CN101967572B - Method for preparing aluminum and titanium master alloy from titanium chips and aluminum at low temperature - Google Patents
Method for preparing aluminum and titanium master alloy from titanium chips and aluminum at low temperature Download PDFInfo
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- CN101967572B CN101967572B CN201010543741A CN201010543741A CN101967572B CN 101967572 B CN101967572 B CN 101967572B CN 201010543741 A CN201010543741 A CN 201010543741A CN 201010543741 A CN201010543741 A CN 201010543741A CN 101967572 B CN101967572 B CN 101967572B
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Abstract
The invention relates to a process for preparing aluminum and titanium master alloy, in particular to a method for preparing the aluminum and titanium master alloy from titanium chips and aluminum at a low temperature. The titanium chips and aluminum generated in a mechanical processing process of a titanium product are alloyed at the low temperature to form the aluminum and titanium master alloy. The method comprises the following steps of: after the melted aluminum and titanium chips are alloyed, rotationally degassing with argon or nitrogen, and when nitrogen content is 0.2 to 0.3ml/100gAl, filtering with a 10 to 20ppi alumina ceramic filter plate; removing impurities from an alloy liquid; and casting the alloy liquid into spindle shaped objects. The waste titanium chips can be reused and the aluminum and titanium master alloy can be produced at a relatively low alloying temperature by the method, so that serious burning loss, oxidation and inspiration of the alloy are avoided and the quality of the aluminum and titanium master alloy is improved.
Description
Technical field
The present invention relates to the manufacturing process of aluminium titanium master alloy, refer in particular to a kind of titanium bits and aluminium method of alloying manufacturing aluminium titanium master alloy at low temperatures of utilizing.
Background technology
The production technique of making aluminium titanium master alloy at present mainly contains, form in high temperature (about 1000 ℃) melting by primary aluminum and titanium sponge grain, common this aluminium titanium master alloy manufacturing needs temperature of aluminum liquid is superheated to more than 1000 ℃ continuously, make aluminum titanium alloy severe oxidation and air-breathing, worsened the performance of aluminium titanium master alloy.Make and produce a large amount of oxide inclusions and gas in the master alloy and bring (as being used for the A356 alloy that automotive hub is made) in the alloy that needs to add into.Another method of making aluminium titanium master alloy is to utilize the potassium fluotitanate thermite reaction, though this method need melting under the hyperthermia and superheating condition, but its shortcoming is the salt by-product that reaction produces is difficult to thorough removal, remains in the aluminum titanium alloy, has a strong impact on the quality of subsequent product.Also have, in temperature is 1150～1300 ℃ cryolite melts, with TiO2 is that raw material, Al are that reductive agent makes the Al-Ti alloy, although this kind method production cost is lower, but yield rate is also relatively low, and in the reaction process, because temperature is too high, more be easy to generate impurity and gas, had a strong impact on quality product.
Aluminium titanium master alloy is formed with the alloying reaction manufacturing under hot conditions (about 1000 ℃) of titanium sponge grain by fine aluminium usually.The composition that this high titaniferous amount master alloy (AlTi5, AlTi10, AlTi15 etc.) is used for the Ti-contained Al alloy material adds, especially for making the melting of automotive hub with the A356 alloy.The manufacturing of common this aluminium titanium master alloy needs temperature of aluminum liquid is superheated to alloying more than 1000 ℃ continuously, to making aluminum titanium alloy severe oxidation and air-breathing, has worsened the performance of aluminium titanium master alloy.Make to produce a large amount of oxide inclusions and gas in the master alloy, and these inclusiones and gas are brought in the alloy that is added into.The another kind of method of making aluminium titanium master alloy is to utilize the potassium fluotitanate thermite reaction, though this method need melting under the hyperthermia and superheating condition, but its shortcoming is the salt by-product that reaction produces is difficult to thorough removal, remain in the aluminium titanium master alloy, have a strong impact on the quality of subsequent product (as automotive hub A356 alloy).
Summary of the invention
The objective of the invention is to be improved and innovate at the shortcoming that exists in the background technology and problem, provide a kind of production technique simple, production cost is low, yield rate, cleanliness factor are high utilize titanium bits and aluminium at low temperatures alloying make the method for aluminium titanium master alloy.
The inventive method is earlier the titanium bits to be carried out oil removing and shear pulverizing, and then grinds to form the size less than 20mm.Be pressed into the titanium cake after adding small amount of binder.The titanium cake of gained is added the 780-820 ℃ of molten aluminum liquid interalloyization that sprinkles insulating covering agent.After composition stirred alloying in 30-40 minute, through being cast into the ingot shape again after the degasification of aluminium liquid, removal of impurities, the filtration treatment.Specifically may further comprise the steps:
The first step, the titanium bits that machining is cut carry out oil removal treatment, shear on shear pulverizer and are crushed to the sheet that overall dimension is not more than 20mm.And then make pulverizing mill at abrasive disc by wear resisting steel and grind to form powdery, being milled to and making it to be qualified by 10 purpose screen clothes.Again the powder that is ground to form is sneaked into small amount of binder (aluminium powder or aluminum stearate etc. are as the criterion with energy compression moulding), on oil press, be pressed into the titanium cake (piece) of every 0.5-2.0 kilogram.Above-mentioned titanium bits are thickness≤2mm, and the titaniferous amount is considered to be worth doing greater than 98% titanium.
Second step with fine aluminium fusing, sprinkled special high temperature covering agent in aluminium liquid surface, and the composition of insulating covering agent is a sodium-chlor: Repone K: aluminum fluoride equals the 5:4:1(weight ratio), and aluminium liquid is warming up to 780-820 ℃.
In the 3rd step, the titanium cake (piece) that has calculated weight is dropped in the aluminium liquid, and the worker that constantly chooses (perhaps electromagnetism) stirs alloying.Approximately stop after 30-40 minute stirring and sampling analysis.Above technology is added and repeated to off analysis again, to qualified to composition.
The 4th step, under temperature 740-780 ℃, utilize the rotation getter with argon or nitrogen to processings that outgas of aluminium liquid, and utilize hydrogen meter device measurement hydrogen richness, when hydrogen richness reaches 0.2-0.3ml/100gAl, stop degasification and skimming.
The 5th step under temperature 740-780 ℃, imported filter box with aluminium liquid, by the alumina-ceramic screen plate filtration treatment of 10-20ppi, removed the inclusion in the alloy liquid.
The 6th step under 720-740 ℃ of condition, was cast into air content less than 0.3ml/100gAl with aluminium alloy liquid at temperature of aluminum liquid, and the aluminium titanium intermediate alloy ingot that dregginess is low needs in the casting process constantly aluminium liquid to be stirred all the time.
Advantage of the present invention and beneficial effect:
The present invention is by a kind of new aluminium titanium master alloy manufacturing process, and useless titanium bits of utilization and aluminium alloying at low temperatures produce the aluminium titanium master alloy that a kind of price is relatively low and quality is higher.Compared with prior art, utilize the metal titanium bits and the alloying of aluminium under cold condition that reclaim, manufacturing cost is reduced relatively.Master alloy is overheated at high temperature (about 1000 ℃) for a long time owing to not needing simultaneously, and makes the quality of aluminium titanium master alloy improve relatively.Be both, produce aluminium titanium master alloy with thermite process and compare, can not contain byproduct of reaction fluoride salt inclusion in the product, purer.
The present invention is a kind of metal titanium bits (machining bits such as car bits, shavings, sawdust) that utilize Ti product to produce in mechanical processing process are made aluminium titanium master alloy at low temperatures with the molten aluminium alloying a method, this method biggest advantage is both processing back depleted titanium bits can be utilized again, alloying is produced aluminium titanium master alloy at a lower temperature again, can avoid scaling loss, oxidation and alloy air-breathing greatly, and improved aluminium titanium master alloy quality and reduce production costs.This kind method all has great propelling meaning to the cost and the environment protection of producing aluminium titanium master alloy.
Embodiment
Embodiment 1: utilize titanium bits and aluminium alloying under cold condition to make the AlTi10 master alloy
The aluminium titanium master alloy of titaniferous 10% is a kind of master alloy commonly used of the A356 of being widely used in alloy production.
The pure titanium bits (the titaniferous amount is greater than 98%) of machining cutting are carried out oil removal treatment, on shear pulverizer, shear again and be crushed to the sheet that overall dimension is not more than 20mm.And then make pulverizing mill by wear resisting steel and grind to form powdery, being milled to and making it to be qualified by 10 purpose screen clothes.Again the powder that is ground to form is sneaked into the small amount of binder aluminum stearate according to part by weight 97:3, on oil press, be pressed into the right cylinder (titanium cake) of every .0.5 kilogram.Will the 900kg99.7% aluminium ingot add in the medium-frequency induction furnace and melt, treat to sprinkle insulating covering agent in aluminium liquid surface after the fusing of aluminium liquid, the composition of insulating covering agent is a sodium-chlor: Repone K: Sodium Fluoride equals the 5:4:1(weight ratio), and aluminium liquid is warming up to 780 ℃.105kg titanium cake is dropped in the aluminium liquid in batches, and the worker that constantly chooses stirs alloying.Stop after 40 minutes stirring, sampling analysis, its composition are Ti:9.80%, Fe:0.19%, and Si:0.26%, composition is qualified.Under 740 ℃ of temperature, utilize the rotation getter to outgas and handled 30 minutes with argon gas, spinner velocity is 500rmp, gas flow is 12 liters/minute, and utilize dynamic hydrogen meter device to measure hydrogen richness, when hydrogen richness reaches 0.25ml/100gAl, stop degasification and skimming.Under 740 ℃ of temperature, aluminium liquid is imported filter box, by 300mmX300mmX50mm, after the alumina-ceramic screen plate filtration treatment of 10ppi, aluminum alloy melt is cast into the AlTi10 China husband ingot that every weight is about 7 kilogram weights, about 1000 kilograms of aluminium titanium intermediate alloy ingot altogether.All the time need in the casting process constantly aluminium liquid to be carried out hand mixing.
Embodiment 2: utilize titanium bits and aluminium alloying under cold condition to make the AlTi15 master alloy
The pure titanium bits (the titaniferous amount is greater than 98%) of machining cutting are carried out oil removal treatment, on shear pulverizer, shear again and be crushed to the sheet that overall dimension is not more than 20mm.And then make pulverizing mill by wear resisting steel and grind to form powdery, being milled to and making it to be qualified by 10 purpose screen clothes.Again the powder that is ground to form is sneaked into binding agent aluminum stearate and aluminium powder according to part by weight 95:4:1, on oil press, be pressed into every 0.5 kilogram right cylinder (titanium cake).Will the 850kg99.7% aluminium ingot add in the medium-frequency induction furnace and melt, treat to sprinkle insulating covering agent in aluminium liquid surface after the fusing of aluminium liquid, the composition of insulating covering agent is a sodium-chlor: Repone K: Sodium Fluoride equals the 5:4:1(weight ratio), and aluminium liquid is warming up to 820 ℃.165kg titanium cake is dropped in the aluminium liquid in batches, and constantly electricity consumption magnetic stirs alloying.Stop after 40 minutes stirring, sampling analysis, its composition are Ti:10.3%, Fe:0.20%, and Si:0.22%, composition is qualified.Under 780 ℃ of temperature, utilize the rotation getter to outgas and handled 30 minutes with argon gas, spinner velocity is 500rmp, gas flow is 12 liters/minute, and utilize dynamic hydrogen meter device to measure hydrogen richness, when hydrogen richness reaches 0.25ml/100gAl, stop degasification and skimming.Under 780 ℃ of temperature, aluminium liquid is imported filter box, by 300mmX300mmX50mm, after the alumina-ceramic screen plate filtration treatment of 10ppi, aluminum alloy melt is cast into the AlTi15 China husband ingot that every weight is about 7 kilogram weights, about 1000 kilograms of aluminium titanium intermediate alloy ingot altogether.All the time need in the casting process constantly aluminium liquid to be carried out hand mixing.
Embodiment of the present invention only is the description that preferred implementation of the present invention is carried out; be not that design of the present invention and scope are limited; under the prerequisite that does not break away from design philosophy of the present invention; engineering technical personnel make technical scheme of the present invention in this area various modification and improvement; all should fall into protection scope of the present invention; the technology contents that the present invention asks for protection all is documented in claims.
Claims (4)
1. one kind is utilized titanium bits and the aluminium method of alloying manufacturing aluminium titanium master alloy at low temperatures, it is characterized in that may further comprise the steps:
1) after the titanium bits that will process cutting carries out oil removal treatment, on shear pulverizer, shear the sheet that is ground into overall dimension≤20mm, make pulverizing mill with wear resisting steel again and grind to form the powder that can pass through 10 eye mesh screens, again the powder that is ground to form is sneaked into small amount of binder, on oil press, be pressed into the titanium cake or the titanium piece of every 0.5-2.0 kilogram;
2) sprinkle insulating covering agent with the fine aluminium fusing, and on aluminium liquid surface;
3) aluminium liquid is warming up to 780-820 ℃ after, will calculate the titanium cake or the titanium piece of weight drop in the aluminium liquid, and constantly stir alloying, stop after 30-40 minute stirring, sampling analysis is qualified;
4) under temperature of aluminum liquid 740-780 ℃ condition, utilize the rotation getter with the processing that outgases of argon or nitrogen, detect the hydrogen content of aluminium liquid when being 0.2-0.3ml/100gAl, stop degasification and skimming;
5) under temperature of aluminum liquid 740-780 ℃ condition, the aluminium alloy liquid after will outgasing with the alumina-ceramic screen plate of 10-20ppi carries out filtration treatment, removes the inclusion in the alloy liquid;
6) under temperature of aluminum liquid 720-740 ℃ condition, aluminium alloy liquid is cast into ingot, promptly gets air content, the aluminium titanium intermediate alloy ingot that dregginess is low less than 0.3ml/100gAl.
2. a kind of titanium bits and aluminium method of alloying manufacturing aluminium titanium master alloy at low temperatures of utilizing according to claim 1 is characterized in that described titanium bits are thickness≤2mm, and the titaniferous amount is considered to be worth doing greater than 98% titanium.
3. a kind of titanium bits and aluminium method of alloying manufacturing aluminium titanium master alloy at low temperatures of utilizing according to claim 1 is characterized in that aluminium powder or the aluminum stearate of described binding agent for energy compression moulding.
4. a kind of titanium bits and aluminium method of alloying manufacturing aluminium titanium master alloy at low temperatures of utilizing according to claim 1 is characterized in that described insulating covering agent is the special insulating covering agent that sodium-chlor, Repone K and aluminum fluoride are formed by the weight ratio of 5:4:1.
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| CN102912139A (en) * | 2012-10-26 | 2013-02-06 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for producing titanium or titanium alloy casting through titanium scrap |
| CN102965527B (en) * | 2012-11-29 | 2014-07-09 | 哈尔滨理工大学 | Method for preparing aluminium-chromium intermediate alloy by using chromium shavings |
| CN103849839A (en) * | 2012-12-04 | 2014-06-11 | 光洋应用材料科技股份有限公司 | Aluminum-titanium alloy sputtering target material and production method thereof |
| CN103773979B (en) * | 2014-03-04 | 2016-03-30 | 哈尔滨理工大学 | The method of aluminium titanium master alloy prepared by a kind of regeneration titanium bits or titanium scrap stock |
| CN103966452B (en) * | 2014-05-23 | 2015-12-02 | 哈尔滨理工大学 | A kind of recoverying and utilizing method of the magnesium alloy scrap containing aluminium |
| CN104805332A (en) * | 2015-04-22 | 2015-07-29 | 铜山县超特有色金属添加剂厂 | Production technology of aluminum-titanium alloy AlTi15 |
| CN104762496A (en) * | 2015-04-22 | 2015-07-08 | 铜山县超特有色金属添加剂厂 | Production process of aluminum-titanium alloy AlTi10 |
| CN105063387B (en) * | 2015-08-28 | 2018-02-13 | 重庆润际远东新材料科技有限公司 | It is a kind of to be used to produce titanium agent of aluminium alloy and preparation method thereof |
| CN105039755B (en) * | 2015-08-28 | 2018-04-24 | 重庆润际远东新材料科技有限公司 | It is a kind of to be used to produce fine powder chalybeate of aluminium alloy and preparation method thereof |
| CN106521201A (en) * | 2016-11-07 | 2017-03-22 | 湖南金联星特种材料股份有限公司 | Preparing method for Al-Ti-RE intermediate alloy |
| CN109371312A (en) * | 2018-10-12 | 2019-02-22 | 江苏裕虎新材料科技发展有限公司 | The Ti Alloying method of molten steel |
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| CN1116440C (en) * | 1999-12-03 | 2003-07-30 | 郑州大学 | Process for preparing Ti-contained Al alloy |
| CN101413061A (en) * | 2008-12-05 | 2009-04-22 | 西北有色金属研究院 | Electron beam cold hearth melting recovery method for titanium and titanium alloy chip scrap |
| CN101514418A (en) * | 2009-01-09 | 2009-08-26 | 毕祥玉 | Aluminum titanium intermediate alloy and preparation method thereof |
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Owner name: HU NAN JINLIANXING SPECIAL MATERIAL CO., LTD. Free format text: FORMER OWNER: HUNAN JINLIANXING METALLURGICAL MATERIALS TECHNOLOGY CO., LTD. Effective date: 20111223 |
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Effective date of registration: 20111223 Address after: 414000 Junshan Road, Junshan District, Hunan, No. 6888, No. Patentee after: Hunan Jinlianxing Metallurgical Materials Co., Ltd. Address before: 414000 Junshan Road, Junshan District, Hunan, No. 6888, No. Patentee before: Hunan Jinlianxing Metallurgical Materials Technology Co., Ltd. |