CN104878233A - Preparation method of aluminum-titanium-boron alloy ingot - Google Patents
Preparation method of aluminum-titanium-boron alloy ingot Download PDFInfo
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- CN104878233A CN104878233A CN201510252071.5A CN201510252071A CN104878233A CN 104878233 A CN104878233 A CN 104878233A CN 201510252071 A CN201510252071 A CN 201510252071A CN 104878233 A CN104878233 A CN 104878233A
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Abstract
The invention discloses a preparation method of an aluminum-titanium-boron alloy ingot, belonging to the field of preparation of refiner materials. The method is characterized in that the aluminum-titanium-boron alloy ingot is prepared by carrying out hot pressing on aluminum-titanium-boron alloy powder in vacuum. The method comprises the following steps: 1. heating to melt an aluminum ingot, adding potassium fluotitanate and potassium borofluoride, stirring, and deslagging to obtain an aluminum-titanium-boron alloy solution; 2. atomizing the aluminum-titanium-boron alloy into powder; 3. screening the aluminum-titanium-boron alloy powder; and 4. carrying out hot pressing on the aluminum-titanium-boron alloy in vacuum to obtain the aluminum-titanium-boron alloy ingot. The powder vacuum hot pressing method for preparing the aluminum-titanium-boron alloy ingot overcomes the defects of large TiAl3 phase size and TiB2 particle aggregation in the traditional cast aluminum-titanium-boron alloy ingot. The aluminum-titanium-boron alloy prepared by the method has the advantages of small TiAl3 phase size, uniform TiB2 particle distribution and higher grain refinement capacity.
Description
Technical field
The invention belongs to fining agent field of material preparation, be specifically related to a kind of preparation method of Al-Ti-B alloy ingot.
Background technology
Al-Ti-B alloy ingot is fining agent conventional during fine aluminium and aluminum alloy gravity casting, low-pressure casting, Hpdc, investment cast etc. are produced, using method be Al-Ti-B alloy ingot is directly joined pure Al and Alalloy smelting furnace or holding furnace in, then Foundry Production is carried out, the crystal grain of refinement fine aluminium and aluminum alloy casting, improves homogeneity of structure and the mechanical property of foundry goods.
Existing Al-Ti-B alloy ingot mainly adopts casting to produce, and is directly poured in metal pattern by Al-Ti-B alloy liquid, obtains Al-Ti-B alloy ingot after cooled and solidified.Owing to there is nonequilibrium freezing characteristic in Al-Ti-B alloy liquid process of setting, add the TiB in Al-Ti-B alloy liquid
2number of particles is numerous and have very strong affinity between particle, causes TiAl in cast aluminum-molykote composite material Ti-B alloy ingot
3mutually in thick bulk or lath-shaped, TiB
2particle is then in reunion shape.TiAl
3thick and the TiB of phase size
2particle aggregation all can reduce the grain refining capability of Al-Ti-B alloy ingot.
Find literature retrieval, prior art have employed methods such as comprising supersound process, induction stirring, copper mold rapid cooling to prepare Al-Ti-B alloy ingot.Although the thinning TiAl that these methods can be suitable
3the size of phase and improve TiB
2the distributing homogeneity of particle, but effect is not very desirable, particularly can not overcome TiB completely
2the agglomeration traits of particle.
Chinese patent CN102367534A discloses a kind of method of preparing cast aluminum alloy with composite grain refiner, its technical scheme adopts atomization to prepare Al-Ti-B-C and Cu-P alloy powder respectively, and then two kinds of alloy powders are mixed into composite refining agent are used for refinement cast aluminium alloy, its main purpose is the proportions problem of solution two kinds of fining agents.
Chinese patent CN102776422A discloses a kind of High-efficiency magnesium alloy grain refiner and preparation method thereof, and its technical scheme adopts atomization or ball milled to prepare the Powdered fining agent of Al-C-Si-Ca-Re, its main purpose be solve graphite C powder add problem.
Chinese patent CN1312396A discloses a kind of production method of fast solidified granular metal fining modifier of aluminium alloy, its technical scheme adopts mechanical vibration to add water quenching or high pressure gas winding-up atomization or mechanical centrifugal atomization to prepare the Powdered fining modifiers such as Al-Ti-B-Sr, and its main purpose reduces or eliminates thick second-phase.
Although above-mentioned patent all relates to atomization and prepares refiner alloy powder, all do not relate to the preparation of alloy pig, and the use of Powdered fining agent is very inconvenient, cannot meet the needs of fine aluminium and aluminium alloy Foundry Production.
Summary of the invention
For prior art Problems existing with not enough, the invention provides a kind of preparation method of Al-Ti-B alloy ingot, can TiAl be obtained
3phase size is tiny, TiB
2the uniform Al-Ti-B alloy ingot of particle distribution, improves the grain refining capability of Al-Ti-B alloy ingot.
It is formed by the vacuum hotpressing of Al-Ti-B alloy powder that the present invention realizes the technical scheme that above-mentioned purpose adopts, and is made up of following steps:
The first step: aluminium ingot heat fused is warming up to 850 ~ 900 DEG C, then adds potassium fluotitanate and potassium fluoborate, stir after 60 ~ 90 minutes, remove the scum silica frost on aluminium alloy surface, obtain Al-Ti-B alloy liquid;
Second step: under nitrogen protection Al-Ti-B alloy liquid is atomized into powder, atomization temperature is 800 ~ 820 DEG C, and the pressure of atomization nitrogen is 2 ~ 3MPa;
3rd step: screen Al-Ti-B alloy powder, obtains the Al-Ti-B alloy powder of particle diameter≤154 micron;
4th step: Al-Ti-B alloy powder Vacuum Heat is pressed into Al-Ti-B alloy ingot, vacuum tightness is 10
-3pa, pressure is 400 ~ 420MPa, and temperature is 580 ~ 590 DEG C.
The mass ratio of described aluminium ingot and potassium fluotitanate is 100: 22.5 ~ 27.5, and the mass ratio of aluminium ingot and potassium fluoborate is 100: 9.2 ~ 13.7.
Al-Ti-B alloy liquid is first atomized into powder by the present invention, and then Vacuum Heat is pressed into Al-Ti-B alloy ingot, because powder by atomization is a kind of fast solidification technology, Al-Ti-B alloy liquid is first atomized into tiny microlayer model under the jetting action of high pressure nitrogen, and speed of cooling can up to 10 in flight course for microlayer model
3~ 10
5k/s, cooling can suppress TiAl in microlayer model fast
3growing up and TiB of phase
2the segregation of particle is reunited, when microlayer model cooled and solidified becomes powder, then after powder Vacuum Heat is pressed into Al-Ti-B alloy ingot, and TiAl
3phase and TiB
2particle is all uniformly distributed in Al-Ti-B alloy ingot.
Al-Ti-B alloy ingot of the present invention contains the titanium of quality 4.5 ~ 5.5% and the boron of 0.8 ~ 1.2%.
The invention has the beneficial effects as follows: instant invention overcomes TiAl in conventional cast Al-Ti-B alloy ingot
3thick and the TiB of phase size
2the problem of particle aggregation, adopts Al-Ti-B alloy ingot prepared by the present invention, TiAl
3phase size is more tiny, TiB
2particle distribution is even, there is not TiB
2particle aggregation phenomenon, improves the grain refining capability of Al-Ti-B alloy ingot.
Compared with conventional cast Al-Ti-B alloy ingot, the Al-Ti-B alloy ingot prepared due to the present invention has stronger grain refining capability, fine aluminium and aluminum alloy casting can be made to obtain more tiny crystal grain, can further improve homogeneity of structure and the mechanical property of foundry goods.
Accompanying drawing explanation
Fig. 1 is the microstructure scanning electron microscope (SEM) photograph that the Al-Ti-B alloy ingot of embodiment 1 amplifies 500 times.
Fig. 2 is the microstructure scanning electron microscope (SEM) photograph that the Al-Ti-B alloy ingot of embodiment 1 amplifies 2000 times.
Fig. 3 is the microstructure scanning electron microscope (SEM) photograph that the Al-Ti-B alloy ingot of conventional cast amplifies 500 times.
Fig. 4 is the macrograin organization chart of fine aluminium after the Al-Ti-B alloy ingot that with the addition of embodiment 1.
Fig. 5 is the macrograin organization chart of fine aluminium after the Al-Ti-B alloy ingot that with the addition of conventional cast.
Embodiment
Embodiment 1
Adopt the present invention to prepare the Al-Ti-B alloy ingot that Ti constituent content is 5%, B element content is 1%, major equipment is medium frequency induction melting furnace, powder by atomization machine, vibrations sifting machine and vacuum induction hot pressing furnace, and preparation method is as follows:
The first step: heat fused aluminium ingot in medium-frequency induction furnace is also warming up to 875 DEG C, and then adds the potassium fluotitanate of quality of ingot aluminum 25% and the potassium fluoborate of 11.5%, stirs after 80 minutes, removes the scum silica frost on aluminium alloy surface, obtain Al-Ti-B alloy liquid;
Second step: Al-Ti-B alloy liquid is transferred in powder by atomization machine, under nitrogen protection Al-Ti-B alloy liquid is atomized into powder, atomization temperature is 810 DEG C, and the pressure of atomization nitrogen is 2.5MPa;
3rd step: with 100 objects vibrations sifting machines, Al-Ti-B alloy powder is screened, obtain the Al-Ti-B alloy powder of particle diameter≤154 micron;
4th step: be loaded in stainless steel pressing mold by Al-Ti-B alloy powder, puts into vacuum induction hot pressing furnace, is 10 in vacuum tightness
-3pa, pressure are 410MPa, temperature is that under the condition of 585 DEG C, Vacuum Heat is pressed into Al-Ti-B alloy ingot.
Can see from Fig. 1 and Fig. 2, the Al-Ti-B alloy ingot of the present embodiment, TiAl
3phase and TiB
2grain is all evenly distributed, TiAl
3be tiny bulk or strip mutually, size is less than 5 microns, has no TiB
2there is agglomeration in particle.
The one-tenth of conventional cast Al-Ti-B alloy ingot is grouped into and mass ratio is similarly: the Ti of 5%, the B of 1%, and surplus is Al.Can see from Fig. 3, TiAl in conventional cast Al-Ti-B alloy ingot
3mutually in thick bulk or lath-shaped, overall dimension reaches 50 microns, TiB
2particle is then distributed in aluminum substrate in reunion shape.
Can be seen by comparison diagram 1, Fig. 2 and Fig. 3, the TiAl of the Al-Ti-B alloy ingot adopting the present invention to prepare
3phase size is more tiny, TiB
2particle distribution is even, TiB
2there is not any agglomeration in particle.
In order to check the grain refining capability of the present embodiment Al-Ti-B alloy ingot, according to the grain refining capability test method that People's Republic of China (PRC) non-ferrous metal industry standard YS/T 447.1-2011 provides, respectively the grain refining capability of the present embodiment Al-Ti-B alloy ingot and conventional cast Al-Ti-B alloy ingot is detected.
Can see from Fig. 4, after with the addition of the Al-Ti-B alloy ingot of the present embodiment, the crystal grain of fine aluminium is refined to the equiax crystal that mean diameter is 84 microns.
Can see from Fig. 5, after with the addition of the Al-Ti-B alloy ingot of conventional cast, the crystal grain of fine aluminium is only refined to the equiax crystal that mean diameter is 102 microns.
Can be found out by comparison diagram 4 and Fig. 5, Al-Ti-B alloy ingot prepared by the present invention has stronger grain refining capability than the Al-Ti-B alloy ingot of conventional cast.
Embodiment 2
Adopt the present invention to prepare the Al-Ti-B alloy ingot that Ti constituent content is 4.5%, B element content is 0.8%, major equipment is medium frequency induction melting furnace, powder by atomization machine, vibrations sifting machine and vacuum induction hot pressing furnace, and preparation method is as follows:
The first step: heat fused aluminium ingot in medium-frequency induction furnace is also warming up to 850 DEG C, and then adds the potassium fluotitanate of quality of ingot aluminum 22.5% and the potassium fluoborate of 9.2%, stirs after 60 minutes, removes the scum silica frost on aluminium alloy surface, obtain Al-Ti-B alloy liquid;
Second step: Al-Ti-B alloy liquid is transferred in powder by atomization machine, under nitrogen protection Al-Ti-B alloy liquid is atomized into powder, atomization temperature is 800 DEG C, and atomization nitrogen pressure is 2MPa;
3rd step: with 100 objects vibrations sifting machines, Al-Ti-B alloy powder is screened, obtain the Al-Ti-B alloy powder of particle diameter≤154 micron;
4th step: be loaded in stainless steel pressing mold by Al-Ti-B alloy powder, puts into vacuum induction hot pressing furnace, is 10 in vacuum tightness
-3pa, pressure are 400MPa, temperature is that under the condition of 580 DEG C, Vacuum Heat is pressed into Al-Ti-B alloy ingot.
Embodiment 3
Adopt the present invention to prepare the Al-Ti-B alloy ingot that Ti constituent content is 5.5%, B element content is 1.2%, major equipment is medium frequency induction melting furnace, powder by atomization machine, vibrations sifting machine and vacuum induction hot pressing furnace, and preparation method is as follows:
The first step: heat fused aluminium ingot in medium-frequency induction furnace is also warming up to 900 DEG C, and then adds the potassium fluotitanate of quality of ingot aluminum 27.5% and the potassium fluoborate of 13.7%, stirs after 90 minutes, removes the scum silica frost on aluminium alloy surface, obtain Al-Ti-B alloy liquid;
Second step: Al-Ti-B alloy liquid is transferred in powder by atomization machine, under nitrogen protection Al-Ti-B alloy liquid is atomized into powder, atomization temperature is 820 DEG C, and atomization nitrogen pressure is 3MPa;
3rd step: with 100 objects vibrations sifting machines, Al-Ti-B alloy powder is screened, obtain the Al-Ti-B alloy powder of particle diameter≤154 micron;
4th step: be loaded in stainless steel pressing mold by Al-Ti-B alloy powder, puts into vacuum induction hot pressing furnace, is 10 in vacuum tightness
-3pa, pressure are 420MPa, temperature is that under the condition of 590 DEG C, Vacuum Heat is pressed into Al-Ti-B alloy ingot.
Claims (3)
1. a preparation method for Al-Ti-B alloy ingot, is characterized in that described Al-Ti-B alloy ingot is formed by the vacuum hotpressing of Al-Ti-B alloy powder, is made up of following steps:
The first step: aluminium ingot heat fused is warming up to 850 ~ 900 DEG C, then adds potassium fluotitanate and potassium fluoborate, stir after 60 ~ 90 minutes, remove the scum silica frost on aluminium alloy surface, obtain Al-Ti-B alloy liquid;
Second step: under nitrogen protection Al-Ti-B alloy liquid is atomized into powder, atomization temperature is 800 ~ 820 DEG C, and the pressure of atomization nitrogen is 2 ~ 3MPa;
3rd step: screen Al-Ti-B alloy powder, obtains the Al-Ti-B alloy powder of particle diameter≤154 micron;
4th step: Al-Ti-B alloy powder Vacuum Heat is pressed into Al-Ti-B alloy ingot, vacuum tightness is 10
-3pa, pressure is 400 ~ 420MPa, and temperature is 580 ~ 590 DEG C.
2. the preparation method of a kind of Al-Ti-B alloy ingot according to claim 1, is characterized in that the mass ratio of described aluminium ingot and potassium fluotitanate is 100: 22.5 ~ 27.5.
3. the preparation method of a kind of Al-Ti-B alloy ingot according to claim 1, is characterized in that the mass ratio of described aluminium ingot and potassium fluoborate is 100: 9.2 ~ 13.7.
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Cited By (9)
Publication number | Priority date | Publication date | Assignee | Title |
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CN107737941A (en) * | 2017-11-02 | 2018-02-27 | 长沙新材料产业研究院有限公司 | TiB for increasing material manufacturing2Strengthen the preparation method of Al alloy powder |
CN109576496A (en) * | 2018-12-29 | 2019-04-05 | 中北大学 | Waste aluminum recovery prepares method, product and the equipment that powder is used in selective laser fusing |
CN109694972A (en) * | 2019-03-11 | 2019-04-30 | 江苏华企铝业科技股份有限公司 | The high-densit aluminium titanium boron wire of high-purity and its manufacturing method |
CN110670008A (en) * | 2019-10-18 | 2020-01-10 | 靖江新舟合金材料有限公司 | Novel alloy adjusting ingot and preparation method thereof |
CN110976847A (en) * | 2019-12-23 | 2020-04-10 | 江西理工大学 | Preparation and use method of aluminum-titanium-boron nuclear rod |
CN111349822A (en) * | 2020-03-20 | 2020-06-30 | 永城金联星铝合金有限公司 | Aluminum-titanium-boron-strontium-rare earth alloy wire and preparation method thereof |
CN111593218A (en) * | 2020-05-12 | 2020-08-28 | 大连理工大学 | Micro-nano particle reinforced aluminum-based composite material and preparation method thereof |
CN114294950A (en) * | 2021-12-27 | 2022-04-08 | 福建省漳平市九鼎氟化工有限公司 | Setting and method for preparing aluminum-titanium-boron alloy refiner |
CN115558821A (en) * | 2022-12-06 | 2023-01-03 | 北京航空航天大学 | Realize TiB 2 Preparation method of size-controllable Al-Ti-B refiner |
Citations (2)
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CN1312396A (en) * | 2000-12-29 | 2001-09-12 | 刘庆德 | Production process of fast solidified granular metal fining modifier for aluminium alloy |
CN1322854A (en) * | 2001-05-10 | 2001-11-21 | 山东大学 | Intermediate Al-Sr alloy and its prepn |
-
2015
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Patent Citations (2)
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CN1312396A (en) * | 2000-12-29 | 2001-09-12 | 刘庆德 | Production process of fast solidified granular metal fining modifier for aluminium alloy |
CN1322854A (en) * | 2001-05-10 | 2001-11-21 | 山东大学 | Intermediate Al-Sr alloy and its prepn |
Cited By (11)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN107737941A (en) * | 2017-11-02 | 2018-02-27 | 长沙新材料产业研究院有限公司 | TiB for increasing material manufacturing2Strengthen the preparation method of Al alloy powder |
CN109576496A (en) * | 2018-12-29 | 2019-04-05 | 中北大学 | Waste aluminum recovery prepares method, product and the equipment that powder is used in selective laser fusing |
CN109694972A (en) * | 2019-03-11 | 2019-04-30 | 江苏华企铝业科技股份有限公司 | The high-densit aluminium titanium boron wire of high-purity and its manufacturing method |
CN110670008A (en) * | 2019-10-18 | 2020-01-10 | 靖江新舟合金材料有限公司 | Novel alloy adjusting ingot and preparation method thereof |
CN110976847A (en) * | 2019-12-23 | 2020-04-10 | 江西理工大学 | Preparation and use method of aluminum-titanium-boron nuclear rod |
CN110976847B (en) * | 2019-12-23 | 2021-10-08 | 江西理工大学 | Preparation and use method of aluminum-titanium-boron nuclear rod |
CN111349822A (en) * | 2020-03-20 | 2020-06-30 | 永城金联星铝合金有限公司 | Aluminum-titanium-boron-strontium-rare earth alloy wire and preparation method thereof |
CN111593218A (en) * | 2020-05-12 | 2020-08-28 | 大连理工大学 | Micro-nano particle reinforced aluminum-based composite material and preparation method thereof |
CN114294950A (en) * | 2021-12-27 | 2022-04-08 | 福建省漳平市九鼎氟化工有限公司 | Setting and method for preparing aluminum-titanium-boron alloy refiner |
CN114294950B (en) * | 2021-12-27 | 2024-02-13 | 福建省漳平市九鼎氟化工有限公司 | Setting and method for preparing aluminum-titanium-boron alloy refiner |
CN115558821A (en) * | 2022-12-06 | 2023-01-03 | 北京航空航天大学 | Realize TiB 2 Preparation method of size-controllable Al-Ti-B refiner |
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