CN1769240A - Aluminum oxide granule reinforced aluminum titanium carbide base composite material and its preparation method - Google Patents
Aluminum oxide granule reinforced aluminum titanium carbide base composite material and its preparation method Download PDFInfo
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- CN1769240A CN1769240A CN 200410050692 CN200410050692A CN1769240A CN 1769240 A CN1769240 A CN 1769240A CN 200410050692 CN200410050692 CN 200410050692 CN 200410050692 A CN200410050692 A CN 200410050692A CN 1769240 A CN1769240 A CN 1769240A
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- sintering
- alumina particle
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- titanium carbide
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Abstract
The invention relates to a method for preparation of Ti2Al2/ Al2O3 composite by an in-situ hot pressing/ solid- liquid phase reaction. The pottery can be prepared by using Al2O3 particles strengthening Ti3AlC2 ternary layer, alumina particle strengthening phase being 5-30% by volume ratio; and the specific method for preparation is as following: using titanium powder, aluminum powder, graphite powder, and alumina powder as the raw material with the molar ration of Ti: Al: C being 3: (0.9-1.1): (1.8-2.0), adding the alumina powder by predetermined volume ratio; mixing the material powders for 8-24 hours by physics machine means, adding into graphite die for cold press with pressure of 10-20MPa, and sintering in a hot-pressing stove in a protective atmosphere, with the heating-up speed of 5-50Deg. C/ min, sintering temperature of 1400-1600Deg. C, sintering time of 0.5-2 hours, and sintering pressure of 20-40MPa. In the invention, aluminum-titanium carbide composite reinforced by alumina particle with high purity, high strength and thermostability can be prepared in lower temperature, shorter time.
Description
Technical field
The present invention relates to ceramic matric composite and preparation method, be specially a kind of in-situ hot pressing/solid-liquid phase reaction and prepare aluminum oxide (Al
2O
3) particle-reinforced aluminum titanium carbide (Ti
3AlC
2) based composites and preparation method thereof.
Background technology
Ti
3AlC
2It is a kind of novel ternary layered ceramic material.Document 1: material journal (Acta Materialia50,3141 (2002)) studies show that in that it combines the plurality of advantages of pottery and metal, have high-modulus, soft, high specific conductivity and thermal conductivity and easy characteristics such as processing, thereby have broad application prospects.But as a kind of structured material, its intensity and hardness are on the low side, have limited its widespread use.Introducing hard ceramic particles is one of effective ways that improve ternary layered ceramic intensity, does not also have Ti at present
3AlC
2The report of reinforcement aspect.Existing work only concentrates on another kind and Ti
3AlC
2The ceramic layered Ti that structure is similar with performance
3SiC
2Particle strengthening on.Titanium carbide, silicon carbide and aluminum oxide are added into as strengthening phase or the synthetic preparation of original position Ti
3SiC
2Based composites, but there is the conclusion of many contradictions on the performance.For example, be a kind of Ti equally
3SiC
2/ Al
2O
3Matrix material, people's such as Luo studies show that the bending strength of matrix material descends gradually along with the increasing of aluminum oxide add-on in the U.S. pottery association journal (Journal of American Ceramic Society 85,3099 (2002)); And people's such as Wang result of study shows and adds that the intensity of matrix material increases behind the aluminum oxide in the international pottery (Ceramic International 28,931 (2002)).On the other hand, above-mentioned Ti
3SiC
2/ Al
2O
3The preparation of matrix material all is to adopt earlier synthetic silicon titanium carbide (Ti
3SiC
2) powder, again with the aluminum oxide mixed sintering, the technology more complicated, and in the follow-up sintering process, produce titanium carbide impurity inevitably, will influence the high-temperature oxidation resistance of material.
Summary of the invention
The object of the present invention is to provide that a kind of mechanical property is good, purity is high, simple to operate, easy control of process conditions, alumina particle that cost is low strengthen aluminum titanium carbide base (Ti
3AlC
2/ Al
2O
3) matrix material and preparation method thereof.
Technical scheme of the present invention is:
A kind of alumina particle strengthens the aluminum titanium carbide based composites, by aluminum oxide (Al
2O
3) particle wild phase and aluminum titanium carbide (Ti
3AlC
2) the matrix composition, wherein the percent by volume of alumina particle wild phase is 5～30%.
Described alumina particle strengthens the preparation method of aluminum titanium carbide based composites; with the simple substance titanium valve; aluminium powder; Graphite Powder 99 and aluminum oxide powder are as raw material; wherein the mol ratio of Ti: Al: C is 3: (0.9～1.1): (1.8～2.0); aluminum oxide powder adds by predetermined volume ratio; raw material powder was mixed 8～24 hours through physical mechanical method; pack into and cold pressing in the graphite jig; the pressure that applies is 10～20MPa; sintering in the hot pressing furnace that is connected with protection of inert gas atmosphere; temperature rise rate is 5～50 ℃/minute, and sintering temperature is 1400～1600 ℃; sintering time is 0.5～2 hour; sintering pressure is 20～40MPa.The present invention can prepare have high purity, high strength, high tenacity, alumina particle high temperature resistant and that over-all properties such as can process strengthen titanium aluminium carbide based composites.
The titanium valve of described adding, aluminium powder, Graphite Powder 99 size range are 200～400 orders, and the alumina particle diameter of adding is 0.1～10 micron; Described sintering processing is hot pressed sintering or HIP sintering; Described rare gas element is argon gas, helium or neon; Described physical mechanical method mixes the ball milled that adopts under the alcohol medium.
Advantage of the present invention is 2
L, purity height, mechanical property are good.Adopt the Ti of the inventive method preparation
3AlC
2/ Al
2O
3Matrix material does not contain other impurity only by aluminum titanium carbide and aluminum oxide two phase composites, as titanium carbide etc.This has just given full play to the reinforcing edge of aluminum oxide, has both improved the mechanical property of material, can guarantee that again material oxidation-resistance in high temperature is used can not descend, even strengthen to some extent.Utilize the present invention, aluminium oxide particles can be evenly distributed in the titanium aluminium carbide matrix, and reinforced effects is strengthened greatly.Ti
3AlC
2/ Al
2O
3The hardness of matrix material, compressive strength, tensile strength are all than pure Ti
3AlC
2Improve 30～80%, especially when the content of wild phase was the 10vol.% left and right sides, the fracture toughness property of material reached 8.8MPam
1/2, than pure Ti
3AlC
2Improved about 20%.In addition, experimental results show that at high temperature Ti
3AlC
2/ Al
2O
3Matrix material still can keep above-mentioned reinforced effects.
2, technology is simple, and cost is low.The present invention is that sintering and densification are carried out simultaneously by in-situ hot pressing/solid-liquid phase reaction, simultaneously, because aluminum oxide is very stable, does not participate in reaction in sintering process, thereby finally obtains Ti
3AlC
2/ Al
2O
3Matrix material.Because the appearance of liquid phase is arranged in sintering process, utilize the quick mass transfer process of liquid phase, chemical time is shortened greatly, make densification process become very easy again.With respect to earlier synthetic two phase ceramics, the remix sintering had both made technical process become simply, had saved expense again.
Description of drawings
Fig. 1 is Ti
3AlC
2/ 10vol.%Al
2O
3Backscattered electron photo after the matrix material polishing.
Fig. 2 is Ti
3AlC
2/ 10vol.%Al
2O
3The crooked fracture stereoscan photograph of matrix material.
Fig. 3 is Ti
3AlC
2And Ti
3AlC
2/ 10vol.%Al
2O
3The room temperature of matrix material and the contrast of high-temperature bending strength.Crossbeam speed is 0.5mm/min.
Embodiment
Below by example in detail the present invention is described in detail.
With size range is 200～400 purpose titanium valves, 140.5 grams, aluminium powder 28.01 grams, graphite 21.28 grams and 9.48 gram aluminum oxide powder (5vol.%, particle diameter is 2～5 microns) ball milling 8 hours in the alcohol medium, the coldmoulding in the graphite jig of packing into afterwards, the pressure that applies is 10MPa, puts into the hot pressing furnace hot pressed sintering.Temperature rise rate is 10 ℃/minute, is heated to 1500 ℃ of insulations 1 hour, and pressure is added to 25MPa gradually simultaneously.Whole sintering process all is to carry out under argon shield, and the reaction product of acquisition is Ti through X-ray diffraction analysis
3AlC
2And Al
2O
3The density that Archimedes's method records is 4.18g/cm
3, be 99.2% of theoretical density.Ti
3AlC
2/ 5vol.%Al
2O
3The Vickers' hardness of matrix material is 3.93GPa; Compressive strength is 781MPa; Bending strength is 386MPa, and fracture toughness is 8.5MPam
1/2
With size range is 200～400 purpose titanium valves, 135.4 grams, aluminium powder 23.52 grams, graphite 22.08 grams and 19 gram aluminum oxide powder (10vol.%, particle diameter is 5～10 microns) ball milling 16 hours in the alcohol medium, the coldmoulding in the graphite jig of packing into afterwards, the pressure that applies is 15MPa, puts into the hot pressing furnace hot pressed sintering.Temperature rise rate is 20 ℃/minute, is heated to 1550 ℃ of insulations 1 hour, and pressure is added to 30MPa gradually simultaneously.Whole sintering process all is to carry out under argon shield, and the reaction product of acquisition is Ti through X-ray diffraction analysis
3AlC
2And Al
2O
3The density that Archimedes's method records is 4.17g/cm
3, be 99.5% of theoretical density.Ti
3AlC
2/ 10vol.%Al
2O
3The Vickers' hardness of matrix material is 4.46GPa; Compressive strength is 879MPa; Bending strength is 423MPa, and fracture toughness is 8.8MPam
1/21100 ℃ anti-bending test shows Ti
3AlC
2/ 10vol.%Al
2O
3The bending strength of matrix material is 236.1MPa.
With size range is 200～400 purpose titanium valves, 119.24 grams, aluminium powder 24.48 grams, graphite 19.86 grams and 38.22 gram aluminum oxide powder (20vol.%, particle diameter is 0.1～2 micron) ball milling 24 hours in the alcohol medium, the coldmoulding in the graphite jig of packing into afterwards, the pressure that applies is 20MPa, puts into the hot pressing furnace HIP sintering.Temperature rise rate is 50 ℃/minute, is heated to 1600 ℃ of insulations 1 hour, and pressure is added to 40MPa gradually simultaneously.Whole sintering process all is to carry out under argon shield, and the reaction product of acquisition is Ti through X-ray diffraction analysis
3AlC
2And Al
2O
3The density that Archimedes's method records is 4.15g/cm
3, be 99.6% of theoretical density.Ti
3AlC
2/ 20vol.%Al
2O
3The Vickers' hardness of matrix material is 5.47GPa; Compressive strength is 1138MPa; Bending strength is 500MPa, and fracture toughness is 7.1Mpam
1/2
Comparative example
The pure Ti that adopted the prepared identical with embodiment 2
3AlC
2, the density that Archimedes's method records is 4.21g/cm
3, be 99.1% of theoretical density; Vickers' hardness is 3.5GPa; Compressive strength is 749MPa; Bending strength is 356MPa, and fracture toughness is 7.2MPam
1/21100 ℃ bending strength is that the every mechanical performance index of 133MPa. is all far below Ti
3AlC
2/ Al
2O
3Matrix material.Below with Ti
3AlC
2/ 10vol.%Al
2O
3Matrix material is an example, specifies the tissue and the performance variation that add material behind the aluminum oxide.
Fig. 1 is Ti
3AlC
2/ 10vol.%Al
2O
3Backscattered electron photo after the matrix material polishing.The ash light tone be Ti mutually
3AlC
2Matrix, grey black be Al mutually
2O
3Particle.The wild phase particle can be uniformly distributed in the matrix as seen from the figure.Fig. 2 is Ti
3AlC
2/ 10vol.%Al
2O
3The crooked fracture stereoscan photograph of matrix material shows that more clearly aluminium oxide particles both had been distributed in Ti
3AlC
2The crystal boundary place, also may reside in intragranular, this has just improved the effect of particle strengthening.The preparation method of other matrix material of mentioning in this point and the background technology is significantly different, and the former can only be present in Ti by aluminium oxide particles
3AlC
2The crystal boundary place.
Fig. 3 is Ti
3AlC
2And Ti
3AlC
2/ 10vol.%Al
2O
3The room temperature of matrix material and the contrast of high-temperature bending strength.As seen add aluminium oxide particles and not only improved Ti later on
3AlC
2Room temperature strength, and this reinforcement can remain to high temperature, or even 1100 ℃.
By embodiment 1, embodiment 2, embodiment 3 and comparative example as seen, the Ti of present method preparation
3AlC
2/ Al
2O
3Matrix material has purity height, density height, advantage that mechanical property is good, adds room temperature and hot strength that alumina particle has improved the titanium aluminium carbide.
Claims (7)
1, a kind of alumina particle strengthens the aluminum titanium carbide based composites, and it is characterized in that: be made up of alumina particle wild phase and aluminum titanium carbide matrix, wherein the percent by volume of alumina particle wild phase is 5～30%.
2; strengthen the preparation method of aluminum titanium carbide based composites according to the described alumina particle of claim 1; it is characterized in that: with the simple substance titanium valve; aluminium powder; Graphite Powder 99 and aluminum oxide powder are as raw material; wherein the mol ratio of Ti: Al: C is 3: (0.9～1.1): (1.8～2.0); aluminum oxide powder adds by predetermined volume ratio; raw material powder was mixed 8～24 hours through physical mechanical method; pack into and cold pressing in the graphite jig; the pressure that applies is 10～20MPa; sintering in the hot pressing furnace that is connected with protection of inert gas atmosphere; temperature rise rate is 5～50 ℃/minute, and sintering temperature is 1400～1600 ℃; sintering time is 0.5～2 hour; sintering pressure is 20～40MPa.
3, strengthen the preparation method of aluminum titanium carbide based composites according to the described alumina particle of claim 2, it is characterized in that: the volume percent of described alumina particle wild phase is 5～30%.
4, strengthen the preparation method of aluminum titanium carbide based composites according to the described alumina particle of claim 2, it is characterized in that: the alumina particle diameter of described adding is 0.1～10 micron, and the titanium valve of adding, aluminium powder, Graphite Powder 99 size range are 200～400 orders.
5, strengthen the preparation method of aluminum titanium carbide based composites according to the described alumina particle of claim 2, it is characterized in that: described sintering processing is hot pressed sintering or HIP sintering.
6, strengthen the preparation method of aluminum titanium carbide based composites according to the described alumina particle of claim 2, it is characterized in that: described rare gas element is argon gas, helium or neon.
7, strengthen the preparation method of aluminum titanium carbide based composites according to the described alumina particle of claim 2, it is characterized in that: described physical mechanical method mixes employing ball milling in the alcohol medium.
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|---|---|---|---|
| CNB2004100506927A CN1298675C (en) | 2004-10-28 | 2004-10-28 | Aluminum oxide granule reinforced aluminum titanium carbide base composite material and its preparation method |
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|---|---|---|---|
| CNB2004100506927A CN1298675C (en) | 2004-10-28 | 2004-10-28 | Aluminum oxide granule reinforced aluminum titanium carbide base composite material and its preparation method |
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|---|---|
| CN1769240A true CN1769240A (en) | 2006-05-10 |
| CN1298675C CN1298675C (en) | 2007-02-07 |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100418923C (en) * | 2007-04-27 | 2008-09-17 | 武汉理工大学 | Compact Ti2AlC-TiB2 composite material and preparation method therefor |
| CN100463984C (en) * | 2007-01-12 | 2009-02-25 | 西北工业大学 | Preparation method of Titanium Trialuminum radical composite material |
| CN107805071A (en) * | 2017-10-26 | 2018-03-16 | 西南交通大学 | A kind of preparation method of the low glass wetting aluminium two/mullite composite ceramic of carbon of titanium three |
| CN115354182A (en) * | 2022-08-29 | 2022-11-18 | 哈尔滨工业大学 | TiAl in-situ growth 3 Texture of the skeleton Ti 3 AlC 2 Preparation method of reinforced aluminum-based composite material |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1179918C (en) * | 2003-06-20 | 2004-12-15 | 武汉理工大学 | Method for preparing single-phase compact titanium aluminium carbon block body material by using si as adjurant through hot pressing process |
-
2004
- 2004-10-28 CN CNB2004100506927A patent/CN1298675C/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 |
| CN100418923C (en) * | 2007-04-27 | 2008-09-17 | 武汉理工大学 | Compact Ti2AlC-TiB2 composite material and preparation method therefor |
| CN107805071A (en) * | 2017-10-26 | 2018-03-16 | 西南交通大学 | A kind of preparation method of the low glass wetting aluminium two/mullite composite ceramic of carbon of titanium three |
| CN115354182A (en) * | 2022-08-29 | 2022-11-18 | 哈尔滨工业大学 | TiAl in-situ growth 3 Texture of the skeleton Ti 3 AlC 2 Preparation method of reinforced aluminum-based composite material |
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|---|---|
| CN1298675C (en) | 2007-02-07 |
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Granted publication date: 20070207 Termination date: 20091130 |