CN115502400A - Method for rapidly preparing high-performance powder titanium alloy based on titanium hydride raw material - Google Patents
Method for rapidly preparing high-performance powder titanium alloy based on titanium hydride raw material Download PDFInfo
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- CN115502400A CN115502400A CN202211083557.7A CN202211083557A CN115502400A CN 115502400 A CN115502400 A CN 115502400A CN 202211083557 A CN202211083557 A CN 202211083557A CN 115502400 A CN115502400 A CN 115502400A
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- 239000000843 powder Substances 0.000 title claims abstract description 97
- 229910001069 Ti alloy Inorganic materials 0.000 title claims abstract description 68
- 238000000034 method Methods 0.000 title claims abstract description 54
- -1 titanium hydride Chemical compound 0.000 title claims abstract description 43
- 229910000048 titanium hydride Inorganic materials 0.000 title claims abstract description 43
- 239000002994 raw material Substances 0.000 title claims abstract description 31
- 238000010438 heat treatment Methods 0.000 claims abstract description 51
- 238000005242 forging Methods 0.000 claims abstract description 33
- 230000006698 induction Effects 0.000 claims abstract description 25
- 238000005245 sintering Methods 0.000 claims abstract description 18
- 238000009768 microwave sintering Methods 0.000 claims abstract description 14
- 239000012298 atmosphere Substances 0.000 claims abstract description 10
- 230000001681 protective effect Effects 0.000 claims abstract description 9
- 229910045601 alloy Inorganic materials 0.000 claims description 43
- 239000000956 alloy Substances 0.000 claims description 43
- 238000001816 cooling Methods 0.000 claims description 24
- 238000000137 annealing Methods 0.000 claims description 13
- 238000009694 cold isostatic pressing Methods 0.000 claims description 13
- 238000002156 mixing Methods 0.000 claims description 13
- 238000006356 dehydrogenation reaction Methods 0.000 claims description 12
- 238000004321 preservation Methods 0.000 claims description 12
- 239000011812 mixed powder Substances 0.000 claims description 9
- 239000002245 particle Substances 0.000 claims description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 3
- 239000001301 oxygen Substances 0.000 claims description 3
- 229910052760 oxygen Inorganic materials 0.000 claims description 3
- 238000003825 pressing Methods 0.000 claims description 2
- 230000009466 transformation Effects 0.000 claims 1
- 238000002360 preparation method Methods 0.000 abstract description 11
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 abstract description 6
- 239000001257 hydrogen Substances 0.000 abstract description 6
- 229910052739 hydrogen Inorganic materials 0.000 abstract description 6
- 239000013078 crystal Substances 0.000 abstract description 4
- 238000009792 diffusion process Methods 0.000 abstract description 3
- 238000000280 densification Methods 0.000 abstract description 2
- 230000000694 effects Effects 0.000 abstract description 2
- 239000012300 argon atmosphere Substances 0.000 description 7
- 238000004663 powder metallurgy Methods 0.000 description 6
- 229910000883 Ti6Al4V Inorganic materials 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 238000005272 metallurgy Methods 0.000 description 2
- 230000001737 promoting effect Effects 0.000 description 2
- 238000003723 Smelting Methods 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical group [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- XKRFYHLGVUSROY-UHFFFAOYSA-N argon Substances [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000005204 segregation Methods 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/001—Starting from powder comprising reducible metal compounds
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/02—Compacting only
- B22F3/04—Compacting only by applying fluid pressure, e.g. by cold isostatic pressing [CIP]
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/10—Sintering only
- B22F3/105—Sintering only by using electric current other than for infrared radiant energy, laser radiation or plasma ; by ultrasonic bonding
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/17—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces by forging
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/24—After-treatment of workpieces or articles
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/04—Making non-ferrous alloys by powder metallurgy
- C22C1/05—Mixtures of metal powder with non-metallic powder
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C14/00—Alloys based on titanium
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/10—Sintering only
- B22F3/105—Sintering only by using electric current other than for infrared radiant energy, laser radiation or plasma ; by ultrasonic bonding
- B22F2003/1053—Sintering only by using electric current other than for infrared radiant energy, laser radiation or plasma ; by ultrasonic bonding by induction
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- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/10—Sintering only
- B22F3/105—Sintering only by using electric current other than for infrared radiant energy, laser radiation or plasma ; by ultrasonic bonding
- B22F2003/1054—Sintering only by using electric current other than for infrared radiant energy, laser radiation or plasma ; by ultrasonic bonding by microwave
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- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/17—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces by forging
- B22F2003/175—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces by forging by hot forging, below sintering temperature
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- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/24—After-treatment of workpieces or articles
- B22F2003/248—Thermal after-treatment
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- Y02P10/25—Process efficiency
Abstract
The invention relates to a method for rapidly preparing a high-performance powder titanium alloy based on a titanium hydride raw material, and belongs to the technical field of powder titanium alloy preparation. The method comprises the steps of preparing a titanium alloy powder sintering blank by using a low-cost titanium hydride powder raw material and adopting protective atmosphere microwave sintering, and finally completing the preparation of a powder titanium alloy component by induction heating and rapid die forging forming. The method has simple process and can realize the rapid preparation of the high-performance powder titanium alloy. By utilizing the characteristics of high microwave sintering and induction heating temperature rise rate, hydrogen in the titanium hydride raw material is reserved in the heating process, and the diffusion capacity of titanium alloy elements is improved, so that the sintering activity is improved, the densification in the forming process is promoted, and the prepared powder titanium alloy has high density, fine crystal grains and excellent comprehensive mechanical property.
Description
Technical Field
The invention belongs to the technical field of powder titanium alloy preparation, and particularly relates to a method for quickly preparing a high-performance powder titanium alloy based on a titanium hydride raw material.
Background
Titanium alloy is known as the third metal, has the advantages of high specific strength, corrosion resistance, biocompatibility and the like, and is widely applied to the fields of aerospace, ocean engineering, biomedicine and the like. The traditional titanium alloy is produced by adopting an ingot metallurgy process, multiple times of vacuum consumable melting are needed to prepare ingots, and the structure and the performance of the alloy are improved through a complex hot processing process.
Powder metallurgy techniques can produce titanium alloy articles with near-net part dimensions by forming and sintering from elemental powders as raw materials. Therefore, the powder metallurgy technology can naturally avoid complex procedures such as vacuum consumable melting of the titanium alloy and the like, and can greatly shorten the production process flow of the titanium alloy. The method has the characteristic of near-net forming, and solves the problem of low utilization rate of ingot metallurgy materials. The titanium alloy part prepared by adopting the powder metallurgy technology has uniform components and fine crystal grains, thereby not only avoiding the problem of component segregation generated in the smelting process, but also reducing the dependence on the hot working process. Therefore, the powder metallurgy technology provides a new route for reducing the production cost of titanium alloy parts.
However, there are problems associated with the use of powder metallurgy in titanium alloys. For example, titanium alloy powders are susceptible to oxidation, resulting in an increase in the overall oxygen content of the powdered titanium alloy, resulting in an alloy with higher strength but much lower plasticity. In addition, the titanium alloy prepared by the powder metallurgy process is easy to form residual pores in the alloy, and also has serious influence on the mechanical property of the alloy.
In order to improve the compactness of the powder titanium alloy and further improve the comprehensive mechanical property level of the alloy, the subsequent hot processing of the titanium alloy powder sintered blank is a simple and effective means, the compactness of the material is improved, and the final forming of the powder blank can be realized. The hydrogen element can improve the sintering density of the titanium alloy, reduce the impurity content in the alloy and improve the plastic deformation capacity of the alloy. Therefore, the sintering compactness can be improved by using titanium hydride powder as a main raw material and promoting the titanium atom diffusion capacity by using hydrogen elements.
However, titanium hydride is easily decomposed at high temperature, and hydrogen or a hydrogen-argon mixed atmosphere is required to obtain a powder sintered compact containing a certain hydrogen content, which increases the safety risk of the process to a certain extent.
Disclosure of Invention
Aiming at the problems in the background art, the application provides a method for quickly preparing high-performance powder titanium alloy based on a titanium hydride raw material.
The purpose of the invention is realized by the following technical scheme:
the method for rapidly preparing the high-performance powder titanium alloy based on the titanium hydride raw material comprises the following steps:
s1: mechanically mixing raw material titanium hydride powder and intermediate alloy powder according to the nominal component proportion of the titanium alloy;
s2: carrying out cold isostatic pressing treatment on the mixed powder obtained in the step S1;
s3: performing powder microwave sintering on the powder subjected to the cold isostatic pressing treatment in the step S2 to obtain a powder sintered blank, and performing furnace cooling after heat preservation for a period of time;
s4: carrying out induction heating and cooling on the powder sintered blank obtained in the step S3;
s5: carrying out rapid die forging on the powder sintering blank subjected to induction heating in the step S4 and cooling;
s6: and (5) carrying out vacuum dehydrogenation annealing on the powder sintered blank subjected to the rapid die forging in the step S5, and carrying out heat preservation and cooling to obtain the high-performance powder titanium alloy.
Further, the average particle diameter of the titanium hydride powder is 13 to 150 μm; the mean particle diameter of the master alloy powder is 13 to 150 μm.
Further, the average oxygen content of the titanium hydride powder is in the range of 0 to 0.25wt%.
Further, in step S1, the mechanical mixing process of the raw material titanium hydride powder and the master alloy powder is performed under vacuum or protective atmosphere.
Further, in step S2, the pressing pressure in the cold isostatic pressing process is 150 to 400MPa.
Further, in step S3, the sintering temperature in the microwave sintering process is 1050-1350 ℃, the heating rate is more than or equal to 50 ℃/min when the sintering temperature is below 750 ℃, and the heat preservation time is 5-60 min.
Further, in step S4, induction heating is performed in a protective atmosphere or air; when induction heating is performed in air, the heating time does not exceed 15min.
Further, in step S5, the forging temperature in the rapid die forging process is not lower than the beta/alpha + beta transition temperature T β Below 60 deg.C, not higher than 1200 deg.C, average deformation rate not less than 1s -1 The integral deformation is more than or equal to 30 percent.
Further, in step S6, the vacuum pressure in the vacuum dehydrogenation annealing process is less than or equal to 10 -2 Pa, the annealing temperature is 250-450 ℃, and the heat preservation time is 0.5-3 h.
The method for rapidly preparing the high-performance powder titanium alloy based on the titanium hydride raw material has the following beneficial effects:
the method utilizes the characteristics of high microwave sintering and induction heating temperature rise rate to retain hydrogen in the titanium hydride raw material in the heating process and improve the diffusion capacity of titanium alloy elements, thereby improving the sintering activity and promoting the densification in the forming process, and the prepared powder titanium alloy has high density, fine crystal grains and excellent comprehensive mechanical property.
Other features of the present application and advantages thereof will become apparent from the following detailed description of exemplary embodiments thereof.
Drawings
FIG. 1 is a flow chart of a method for rapidly preparing a high performance powdered titanium alloy based on a titanium hydride feedstock in accordance with the present invention;
FIG. 2 is an alloy microstructure of a high performance powder titanium alloy prepared in example 3 of the present invention;
FIG. 3 is a room temperature tensile stress strain curve of the high performance powdered titanium alloy prepared in example 3 of the present invention.
Detailed Description
The technical solutions of the present invention will be described clearly and completely with reference to the following embodiments of the present invention, and it should be understood that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
The embodiment provides a method for rapidly preparing a high-performance powder titanium alloy based on a titanium hydride raw material, wherein the prepared titanium alloy is TC4, and the preparation method specifically comprises the following steps:
s1: mixing titanium hydride powder with the average grain size of 45 mu m and Al-V40 master alloy powder with the average grain size of 45 mu m according to the proportion of Ti-6Al-4V, and mechanically mixing for 12h on a V-shaped mixer;
S2: after the mixed powder is packaged, carrying out cold isostatic pressing under the pressure of 350MPa to obtain a powder compact;
s3: performing argon atmosphere microwave sintering on the powder compact, wherein the sintering temperature is 1250 ℃, the heating rate below 750 ℃ is 70 ℃/min, and the temperature is preserved for 30min and then the powder compact is cooled along with the furnace;
s4: carrying out induction heating on the sintered alloy in air for 15 min;
s5: the alloy after induction heating is rapidly die-forged at 970 ℃, and the deformation rate in the forging process is 30s -1 The integral deformation is 50%, and then air cooling is carried out;
s6: at 10 -2 Carrying out dehydrogenation vacuum heat treatment on the alloy subjected to rapid die forging under the vacuum pressure of Pa, raising the temperature to the annealing temperature of 350 ℃ at the heating rate of 10 ℃/min, preserving the heat for 1h, and then cooling along with the furnace; and finally obtaining the dehydrogenated TC4 titanium alloy forging.
Example 2
The embodiment provides a method for rapidly preparing a high-performance powder titanium alloy based on a titanium hydride raw material, the prepared titanium alloy is TA19, and the preparation method specifically comprises the following steps:
s1: mixing titanium hydride powder with the average grain diameter of 45 mu m and Al-V40 master alloy powder with the average grain diameter of 45 mu m mechanically for 12h on a V-shaped mixer according to the proportion of Ti-6Al-2Sn-4Zr-2 Mo;
S2: after the mixed powder is packaged, carrying out cold isostatic pressing under the pressure of 400MPa to obtain a powder compact;
s3: carrying out argon atmosphere microwave sintering on the powder compact, wherein the sintering temperature is 1200 ℃, the heating rate below 750 ℃ is 80 ℃/min, and carrying out furnace cooling after heat preservation for 60 min;
s4: carrying out induction heating on the sintered alloy for 20min in a protective atmosphere;
s5: the alloy after induction heating is subjected to rapid die forging at 1100 ℃, and the deformation rate in the forging process is 30s -1 The integral deformation is 40 percent, and then air cooling is carried out;
s6: at 10 -2 Carrying out dehydrogenation vacuum heat treatment on the alloy subjected to rapid die forging under the vacuum pressure Pa, raising the temperature to the annealing temperature of 400 ℃ at the heating rate of 50 ℃/min, preserving the heat for 2h, and then cooling along with the furnace; finally obtaining the TA19 titanium alloy forged piece after dehydrogenation.
Example 3
The embodiment provides a method for rapidly preparing a high-performance powder titanium alloy based on a titanium hydride raw material, wherein the prepared titanium alloy is TC4, and the preparation method specifically comprises the following steps:
s1: mixing titanium hydride powder with the average grain size of 13 mu m and Al-V40 master alloy powder with the average grain size of 13 mu m according to the proportion of Ti-6Al-4V, and mechanically mixing for 12h on a V-shaped mixer;
S2: after the mixed powder is packaged, carrying out cold isostatic pressing under the pressure of 150MPa to obtain a powder compact;
s3: performing argon atmosphere microwave sintering on the powder compact, wherein the sintering temperature is 1050 ℃, the heating rate below 750 ℃ is 50 ℃/min, and the powder compact is cooled along with the furnace after heat preservation for 5 min;
s4: carrying out induction heating on the sintered alloy in a protective atmosphere for 15 min;
s5: alloy after induction heating at T β Carrying out rapid die forging at the temperature of minus 60 ℃, wherein the deformation rate in the forging process is 1s -1 The integral deformation is 30 percent, and then air cooling is carried out;
s6: at 10 -2 Carrying out dehydrogenation vacuum heat treatment on the alloy subjected to rapid die forging under the vacuum pressure of Pa, raising the temperature to the annealing temperature of 250 ℃ at the heating rate of 50 ℃/min, preserving the heat for 0.5h, and then cooling along with the furnace; and finally obtaining the dehydrogenated TC4 titanium alloy forging.
The alloy microstructure of the TC4 titanium alloy forging prepared in the embodiment 3 is shown in figure 2, and the high compactness and small granularity of crystal grains can be observed; the tensile stress-strain curve at room temperature of the TC4 titanium alloy forged piece prepared in example 3 is shown in fig. 3, the tensile strength Rm =1020MPa, and the elongation at break a =12.0%, and the data shows that the forged piece has excellent comprehensive mechanical properties.
Example 4
The embodiment provides a method for rapidly preparing a high-performance powder titanium alloy based on a titanium hydride raw material, the prepared titanium alloy is TA19, and the preparation method specifically comprises the following steps:
s1: mixing titanium hydride powder with the average grain diameter of 150 mu m and Al-V40 master alloy powder with the average grain diameter of 150 mu m mechanically for 12h on a V-shaped mixer according to the proportion of Ti-6Al-2Sn-4Zr-2 Mo;
s2: after the mixed powder is packaged, carrying out cold isostatic pressing under the pressure of 400MPa to obtain a powder compact;
s3: performing argon atmosphere microwave sintering on the powder compact, wherein the sintering temperature is 1350 ℃, the heating rate below 750 ℃ is 100 ℃/min, and the furnace cooling is carried out after the temperature is kept for 60 min;
s4: carrying out induction heating on the sintered alloy in air for 15 min;
s5: the alloy after induction heating is rapidly die-forged at 1200 ℃, and the deformation rate in the forging process is 40s -1 The integral deformation is 70 percent, and then air cooling is carried out;
s6: at 10 -2 Under the vacuum pressure of Pa, the alloy after the rapid die forging is subjected to dehydrogenation vacuum heat treatment, and the temperature is increased to 10 ℃/minThe annealing temperature is 450 ℃, and the annealing furnace is cooled after heat preservation for 3 hours; and finally obtaining the dehydrogenated TA19 titanium alloy forging.
Example 5
The embodiment provides a method for rapidly preparing a high-performance powder titanium alloy based on a titanium hydride raw material, the prepared titanium alloy is TA19, and the preparation method specifically comprises the following steps:
s1: titanium hydride powder with the average grain diameter of 81.5 mu m and Al-V40 master alloy powder with the average grain diameter of 81.5 mu m are mixed mechanically for 12 hours on a V-type mixer according to the proportion of Ti-6Al-2Sn-4Zr-2 Mo;
s2: after the mixed powder is packaged, carrying out cold isostatic pressing under the pressure of 275MPa to obtain a powder compact;
s3: carrying out argon atmosphere microwave sintering on the powder compact, wherein the sintering temperature is 1200 ℃, the heating rate below 750 ℃ is 80 ℃/min, and the temperature is kept for 32.5min and then is cooled along with the furnace;
s4: carrying out induction heating on the sintered alloy for 30min in a protective atmosphere;
s5: the alloy after induction heating is rapidly die-forged at 1150 ℃, and the deformation rate in the forging process is 30s -1 The integral deformation is 60 percent, and then air cooling is carried out;
s6: at 10 -2 Carrying out dehydrogenation vacuum heat treatment on the alloy subjected to rapid die forging under the vacuum pressure of Pa, raising the temperature to the annealing temperature of 350 ℃ at the heating rate of 10 ℃/min, preserving the heat for 1.75h, and then cooling along with the furnace; and finally obtaining the dehydrogenated TA19 titanium alloy forging.
Example 6
The embodiment provides a method for rapidly preparing a high-performance powder titanium alloy based on a titanium hydride raw material, wherein the prepared titanium alloy is TC4, and the preparation method specifically comprises the following steps:
s1: titanium hydride powder with the average grain diameter of 13 mu m and Al-V40 master alloy powder with the average grain diameter of 150 mu m are proportioned according to Ti-6Al-4V and mechanically mixed for 12 hours on a V-shaped mixer;
s2: after the mixed powder is packaged, carrying out cold isostatic pressing under the pressure of 150MPa to obtain a powder compact;
s3: performing argon atmosphere microwave sintering on the powder compact, wherein the sintering temperature is 1350 ℃, the heating rate below 750 ℃ is 50 ℃/min, and the furnace cooling is carried out after the heat preservation is carried out for 5 min;
s4: carrying out induction heating on the sintered alloy for 15min in a protective atmosphere;
s5: the alloy after induction heating is rapidly die-forged at 1200 ℃, and the deformation rate in the forging process is 10s -1 The integral deformation is 40 percent, and then air cooling is carried out;
s6: at 10 -2 Carrying out dehydrogenation vacuum heat treatment on the alloy subjected to rapid die forging under the vacuum pressure of Pa, raising the temperature to 450 ℃ at the heating rate of 50 ℃/min, preserving the temperature for 0.5h, and then cooling along with the furnace; and finally obtaining the dehydrogenated TC4 titanium alloy forging.
Example 7
The embodiment provides a method for rapidly preparing a high-performance powder titanium alloy based on a titanium hydride raw material, wherein the prepared titanium alloy is TC4, and the preparation method specifically comprises the following steps:
s1: mixing titanium hydride powder with the average grain size of 150 mu m and Al-V40 master alloy powder with the average grain size of 13 mu m according to the proportion of Ti-6Al-4V, and mechanically mixing for 12h on a V-shaped mixer;
s2: after the mixed powder is packaged, carrying out cold isostatic pressing under the pressure of 400MPa to obtain a powder compact;
s3: performing argon atmosphere microwave sintering on the powder compact, wherein the sintering temperature is 1050 ℃, the heating rate below 750 ℃ is 50 ℃/min, and the powder compact is cooled along with the furnace after heat preservation for 60 min;
s4: carrying out induction heating on the sintered alloy in air for 15 min;
s5: alloy after induction heating at T β Rapid die forging is carried out at the temperature of minus 60 ℃, and the deformation rate in the forging process is 20s -1 The whole deformation is 50%, and then air cooling is carried out;
s6: at 10 -2 Carrying out dehydrogenation vacuum heat treatment on the alloy subjected to rapid die forging under the vacuum pressure of Pa, raising the temperature to the annealing temperature of 250 ℃ at the heating rate of 50 ℃/min, preserving the heat for 3h, and then cooling along with the furnace; finally obtaining after dehydrogenationThe TC4 titanium alloy forging of (1).
Claims (9)
1. A method for rapidly preparing high-performance powder titanium alloy based on titanium hydride raw materials is characterized by comprising the following steps:
s1: mixing the raw material titanium hydride powder and the intermediate alloy powder according to the nominal component proportion of the titanium alloy and mechanically mixing;
s2: carrying out cold isostatic pressing treatment on the mixed powder obtained in the step S1;
s3: performing powder microwave sintering on the powder subjected to the cold isostatic pressing treatment in the step S2 to obtain a powder sintered blank, and performing furnace cooling after heat preservation for a period of time;
s4: carrying out induction heating and cooling on the powder sintered blank obtained in the step S3;
s5: carrying out rapid die forging on the powder sintered blank subjected to induction heating in the step S4 and cooling;
s6: and (5) carrying out vacuum dehydrogenation annealing on the powder sintered blank subjected to the rapid die forging in the step S5, and carrying out heat preservation and cooling to obtain the high-performance powder titanium alloy.
2. The method for rapidly preparing the high-performance powder titanium alloy based on the titanium hydride raw material as claimed in claim 1, wherein the titanium hydride powder has an average particle diameter of 13 to 150 μm; the mean particle diameter of the master alloy powder is 13 to 150 μm.
3. The method of claim 1, wherein the average oxygen content of the titanium hydride powder is in the range of 0 to 0.25wt%.
4. The method for rapidly preparing the high-performance powder titanium alloy based on the titanium hydride raw material as claimed in claim 1, wherein the mechanical mixing process of the raw material titanium hydride powder and the master alloy powder in step S1 is performed under vacuum or protective atmosphere.
5. The method for rapidly preparing the high-performance powder titanium alloy based on the titanium hydride raw material as claimed in claim 1, wherein the pressing pressure of the cold isostatic pressing process in the step S2 is 150-400 MPa.
6. The method for rapidly preparing the high-performance powder titanium alloy based on the titanium hydride raw material as claimed in claim 1, wherein in step S3, the sintering temperature in the microwave sintering process is 1050-1350 ℃, the heating rate of the sintering temperature below 750 ℃ is not less than 50 ℃/min, and the holding time is 5-60 min.
7. The method for rapidly preparing the high-performance powder titanium alloy based on the titanium hydride raw material as claimed in claim 1, wherein in the step S4, the induction heating is performed in a protective atmosphere or air; when induction heating is performed in air, the heating time does not exceed 15min.
8. The method for rapidly preparing high-performance powder titanium alloy based on titanium hydride raw material as claimed in claim 1, wherein in step S5, the forging temperature in the rapid die forging process is not lower than β/α + β transformation temperature T β Below 60 deg.C, not higher than 1200 deg.C, average deformation rate not less than 1s -1 The integral deformation is more than or equal to 30 percent.
9. The method for rapidly preparing high-performance powder titanium alloy based on titanium hydride raw material as claimed in claim 1, wherein in step S6, the vacuum pressure of the vacuum dehydrogenation annealing process is less than or equal to 10 -2 Pa, the annealing temperature is 250-450 ℃, and the heat preservation time is 0.5-3 h.
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Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102121078A (en) * | 2011-01-20 | 2011-07-13 | 西北工业大学 | Composite preparation method for fine crystal titanium alloy |
| CN105081314A (en) * | 2015-09-25 | 2015-11-25 | 上海交通大学 | Method for preparing titanium product through titanium hydride powder |
| CN106077656A (en) * | 2016-07-30 | 2016-11-09 | 上海交通大学 | A kind of prepare the Novel powder metallurgy method with nanometer or hyperfine structure titanium article |
| CN107034375A (en) * | 2017-03-10 | 2017-08-11 | 广东省材料与加工研究所 | A kind of method that utilization hydride powder prepares high-compactness titanium article |
| CN107760897A (en) * | 2017-10-30 | 2018-03-06 | 东北大学 | To hydrogenate method of the titanium sponge as raw material manufacture titanium and titanium alloy and its parts |
| CN107848797A (en) * | 2015-07-15 | 2018-03-27 | Hrl实验室有限责任公司 | Spherical nanoparticle hydride and preparation method thereof |
| CN108838404A (en) * | 2018-06-20 | 2018-11-20 | 北京科技大学 | Titanium alloy low cost near-net-shape method |
| CN110373561A (en) * | 2019-07-11 | 2019-10-25 | 中国航发北京航空材料研究院 | A kind of method that power forging prepares high-compactness Fine Grain Ti Alloy |
| CN113046590A (en) * | 2021-02-04 | 2021-06-29 | 江苏大学 | High-entropy alloy/aluminum composite foam type wave-absorbing material and preparation method thereof |
| CN114309603A (en) * | 2022-01-05 | 2022-04-12 | 东北大学 | Method for preparing pure titanium by directly hot extruding sponge titanium particles |
-
2022
- 2022-09-06 CN CN202211083557.7A patent/CN115502400A/en active Pending
Patent Citations (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102121078A (en) * | 2011-01-20 | 2011-07-13 | 西北工业大学 | Composite preparation method for fine crystal titanium alloy |
| CN107848797A (en) * | 2015-07-15 | 2018-03-27 | Hrl实验室有限责任公司 | Spherical nanoparticle hydride and preparation method thereof |
| CN105081314A (en) * | 2015-09-25 | 2015-11-25 | 上海交通大学 | Method for preparing titanium product through titanium hydride powder |
| CN106077656A (en) * | 2016-07-30 | 2016-11-09 | 上海交通大学 | A kind of prepare the Novel powder metallurgy method with nanometer or hyperfine structure titanium article |
| CN107034375A (en) * | 2017-03-10 | 2017-08-11 | 广东省材料与加工研究所 | A kind of method that utilization hydride powder prepares high-compactness titanium article |
| CN107760897A (en) * | 2017-10-30 | 2018-03-06 | 东北大学 | To hydrogenate method of the titanium sponge as raw material manufacture titanium and titanium alloy and its parts |
| WO2019085183A1 (en) * | 2017-10-30 | 2019-05-09 | 东北大学 | Method for fabricating titanium and titanium alloy metallurgical products |
| CN108838404A (en) * | 2018-06-20 | 2018-11-20 | 北京科技大学 | Titanium alloy low cost near-net-shape method |
| CN110373561A (en) * | 2019-07-11 | 2019-10-25 | 中国航发北京航空材料研究院 | A kind of method that power forging prepares high-compactness Fine Grain Ti Alloy |
| CN113046590A (en) * | 2021-02-04 | 2021-06-29 | 江苏大学 | High-entropy alloy/aluminum composite foam type wave-absorbing material and preparation method thereof |
| CN114309603A (en) * | 2022-01-05 | 2022-04-12 | 东北大学 | Method for preparing pure titanium by directly hot extruding sponge titanium particles |
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