CN110238401A - A kind of method that powder rolling prepares high-compactness Fine Grain Ti Alloy - Google Patents
A kind of method that powder rolling prepares high-compactness Fine Grain Ti Alloy Download PDFInfo
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- CN110238401A CN110238401A CN201910628446.1A CN201910628446A CN110238401A CN 110238401 A CN110238401 A CN 110238401A CN 201910628446 A CN201910628446 A CN 201910628446A CN 110238401 A CN110238401 A CN 110238401A
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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
- 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
- B22F3/02—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
- B22F3/1003—Use of special medium during sintering, e.g. sintering aid
- B22F3/1007—Atmosphere
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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
- B22F3/18—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces by using pressure rollers
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- B—PERFORMING OPERATIONS; TRANSPORTING
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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
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
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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
- B22F3/18—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces by using pressure rollers
- B22F2003/185—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces by using pressure rollers by hot rolling, below sintering temperature
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- B—PERFORMING OPERATIONS; TRANSPORTING
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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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- 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
- B22F2998/00—Supplementary information concerning processes or compositions relating to powder metallurgy
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- B22F2999/00—Aspects linked to processes or compositions used in powder metallurgy
Abstract
The present invention is a kind of method that powder rolling prepares high-compactness Fine Grain Ti Alloy, this method includes using titantium hydride and corresponding intermediate alloy powder as raw material, powder compact is prepared by isostatic cool pressing, it is characterized by: this method comprises: preparing hydrogeneous titanium alloy powder sintered blank using hydrogen/argon gas mixed atmosphere sintering；Hot rolling is carried out to hydrogeneous titanium alloy powder sintered blank, then to the sheet alloy or bar progress vacuum heat treatment after rolling, obtains the titanium alloy plate or pieces of bar stock of dehydrogenation.The method of the present invention process flow is short, cost of material is low, stock utilization is high, and the titanium alloy product consistency prepared is high, ingredient is uniform, crystal grain is tiny, excellent in mechanical performance.
Description
Technical field
The present invention is a kind of method that powder rolling prepares high-compactness Fine Grain Ti Alloy, belongs to PM technique neck
Domain.
Technical background
Titanium alloy specific strength is high, corrosion resistance is strong, good biocompatibility, in aerospace, automobile manufacture, sports equipment
Have broad application prospects with fields such as bio-medicals.Traditional titanium alloy preparation process is passed through based on ingot metallurgy method
Molten alloy ingot casting is combined with thermomechanical processings techniques such as forging, rollings, the titanium alloy excellent in mechanical performance prepared, but traditional
Casting forging titanium alloy material utilization rate is low to cause cost high, seriously limits the application field of titanium alloy.Powder metallurgy skill
Art is one of the titanium alloy preparation process of current most economy, can increase substantially stock utilization, and prepare
Titanium alloy even tissue is tiny, functional.However, since titanium alloy high activity, dystectic characteristic make powder metallurgy titanium alloy
Densification is difficult, it usually needs is combined just with expensive spherical pre-alloyed powder with the high-cost forming technology such as hot isostatic pressing
It is able to achieve, this purpose for reducing cost with powder metallurgy is runed counter to.Using element powders as the complex element powder metallurgical technique of raw material
Powder metallurgy titanium alloy is prepared using the forming and reaction-sintered of element powders, does not need to carry out alloy melting process, it can be very big
Low-alloyed preparation cost drops to degree.But there are more hole in the titanium alloy of complex element powder metallurgy process preparation,
The mechanical property of alloy is seriously affected, to reduce the use value of alloy.In conclusion traditional ingot metallurgy technique
Prepare that titanium alloy is had excellent performance but higher cost, powder metallurgical technique have the potentiality that preparation cost of titanium alloy is greatly lowered,
But current technique still can not achieve the combination of high-performance and low cost.
Compared to hot extrusion, isothermal forging, hot rolling can significantly reduce energy consumption, reduce production cost, powder hot rolling is added
Work technique is applied to the molding processing cost that alloy can be significantly reduced in the process of powder metallurgy titanium alloy, fine and close improving alloy
It can also play the role of refining crystal grain while spending.In addition, protium is widely used in titanium powder field of metallurgy, including powder
Prepare, be sintered, setting hydrogen processing etc..Some researches show that protium can be improved atom diffusivity, improve titanium alloy high-temperature
Deformability has significant help to the closing of pores in powder metallurgy titanium alloy thermal deformation process.In addition, hydrogen can also pinning crystal boundary, thus
Refine crystal grain.Therefore titanium hydride powders, hydrogen sintering are combined with setting hydrogen hot rolling, can obtains that even tissue is tiny, cause
The high powder metallurgy titanium alloy with excellent mechanical performances of density.
Summary of the invention
The present invention designs in view of the deficiencies of the prior art to be provided a kind of powder rolling and prepares high-compactness Fine Grain Ti Alloy
Method, the purpose is to prepare high-densit titanium alloy using simple process using titantium hydride as primary raw material.This method technique letter
Single, at low cost, product mechanical property is excellent, applied widely.
The purpose of the present invention is achieved through the following technical solutions:
The method that this kind of powder rolling prepares high-compactness Fine Grain Ti Alloy includes with titantium hydride and corresponding intermediate alloy
Powder is raw material, prepares powder compact by isostatic cool pressing, it is characterised in that: this method comprises:
It is sintered using hydrogen/argon gas mixed atmosphere, prepares hydrogeneous titanium alloy powder sintered blank；
Hot rolling is carried out to hydrogeneous titanium alloy powder sintered blank, then to the sheet alloy or bar progress Vacuum Heat after rolling
Processing, obtains the titanium alloy plate or pieces of bar stock of dehydrogenation.
Further, the technological parameter hydrogeneous titanium alloy powder being sintered are as follows: sintering temperature is 1000~1450 DEG C,
Soaking time is 1~4h, and hydrogen volume score is 10~100% in atmosphere, remaining is argon gas, heating rate is 3~20 DEG C/
min。
Further, titantium hydride and corresponding intermediate alloy powder granularity are 100~500 mesh.
Further, the pressure of the isostatic cool pressing is 150~400MPa.
Further, the rolling temperature of the hot rolling is lower than 10~100 DEG C of transformation temperature, and total deformation is greater than 50%.Often
Passes deflection is 10~30%.
Further, the vacuum degree in the vacuum heat treatment process is≤0.1Pa.
In a kind of implementation, obtained titanium alloy is TC4, wherein joining to the technique that hydrogeneous alloy powder is sintered
Number are as follows: sintering temperature is 1250 DEG C, and heating rate is 10 DEG C/min, keeps the temperature furnace cooling after 4h, hydrogen volume in mixed atmosphere
Score is 30%；
Sintered blank is rolled at 950 DEG C, rolling reduction is 20% per pass, carries out 7 passes, total deformation
It is 80%.
In a kind of implementation, obtained titanium alloy is TB6, wherein joining to the technique that hydrogeneous alloy powder is sintered
Number are as follows: sintering temperature is 1150 DEG C, and heating rate is 5 DEG C/min, keeps the temperature furnace cooling after 2h, hydrogen integral in mixed atmosphere
Number is 50%；
Sintered blank is rolled at 750 DEG C, rolling reduction is 15% per pass, carries out 6 passes, total deformation
It is 62%.
The characteristics of technical solution of the present invention and its innovation effect are:
Innovation of the invention is to participate in protium overall process into titanium alloy powder sintering and powder rolling.And at present about
Influence of the protium to the research of powder metallurgy titanium alloy mainly for protium in sintering process to sintered density and tissue modulation,
And it is not clear to the affecting laws of powder metallurgy titanium alloy densification and crystal grain refinement during powder rolling to protium.For this purpose,
Technical solution of the present invention proposes a kind of titanium for improving titanium alloy densification degree and reducing crystallite dimension by in-depth study
The preparation method of alloy is described as follows this method feature:
First, in the method for the present invention, protium participates in sintering and rolling overall process, using protium to powder in the operation of rolling
The facilitation of last titanium alloy densification and crystal grain refinement promotes powder rolling titanium alloy performance and raising rolling efficiency to realize
Reduce the purpose of cost.
Protium has very important influence to the final performance of powder rolling titanium alloy as interim alloying element, because
This is very crucial to the control of protium, and the method for the present invention is established on a large amount of, systematic research basis.It is logical
It crosses the study found that the variation of hydrogen ratio can all cause the variation of protium content in alloy in sintering temperature and atmosphere, thus
The generation of the subsequent operation of rolling is seriously affected.For example, protium caused by density of hydrogen improves in sintering temperature variation, atmosphere
Content improves, and can promote the raising of alloy plastic deformation's ability, promote the densification of alloy, rolling pass be reduced, to contract
Short processes process, reduces cost；But it may cause alloy in sintering process simultaneously to crack.Opposite, protium content reduces again
The effect that protium refines sintering process alloy grain can be weakened, and densification and crystal grain refinement production to operation of rolling alloy
Raw adverse effect.Therefore, in the method for the present invention, for the titanium alloy of heterogeneity, corresponding sintering process parameter has been formulated, has been wrapped
Sintering temperature, density of hydrogen, type of cooling etc. are included, protium content in sintered blank is precisely controlled with realizing, thus effectively
Ground plays hydrogen to the facilitation of densification and crystal grain refinement in the powder metallurgy titanium alloy operation of rolling；
Second, sintering and rolling mill practice are tight associations to the densification of alloy and crystal grain refinement.For example, sintering temperature
It improves, causes the consistency of sintered blank to improve, but will lead to the increase of crystallite dimension simultaneously.Therefore in subsequent rolling process mistake
Cheng Zhong provides bigger deflection to guarantee that crystal grain sufficiently refines needs.Opposite, sintering temperature reduces, consistency decline, but
Crystallite dimension is lower.It is the full densification for guaranteeing realization powder metallurgy in the subsequent operation of rolling, also needs using biggish
Deflection or higher rolling temperature.Therefore, in the method for the present invention, it is contemplated that the pass between rolling mill practice and sintering process parameter
Connection property, has formulated the rolling mill practice to match on the basis of sintering process.
Third, it is cost effective.Powder rolling titanium alloy can prepare the conjunction of high-performance powder titanium compared to Powder hot isostatic pressure etc.
The technique of gold, the requirement to raw material powder and process equipment is lower, therefore the method for the present invention has the characteristic of low cost.But pass through
The powder metallurgy titanium alloy for the method preparation that the invention provides can have and the quite even superior performance of Powder hot isostatic pressure.
Detailed description of the invention
Fig. 1 is the process flow diagram of the method for the present invention
Fig. 2 is the microstructure picture after the TC4 alloy sintering in embodiment 1
Fig. 3 is the microstructure picture after the TC4 alloy vacuum annealing in embodiment 1
Specific embodiment
Technical solution of the present invention is further described below with reference to drawings and examples:
Embodiment 1
For preparing TC4 alloy, referring to attached drawing 1, the process of preparation method are as follows: with granularity be -500 mesh titantium hydride,
Al-V40 intermediate alloy powder is raw material, is matched according to weight ratio 9:1, and 12h mixing is carried out on V-type batch mixer.To mixed
After conjunction powder is packaged, isostatic cool pressing is carried out under the pressure of 250MPa and obtains powder compact.Atmosphere is carried out to powder compact
Sintering, wherein sintering temperature is 1250 DEG C, and heating rate is 10 DEG C/min, keeps the temperature furnace cooling after 4h, and entire sintering process is burnt
The mixed gas that atmosphere is hydrogen and argon gas is tied, wherein hydrogen volume score is 30%, the microscopic structure of sintered alloy such as Fig. 2 institute
Show.Sintered alloy is rolled at 950 DEG C, rolling reduction is about 20% per pass, carries out 7 passes, total deformation
It is 80%.To furnace cooling after 950 DEG C of deformed alloy progress, 1h vacuum heat treatment, alloy structure after cooling such as Fig. 3 institute
Show.
It can be seen that the TC4 titanium alloy consistency prepared by the method for the invention reaches 100% from Fig. 2,3, and have
There is the characteristics of tiny crystal grain, even tissue.
Embodiment 2
For preparing TB6 alloy, referring to attached drawing 1, the process of preparation method are as follows: with granularity be -500 mesh titantium hydride, -
500 mesh Fe-V-Al, -300 mesh Al-V intermediate alloy powder are raw material, according to the ingredient of Ti-10V-2Fe-3Al (wt.%) alloy
It is matched, 12h mixing is carried out on V-type batch mixer.After being packaged to mixed-powder, carried out under the pressure of 200MPa cold
Equal static pressure obtain powder compact.To powder compact carry out atmosphere sintering, wherein sintering temperature be 1150 DEG C, heating rate be 5 DEG C/
Min keeps the temperature furnace cooling after 2h, and entire sintering process sintering atmosphere is the mixed gas of hydrogen and argon gas, wherein hydrogen volume
Score is 50%.To sintered alloy in 750 DEG C of progress hot rollings, deflection is 15% per pass, carries out 6 passes, total to become
Shape amount is 62%.740 DEG C, water cooling after 1h vacuum heat treatment are carried out to the alloy after hot rolling, using 510 DEG C, 6h ageing treatment,
Obtain the tiny TB6 alloy of even tissue.
Claims (9)
1. a kind of method that powder rolling prepares high-compactness Fine Grain Ti Alloy, this method includes with titantium hydride and intermediate accordingly
Alloy powder is raw material, prepares powder compact by isostatic cool pressing, it is characterised in that: this method comprises:
It is sintered using hydrogen/argon gas mixed atmosphere, prepares hydrogeneous titanium alloy powder sintered blank；
To hydrogeneous titanium alloy powder sintered blank carry out hot rolling, then to after rolling sheet alloy or bar carry out Vacuum Heat at
Reason, obtains the titanium alloy plate or pieces of bar stock of dehydrogenation.
2. the method that powder rolling according to claim 1 prepares high-compactness Fine Grain Ti Alloy, it is characterised in that: to containing
The technological parameter that the titanium alloy powder of hydrogen is sintered are as follows: sintering temperature is 1000~1450 DEG C, and soaking time is 1~4h, gas
Hydrogen volume score is 10~100% in atmosphere, remaining is argon gas, and heating rate is 3~20 DEG C/min.
3. the method that powder rolling according to claim 1 prepares high-compactness Fine Grain Ti Alloy, it is characterised in that: hydrogenation
Titanium and corresponding intermediate alloy powder granularity are 100~500 mesh.
4. the method that powder rolling according to claim 1 prepares high-compactness Fine Grain Ti Alloy, it is characterised in that: described
The pressure of isostatic cool pressing is 150~400MPa.
5. the method that powder rolling according to claim 1 prepares high-compactness Fine Grain Ti Alloy, it is characterised in that: described
The rolling temperature of hot rolling is lower than 10~100 DEG C of transformation temperature, and total deformation is greater than 50%.
6. the method that powder rolling prepares high-compactness Fine Grain Ti Alloy according to claim 1 or 5, it is characterised in that:
Rolling reduction per pass during the hot rolling is 10~30%.
7. the method that powder rolling according to claim 1 prepares high-compactness Fine Grain Ti Alloy, it is characterised in that: described
Vacuum degree in vacuum heat treatment process is≤0.1Pa.
8. the method that powder rolling according to claim 1 prepares high-compactness Fine Grain Ti Alloy, it is characterised in that: gained
The titanium alloy arrived is TC4, wherein the technological parameter being sintered to hydrogeneous alloy powder are as follows: sintering temperature is 1250 DEG C, is risen
Warm rate is 10 DEG C/min, keeps the temperature furnace cooling after 4h, and hydrogen volume score is 30% in mixed atmosphere；
Sintered blank is rolled at 950 DEG C, rolling reduction is 20% per pass, carries out 7 passes, and total deformation is
80%.
9. the method that powder rolling according to claim 1 prepares high-compactness Fine Grain Ti Alloy, it is characterised in that: gained
The titanium alloy arrived is TB6, wherein the technological parameter being sintered to hydrogeneous alloy powder are as follows: sintering temperature is 1150 DEG C, is risen
Warm rate is 5 DEG C/min, keeps the temperature furnace cooling after 2h, and hydrogen volume score is 50% in mixed atmosphere；
Sintered blank is rolled at 750 DEG C, rolling reduction is 15% per pass, carries out 6 passes, and total deformation is
62%.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113278901A (en) * | 2021-05-01 | 2021-08-20 | 上海交通大学 | Multi-cycle hydrogen-placing treatment method for grain refinement of titanium alloy plate |
| CN114082951A (en) * | 2021-11-29 | 2022-02-25 | 太原理工大学 | Strong-plasticity matched titanium alloy composite material and preparation method thereof |
| CN114433859A (en) * | 2022-01-25 | 2022-05-06 | 华中科技大学 | High-quality electrode for titanium alloy powder, and preparation and application thereof |
| CN114672682A (en) * | 2022-02-23 | 2022-06-28 | 北京科技大学 | High-performance powder metallurgy titanium alloy part and preparation method thereof |
| CN114985740A (en) * | 2022-05-06 | 2022-09-02 | 北京科技大学 | Large-deformation titanium-aluminum alloy plate and short-process rolling preparation method thereof |
| CN115475946A (en) * | 2022-08-26 | 2022-12-16 | 贵州航宇科技发展股份有限公司 | Ti 2 Roll forming and heat treatment method of AlNb powder metallurgy ring piece |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113278901A (en) * | 2021-05-01 | 2021-08-20 | 上海交通大学 | Multi-cycle hydrogen-placing treatment method for grain refinement of titanium alloy plate |
| CN114082951A (en) * | 2021-11-29 | 2022-02-25 | 太原理工大学 | Strong-plasticity matched titanium alloy composite material and preparation method thereof |
| CN114082951B (en) * | 2021-11-29 | 2023-09-05 | 太原理工大学 | Strong-plasticity matched titanium alloy composite material and preparation method thereof |
| CN114433859A (en) * | 2022-01-25 | 2022-05-06 | 华中科技大学 | High-quality electrode for titanium alloy powder, and preparation and application thereof |
| CN114433859B (en) * | 2022-01-25 | 2023-02-14 | 华中科技大学 | High-quality electrode for titanium alloy powder, and preparation and application thereof |
| CN114672682A (en) * | 2022-02-23 | 2022-06-28 | 北京科技大学 | High-performance powder metallurgy titanium alloy part and preparation method thereof |
| CN114985740A (en) * | 2022-05-06 | 2022-09-02 | 北京科技大学 | Large-deformation titanium-aluminum alloy plate and short-process rolling preparation method thereof |
| CN115475946A (en) * | 2022-08-26 | 2022-12-16 | 贵州航宇科技发展股份有限公司 | Ti 2 Roll forming and heat treatment method of AlNb powder metallurgy ring piece |
| CN115475946B (en) * | 2022-08-26 | 2024-04-02 | 贵州航宇科技发展股份有限公司 | Ti (titanium) 2 Rolling forming and heat treatment method for AlNb powder metallurgy ring piece |
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Application publication date: 20190917 |