CN101775512B - Method for preparing TiAl alloy bars - Google Patents
Method for preparing TiAl alloy bars Download PDFInfo
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- CN101775512B CN101775512B CN2010103005263A CN201010300526A CN101775512B CN 101775512 B CN101775512 B CN 101775512B CN 2010103005263 A CN2010103005263 A CN 2010103005263A CN 201010300526 A CN201010300526 A CN 201010300526A CN 101775512 B CN101775512 B CN 101775512B
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Abstract
The invention provides a method for preparing TiAl alloy bars, relating to a method for preparing alloy bars. The invention solves the problem of difficult hot extrusion in preparation of the TiAl alloy bars by the existing casting metallurgical method and the problems of easy introduction of impurities and low compactness of the TiAl alloy bars prepared by the powder metallurgical method. The method of the invention is as follows: 1) preparing Ti powder into porous Ti by cold compressing and sintering; 2) forming a hot-pressing piece by the porous Ti and alusil alloy; 3) preparing Ti-Al bimetal complexes by using a vacuum pressure infiltration method; 4) extruding to obtain Ti-Al bimetal composite bars; and 5) performing heat treatment to obtain the TiAl alloy bars. In the invention, the extrusion operation of the bars is carried out at lower temperature, the bar has the advantages that the extrusion is easy, no ball milling process is needed, the impurities are less, the tissues of the bars are uniform and fine, the compactness is 97-99%, and the tensile strength is 730-780 MPa, thereby be capable of being used in the fields of aviation, spaceflight and automobile.
Description
Technical field
The present invention relates to a kind of preparation method of alloy bar material.
Background technology
The TiAl alloy is a lightening fire resistant structured material of new generation, has the fusing point height, density is low, hot strength is high, the good and oxidation resistant advantage of fire retardancy and be widely used in aerospace and automotive field.The preparation method of existing TiAl alloy bar material mainly contains two kinds, the one, adopt the casting metallurgical technology, earlier raw material is cut after casting and obtain blank, be to be squeezed into the TiAl alloy bar material under 1250 ℃～1400 ℃ the condition then with blank in temperature, cast the hot extrusion deformation temperature height of resulting fragility TiAl base alloy cast ingot, extruding is difficulty very; The 2nd, adopt powder metallurgy technology, earlier with raw material powder compression moulding, carry out densification with static pressure or sintering then, this method at first will be carried out ball milling to raw material, oxidation easily takes place in Ti, Al element in mechanical milling process, and very easily introduce impurity, the density of finished product is 85%～90%, and the performance of TiAl alloy is reduced.
Summary of the invention
The present invention easily introduces impurity, problem that density is low for the TiAl alloy bar material that solves difficult hot extrusion that existing casting metallurgy method prepares the TiAl alloy bar material, powder metallurgic method preparation, and a kind of preparation method of TiAl alloy bar material is provided.
The preparation method of a kind of TiAl alloy bar material of the present invention, carry out according to the following steps: one, the sized spherical titanium powder with quality purity 〉=99.5% joins in the steel die, be cold-pressed into porosity and be 45%～55% block, then block is put in the vacuum sintering furnace, after the vacuum tightness of vacuum sintering furnace is evacuated to 0.005Pa～0.01Pa, be warming up to 900 ℃～1200 ℃ and keep 1h～3h, obtain the POROUS TITANIUM precast body; Two, earlier the POROUS TITANIUM precast body is placed steel die, be to take by weighing aluminum silicon alloy at 1: 1 by the mol ratio of titanium in the POROUS TITANIUM precast body that obtains through step 1 and the aluminium in the aluminum silicon alloy again, and aluminum silicon alloy placed on the POROUS TITANIUM precast body in the steel die, form the hot pressing part; Three, will put into the vacuum heating-press sintering stove through the hot pressing part that step 2 is formed, earlier with the vacuum heating-press sintering stove evacuation to 0.001Pa～0.01Pa, be warming up to 590 ℃～640 ℃ and keep 30min～120min, be that 0.001Pa～0.01Pa, temperature are that 590 ℃～640 ℃, pressure are vacuum heating-press sintering 10min～30min under the condition of 5MPa～30MPa in vacuum tightness again, keep vacuum tightness and pressure constant at last, be cooled to room temperature, obtain Ti-Al bimetal complex body; Four, will be after Ti-Al bimetal complex body that step 3 obtains under being 300 ℃～500 ℃ condition, temperature keep 30min～60min earlier, and then by 9～36: 1 extrusion ratio is squeezed into Ti-Al bimetal compound bar with Ti-Al bimetal complex body; Five, will put into resistance furnace through the Ti-Al bimetal compound bar that step 4 obtains, be warming up to 640 ℃～700 ℃ and keep 1h～4h earlier, continue to be warming up to 1100 ℃～1400 ℃ and keep 3h～7h again, be cooled to room temperature then, obtain the TiAl alloy bar material.
The particle diameter of described sized spherical titanium powder is 100 μ m～150 μ m.
Described aluminum silicon alloy is Al-8%Si, Al-12%Si, Al-15%Si or Al-20%Si.
The present invention prepares the good titanium Al bimetal complex body of plasticity by the vacuum pressure infiltration method, under 300 ℃～500 ℃ temperature, be easy to it is hot extruded into bar, and then hot pressure reaction sintering is converted into the TiAl alloy bar material, avoid direct hot extrusion, solved and cast the problem that metallurgy method prepares the difficult hot extrusion of TiAl alloy bar material, and hot extrusion is carried out at low temperatures fragility TiAl alloy cast ingot, extruding has reduced energy waste and preparation cost easily; Adopt the vacuum pressure infiltration legal system to be equipped with the TiAl alloy bar material, this process does not need ball milling to mix powder, can avoid Ti, Al that the introducing of oxidation and impurity takes place, and the TiAl alloy bar material that the vacuum pressure infiltrating method obtains is organized tiny, even, fine and close, its density is 97%～99%, tensile strength is 730MPa～780MPa, TiAl tensile strength of alloys with casting metallurgy method or powder metallurgical technique preparation is generally 450MPa～800MPa, more as can be known, the intensity of the TiAl alloy bar material that obtains of the present invention reaches the prior art level.
Description of drawings
Fig. 1 is the electronic scanning Electronic Speculum figure of embodiment 22 through the titanium Al bimetal complex body of step 3 preparation; Fig. 2 is the electronic scanning Electronic Speculum figure of the TiAl alloy bar material of embodiment 22 preparations.
Embodiment
Embodiment one: the preparation method of the TiAl alloy bar material of present embodiment, carry out according to the following steps: one, the sized spherical titanium powder with quality purity 〉=99.5% joins in the steel die, be cold-pressed into porosity and be 45%～55% block, then block is put in the vacuum sintering furnace, after the vacuum tightness of vacuum sintering furnace is evacuated to 0.005Pa～0.01Pa, be warming up to 900 ℃～1200 ℃ and keep 1h～3h, obtain the POROUS TITANIUM precast body; Two, earlier the POROUS TITANIUM precast body is placed steel die, be to take by weighing aluminum silicon alloy at 1: 1 by the mol ratio of titanium in the POROUS TITANIUM precast body that obtains through step 1 and the aluminium in the aluminum silicon alloy again, and aluminum silicon alloy placed on the POROUS TITANIUM precast body in the steel die, form the hot pressing part; Three, will put into the vacuum heating-press sintering stove through the hot pressing part that step 2 is formed, earlier with the vacuum heating-press sintering stove evacuation to 0.001Pa～0.01Pa, be warming up to 590 ℃～640 ℃ and keep 30min～120min, be that 0.001Pa～0.01Pa, temperature are that 590 ℃～640 ℃, pressure are vacuum heating-press sintering 10min～30min under the condition of 5MPa～30MPa in vacuum tightness again, keep vacuum tightness and pressure constant at last, be cooled to room temperature, obtain Ti-Al bimetal complex body; Four, will be after Ti-Al bimetal complex body that step 3 obtains under being 300 ℃～500 ℃ condition, temperature keep 30min～60min earlier, and then by 9～36: 1 extrusion ratio is squeezed into Ti-Al bimetal compound bar with Ti-Al bimetal complex body; Five, will put into resistance furnace through the Ti-Al bimetal compound bar that step 4 obtains, be warming up to 640 ℃～700 ℃ and keep 1h～4h earlier, continue to be warming up to 1100 ℃～1400 ℃ and keep 3h～7h again, be cooled to room temperature then, obtain the TiAl alloy bar material.
The vacuum sintering furnace of present embodiment, vacuum heating-press sintering stove, resistance furnace are commercially available equipment.
Present embodiment is prepared the good titanium Al bimetal complex body of plasticity by the vacuum pressure infiltration method, under 300 ℃～500 ℃ temperature, be easy to it is hot extruded into bar, and then hot pressure reaction sintering is converted into the TiAl alloy bar material, avoid direct hot extrusion, solved and cast the problem that metallurgy method prepares the difficult hot extrusion of TiAl alloy bar material, and hot extrusion is carried out at low temperatures fragility TiAl alloy cast ingot, predation is easy, and has reduced energy waste and preparation cost; Adopt the vacuum pressure infiltration legal system to be equipped with the TiAl alloy bar material, this process does not need ball milling to mix powder, can avoid Ti, Al that the introducing of oxidation and impurity takes place, and the TiAl alloy bar material that the vacuum pressure infiltrating method obtains is organized tiny, even, fine and close, its density is 97%～99%, and tensile strength is 730MPa～780MPa.
Embodiment two: what present embodiment and embodiment one were different is: the particle diameter of the sized spherical titanium powder described in the step 1 is 100 μ m～150 μ m.Other is identical with embodiment one.
Embodiment three: what present embodiment was different with embodiment one or two is: the particle diameter of the sized spherical titanium powder described in the step 1 is 120 Jing.Other is identical with embodiment one or two.
Embodiment four: what present embodiment and embodiment one to three were different is: the aluminum silicon alloy described in the step 1 is Al-8%Si, Al-12%Si, Al-15%Si or Al-20%Si.Other is identical with embodiment one to three.
Embodiment five: what present embodiment and embodiment one to four were different is: the porosity of the back block of colding pressing in the step 1 is 48%～53%.Other is identical with embodiment one to four.
Embodiment six: what present embodiment and embodiment one to five were different is: the porosity of the back block of colding pressing in the step 1 is 50%.Other is identical with embodiment one to five.
Embodiment seven: what present embodiment and embodiment one to six were different is: the vacuum tightness of vacuum sintering furnace is 0.006Pa～0.009Pa in the step 1.Other is identical with embodiment one to six.
Embodiment eight: what present embodiment and embodiment one to seven were different is: the vacuum tightness of vacuum sintering furnace is 0.008Pa in the step 1.Other is identical with embodiment one to seven.
Embodiment nine: what present embodiment and embodiment one to eight were different is: the temperature of vacuum sintering furnace is that 950 ℃～1100 ℃, soaking time are 1.5h～2.5h in the step 1.Other is identical with embodiment one to eight.
Embodiment ten: what present embodiment and embodiment one to nine were different is: the temperature of vacuum sintering furnace is that 1000 ℃, soaking time are 2h in the step 1.Other is identical with embodiment one to nine.
Embodiment 11: what present embodiment and embodiment one to ten were different is: be warming up to 600 ℃～630 ℃ and keep 40min～110min in the step 3 earlier.Other is identical with embodiment one to ten.
Embodiment 12: what present embodiment and embodiment one to 11 were different is: be warming up to 610 ℃ and keep 90min in the step 3 earlier.Other is identical with embodiment one to 11.
Embodiment 13: what present embodiment and embodiment one to 12 were different is: be that 0.002Pa～0.008Pa, temperature are that 600 ℃～630 ℃, pressure are vacuum heating-press sintering 1 5min～25min under the condition of 10MPa～25MPa in vacuum tightness in the step 3.Other is identical with embodiment one to 12.
Embodiment 14: what present embodiment and embodiment one to 13 were different is: be that 0.005Pa, temperature are that 620 ℃, pressure are vacuum heating-press sintering 20min under the condition of 20MPa in vacuum tightness in the step 3.Other is identical with embodiment one to 13.
Embodiment 15: what present embodiment and embodiment one to 14 were different is: keep 35min～55min earlier under temperature is 350 ℃～450 ℃ condition in the step 4.Other is identical with embodiment one to 14.
Embodiment 16: what present embodiment and embodiment one to 15 were different is: keep 45min earlier under temperature is 400 ℃ condition in the step 4.Other is identical with embodiment one to 15.
Embodiment 17: what present embodiment and embodiment one to 16 were different is: the extrusion ratio in the step 4 is 12～33: 1.Other is identical with embodiment one to 16.
Embodiment 18: what present embodiment and embodiment one to 17 were different is: the extrusion ratio in the step 4 is 12～33: 1.Other is identical with embodiment one to 17.
Embodiment 19: what present embodiment and embodiment one to 18 were different is: the extrusion ratio in the step 4 is 22: 1.Other is identical with embodiment one to 18.
Embodiment 20: what present embodiment and embodiment one to 19 were different is: be warming up to 650 ℃～680 ℃ and keep 1.5h～3.5h in the step 5 earlier, continue to be warming up to 1150 ℃～1350 ℃ and keep 3.5h～6.5h again.Other is identical with embodiment one to 19.
Embodiment 21: what present embodiment and embodiment one to 20 were different is: be warming up to 660 ℃ and keep 2.5h in the step 5 earlier, continue to be warming up to 1250 ℃ and keep 5h again.Other is identical with embodiment one to 20.
Embodiment 22: the preparation method of the TiAl alloy bar material of (referring to Fig. 1, Fig. 2) present embodiment carries out according to the following steps: the sized spherical titanium powder that, with quality purity 〉=99.5% and grain diameter is 100 μ m joins in the steel die, be cold-pressed into porosity and be 53% block, then block is put in the vacuum sintering furnace, after the vacuum tightness of vacuum sintering furnace is evacuated to 0.01Pa, be warming up to 1000 ℃ and keep 2h, obtain the POROUS TITANIUM precast body; Two, earlier the POROUS TITANIUM precast body is placed steel die, be to take by weighing aluminum silicon alloy at 1: 1 by the mol ratio of aluminium among titanium and the Al-12%Si in the POROUS TITANIUM precast body that obtains through step 1 again, and aluminum silicon alloy placed on the POROUS TITANIUM precast body in the steel die, form the hot pressing part; Three, will put into the vacuum heating-press sintering stove through the hot pressing part that step 2 is formed, earlier with the vacuum heating-press sintering stove evacuation to 0.001MPa, be warming up to 640 ℃ and keep 30min, be that 0.005MPa, temperature are that 640 ℃, pressure are vacuum heating-press sintering 10min under the condition of 30MPa in vacuum tightness again, keep vacuum tightness and pressure constant at last, be cooled to room temperature, obtain Ti-Al bimetal complex body; Four, will be after Ti-Al bimetal complex body that step 3 obtains under being 400 ℃ condition, temperature keep 100min earlier, then Ti-Al bimetal complex body is squeezed into Ti-Al bimetal compound bar by 16: 1 extrusion ratio; Five, will put into resistance furnace through the Ti-Al bimetal compound bar that step 4 obtains, be warming up to 650 ℃ and keep 1.5h earlier, continue to be warming up to 1200 ℃ and keep 6h again, be cooled to room temperature then, obtain the TiAl alloy bar material.
Present embodiment is prepared the good titanium Al bimetal complex body of plasticity by the vacuum pressure infiltration method of step 3, the electronic scanning Electronic Speculum of titanium Al bimetal complex body as shown in Figure 1, as can be seen from Figure 1, titanium, two kinds of metals of aluminium are evenly distributed in complex body in the titanium Al bimetal complex body.Under 400 ℃ of temperature, be easy to titanium Al bimetal complex body is hot extruded into bar, and then be converted into the TiAl alloy bar material through hot pressure reaction sintering, avoid direct hot extrusion to fragility TiAl alloy cast ingot, solved the problem that metallurgy method prepares the difficult hot extrusion of TiAl alloy bar material of casting, and hot extrusion carries out at low temperatures, and extruding easily and reduced energy waste and preparation cost; Adopt the vacuum pressure infiltration legal system to be equipped with the TiAl alloy bar material, this process does not need ball milling to mix powder, can avoid the introducing of Ti, Al generation oxidation and impurity, and the TiAl alloy bar material that obtains of vacuum pressure infiltrating method.The scanning electron microscope of the TiAl alloy bar material of present embodiment preparation as shown in Figure 2, as can be seen from Figure 2, that the TiAl alloy bar material is organized is tiny, be evenly distributed, densification, its density is 98%, tensile strength is 780MPa.TiAl tensile strength of alloys with casting metallurgy method or powder metallurgical technique preparation is generally 450MPa～800MPa, and data are compared, and the intensity of the TiAl alloy bar material of present embodiment preparation is higher as can be known.
Claims (10)
1. the preparation method of a TiAl alloy bar material, the preparation method who it is characterized in that a kind of TiAl alloy bar material carries out according to the following steps: one, the sized spherical titanium powder with quality purity 〉=99.5% joins in the steel die, be cold-pressed into porosity and be 45%～55% block, then block is put in the vacuum sintering furnace, after the vacuum tightness of vacuum sintering furnace is evacuated to 0.005Pa～0.01Pa, be warming up to 900 ℃～1200 ℃ and keep 1h～3h, obtain the POROUS TITANIUM precast body; Two, earlier the POROUS TITANIUM precast body is placed steel die, mol ratio by titanium in the POROUS TITANIUM precast body that obtains through step 1 and the aluminium in the aluminum silicon alloy is that 1:1 takes by weighing aluminum silicon alloy again, and aluminum silicon alloy placed on the POROUS TITANIUM precast body in the steel die, form the hot pressing part; Three, will put into the vacuum heating-press sintering stove through the hot pressing part that step 2 is formed, earlier with the vacuum heating-press sintering stove evacuation to 0.001Pa～0.01Pa, be warming up to 590 ℃～640 ℃ and keep 30min～120min, be that 0.001Pa～0.01Pa, temperature are that 590 ℃～640 ℃, pressure are vacuum heating-press sintering 10min～30min under the condition of 5MPa～30MPa in vacuum tightness again, keep vacuum tightness and pressure constant at last, be cooled to room temperature, obtain Ti-Al bimetal complex body; Four, will be after Ti-Al bimetal complex body that step 3 obtains under being 300 ℃～500 ℃ condition, temperature keep 30min～60min earlier, and then the extrusion ratio by 9～36:1 is squeezed into Ti-Al bimetal compound bar with Ti-Al bimetal complex body; Five, will put into resistance furnace through the Ti-Al bimetal compound bar that step 4 obtains, be warming up to 640 ℃～700 ℃ and keep 1h～4h earlier, continue to be warming up to 1100 ℃～1400 ℃ and keep 3h～7h again, be cooled to room temperature then, obtain the TiAl alloy bar material.
2. the preparation method of a kind of TiAl alloy bar material according to claim 1, the particle diameter that it is characterized in that the sized spherical titanium powder described in the step 1 is 100 μ m～150 μ m.
3. the preparation method of a kind of TiAl alloy bar material according to claim 1 and 2 is characterized in that aluminum silicon alloy is Al-8%Si, Al-12%Si, Al-15%Si or Al-20%Si in the step 2.
4. the preparation method of a kind of TiAl alloy bar material according to claim 3, the porosity of block is 48%～53% after it is characterized in that colding pressing in the step 1.
5. according to the preparation method of claim 1,2 or 4 described a kind of TiAl alloy bar materials, the vacuum tightness that it is characterized in that vacuum sintering furnace in the step 1 is 0.006Pa～0.009Pa.
6. the preparation method of a kind of TiAl alloy bar material according to claim 5, the temperature that it is characterized in that vacuum sintering furnace in the step 1 are that 950 ℃～1100 ℃, soaking time are 1.5h～2.5h.
7. according to the preparation method of claim 1,2,4 or 6 described a kind of TiAl alloy bar materials, it is characterized in that in the step 3 in vacuum tightness being that 0.002Pa～0.008Pa, temperature are that 600 ℃～630 ℃, pressure are vacuum heating-press sintering 15min～25min under the condition of 10MPa～25MPa.
8. the preparation method of a kind of TiAl alloy bar material according to claim 7 is characterized in that in the step 4 earlier keeping 35min～55min under temperature is 350 ℃～450 ℃ condition.
9. according to the preparation method of claim 1,2,4,6 or 8 described a kind of TiAl alloy bar materials, it is characterized in that the extrusion ratio in the step 4 is 12～33:1.
10. the preparation method of a kind of TiAl alloy bar material according to claim 9 is characterized in that being warming up to earlier in the step 5 650 ℃～680 ℃ and keep 1.5h～3.5h, continues to be warming up to 1150 ℃～1350 ℃ and keep 3.5h～6.5h again.
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| CN103710554B (en) * | 2014-01-23 | 2015-10-28 | 哈尔滨工业大学 | A kind of vacuum pressure infiltration legal system of using is for Ti 2the method of AlNb alloy |
| CN103725910B (en) * | 2014-01-23 | 2016-02-10 | 哈尔滨工业大学 | The method of TiAl alloy bar is prepared in a kind of composite granule semi-solid state hot extrusion based on Ti powder and Al alloy powder |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0396389A1 (en) * | 1989-05-03 | 1990-11-07 | Alcan International Limited | Production of aluminum master alloy rod |
| CN101457331A (en) * | 2007-12-12 | 2009-06-17 | 中国科学院金属研究所 | Method for preparing TiAl alloy bar material |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0396389A1 (en) * | 1989-05-03 | 1990-11-07 | Alcan International Limited | Production of aluminum master alloy rod |
| CN101457331A (en) * | 2007-12-12 | 2009-06-17 | 中国科学院金属研究所 | Method for preparing TiAl alloy bar material |
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