CN100432253C - Process for preporing auto-nano Al203/TiAl base composite material - Google Patents
Process for preporing auto-nano Al203/TiAl base composite material Download PDFInfo
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- CN100432253C CN100432253C CNB2005100960882A CN200510096088A CN100432253C CN 100432253 C CN100432253 C CN 100432253C CN B2005100960882 A CNB2005100960882 A CN B2005100960882A CN 200510096088 A CN200510096088 A CN 200510096088A CN 100432253 C CN100432253 C CN 100432253C
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Abstract
The present invention relates to a preparation process of nanometer Al2 O3 /TiAl base composite materials, which comprises the steps that firstly, Ti, Al, TiO2 and Nb2O5 are mixed, and then rare earth oxides such as La2 O3 or Y2O3 are added to prepare a mixture; the mixture uses ethanol as a medium and is milled in a high-aluminum ball milling pot; the milled mixture is pressed into block-shaped prefabricated bodies on a single-direction oil hydraulic press; the mixed powder of graphite and alumina powder is coated on the prefabricated bodies, or is sintered in vacuum or under the condition of atmosphere protection; pressurization and heat insulation are carried out when the mixed powder is at the highest temperature, and then the mixed powder is naturally cooled. The present invention has the advantages that alumina whiskers are generated by reacting in a TiAl intermetallic compound basal body, and the whiskers have narrow size distribution and have a diameter of 20 to 30 nm. The whiskers uniformly dispersed in the basal bodies have a certain improvement to material properties.
Description
Technical field
The present invention relates to the preparation technology of intermetallic compound composite material, particularly a kind of spontaneous nanometer Al
2O
3The preparation technology of/TiAl based composites
Background technology
The TiAl intermetallic compound is the high-temperature structural material that a new generation has wide application prospect owing to dual key (metallic bond and Gong Jia Key coexistence) and atom long-range order ordered state have nearly ceramic high temperature intensity and near Plastic Deformation.Wherein γ-TiAl also has good high-temperature oxidation-resistance and low density, uses more attractively on all kinds of engines, becomes the focus of research and development.But because ordered structure of its height makes its room temperature ductility poor, be difficult to machining deformation and non-oxidizability deficiency more than 850 ℃, seriously hindered its practical application.
Adopt alloying, special preparation technology and different methods such as thermal treatment, make the performance of this material that bigger improvement arranged, 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 the preparation intermetallic compound based composite material, can obtain the good mechanical performance, and keep the low characteristic of matrix density simultaneously.
Though strengthen the research of intermetallic compound about ceramic fibre certain progress is arranged, be mostly by the compound method of plus fiber.And owing to interface, matched coefficients of thermal expansion, fiber dispersion, the fibre strength loss in technological process or the like reason, whether it can use in practice waits further investigation.Whisker and continuous fiber have same toughening effect, and size and the ceramic particle of whisker are close, process than being easier to, but its manufacturing cost costliness, the dispersing technology complexity, and directly contacted carcinogenic harm etc. with human body.
Summary of the invention
The objective of the invention is to overcome the shortcoming of above-mentioned prior art, provide a kind of and strengthened the Intermatallic Ti-Al compound matrix by the synthetic In-situ whisker of reaction, it is simple to reach preparation technology, and cost is low, the finely dispersed spontaneous nanometer Al of whisker
2O
3The preparation technology of/TiAl based composites.
For achieving the above object, the technical solution used in the present invention is: at first with purity greater than 99%, fineness is greater than 200 purpose Ti, the Al powder Ti by weight 35-50%, the Al of 35-50%, the TiO of 8-13%
2And the Nb of 0-5%
2O
5Mix, and then add the rare earth oxide La of mixture quality 0.5-2%
2O
3Or Y
2O
3Make mixture; To 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; graphite and alumina powder mixed powder covered be embedded in that the speed with 3-8 ℃/minute is warming up to 1200-1250 ℃ of sintering on the precast body; with precast body 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 thermite reaction, principle of oxidation and reduction, spontaneous whisker strengthens body in the generative process of material, can not only make material synthetic under lower temperature, saved the energy, simplified production technique, and having reduced the loss of strength of whisker in technological process, spontaneous whisker has not only reduced manufacturing cost, has simplified production technique, and the whisker that this mode generates possesses clean phase boundary, no foreign matter, pollute generation, make whisker in TiAl intermetallic compound base body, better chemical and physical compatibility are arranged, the present invention is in TiAl intermetallic compound base body, the self-formed from reaction alumina whisker, whisker narrow size distribution, the about 20-30nm of diameter, in matrix, disperse comparatively evenly, material property is had certain improvement.
Description of drawings
Fig. 1 is the spontaneous nanometer Al that makes according to preparation method of the present invention
2O
3The XRD analysis figure of/TiAl based composites;
Fig. 2 is the sem analysis figure of the spontaneous whisker of the present invention, and wherein X-coordinate is the diffraction angle number of degrees, and ordinate zou is an intensity;
Fig. 3 is energy dispersive spectrometry (EDS) analysis chart of the spontaneous whisker of the present invention, and wherein ordinate zou is an intensity, and X-coordinate is an X-ray 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 is greater than 200 purpose Ti, the Al powder Ti by weight 35%, 50% Al, 10% TiO
2And 5% Nb
2O
5Mix, and then add the rare earth oxide La of mixture quality 2%
2O
3Make mixture; To be medium fully mixed mixture in 20 minutes with 900 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 45Mpa 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 in that the speed with 8 ℃/minute is warming up to 1200 ℃ of sintering on the precast body, after applying the pressure of 150Mpa during to 1200 ℃ and being incubated 10.8 hours, cooling gets final product naturally.
Embodiment 2: at first with purity greater than 99%, fineness is greater than 200 purpose Ti, the Al powder Ti by weight 50%, 40% Al, 10% TiO
2Mix, and then add the rare earth oxide Y of mixture quality 0.8%
2O
3Make mixture; To be medium fully mixed mixture in 35 minutes with 860 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 in that the speed with 5 ℃/minute is warming up to 1230 ℃ of sintering on the precast body, after applying the pressure of 60Mpa during to 1230 ℃ and being incubated 0.8 hour, cooling gets final product naturally.
Embodiment 3: at first with purity greater than 99%, fineness is greater than 200 purpose Ti, the Al powder Ti by weight 48%, 35% Al, 13% TiO
2And 4% Nb
2O
5Mix, and then add the rare earth oxide La of mixture quality 1.6%
2O
3Make mixture; To be medium fully mixed mixture in 42 minutes with 820 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 1210 ℃ of sintering, and after applying the pressure of 30Mpa during to 1210 ℃ and being incubated 0.6 hour, cooling gets final product naturally.
Embodiment 4: at first with purity greater than 99%, fineness is greater than 200 purpose Ti, the Al powder Ti by weight 45%, 45% Al, 8% TiO
2And 2% Nb
2O
5Mix, and then add the rare earth oxide Y of mixture quality 1.0%
2O
3Make mixture; To be medium fully mixed mixture in 50 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 35Mpa 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 0.7 hour, cooling gets final product naturally.
Embodiment 5: at first with purity greater than 99%, fineness is greater than 200 purpose Ti, the Al powder Ti by weight 40%, 47% Al, 12% TiO
2And 1% Nb
2O
5Mix, and then add the rare earth oxide La of mixture quality 0.5%
2O
3Make mixture; To be medium fully mixed mixture in 26 minutes with 890 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 42Mpa 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 1250 ℃ of sintering, and after applying the pressure of 120Mpa during to 1250 ℃ and being incubated 0.9 hour, cooling gets final product naturally.
Embodiment 6: at first with purity greater than 99%, fineness is greater than 200 purpose Ti, the Al powder Ti by weight 50%, 38% Al, 9% TiO
2And 3% Nb
2O
5Mix, and then add the rare earth oxide Y of mixture quality 1.5%
2O
3Make mixture; To be medium fully mixed mixture in 30 minutes with 850 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 48Mpa on unidirectional hydraulic press is pressed into block precast body; Again with graphite: precast body speed with 7 ℃/minute under the atmosphere protection condition is warming up to 1220 ℃ of sintering, and after applying the pressure of 80Mpa during to 1220 ℃ and being incubated 0.5 hour, cooling gets final product naturally.
Referring to Fig. 1, according to preparation method of the present invention, the material principal crystalline phase of preparation is TiAl, and inferior crystalline phase is NbAl
3, Al
2O
3
Referring to Fig. 2, spontaneous whisker any surface finish in the material, length-to-diameter ratio is about 1: 50.
Referring to Fig. 3, the whisker composition in the material is Al
2O
3
Claims (7)
1, spontaneous nanometer Al
2O
3The preparation technology of/TiAl based composites is characterized in that:
1) at first with purity greater than 99%, fineness is greater than 200 purpose Ti, the Al powder Ti by weight 35-50%, the Al of 35-50%, the TiO of 8-13%
2And the Nb of 0-5%
2O
5Mix, and then add the rare earth oxide La of mixture quality 0.5-2%
2O
3Or Y
2O
3Make mixture;
2) 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;
3) the mixture pressure with 30-50Mpa on unidirectional oil press after will sieving is pressed into block precast body;
4) again with graphite: aluminum oxide powder is by 1: the mass ratio of 1-3 is made graphite and aluminum oxide powder mixed powder; graphite and aluminum oxide powder mixed powder covered be embedded in that the speed with 3-8 ℃/minute is warming up to 1200-1250 ℃ of sintering on the precast body; with precast body 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, spontaneous nanometer Al according to claim 1
2O
3The preparation technology of/TiAl based composites is characterized in that: at first with purity greater than 99%, fineness is greater than 200 purpose Ti, the Al powder Ti by weight 35%, 50% Al, 10% TiO
2And 5% Nb
2O
5Mix, and then add the rare earth oxide La of mixture quality 2%
2O
3Make mixture; To be medium fully mixed mixture in 20 minutes with 900 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 45Mpa 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 in that the speed with 8 ℃/minute is warming up to 1200 ℃ of sintering on the precast body, after applying the pressure of 150Mpa during to 1200 ℃ and being incubated 10.8 hours, cooling gets final product naturally.
3, spontaneous nanometer Al according to claim 1
2O
3The preparation technology of/TiAl based composites is characterized in that: at first with purity greater than 99%, fineness is greater than 200 purpose Ti, the Al powder Ti by weight 50%, 40% Al, 10% TiO
2Mix, and then add the rare earth oxide Y of mixture quality 0.8%
2O
3Make mixture; To be medium fully mixed mixture in 35 minutes with 860 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 in that the speed with 5 ℃/minute is warming up to 1230 ℃ of sintering on the precast body, after applying the pressure of 60Mpa during to 1230 ℃ and being incubated 0.8 hour, cooling gets final product naturally.
4, spontaneous nanometer Al according to claim 1
2O
3The preparation technology of/TiAl based composites is characterized in that: at first with purity greater than 99%, fineness is greater than 200 purpose Ti, the Al powder Ti by weight 48%, 35% Al, 13% TiO
2And 4% Nb
2O
5Mix, and then add the rare earth oxide La of mixture quality 1.6%
2O
3Make mixture; To be medium fully mixed mixture in 42 minutes with 820 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 1210 ℃ of sintering, and after applying the pressure of 30Mpa during to 1210 ℃ and being incubated 0.6 hour, cooling gets final product naturally.
5, spontaneous nanometer Al according to claim 1
2O
3The preparation technology of/TiAl based composites is characterized in that: at first with purity greater than 99%, fineness is greater than 200 purpose Ti, the Al powder Ti by weight 45%, 45% Al, 8% TiO
2And 2% Nb
2O
5Mix, and then add the rare earth oxide Y of mixture quality 1.0%
2O
3Make mixture; To be medium fully mixed mixture in 50 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 35Mpa 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 0.7 hour, cooling gets final product naturally.
6, spontaneous nanometer Al according to claim 1
2O
3The preparation technology of/TiAl based composites is characterized in that: at first with purity greater than 99%, fineness is greater than 200 purpose Ti, the Al powder Ti by weight 40%, 47% Al, 12% TiO
2And 1% Nb
2O
5Mix, and then add the rare earth oxide La of mixture quality 0.5%
2O
3Make mixture; To be medium fully mixed mixture in 26 minutes with 890 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 42Mpa 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 1250 ℃ of sintering, and after applying the pressure of 120Mpa during to 1250 ℃ and being incubated 0.9 hour, cooling gets final product naturally.
7, spontaneous nanometer Al according to claim 1
2O
3The preparation technology of/TiAl based composites is characterized in that: at first with purity greater than 99%, fineness is greater than 200 purpose Ti, the Al powder Ti by weight 50%, 38% Al, 9% TiO
2And 3% Nb
2O
5Mix, and then add the rare earth oxide Y of mixture quality 1.5%
2O
3Make mixture; To be medium fully mixed mixture in 30 minutes with 850 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 48Mpa on unidirectional hydraulic press is pressed into block precast body; Again with graphite: precast body speed with 7 ℃/minute under the atmosphere protection condition is warming up to 1220 ℃ of sintering, and after applying the pressure of 80Mpa during to 1220 ℃ and being incubated 0.5 hour, cooling gets final product naturally.
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CN105274380A (en) * | 2014-07-07 | 2016-01-27 | 陈焕铭 | Method for improving wettability of Al2O3 porous perform and NbAl molten alloy |
CN106367633A (en) * | 2016-09-12 | 2017-02-01 | 江苏大学 | La2O3-microalloyed TiAl-based alloy being high in acid corrosion resistance |
CN108165865A (en) * | 2017-12-27 | 2018-06-15 | 济南大学 | A kind of novel TiAl-base alloy material and preparation method |
Citations (3)
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US4865666A (en) * | 1987-10-14 | 1989-09-12 | Martin Marietta Corporation | Multicomponent, low density cubic L12 aluminides |
EP0362470A1 (en) * | 1988-10-03 | 1990-04-11 | General Electric Company | Manganese and niobium-modified titanium aluminum alloys |
US6294132B1 (en) * | 1996-10-28 | 2001-09-25 | Mitsubishi Heavy Industries Ltd. | TiAl intermetallic compound-based alloy |
-
2005
- 2005-09-29 CN CNB2005100960882A patent/CN100432253C/en not_active Expired - Fee Related
Patent Citations (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 |
EP0362470A1 (en) * | 1988-10-03 | 1990-04-11 | General Electric Company | Manganese and niobium-modified titanium aluminum alloys |
US6294132B1 (en) * | 1996-10-28 | 2001-09-25 | Mitsubishi Heavy Industries Ltd. | TiAl intermetallic compound-based alloy |
Non-Patent Citations (6)
Title |
---|
Al2O3/Ti-Al复合材料的抗高温氧化性研究. 吕臣敬,王芬,朱剑锋.陕西科技大学学报,第23卷第3期. 2005 |
Al2O3/Ti-Al复合材料的抗高温氧化性研究. 吕臣敬,王芬,朱剑锋.陕西科技大学学报,第23卷第3期. 2005 * |
Al-Ti-TiO2体系燃烧合成及其反应过程研究. 李志强,曲伟,韩杰才,赫晓东.无机材料学报,第17卷第2期. 2002 |
Al-Ti-TiO2体系燃烧合成及其反应过程研究. 李志强,曲伟,韩杰才,赫晓东.无机材料学报,第17卷第2期. 2002 * |
原位合成Al2O3/Ti-Al复合材料的研究. 吕臣敬,王芬,张希清.宇航材料工艺,第4期. 2005 |
原位合成Al2O3/Ti-Al复合材料的研究. 吕臣敬,王芬,张希清.宇航材料工艺,第4期. 2005 * |
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