CN102641890A - Preparation method of powder metallurgy superfine crystal titanium aluminum base alloy panel - Google Patents

Preparation method of powder metallurgy superfine crystal titanium aluminum base alloy panel Download PDF

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CN102641890A
CN102641890A CN2012101312069A CN201210131206A CN102641890A CN 102641890 A CN102641890 A CN 102641890A CN 2012101312069 A CN2012101312069 A CN 2012101312069A CN 201210131206 A CN201210131206 A CN 201210131206A CN 102641890 A CN102641890 A CN 102641890A
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base alloy
rolling
aluminium base
titanium aluminium
powder metallurgy
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CN102641890B (en
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刘咏
梁霄鹏
李慧中
黄岚
黄伯云
曾敏
李建波
周灿旭
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Central South University
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Abstract

Provided is a preparation method of a powder metallurgy superfine crystal titanium aluminum base alloy panel. Alloy components, by atomic percent, are Ti-(46-48) AI-(1-3) Cr-(2-3) Nb-(0.1-0.3) W. The preparation method is (1) preparing ingot blanks by using a method that hot isostatic pressure is carried out on alloyed powder; (2) cutting the blanks to be rolled from the hot isostatic pressure ingot blanks and conducting wrapping anti-oxidation treatment; (3) enabling the blanks obtained in the step (2) to stay at even temperature of 1150-1250 DEG C, rolling on a common two-roller reversible hot mill, adopting rapid rolling and gate large deformation methods to achieve high strain rate deformation during rolling, and stopping rolling when total deformation amount is larger than 85%; and (4) enabling the panel to be annealed at the temperature of 850-900 DEG C for 3-5 hours after completion of the rolling and then conducting air cooling. The preparation method achieves a purpose for preparing superfine crystal titanium aluminum base alloy, enables grain size to be as small as two orders of magnitudes compared with the existing rolling panel, and achieves the nanocrystalline size of 200-300nm. Simultaneously, the preparation method has the advantages of being simple in process, low in requirement for rolling equipment, short in rolling cycle and high in production efficiency.

Description

The ultra-fine brilliant titanium aluminium base alloy preparation of plates method of a kind of powder metallurgy
Technical field
The present invention relates to ultra-fine brilliant titanium aluminium base alloy preparation of plates method, speciality is the ultra-fine brilliant titanium aluminium base alloy preparation of plates method of a kind of powder metallurgy; Belong to the powdered metallurgical material processing technique field.
Background technology
The titanium aluminium base alloy specific strength is high, specific stiffness is high, density is low, fire resistance and high-temperature oxidation resistant, creep-resistant property are good, is a kind of very potential lightweight high-temperature structural material, at industrial circles such as Aero-Space, automobile makings wide application prospect is arranged.Titanium aluminium base alloy sheet material is except can directly being used as the structural material; Can also be as the preform material of superplasticforming; And be used for near-net-shape Aeronautics and Astronautics engine zero, the wing, housing, the hot-zone covering of parts and super speed vehicle, turbo blade, missile tail etc.Yet titanium aluminium base alloy is more crisp, belongs to difficult-to-deformation material, and all very difficulty, the especially rolling deformation of sheet material are difficult especially for room temperature and high temperature process distortion.
3 conditions have just been summed up as far back as nineteen ninety-five Koeppe: 1. be similar to the rolling of isothermal at high temperature α+γ phase region with casting metallurgical prepared TiAl base latten; 2. strict controlled rolling technological parameter (mill speed and reduction in pass); 3. take the necessary measures and prevent that TiAl base alloy is oxidized in deformation process.(Koeppe?C,Bartels?A,Clement?H,et?al.Optimizing?Properties?of?TiAl?Sheet?Material?for?Application?in?Heat?Protection?Shields?or?Propulsion?Systems.Materials?Science?and?Engineering?A,1995,201:182~193.)。Thereafter for over ten years; No matter adopting the ingot metallurgy method still is that powder metallurgic method prepares titanium aluminium base alloy sheet material; Its technology guiding theory all is to carry out design technology according to the condition that Koeppe provides; Aspect the nearly ausrolling of realization, developed the roll that can be heated to 1100 ℃ and realized ausrolling; At the controlled rolling process aspect, all adopt low speed at present, depress the rolling mill practice of multi-pass less, just adopt the low mill speed of trying one's best, it is rolling that less pass deformation carries out multi-pass; Aspect anti-oxidation, adopt jacket and the anti-oxidation method of painting to realize.In these 3 conditions, realize ausrolling, higher to equipment requirements, need special material preparation roll; Therefore, can realize ausrolling mechanism seldom, aspect anti-oxidation, technology is simple; Do not had technical barrier, and at the controlled rolling process aspect, low speed is depressed the deformation condition that is reflected less and is the low strain rate distortion, in reporting at present; No matter be numerical simulation, physical analogy or experimental verification, its strain rate that is embodied as the rolling time control of merit is all less than 1s -1Scope in since when strain rate less than 0.1s -1The time, deformation velocity is too slow, is not suitable for actual rollingly, therefore thinks that strain rate is at 0.1s -1To 1s -1Scope be proper machining area.Even if but 1s -1Strain rate distortion, be 10% to calculate to time deflection, make total deformation reach 80% needs about 20 passages, considers temperature retention time between passage again, the rolling time of a rolling sheet material was at least 2.5 hours, it is thus clear that rolling efficiency is very low.Rolling pass is many simultaneously; Temperature retention time between passage is also long; The result who causes is that the little crystal grain of crystallization again that the insulation between passage makes the operation of rolling produce is grown up; So the crystallite dimension of the titanium aluminium base alloy rolled plate that document is reported is basically more than 50 μ m, even can make grain size reach not easy about 10 μ m through the special thermal treatment in later stage.Yet grain size has significant effects to alloy mechanical property, and crystal grain is more little, and the intensity of alloy and percentage elongation are also just high more.Thereby preparation fine grained texture is an important channel of realizing the high-performance titanium aluminium base alloy.
Summary of the invention
The objective of the invention is to overcome the deficiency of prior art and provide a kind of technology simple, the rolling cycle is short, and production efficiency is high, and the rolling sheet deformation that obtains is even, the ultra-fine brilliant titanium aluminium base alloy preparation of plates method of the powder metallurgy that crystallite dimension is little.
The ultra-fine brilliant titanium aluminium base alloy preparation of plates method of a kind of powder metallurgy of the present invention comprises the steps:
The first step: high temperature insostatic pressing (HIP) prepares the titanium aluminium base alloy ingot blank
According to the titanium aluminium base alloy constituent atoms percentage of design, get each component metals powder respectively, the metal dust granularity is 80~100 orders, is shaped as sphere; With the metal dust mild steel jacket of packing into, carry out high temperature insostatic pressing (HIP) in 1235~1265 ℃, the preparation density is more than or equal to 98%, and oxygen content is smaller or equal to the titanium aluminium base alloy ingot blank of 1000ppm;
Second step: intercepting is equipped with rolling stock
The titanium aluminium base alloy ingot blank that obtains from the first step cuts rolling stock fully, adopts pure titanium plate to coat and is equipped with rolling stock, and welded behind the anti-oxidation glass coating of pure titanium plate surface-coated, is rolled fully;
The 3rd step: rolling
After gained was equipped with rolling stock and was heated to 1200~1250 ℃ of sammings second step, it was rolling to carry out multi-pass, and rolling total deformation is 85%~90%; Control passage finishing temperature is more than or equal to 1100 ℃, after every time is rolling, melts down that to carry out next passage behind samming to 1200~1250 ℃ rolling, makes powder metallurgy titanium aluminium base alloy sheet material; When being equipped with the rolling stock total deformation smaller or equal to 35% the time, the roll linear velocity is 1~2m/min, and pass deformation is 8~10%; When the rolling stock total deformation was 35%~90% fully, the roll linear velocity was 20~30m/min, and pass deformation is 50~60%;
The 4th step: annealing
The powder metallurgy titanium aluminium base alloy sheet material that the 3rd step was obtained was heated to 850~900 ℃ of insulation annealings after 3~5 hours, and the air cooling of coming out of the stove obtains the ultra-fine brilliant titanium aluminium base alloy sheet material of powder metallurgy.
The ultra-fine brilliant titanium aluminium base alloy preparation of plates method of a kind of powder metallurgy of the present invention, in the first step, said titanium aluminium base alloy constituent atoms percentage is: Al:46~48, Cr:1~3, Nb:2~3, W:0.1~0.3, all the other are Ti.
The ultra-fine brilliant titanium aluminium base alloy preparation of plates method of a kind of powder metallurgy of the present invention, in the first step, said metal dust is to adopt the rotation electrode atomization to produce.
The ultra-fine brilliant titanium aluminium base alloy preparation of plates method of a kind of powder metallurgy of the present invention, in the first step, the pressure of said high temperature insostatic pressing (HIP) is 130 ± 10MPa MPa, 3~6 hours high temperature insostatic pressing (HIP) time.
The ultra-fine brilliant titanium aluminium base alloy preparation of plates method of a kind of powder metallurgy of the present invention, in second step, said rolling stock width fully is 100~150mm, length is 80~100mm, thickness 10 ± 1mm; Coating the pure titanium plate thickness that is equipped with rolling stock is to be equipped with 10%~15% of rolling stock thickness.
The ultra-fine brilliant titanium aluminium base alloy preparation of plates method of a kind of powder metallurgy of the present invention, in second step, said anti-oxidation glass coating comprises following compositions in weight percentage composition:
SiO 2 80%,
Na 2O 12%,
CaO 8%。
The ultra-fine brilliant titanium aluminium base alloy preparation of plates method of a kind of powder metallurgy of the present invention, in the 3rd step, said rollingly on two roller reversible hot milling rolls, carry out.
The ultra-fine brilliant titanium aluminium base alloy preparation of plates method of a kind of powder metallurgy of the present invention in the 3rd step, when being equipped with the rolling stock total deformation smaller or equal to 35% the time, adopts the low strain rate rolling deformation, and its strain rate is less than 0.2s -1
The ultra-fine brilliant titanium aluminium base alloy preparation of plates method of a kind of powder metallurgy of the present invention in the 3rd step, reaches after 35% when being equipped with the rolling stock total deformation, adopts the high strain rate rolling deformation, and its strain rate is 30~50s -1
The ultra-fine brilliant titanium aluminium base alloy preparation of plates method of a kind of powder metallurgy of the present invention, the ultra-fine brilliant titanium aluminium base alloy sheet material grain size of the powder metallurgy of preparation is 200~300nm.
The present invention is owing to adopting above-mentioned process, according to the attribute of titanium aluminium base alloy itself and the principle of plastic working, promptly when the pyroplastic deformability of titanium aluminium base alloy occurs to a certain degree; Continuation is during to its thermal deformation; Dynamic recrystallization takes place easily in alloy in plastic history, and dynamic recrystallization crystal grain has plasticity preferably, at first adopts first low strain rate distortion; Make alloy that plastic deformation to a certain degree take place; Adopt the high strain rate distortion then, the small grains that the dynamic recrystallization generation takes place when utilizing the high strain rate distortion is impelled the performance of its plasticity, and realizes good mouldability.Compare with other milling methods, the titanium aluminium base alloy sheet material of this method preparation not only crystallite dimension significantly reduces (200~300nm), and the operation of rolling only needs to have significantly improved production efficiency about about 7 passages (30~40 minutes).
In sum, technology of the present invention is simple, and the rolling cycle is short; Production efficiency is high, and the rolling sheet deformation that obtains is even, and crystallite dimension is little; Not only solved the difficult problem that titanium aluminium base alloy is difficult to prepare through rolling deformation sheet material, realized preparing the purpose of ultra-fine brilliant titanium aluminium base alloy simultaneously, its crystallite dimension is crystal grain little at least two one magnitude of rolled plate at present; Reach the nanocrystalline size of 200~300nm, low to the rolling equipment requirement, be suitable for large-scale production.
Description of drawings
Accompanying drawing 1 is the macro morphology behind the alloy rolling of embodiment 1.
Accompanying drawing 2 is the projection Electronic Speculum microscopic structure behind the alloy rolling of embodiment 1, and the crystallite dimension of its alloy is 200~300nm
The specific embodiment
Embodiment 1
Adopt the rotation electrode atomization to produce key component (at.%) and be Al:47.5, Cr:2, Nb:2; W:0.2, all the other are the spherical alloy powder of Ti, its powder size is 80~100 orders; The powder mild steel of packing into is fit over 1250 ± 15 ℃; 130 ± 10MPa carries out high temperature insostatic pressing (HIP) and produced ingot blank in 4 hours, and its ingot blank density is greater than 98%, and oxygen content is less than 1000ppm.Cutting width from the high temperature insostatic pressing (HIP) ingot blank is 120mm, and length is 100mm, the ingot blank of thickness 10mm, and adopt pure titanium plate to coat six faces of blank; And the welding slit, its titanium plate thickness is the 1mm of ingot blank thickness, then at the anti-oxidation glass coating of pure titanium plate surface-coated; With the blank that coats protective coating through 1250 ± 10 ℃ the insulation 1 hour after, rolling on the common two roller reversible hot milling rolls of Φ 500 * 600mm, the rolling mill speed of preceding 5 passages is 1.5m/min; Reduction in pass is 10%, the five after this accomplishes, to melt down insulation 5min, and mill speed is adjusted to 30m/min; Drafts is that 60% to carry out the 6th passage rolling, and loop insulation thereafter was 30m/min according to mill speed after five minutes; Drafts is that 50% to carry out the 7th passage rolling, after putting into 900 ℃ electric furnace then and annealing 3~5 hours, and air cooling.Obtaining thickness is the titanium aluminium base alloy sheet material of 1.2mm, and its total deformation is 88%.
Embodiment 2
Adopt the rotation electrode atomization to produce key component (at.%) and be Al:47.5, Cr:2, Nb:2; W:0.2, all the other are the spherical alloy powder of Ti, its powder size is 80~100 orders; The powder mild steel of packing into is fit over 1250 ± 15 ℃; 130 ± 10MPa carries out high temperature insostatic pressing (HIP) and produced ingot blank in 4 hours, and its ingot blank density is greater than 98%, and oxygen content is less than 1000ppm.Cutting width from the high temperature insostatic pressing (HIP) ingot blank is 120mm, and length is 100mm, the ingot blank of thickness 10mm, and adopt pure titanium plate to coat six faces of blank; And the welding slit, its titanium plate thickness is the 1mm of ingot blank thickness, then at the anti-oxidation glass coating of pure titanium plate surface-coated; With the blank that coats protective coating through 1250 ± 10 ℃ the insulation 1 hour after, rolling on the common two roller reversible hot milling rolls of Φ 500 * 600mm, the rolling mill speed of preceding 4 passages is 2m/min; Reduction in pass is 8%, the five after this accomplishes, to melt down insulation 5min, and mill speed is adjusted to 25m/min; Drafts is that 50% to carry out the 6th passage rolling, and loop insulation thereafter was 20m/min according to mill speed after five minutes; Drafts is that 60% to carry out the 7th passage rolling, after putting into 900 ℃ electric furnace then and annealing 3~5 hours, and air cooling.Obtaining thickness is the titanium aluminium base alloy sheet material of 1.3mm, and its total deformation is 87%.
Embodiment 3
Adopt the rotation electrode atomization to produce key component (at.%) and be Al:47.5, Cr:2, Nb:2; W:0.2, all the other are the spherical alloy powder of Ti, its powder size is 80~100 orders; The powder mild steel of packing into is fit over 1250 ± 15 ℃; 130 ± 10MPa carries out high temperature insostatic pressing (HIP) and produced ingot blank in 4 hours, and its ingot blank density is greater than 98%, and oxygen content is less than 1000ppm.Cutting width from the high temperature insostatic pressing (HIP) ingot blank is 120mm, and length is 100mm, the ingot blank of thickness 10mm, and adopt pure titanium plate to coat six faces of blank; And the welding slit, its titanium plate thickness is the 1mm of ingot blank thickness, then at the anti-oxidation glass coating of pure titanium plate surface-coated; With the blank that coats protective coating through 1250 ± 10 ℃ the insulation 1 hour after, rolling on the common two roller reversible hot milling rolls of Φ 500 * 600mm, the rolling mill speed of preceding 4 passages is 2m/min; Reduction in pass is 10%, the five after this accomplishes, to melt down insulation 5min, and mill speed is adjusted to 25m/min; Drafts is that 60% to carry out the 6th passage rolling, and loop insulation thereafter was 30m/min according to mill speed after five minutes; Drafts is that 60% to carry out the 7th passage rolling, after putting into 900 ℃ electric furnace then and annealing 3~5 hours, and air cooling.Obtaining thickness is the titanium aluminium base alloy sheet material of 1.0mm, and its total deformation is 90%.

Claims (10)

1. the ultra-fine brilliant titanium aluminium base alloy preparation of plates method of powder metallurgy comprises the steps:
The first step: high temperature insostatic pressing (HIP) prepares the titanium aluminium base alloy ingot blank
According to the titanium aluminium base alloy constituent atoms percentage of design, get each component metals powder respectively, the metal dust granularity is 80~100 orders, is shaped as sphere; With the metal dust mild steel jacket of packing into, carry out high temperature insostatic pressing (HIP) in 1235~1265 ℃, the preparation density is more than or equal to 98%, and oxygen content is smaller or equal to the titanium aluminium base alloy ingot blank of 1000ppm;
Second step: intercepting is equipped with rolling stock
The titanium aluminium base alloy ingot blank that obtains from the first step cuts rolling stock fully, adopts pure titanium plate to coat and is equipped with rolling stock, and welded behind the anti-oxidation glass coating of pure titanium plate surface-coated, is rolled fully;
The 3rd step: rolling
After gained was equipped with rolling stock and was heated to 1200~1250 ℃ of sammings second step, it was rolling to carry out multi-pass, and rolling total deformation is 85%~90%; Control passage finishing temperature is more than or equal to 1100 ℃, after every time is rolling, melts down that to carry out next passage behind samming to 1200~1250 ℃ rolling, makes powder metallurgy titanium aluminium base alloy sheet material; When being equipped with the rolling stock total deformation smaller or equal to 35% the time, the roll linear velocity is 1~2m/min, and pass deformation is 8~10%; When the rolling stock total deformation was 35%~90% fully, the roll linear velocity was 20~30m/min, and pass deformation is 50~60%;
The 4th step: annealing
The powder metallurgy titanium aluminium base alloy sheet material that the 3rd step was obtained was heated to 850~900 ℃ of insulation annealings after 3~5 hours, and the air cooling of coming out of the stove obtains the ultra-fine brilliant titanium aluminium base alloy sheet material of powder metallurgy.
2. the ultra-fine brilliant titanium aluminium base alloy preparation of plates method of a kind of powder metallurgy according to claim 1 is characterized in that: in the first step, said titanium aluminium base alloy constituent atoms percentage is: Al:46~48; Cr:1~3; Nb:2~3, W:0.1~0.3, all the other are Ti.
3. the ultra-fine brilliant titanium aluminium base alloy preparation of plates method of a kind of powder metallurgy according to claim 23 is characterized in that: in the first step, said metal dust is to adopt the rotation electrode atomization to produce.
4. the ultra-fine brilliant titanium aluminium base alloy preparation of plates method of a kind of powder metallurgy according to claim 3, it is characterized in that: in the first step, the pressure of said high temperature insostatic pressing (HIP) is 130 ± 10MPa MPa, 3~6 hours high temperature insostatic pressing (HIP) time.
5. the ultra-fine brilliant titanium aluminium base alloy preparation of plates method of a kind of powder metallurgy according to claim 4 is characterized in that: in second step, said rolling stock width fully is 100~150mm, and length is 80~100mm, thickness 10 ± 1mm; Coating the pure titanium plate thickness that is equipped with rolling stock is to be equipped with 10%~15% of rolling stock thickness.
6. the ultra-fine brilliant titanium aluminium base alloy preparation of plates method of a kind of powder metallurgy according to claim 5 is characterized in that: in second step, said anti-oxidation glass coating comprises following compositions in weight percentage composition:
SiO 2 80%,
Na 2O 12%,
CaO 8%。
7. the ultra-fine brilliant titanium aluminium base alloy preparation of plates method of a kind of powder metallurgy according to claim 6 is characterized in that: in the 3rd step, and said rollingly on two roller reversible hot milling rolls, carry out.
8. the ultra-fine brilliant titanium aluminium base alloy preparation of plates method of a kind of powder metallurgy according to claim 7 is characterized in that: the ultra-fine brilliant titanium aluminium base alloy sheet material grain size of the powder metallurgy of preparation is 200~300nm.
9. the ultra-fine brilliant titanium aluminium base alloy preparation of plates method of a kind of powder metallurgy according to claim 8 is characterized in that: in the 3rd step, when being equipped with the rolling stock total deformation smaller or equal to 35% the time, adopt the low strain rate rolling deformation, its strain rate is less than 0.2s -1
10. the ultra-fine brilliant titanium aluminium base alloy preparation of plates method of a kind of powder metallurgy according to claim 9 is characterized in that: in the 3rd step, reach after 35% when being equipped with the rolling stock total deformation, adopt the high strain rate rolling deformation, its strain rate is 30~50s -1
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CN115074582A (en) * 2022-06-20 2022-09-20 中南大学 Preparation method of hypoeutectic Al-Ce alloy with bimodal grain structure

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CN108097962A (en) * 2017-12-29 2018-06-01 中南大学 A kind of preparation method of Nb toughenings titanium aluminium base alloy composite material
CN115074582A (en) * 2022-06-20 2022-09-20 中南大学 Preparation method of hypoeutectic Al-Ce alloy with bimodal grain structure

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