CN1775975A - Method for preparing Al 203 fiber-reinforced TiAl3 base composite material - Google Patents
Method for preparing Al 203 fiber-reinforced TiAl3 base composite material Download PDFInfo
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- CN1775975A CN1775975A CN 200510096089 CN200510096089A CN1775975A CN 1775975 A CN1775975 A CN 1775975A CN 200510096089 CN200510096089 CN 200510096089 CN 200510096089 A CN200510096089 A CN 200510096089A CN 1775975 A CN1775975 A CN 1775975A
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Abstract
The invention relates to a manufacture method for Al2O3 fiber enhancing TiAl3 basal compounding material that includes the following steps: mixing the Ti powder and Al powder according to the weight ratio of 1:1-4; adding TiO2 and Nb2O5 into the mixture; grinding in the high aluminum ball mill jar using alcohol as medium and filtering through 200 eyes; pressing into massive prefabricated material on unilateralism oil press; sintering the mixture covering on the prefabricated material, and cooling naturally. The invention uses alumino-thermit reaction, saves energy and simplifies working process.
Description
Technical field
The invention belongs to the preparation method of TiAl intermetallic compound composite material, particularly a kind of Al
2O
3Fiber Reinforced Ti Al
3The preparation method of based composites.
Background technology
In numerous intermetallic compounds and superalloy, the TiAl compound is with its room temperature and high temperature specific tenacity (strength/density) height, and antifatigue, resistance of oxidation are strong, and density but claims work much smaller than superalloy.The high-temperature material that has significant advantage as a new generation, more be applicable to and make structural material, engine components or the engine for automobile parts etc. that Aero-Space are used body, and be hopeful significantly lightweight and improve its performance, thereby the extremely concern of new material research application.But, be difficult to machining deformation and the oxidation-resistance deficiency has seriously hindered it more than 800 ℃ practical application because ordered structure of its height makes its room temperature ductility poor.Countries in the world are the deformation modes of Knowing material to the research emphasis of this material at present, grasp the low mechanism of temperature-room type plasticity, find the effective way of strengthening its good high-temperature behavior and improving temperature-room type plasticity.
Adopt alloying, special preparation technology and different methods such as thermal treatment, the performance of this material is had greatly improved, but from its performance mechanical property particularly, simple intermetallic compound can't satisfy the composite request of some special aerospace partses to hot strength, creep resistance and enduring quality, and preparation intermetallic compound based composite material (Intermetallic matrix composites, IMCs) can obtain the good mechanical performance, and keep the low characteristic of matrix density simultaneously.Based on sapphire whisker good high-temperature performance, once had directly to be introduced into the TiAl matrix or fiber is carried out introducing the toughened and reinforced method of matrix again after coating is handled.But in the first method, fiber is in the building-up process of material, and loss of strength is up to 50%; The complex process of second method, cost height.
Summary of the invention
The objective of the invention is to overcome the shortcoming of above-mentioned prior art, provide a kind of can be in TiAl intermetallic compound base body the Al of self-generating alumina fibre
2O
3Fiber Reinforced Ti Al
3The preparation method of based composites.
For achieving the above object, the preparation method that the present invention adopts is: at first with purity greater than 99%, fineness greater than 200 purpose Ti powder and Al powder by Ti: Al=1: 1～4 mass ratio is mixed and made into Ti, Al mixture; In Ti, Al mixture, add then the fineness of Ti, Al mixture quality 8～10% greater than 200 purpose TiO
2Nb with 0-5%
2O
5To be medium fully mixed mixture in 20-50 minute with 800-900 rev/min rotating speed mix grinding to 45～50% absolute ethyl alcohols that add mixture in the high aluminium ball grinding jar and add mixture quality, and cross 200 mesh sieves; Mixture after sieving pressure with 30-50Mpa on unidirectional hydraulic press is pressed into block precast body; Again with graphite: alumina powder is by 1: the mass ratio of 1-3 is made graphite and alumina powder mixed powder; with graphite and alumina powder mixed powder cover be embedded on the precast body or vacuum or under the atmosphere protection condition speed with 3-8 ℃/minute be warming up to 1200-1250 ℃ of sintering; apply the pressure of 30-150Mpa during to maximum temperature and be incubated 0.5-1 hour, rear naturally cooling gets final product.
The present invention utilizes thermit reaction, principle of oxidation and reduction, and in-situ fiber strengthens body in the generative process of material, can not only make material synthetic under lower temperature, save the energy, simplified production technology, and reduced the loss of strength of in-situ fiber in technical process.In-situ fiber has not only reduced the manufacturing cost of fiber, and the fiber that this mode generates possesses clean phase boundary, no foreign matter, pollutes and produces, and makes fiber in TiAl intermetallic compound base body, and better chemical and physical compatibility are arranged.
Description of drawings
Fig. 1 is the Al that makes according to preparation method of the present invention
2O
3 (f)/ TiAl
3The XRD analysis figure of matrix material, wherein ordinate zou is an intensity, is the X-coordinate diffraction angle number of degrees.
Fig. 2 is the sem analysis figure of in-situ fiber,
Fig. 3 is energy dispersive spectrometry (EDS) analysis chart of in-situ fiber, and wherein X-coordinate is an intensity, and ordinate zou is a photon energy.
Embodiment
Below in conjunction with drawings and Examples the present invention is described in further detail.
Embodiment 1: at first with purity greater than 99%, fineness greater than 200 purpose Ti powder and Al powder by Ti: Al=1: 4 mass ratio is mixed and made into Ti, Al mixture; In Ti, Al mixture, add then the fineness of Ti, Al mixture quality 10% greater than 200 purpose TiO
2To be medium fully mixed mixture in 20 minutes with 850 rev/mins rotating speed mix grinding to 45% absolute ethyl alcohol that adds mixture in the high aluminium ball grinding jar and add mixture quality, and cross 200 mesh sieves; Mixture after sieving pressure with 40Mpa on unidirectional hydraulic press is pressed into block precast body; Again with graphite: alumina powder is made graphite and alumina powder mixed powder by 1: 1 mass ratio, graphite and alumina powder mixed powder covered be embedded on the precast body, be warming up to 1250 ℃ of sintering with 8 ℃/minute speed, after applying the pressure of 150Mpa during to 1250 ℃ and being incubated 0.5 hour, cooling gets final product naturally.
Embodiment 2: at first with purity greater than 99%, fineness greater than 200 purpose Ti powder and Al powder by Ti: Al=1: 2 mass ratio is mixed and made into Ti, Al mixture; In Ti, Al mixture, add then the fineness of Ti, Al mixture quality 8% greater than 200 purpose TiO
2With 1% Nb
2O
5To be medium fully mixed mixture in 50 minutes with 820 rev/mins rotating speed mix grinding to 46% absolute ethyl alcohol that adds mixture in the high aluminium ball grinding jar and add mixture quality, and cross 200 mesh sieves; Mixture after sieving pressure with 30Mpa on unidirectional hydraulic press is pressed into block precast body; Again with graphite: alumina powder is made graphite and alumina powder mixed powder by 1: 3 mass ratio, graphite and alumina powder mixed powder covered be embedded on the precast body, be warming up to 1230 ℃ of sintering with 5 ℃/minute speed, after applying the pressure of 120Mpa during to 1230 ℃ and being incubated 0.8 hour, cooling gets final product naturally.
Embodiment 3: at first with purity greater than 99%, fineness greater than 200 purpose Ti powder and Al powder by Ti: Al=1: 3 mass ratio is mixed and made into Ti, Al mixture; In Ti, Al mixture, add then the fineness of Ti, Al mixture quality 9% greater than 200 purpose TiO
2With 2% Nb
2O
5To be medium fully mixed mixture in 40 minutes with 900 rev/mins rotating speed mix grinding to 48% absolute ethyl alcohol that adds mixture in the high aluminium ball grinding jar and add mixture quality, and cross 200 mesh sieves; Mixture after sieving pressure with 50Mpa on unidirectional hydraulic press is pressed into block precast body; Precast body speed with 3 ℃/minute under the vacuum protection condition is warming up to 1220 ℃ of sintering, and after applying the pressure of 30Mpa during to 1220 ℃ and being incubated 1.0 hours, cooling gets final product naturally.
Embodiment 4: at first with purity greater than 99%, fineness greater than 200 purpose Ti powder and Al powder by Ti: Al=1: 1 mass ratio is mixed and made into Ti, Al mixture; In Ti, Al mixture, add then the fineness of Ti, Al mixture quality 8% greater than 200 purpose TiO
2With 5% Nb
2O
5To be medium fully mixed mixture in 35 minutes with 800 rev/mins rotating speed mix grinding to 50% absolute ethyl alcohol that adds mixture in the high aluminium ball grinding jar and add mixture quality, and cross 200 mesh sieves; Mixture after sieving pressure with 38Mpa on unidirectional hydraulic press is pressed into block precast body; Precast body speed with 6 ℃/minute under the vacuum protection condition is warming up to 1240 ℃ of sintering, and after applying the pressure of 100Mpa during to 1240 ℃ and being incubated 0.6 hour, cooling gets final product naturally.
Embodiment 5: at first with purity greater than 99%, fineness greater than 200 purpose Ti powder and Al powder by Ti: Al=1: 3 mass ratio is mixed and made into Ti, Al mixture; In Ti, Al mixture, add then the fineness of Ti, Al mixture quality 10% greater than 200 purpose TiO
2With 3% Nb
2O
5To be medium fully mixed mixture in 28 minutes with 870 rev/mins rotating speed mix grinding to 47% absolute ethyl alcohol that adds mixture in the high aluminium ball grinding jar and add mixture quality, and cross 200 mesh sieves; Mixture after sieving pressure with 47Mpa on unidirectional hydraulic press is pressed into block precast body; Precast body speed with 4 ℃/minute under the atmosphere protection condition is warming up to 1210 ℃ of sintering, and after applying the pressure of 80Mpa during to 1210 ℃ and being incubated 0.9 hour, cooling gets final product naturally.
Embodiment 6: at first with purity greater than 99%, fineness greater than 200 purpose Ti powder and Al powder by Ti: Al=1: 4 mass ratio is mixed and made into Ti, Al mixture; In Ti, Al mixture, add then the fineness of Ti, Al mixture quality 9% greater than 200 purpose TiO
2With 4% Nb
2O
5To be medium fully mixed mixture in 45 minutes with 890 rev/mins rotating speed mix grinding to 49% absolute ethyl alcohol that adds mixture in the high aluminium ball grinding jar and add mixture quality, and cross 200 mesh sieves; Mixture after sieving pressure with 35Mpa on unidirectional hydraulic press is pressed into block precast body; Precast body speed with 7 ℃/minute under the atmosphere protection condition is warming up to 1200 ℃ of sintering, and after applying the pressure of 50Mpa during to 1200 ℃ and being incubated 0.7 hour, cooling gets final product naturally.
Referring to Fig. 1, as seen from the figure, forming Ti: Al at primary raw material is 1: 4 o'clock, and the principal crystalline phase of material is TiAl
3, inferior crystalline phase is NbAl
3, Al
2O
3, because aluminium content is higher in the raw material composition, so have a small amount of Al phase in the material last phase.
Referring to Fig. 2, as seen from Figure 2, fiber surface spontaneous in the material is bright and clean, and length-to-diameter ratio is bigger.
Referring to Fig. 3, analyze demonstration by Fig. 3, the fiber in the material is Al
2O
3Fiber.
The present invention utilizes thermit reaction, principle of oxidation and reduction, and in-situ fiber strengthens body in the generative process of material, can not only make material synthetic under lower temperature, save the energy, simplified production technology, and reduced the loss of strength of in-situ fiber in technical process.
In-situ fiber has not only reduced the manufacturing cost of fiber, and the fiber that this mode generates possesses clean phase boundary, no foreign matter, pollutes and produces, and makes fiber in TiAl intermetallic compound base body, and better chemical and physical compatibility are arranged.
The sapphire whisker of the present invention's self-generating in the titanium aluminum substrate, fiber surface is bright and clean, and length-to-diameter ratio is bigger.When Materials Fracture, the dial-out of fiber, fracture etc., all to consume certain energy, therefore, Materials Fracture performance etc. there is certain improvement.
Claims (7)
1, Al
2O
3Fiber Reinforced Ti Al
3The preparation method of based composites is characterized in that:
1) at first with purity greater than 99%, fineness greater than 200 purpose Ti powder and Al powder by Ti: Al=1: 1～4 mass ratio is mixed and made into Ti, Al mixture;
2) in Ti, Al mixture, add then the fineness of Ti, Al mixture quality 8～10% greater than 200 purpose TiO
2Nb with 0-5%
2O
5
3) to be medium made the mixture thorough mixing in 20-50 minute with 800-900 rev/min rotating speed mix grinding to 45～50% dehydrated alcohols that mixture added in the high alumina ball grinder and add mixture quality, and cross 200 mesh sieves;
4) the mixture pressure with 30-50Mpa on unidirectional oil press after will sieving is pressed into block precast body;
5) again with graphite: aluminum oxide powder is by 1: the mass ratio of 1-3 is made graphite and aluminum oxide powder mixed powder; with graphite and aluminum oxide powder mixed powder cover be embedded on the precast body or vacuum or under the atmosphere protection condition speed with 3-8 ℃/minute be warming up to 1200-1250 ℃ of sintering; apply the pressure of 30-150Mpa during to top temperature and be incubated 0.5-1 hour, back naturally cooling gets final product.
2, Al according to claim 1
2O
3Fiber Reinforced Ti Al
3The preparation method of based composites is characterized in that: at first with purity greater than 99%, fineness greater than 200 purpose Ti powder and Al powder by Ti: Al=1: 4 mass ratio is mixed and made into Ti, Al mixture; In Ti, Al mixture, add then the fineness of Ti, Al mixture quality 10% greater than 200 purpose TiO
2To be medium fully mixed mixture in 20 minutes with 850 rev/mins rotating speed mix grinding to 45% absolute ethyl alcohol that adds mixture in the high aluminium ball grinding jar and add mixture quality, and cross 200 mesh sieves; Mixture after sieving pressure with 40Mpa on unidirectional hydraulic press is pressed into block precast body; Again with graphite: alumina powder is made graphite and alumina powder mixed powder by 1: 1 mass ratio, graphite and alumina powder mixed powder covered be embedded on the precast body, be warming up to 1250 ℃ of sintering with 8 ℃/minute speed, after applying the pressure of 150Mpa during to 1250 ℃ and being incubated 0.5 hour, cooling gets final product naturally.
3, Al according to claim 1
2O
3Fiber Reinforced Ti Al
3The preparation method of based composites is characterized in that: at first with purity greater than 99%, fineness greater than 200 purpose Ti powder and Al powder by Ti: Al=1: 2 mass ratio is mixed and made into Ti, Al mixture; In Ti, Al mixture, add then the fineness of Ti, Al mixture quality 8% greater than 200 purpose TiO
2With 1% Nb
2O
5To be medium fully mixed mixture in 50 minutes with 820 rev/mins rotating speed mix grinding to 46% absolute ethyl alcohol that adds mixture in the high aluminium ball grinding jar and add mixture quality, and cross 200 mesh sieves; Mixture after sieving pressure with 30Mpa on unidirectional hydraulic press is pressed into block precast body; Again with graphite: alumina powder is made graphite and alumina powder mixed powder by 1: 3 mass ratio, graphite and alumina powder mixed powder covered be embedded on the precast body, be warming up to 1230 ℃ of sintering with 5 ℃/minute speed, after applying the pressure of 120Mpa during to 1230 ℃ and being incubated 0.8 hour, cooling gets final product naturally.
4, Al according to claim 1
2O
3Fiber Reinforced Ti Al
3The preparation method of based composites is characterized in that: at first with purity greater than 99%, fineness greater than 200 purpose Ti powder and Al powder by Ti: Al=1: 3 mass ratio is mixed and made into Ti, Al mixture; In Ti, Al mixture, add then the fineness of Ti, Al mixture quality 9% greater than 200 purpose TiO
2With 2% Nb
2O
5To be medium fully mixed mixture in 40 minutes with 900 rev/mins rotating speed mix grinding to 48% absolute ethyl alcohol that adds mixture in the high aluminium ball grinding jar and add mixture quality, and cross 200 mesh sieves; Mixture after sieving pressure with 50Mpa on unidirectional hydraulic press is pressed into block precast body; Precast body speed with 3 ℃/minute under the vacuum protection condition is warming up to 1220 ℃ of sintering, and after applying the pressure of 30Mpa during to 1220 ℃ and being incubated 1.0 hours, cooling gets final product naturally.
5, Al according to claim 1
2O
3Fiber Reinforced Ti Al
3The preparation method of based composites is characterized in that: at first with purity greater than 99%, fineness greater than 200 purpose Ti powder and Al powder by Ti: Al=1: 1 mass ratio is mixed and made into Ti, Al mixture; In Ti, Al mixture, add then the fineness of Ti, Al mixture quality 8% greater than 200 purpose TiO
2With 5% Nb
2O
5To be medium fully mixed mixture in 35 minutes with 800 rev/mins rotating speed mix grinding to 50% absolute ethyl alcohol that adds mixture in the high aluminium ball grinding jar and add mixture quality, and cross 200 mesh sieves; Mixture after sieving pressure with 38Mpa on unidirectional hydraulic press is pressed into block precast body; Precast body speed with 6 ℃/minute under the vacuum protection condition is warming up to 1240 ℃ of sintering, and after applying the pressure of 100Mpa during to 1240 ℃ and being incubated 0.6 hour, cooling gets final product naturally.
6, Al according to claim 1
2O
3Fiber Reinforced Ti Al
3The preparation method of based composites is characterized in that: at first with purity greater than 99%, fineness greater than 200 purpose Ti powder and Al powder by Ti: Al=1: 3 mass ratio is mixed and made into Ti, Al mixture; In Ti, Al mixture, add then the fineness of Ti, Al mixture quality 10% greater than 200 purpose TiO
2With 3% Nb
2O
5To be medium fully mixed mixture in 28 minutes with 870 rev/mins rotating speed mix grinding to 47% absolute ethyl alcohol that adds mixture in the high aluminium ball grinding jar and add mixture quality, and cross 200 mesh sieves; Mixture after sieving pressure with 47Mpa on unidirectional hydraulic press is pressed into block precast body; Precast body speed with 4 ℃/minute under the atmosphere protection condition is warming up to 1210 ℃ of sintering, and after applying the pressure of 80Mpa during to 1210 ℃ and being incubated 0.9 hour, cooling gets final product naturally.
7, Al according to claim 1
2O
3Fiber Reinforced Ti Al
3The preparation method of based composites is characterized in that: at first with purity greater than 99%, fineness greater than 200 purpose Ti powder and Al powder by Ti: Al=1: 4 mass ratio is mixed and made into Ti, Al mixture; In Ti, Al mixture, add then the fineness of Ti, Al mixture quality 9% greater than 200 purpose TiO
2With 4% Nb
2O
5To be medium fully mixed mixture in 45 minutes with 890 rev/mins rotating speed mix grinding to 49% absolute ethyl alcohol that adds mixture in the high aluminium ball grinding jar and add mixture quality, and cross 200 mesh sieves; Mixture after sieving pressure with 35Mpa on unidirectional hydraulic press is pressed into block precast body; Precast body speed with 7 ℃/minute under the atmosphere protection condition is warming up to 1200 ℃ of sintering, and after applying the pressure of 50Mpa during to 1200 ℃ and being incubated 0.7 hour, cooling gets final product naturally.
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|---|---|---|---|
| CNB2005100960897A CN100432254C (en) | 2005-09-29 | 2005-09-29 | Method for preparing Al 203 fiber-reinforced TiAl3 base composite material |
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|---|---|---|---|
| CNB2005100960897A CN100432254C (en) | 2005-09-29 | 2005-09-29 | Method for preparing Al 203 fiber-reinforced TiAl3 base composite material |
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| CN1775975A true CN1775975A (en) | 2006-05-24 |
| CN100432254C CN100432254C (en) | 2008-11-12 |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100463984C (en) * | 2007-01-12 | 2009-02-25 | 西北工业大学 | Preparation method of Titanium Trialuminum radical composite material |
| CN102730730A (en) * | 2012-07-03 | 2012-10-17 | 武汉科技大学 | Submicron Al2O3 fibre and preparation method thereof |
| CN109694971A (en) * | 2019-01-24 | 2019-04-30 | 重庆大学 | A kind of powder metallurgy titanium-aluminium matrix composites and preparation method thereof |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4865666A (en) * | 1987-10-14 | 1989-09-12 | Martin Marietta Corporation | Multicomponent, low density cubic L12 aluminides |
| US4897127A (en) * | 1988-10-03 | 1990-01-30 | General Electric Company | Rapidly solidified and heat-treated manganese and niobium-modified titanium aluminum alloys |
| JP3492118B2 (en) * | 1996-10-28 | 2004-02-03 | 三菱重工業株式会社 | TiAl intermetallic compound based alloy |
-
2005
- 2005-09-29 CN CNB2005100960897A patent/CN100432254C/en not_active Expired - Fee Related
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100463984C (en) * | 2007-01-12 | 2009-02-25 | 西北工业大学 | Preparation method of Titanium Trialuminum radical composite material |
| CN102730730A (en) * | 2012-07-03 | 2012-10-17 | 武汉科技大学 | Submicron Al2O3 fibre and preparation method thereof |
| CN102730730B (en) * | 2012-07-03 | 2014-06-18 | 武汉科技大学 | Submicron Al2O3 fibre and preparation method thereof |
| CN109694971A (en) * | 2019-01-24 | 2019-04-30 | 重庆大学 | A kind of powder metallurgy titanium-aluminium matrix composites and preparation method thereof |
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| CN100432254C (en) | 2008-11-12 |
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Granted publication date: 20081112 Termination date: 20110929 |