of fine aluminium weight, NaCl, KCl and Na at aluminium liquid surface coverage one deck through processed
3alF
6with the composite salt insulating covering agent of 30:47:23 weight ratio preparation, melt is stirred and standing 240s respectively, aluminium liquid is poured in punching block, the demoulding, water-cooled is to room temperature.
By the aluminium ingot of having cast, at 20mm above bottom, cut at place, prepare metallographic specimen, observe microstructure, measure grain-size, utilize HXD-1000TMC micro Vickers to carry out hardness measurement to sample.
Embodiment 3
The particle diameter that adopts Changsha Tian Jiu metallic substance company limited to produce is less than 300 object aluminium powders, the nano titanium powder that the mean particle size that Shanghai Chao Wei nanosecond science and technology company limited produces is 800nm, two kinds of powder be take to mass ratio and divide another name sample as 9:1 proportioning, preparation Al-Ti mixed powder; In XQM-1 type planetary ball mill with the rotating speed ball milling 2.5h of 150r/min, again powder is shaped with 11MPa pressure compressing tablet on tabletting machine, compressing tablet diameter is 8mm, thickness is 2mm, then compressing tablet sample is put into corundum crucible, utilize and to assemble voluntarily vacuum unit and be sealed in silica tube, the vacuum tightness in silica tube is less than 0.1pa, by the sample of sealing in KBF1400 box-annealing furnace 625
lower sintering 10h, puts into plumbago crucible 710 by commercial-purity aluminium and refining agent
pit furnace in be heated to melting, insulation 10min, joins the aluminium titanium master alloy of preparation in the aluminium liquid of melting, the add-on of master alloy is 0.3% of fine aluminium weight, at aluminium liquid surface coverage one deck through NaCl, KCl and the Na of processed
3alF
6with the composite salt insulating covering agent of 30:47:23 weight ratio preparation, melt is stirred and standing 60s respectively, aluminium liquid is poured in punching block, the demoulding, water-cooled is to room temperature.
By the aluminium ingot of having cast, at 20mm above bottom, cut at place, prepare metallographic specimen, observe microstructure, measure grain-size, utilize HXD-1000TMC micro Vickers to carry out hardness measurement to sample.
Embodiment 4
The particle diameter that adopts Changsha Tian Jiu metallic substance company limited to produce is less than 300 object aluminium powders, the nano titanium powder that the mean particle size that Shanghai Chao Wei nanosecond science and technology company limited produces is 800nm, two kinds of powder be take to mass ratio and divide another name sample as 9:1 proportioning, preparation Al-Ti mixed powder, in XQM-1 type planetary ball mill with the rotating speed ball milling 2.5h of 150r/min, again powder is shaped with 11MPa pressure compressing tablet on tabletting machine, compressing tablet diameter is 8mm, thickness is 2mm, then compressing tablet sample is put into corundum crucible, utilization is assembled voluntarily vacuum unit and is sealed in silica tube, vacuum tightness in silica tube is less than 0.1pa.By the sample of sealing in KBF1400 box-annealing furnace 625
lower sintering 10h, puts into plumbago crucible 710 by commercial-purity aluminium and refining agent
pit furnace in be heated to melting, insulation 10min, joins the aluminium titanium master alloy of preparation in the aluminium liquid of melting, the add-on of master alloy is 0.6% of fine aluminium weight, at aluminium liquid surface coverage one deck through NaCl, KCl and the Na of processed
3alF
6with the composite salt insulating covering agent of 30:47:23 weight ratio preparation, melt is stirred and standing 90s respectively, aluminium liquid is poured in punching block, the demoulding, water-cooled is to room temperature.
By the aluminium ingot of having cast, at 20mm above bottom, cut at place, prepare metallographic specimen, observe microstructure, measure grain-size, utilize HXD-1000TMC micro Vickers to carry out hardness measurement to sample.
Embodiment 5
The particle diameter that adopts Changsha Tian Jiu metallic substance company limited to produce is less than 300 object aluminium powders, the nano titanium powder that the mean particle size that Shanghai Chao Wei nanosecond science and technology company limited produces is 800nm, two kinds of powder be take to mass ratio and divide another name sample as 9:1 proportioning, preparation Al-Ti mixed powder; In XQM-1 type planetary ball mill with the rotating speed ball milling 2.5h of 150r/min, again powder is shaped with 11MPa pressure compressing tablet on tabletting machine, compressing tablet diameter is 8mm, thickness is 2mm, then compressing tablet sample is put into corundum crucible, utilization is assembled voluntarily vacuum unit and is sealed in silica tube, and the vacuum tightness in silica tube is less than 0.1pa.By the sample of sealing in KBF1400 box-annealing furnace 625
lower sintering 10h; Commercial-purity aluminium and refining agent are put into plumbago crucible 690
pit furnace in be heated to melting, insulation 15min; The aluminium titanium master alloy of preparation is joined in the aluminium liquid of melting, and the add-on of master alloy is 1.0% of fine aluminium weight, NaCl, KCl and Na at aluminium liquid surface coverage one deck through processed
3alF
6with the composite salt insulating covering agent of 30:47:23 weight ratio preparation, melt is stirred and standing 120s respectively, aluminium liquid is poured in punching block, the demoulding, water-cooled is to room temperature.
By the aluminium ingot of having cast, at 20mm above bottom, cut at place, prepare metallographic specimen, observe microstructure, measure grain-size, utilize HXD-1000TMC micro Vickers to carry out hardness measurement to sample.
Under commercial-purity aluminium and embodiment 1～5 thinning method, grain size and micro-hardness testing the results are shown in Table 1.Can find out, add after aluminium titanium master alloy prepared by present method in commercial-purity aluminium, and along with the increase of master alloy add-on, fine aluminium grain-size obviously reduces, microhardness is obvious ascendant trend.
Therefore adopt aluminium titanium master alloy refinement commercial-purity aluminium method of the present invention, in commercial-purity aluminium liquid, add the aluminium titanium master alloy of preparing through sintering process, compare with patent CN 102994788 A, when identical titanium add-on, the grain-size of commercial-purity aluminium prepared by present method is better tiny.Under the experiment condition described in this patent, the commercial-purity aluminium grain-size after rotten processing, at 100 ~ 165 μ m, can obtain good mechanical property.
Crystal grain mean size and microhardness under table 1 commercial-purity aluminium and embodiment 1～5 thinning method
Claims (6)
1. a method for aluminium titanium master alloy refinement commercial-purity aluminium, is characterized in that comprising the steps:
A: aluminium titanium master alloy preparation
By aluminium powder with through the nano titanium powder of modifying, take mass ratio as 9:1 ball milling mixing in medium-acetone, by aluminium titanium mixed powder compressing tablet, the vacuum sintering of drying, prepare Al
3the Al-10wt.%Ti master alloy that Ti phase small and dispersed distributes;
B: technical pure aluminium block and the conventional refining agent using are put into plumbago crucible 690 ~ 710
pit furnace in be heated to fusing, be incubated 10 ~ 15min, Al-10wt.%Ti master alloy is joined in the aluminium liquid of melting, by controlling add-on and the rotten treatment time of aluminium titanium master alloy, obtain modification effect good fine aluminium liquid;
C: the industrial aluminum liquid after rotten is poured into and is chilled to room temperature in punching block and obtains required commercial-purity aluminium foundry goods.
2. the method for a kind of aluminium titanium master alloy refinement commercial-purity aluminium as claimed in claim 1, is characterized in that: in steps A, aluminium powder mean particle size is below 300 orders, and the mean particle size of nano titanium powder is 800nm.
3. the method for a kind of aluminium titanium master alloy refinement commercial-purity aluminium as claimed in claim 1, it is characterized in that: described by aluminium powder with take mass ratio through the nano titanium powder of modifying and refer to as 9:1 ball milling in medium-acetone mixes: first with acetone and nano titanium powder, to be made into suspension liquid, the volume fraction of nano titanium powder is the 1vol% of acetone, the add-on of Tween 80 is the 1vol% of acetone, utilize formic acid and ammoniacal liquor to regulate the pH value to 7 of suspension liquid, then carry out the supersound process of 30min; Aluminium powder is joined in nano titanium powder suspension liquid, according to aluminium powder with through the nano titanium powder of modifying, take mass ratio as 9:1, configuration aluminium titanium mixed powder suspension liquid; By aluminium titanium mixed powder suspension liquid wet ball grinding, the rotating speed of ball milling is 150r/min, and Ball-milling Time is 2.5 hours.
4. the method for a kind of aluminium titanium master alloy refinement commercial-purity aluminium as claimed in claim 1, is characterized in that: the pressure of described compressing tablet is 11MPa, and compressing tablet diameter is 8mm, and thickness is 2mm; Sintering temperature is 625
, soaking time is 10 hours, vacuum tightness is less than 0.1pa; Al in aluminium titanium master alloy after sintering
3ti phase granular size is 2 ~ 6
.
5. the method for a kind of aluminium titanium master alloy refinement commercial-purity aluminium as claimed in claim 1, is characterized in that: the smelting temperature of the commercial-purity aluminium in step B is 690 ~ 710
, the smelting temperature while processing than the common alterant of employing is low by 30 ~ 50
; The corresponding time shorten of rotten processing, controlling stirring and time of repose is 30 ~ 300 seconds, when the time is only 30 ~ 120 seconds, just can obtain preferably modification effect.
6. the method for a kind of aluminium titanium master alloy refinement commercial-purity aluminium as claimed in claim 1, is characterized in that: in step B, the add-on of master alloy is 0.1 ~ 1.0% of commercial-purity aluminium weight, and the average grain size of the commercial-purity aluminium after going bad is at 100-165
between; Compare with common alterant, when agent add-on is on the turn identical, the alterant modification effect that the present invention adopts is better.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112522549A (en) * | 2020-11-27 | 2021-03-19 | 山东创新精密科技有限公司 | High-strength, high-conductivity, corrosion-resistant, weldable and good-thermal-forming-performance 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 |
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| CN102994788A (en) * | 2012-11-21 | 2013-03-27 | 常州大学 | Method for refining pure aluminum of Al-5% Ti intermediate alloy |
-
2013
- 2013-11-05 CN CN201310544122.2A patent/CN103627917B/en active Active
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102994788A (en) * | 2012-11-21 | 2013-03-27 | 常州大学 | Method for refining pure aluminum of Al-5% Ti intermediate alloy |
Non-Patent Citations (3)
| Title |
|---|
| JIANHUA WANG ET AL: "Microstructural Evolution and Grain Refining Efficiency of Al-10Ti Master Alloy Improved by Copper Mold Die Casting", 《JOURNAL OF MATERIALS ENGINEERING AND PERFORMANCE》, vol. 22, no. 7, 31 July 2013 (2013-07-31), pages 2012 - 2018, XP035372134, DOI: 10.1007/s11665-013-0490-6 * |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112522549A (en) * | 2020-11-27 | 2021-03-19 | 山东创新精密科技有限公司 | High-strength, high-conductivity, corrosion-resistant, weldable and good-thermal-forming-performance 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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