CN101417878B - TaC-SiC ceramic composite material synthesized by hot pressing at in-situ reaction - Google Patents
TaC-SiC ceramic composite material synthesized by hot pressing at in-situ reaction Download PDFInfo
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- 239000000919 ceramic Substances 0.000 title claims abstract description 32
- 239000002131 composite material Substances 0.000 title claims abstract description 32
- 238000007731 hot pressing Methods 0.000 title claims abstract description 21
- 238000006243 chemical reaction Methods 0.000 title claims abstract description 15
- 238000011065 in-situ storage Methods 0.000 title claims abstract description 10
- 238000005245 sintering Methods 0.000 claims abstract description 30
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 24
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims abstract description 22
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 claims abstract description 14
- 229910052786 argon Inorganic materials 0.000 claims abstract description 11
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 11
- 239000010439 graphite Substances 0.000 claims abstract description 11
- 239000011347 resin Substances 0.000 claims abstract description 11
- 229920005989 resin Polymers 0.000 claims abstract description 11
- 239000000203 mixture Substances 0.000 claims abstract description 6
- 238000007873 sieving Methods 0.000 claims abstract description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 24
- 235000013312 flour Nutrition 0.000 claims description 12
- 239000000377 silicon dioxide Substances 0.000 claims description 12
- 238000000498 ball milling Methods 0.000 claims description 10
- 238000012856 packing Methods 0.000 claims description 9
- 239000002994 raw material Substances 0.000 claims description 4
- 239000007789 gas Substances 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 2
- 238000004321 preservation Methods 0.000 claims description 2
- 238000000034 method Methods 0.000 abstract description 22
- 239000000463 material Substances 0.000 abstract description 8
- 238000010189 synthetic method Methods 0.000 abstract description 6
- 230000003647 oxidation Effects 0.000 abstract description 4
- 238000007254 oxidation reaction Methods 0.000 abstract description 4
- 230000001590 oxidative effect Effects 0.000 abstract description 3
- 238000002679 ablation Methods 0.000 abstract description 2
- 229910052715 tantalum Inorganic materials 0.000 abstract description 2
- 239000000843 powder Substances 0.000 abstract 2
- 230000003064 anti-oxidating effect Effects 0.000 abstract 1
- 239000011153 ceramic matrix composite Substances 0.000 abstract 1
- 238000000465 moulding Methods 0.000 abstract 1
- 239000011863 silicon-based powder Substances 0.000 abstract 1
- 229910010271 silicon carbide Inorganic materials 0.000 description 73
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 45
- 229910003468 tantalcarbide Inorganic materials 0.000 description 25
- 239000011159 matrix material Substances 0.000 description 10
- 238000002441 X-ray diffraction Methods 0.000 description 9
- 239000007795 chemical reaction product Substances 0.000 description 7
- 238000009413 insulation Methods 0.000 description 7
- 238000005516 engineering process Methods 0.000 description 5
- 238000000280 densification Methods 0.000 description 4
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- 230000003078 antioxidant effect Effects 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 229910003465 moissanite Inorganic materials 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 230000000630 rising effect Effects 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- HPNSNYBUADCFDR-UHFFFAOYSA-N chromafenozide Chemical compound CC1=CC(C)=CC(C(=O)N(NC(=O)C=2C(=C3CCCOC3=CC=2)C)C(C)(C)C)=C1 HPNSNYBUADCFDR-UHFFFAOYSA-N 0.000 description 1
- 238000000748 compression moulding Methods 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 210000000867 larynx Anatomy 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 150000001247 metal acetylides Chemical class 0.000 description 1
- NFFIWVVINABMKP-UHFFFAOYSA-N methylidynetantalum Chemical compound [Ta]#C NFFIWVVINABMKP-UHFFFAOYSA-N 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
- 238000009827 uniform distribution Methods 0.000 description 1
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Abstract
The invention relates to a ceramic matrix composite material and a synthetic method thereof, which are concretely an in-situ reactive synthesized TaC-SiC ceramic composite material by hot pressing and a synthetic method thereof. The method aims at solving the problems that the oxidation resistance of TaC is not ideal and loose surface oxide layers are easy to form in an oxidizing atmosphere, and the like. Two composition phases of TaC and SiC are in-situ formed and the percentage content of SiC is 0 to 50vol. percent. The concrete synthetic method is as follows: tantalum powders, silicon powders and graphite powders are used as materials which are ball milled for 10 to 40 hours under dry condition in a resin tank, after sieving the materials are put in a graphite die for cold molding (5 to 20 MPa), and then the materials are sintered in vacuum or a hot pressing furnace introduced with argon, with the sintering temperature of 1950 to 2150 DEG C, heat preserving sintering time of 1 to 2 hours and sintering pressure of 30 to 40 MPa. The synthetic method can synthesize the TaC-SiC ceramic composite materials by in-situ reaction, the prepared TaC-SiC ceramic composite materials are mainly used for structural components of ablation resistance under high temperature and anti-oxidation and the materials are applied to the aerospace field.
Description
Technical field
The present invention relates to ceramic matric composite, be specially a kind of TaC-SiC ceramic composite material synthesized by hot pressing at in-situ reaction.
Background technology
Transition metal carbides TaC has the NaCl type crystal structure and since the existence of covalent linkage it have high Young's modulus (560GPa), high hardness (15GPa) and high fusing point (3985 ℃).Utilize its high fusing point, TaC can be used as the anti-ablator of high temperature, for example is applied as the throat liner material of aerospace engine jet pipe.Lockheed Martin Corporation (U.S.) once developed a kind of TaC pottery larynx lining that ablate, pure compression molding (density is 95%) hardly, and than traditional carbon-to-carbon material, the production cycle shortens (airborne weapon, 2 (2004) 48) greatly.But the antioxidant property of very important is TaC is undesirable, is easy to form loose surface oxide layer in oxidizing atmosphere.
Summary of the invention
The object of the present invention is to provide a kind of easy control of process conditions, TaC-SiC ceramic composite material synthesized by hot pressing at in-situ reaction that cost is low, undesirable with the antioxidant property that solves TaC, in oxidizing atmosphere, be easy to form loose problems such as surface oxide layer.
Technical scheme of the present invention is:
A kind of TaC-SiC ceramic composite material synthesized by hot pressing at in-situ reaction, TaC become the phase-splitting reaction in to generate with two kinds of SiC, percentage composition meter by volume, and the content of SiC is 0~50% (preferable range is 10~30%), all the other are TaC; The SiC type is a cube phase β-SiC.
The synthetic method of above-mentioned TaC-SiC ceramic composite material synthesized by hot pressing at in-situ reaction, synthetic by the reaction in hot-pressing technique, wherein the content of TaC and SiC in the matrix can be regulated by the content of Ta, Si and C in the original proportioning.Concrete synthetic method is:
With tantalum powder, silica flour and Graphite Powder 99 is raw material, ball milling is 10~40 hours in resin container, the coldmoulding (5~20MPa) in the graphite jig of packing into after sieving, in vacuum or be connected with sintering in the hot pressing furnace of argon gas, temperature rise rate is 10~15 ℃/minute, and sintering temperature is that 1950~2150 ℃, heat preservation sintering time are that 1~2 hour, sintering pressure are 30~40MPa.Thereby, under lower temperature, synthesize the TaC-SiC ceramic composite of high-compactness fast.
The tantalum powder of described adding, silica flour and Graphite Powder 99 size range are 200~600 orders; Described sintering processing is a hot pressed sintering; Described sintering atmosphere is that (vacuum tightness is 10 to vacuum
-4~10
-2MPa) or argon gas; Described mixing method adopts the ball milled under drying conditions.
Advantage of the present invention is:
1. technology is simple.The present invention is a raw material with tantalum powder, silica flour and Graphite Powder 99, and synthetic 1950~2150 ℃ of hot pressing by reaction in, sintering and densification are carried out simultaneously.The agglomerating TaC-SiC of institute ceramic composite is by tantalum carbide and silicon carbide two phase composites.With respect to earlier synthetic two phase ceramics, the remix sintering makes technical process become simple.
2. the TaC-SiC matrix material of the present invention's acquisition is applied to the aerospace field mainly as the anti-ablation of high temperature, oxidation resistant structural part.
3.SiC have excellent high temperature oxidation resistance, can the highlyest in 1600 ℃ air, use.Therefore, the present invention's design strengthens TaC and improves its high-temperature oxidation resistance with SiC.TaC and SiC are by the reaction in synthetic among the present invention.Use reaction in hot pressing synthetic technology, its principle is with raw material proportioning on request, makes it that chemical reaction take place and generates target product, uses heat pressing process to obtain dense material simultaneously.Its advantage is that technology is simple, the product original position is synthetic, has avoided outside contamination, interface cleanness.
Description of drawings
Fig. 1 is that the X-ray diffraction phase composition of TaC-SiC ceramic composite is analyzed.Wherein (a) is TAS0, (b) is TAS5, (c) is TAS10, (d) is TAS20, (e) is TAS30, (f) is TAS40, (g) is TAS50.
Fig. 2 is the density of TaC-SiC ceramic composite and the density change curve with SiC content.
Fig. 3 (a)-(e) is the distribution mutually (secondary electron phase) of TaC-SiC ceramic composite glazed surface.Wherein, Fig. 3 (a) is TAS10, and Fig. 3 (b) is TAS20, and Fig. 3 (c) is TAS30, and Fig. 3 (d) is TAS40, and Fig. 3 (e) is TAS50.
Fig. 4 is the change curve of the Vickers' hardness of TaC-SiC ceramic composite with SiC content.
Fig. 5 is the flexural strength of TaC-SiC ceramic composite and the fracture toughness property change curve with SiC content.
Fig. 6 is that the Young's modulus of TaC-SiC ceramic composite is with the variation of temperature curve.
Embodiment
Below by example in detail the present invention is described in detail, for ease of comparing, single-phase TaC also adopts same technology synthetic.
Embodiment 1 (TaC-5vol.%SiC, TAS5)
With size range is 200~600 purpose tantalum powder 90.3g, silica flour 0.80g and Graphite Powder 99 5.71g, and ball milling is 40 hours in resin container, crosses 200 mesh sieves, coldmoulding in the graphite jig of packing into afterwards, and the pressure that applies is 10MPa, puts into the hot pressing furnace hot pressed sintering.Temperature rise rate is 15 ℃/minute, is heated to 1950 ℃ of insulations 2 hours, and exerting pressure is 30MPa.Whole sintering process all is to carry out under argon shield, and the reaction product of acquisition is TaC through X-ray diffraction analysis, because diffraction peak does not appear in the content of SiC less.The density that Archimedes's method records is 12.58g/cm
3, be 90.4% of theoretical density.Vickers' hardness is 6.3GPa, and flexural strength is 309MPa, and fracture toughness property is 2.9MPam
1/2, Young's modulus is 353GPa.
Embodiment 2 (TaC-10vol.%SiC, TAS10)
With size range is 200~600 purpose tantalum powder 91.67g, silica flour 1.71g and Graphite Powder 99 6.12g, and ball milling is 10 hours in resin container, crosses 200 mesh sieves, coldmoulding in the graphite jig of packing into afterwards, and the pressure that applies is 20MPa, puts into the hot pressing furnace hot pressed sintering.Temperature rise rate is 15 ℃/minute, is heated to 2050 ℃ of insulations 1 hour, and exerting pressure is 40MPa.Whole sintering process all is to carry out under argon shield, and the reaction product of acquisition is TaC and β-SiC through X-ray diffraction analysis.The density that Archimedes's method records is 12.69g/cm
3, be 95.0% of theoretical density.Vickers' hardness is 8.9GPa, and flexural strength is 341MPa, and fracture toughness property is 2.6MPam
1/2, Young's modulus is 410GPa.
Enforcement 3 (TaC-20vol.%SiC, TAS20)
With size range is 200~600 purpose tantalum powder 90.55g, silica flour 3.75g and Graphite Powder 99 6.85g, and ball milling is 20 hours in resin container, crosses 200 mesh sieves, coldmoulding in the graphite jig of packing into afterwards, and the pressure that applies is 5MPa, puts into the hot pressing furnace hot pressed sintering.Temperature rise rate is 10 ℃/minute, is heated to 1950 ℃ of insulations 1 hour, and exerting pressure is 40MPa.Whole sintering process all is to carry out under argon shield, and the reaction product of acquisition is TaC and β-SiC through X-ray diffraction analysis.The density that Archimedes's method records is 11.70g/cm
3, be 95.7% of theoretical density.Vickers' hardness is 8.4GPa, and flexural strength is 309MPa, and fracture toughness property is 3.9MPam
1/2, Young's modulus is 398GPa.
Embodiment 4 (TaC-30vol.%SiC, TAS30)
With size range is 200~600 purpose tantalum powder 79.2g, silica flour 5.65g and Graphite Powder 99 6.9g, and ball milling is 30 hours in resin container, crosses 200 mesh sieves, coldmoulding in the graphite jig of packing into afterwards, and the pressure that applies is 10MPa, puts into the hot pressing furnace hot pressed sintering.Temperature rise rate is 10 ℃/minute, is heated to 2150 ℃ of insulations 2 hours, and exerting pressure is 35MPa.Whole sintering process all is to carry out under argon shield, and the reaction product of acquisition is TaC through X-ray diffraction analysis, β-SiC and a small amount of TaSi
2The density that Archimedes's method records is 11.26 g/cm
3, being 101.4% of theoretical density, this is attributed to than SiC density (3.22g/cm
3) high TaSi
2(density, 9.84g/cm
3) influence.Vickers' hardness is 13.9GPa, and flexural strength is 289MPa, and fracture toughness property is 5.5MPam
1/2, Young's modulus is 459GPa.
Embodiment 5 (TaC-40vol.%SiC, TAS40)
With size range is 200~600 purpose tantalum powder 67.9g, silica flour 7.55g and Graphite Powder 99 6.95g, and ball milling is 20 hours in resin container, crosses 200 mesh sieves, coldmoulding in the graphite jig of packing into afterwards, and the pressure that applies is 5MPa, puts into the hot pressing furnace hot pressed sintering.Temperature rise rate is 10 ℃/minute, is heated to 1950 ℃ of insulations 1 hour, and exerting pressure is 30MPa.Whole sintering process all is to carry out under argon shield, and the reaction product of acquisition is TaC through X-ray diffraction analysis, β-SiC and a small amount of TaSi
2The density that Archimedes's method records is 10.28g/cm
3, being 103.0% of theoretical density, this is attributed to than SiC density (3.22g/cm
3) high TaSi
2(density, 9.84g/cm
3) influence.Vickers' hardness is 14.9GPa, and flexural strength is 331MPa, and fracture toughness property is 5.5MPam
1/2, Young's modulus is 465GPa.
Embodiment 6 (TaC-50vol.%SiC, TAS50)
With size range is 200~600 purpose tantalum powder 67.92g, silica flour 11.28g and Graphite Powder 99 8.4g, and ball milling is 20 hours in resin container, crosses 200 mesh sieves, coldmoulding in the graphite jig of packing into afterwards, and the pressure that applies is 5MPa, puts into the hot pressing furnace hot pressed sintering.Temperature rise rate is 10 ℃/minute, is heated to 2050 ℃ of insulations 1 hour, and exerting pressure is 30MPa.Whole sintering process all is to carry out under argon shield, and the reaction product of acquisition is TaC through X-ray diffraction analysis, β-SiC and a small amount of TaSi
2The density that Archimedes's method records is 8.93g/cm
3, being 100.1% of theoretical density, this is attributed to than SiC density (3.22g/cm
3) high TaSi
2(density, 9.84g/cm
3) influence.Vickers' hardness is 13.9GPa, and flexural strength is 340MPa, and fracture toughness property is 5.2MPam
1/2, Young's modulus is 438GPa.
Comparative example (single-phase TaC, TAS0)
With size range is 200~600 purpose tantalum powder 101.84g and Graphite Powder 99 6.08g, and ball milling is 40 hours in resin container, crosses 200 mesh sieves, coldmoulding in the graphite jig of packing into afterwards, and the pressure that applies is 10MPa, puts into the hot pressing furnace hot pressed sintering.Temperature rise rate is 15 ℃/minute, is heated to 2050 ℃ of insulations 1 hour, and exerting pressure is 30MPa.Whole sintering process all is to carry out under argon shield, and the reaction product of acquisition is TaC through X-ray diffraction analysis.The density that Archimedes's method records is 10.93g/cm
3, be 75.5% of theoretical density.Vickers' hardness is 1.4GPa, and flexural strength is 69MPa, and fracture toughness property is 1.2MPam
1/2, Young's modulus is 136GPa.As seen synthetic TaC-SiC ceramic composite can be realized densification and enhancement by adding SiC under the same process condition, obtains room-temperature mechanical property preferably.
Following mask body is introduced the phase composition of TaC-SiC ceramic composite, density, and microstructure, Vickers' hardness, flexural strength and fracture toughness property, and high-temperature elastic modulus is with the variation relation of SiC content.
Fig. 1 (a)-(g) is that the X-ray diffraction phase composition of TaC-SiC ceramic composite is analyzed.With the increase of SiC content in the matrix material, the diffraction peak of SiC is grow gradually.(a) be single-phase TaC; (b) diffraction peak that does not have SiC in is because the diffraction peak of TaC is bigger by force, has hidden the diffraction peak of SiC.(e)-(g) contain a spot of TaSi in the show sample in
2Fig. 2 is the density of matrix material and the change curve that density increases with the SiC volumn concentration.When showing among the figure that content as SiC is greater than 10vol.%, the density of matrix material is all more than 95%, and its density is on a declining curve with the increase of SiC content.But, just there is a spot of TaSi in the sample of preparation when the content of SiC during greater than 30vol.%
2, because its density (9.84g/cm
3) greater than the density (3.22g/cm of SiC
3), the density value that causes being calculated is greater than 1.Fig. 3 (a)-(e) is the pattern of TaC-SiC ceramic composite glazed surface and distribute mutually (secondary electron phase).Greyish white form and aspect among the figure are TaC, and black is SiC mutually, and the SiC particle is uniform distribution in the TaC matrix, and a little reunion is arranged.Fig. 3 (a) and (b) in have a small amount of sealed porosity, corresponding their lower densityes.And scheme not have in (c)-(e) existence of sealed porosity, the increase of this explanation SiC content has promoted the densification of material.On the other hand, low melting point TaSi
2The existence of (2040 ℃) also may promote the densification of sample.Fig. 4 is the change curve of the Vickers' hardness of TaC-SiC ceramic composite with SiC content.With the increase of SiC content, the hardness of matrix material is in rising trend.The variation of this hardness is corresponding with the variation of density on the one hand; Be that (hardness, 26GPa) content increases the SiC higher than TaC hardness (15GPa), also improves the hardness of matrix material on the other hand.Fig. 5 is the flexural strength of TaC-SiC ceramic composite and the change curve that fracture toughness property increases with SiC content.The fracture toughness property of matrix material is in rising trend with the increase of SiC content.As the SiC content fracture toughness property value of tending towards stability 5.5MPam during greater than 30vol.%
1/2Flexural strength has maximum 341MPa at SiC content during for 10vol.%, and the raising with SiC content descends then.Fig. 6 is that the Young's modulus of TaC-SiC ceramic composite is with the variation of temperature curve.The high temperature rigid of TAS10 shown in the figure and TAS30 all is maintained to 1400 ℃, has shown high temperature application, and the TAS50 high temperature rigid is poor slightly.From above interpretation of result as can be seen, when the content of SiC was 10~30vol.%, matrix material can obtain better comprehensive mechanical property.
By embodiment 1, embodiment 2, embodiment 3, embodiment 4, embodiment 5, embodiment 6 and comparative example as seen, present method can original position be synthesized the TaC-SiC ceramic composite, when SiC content is 10~30vol.%, has better comprehensive mechanical property.
Claims (5)
1. TaC-SiC ceramic composite material synthesized by hot pressing at in-situ reaction is characterized in that: percentage composition meter by volume, and the content of 0<SiC≤50%, all the other are TaC; TaC becomes the phase-splitting reaction in to generate with two kinds of SiC, with tantalum powder, silica flour and Graphite Powder 99 is raw material, ball milling is 10~40 hours in resin container, the coldmoulding in the graphite jig of packing into after sieving, forming pressure 5~20MPa, sintering in being connected with the hot pressing furnace of argon gas, temperature rise rate are 10~15 ℃/minute, and sintering temperature is that 1950~2150 ℃, heat preservation sintering time are that 1~2 hour, sintering pressure are 30~40MPa.
2. according to the described TaC-SiC ceramic composite of claim 1, it is characterized in that: per-cent meter by volume, the content of SiC is 10~30%.
3. according to the described TaC-SiC ceramic composite of claim 1, it is characterized in that: the content of TaC and SiC, regulate according to the content of tantalum powder, silica flour and Graphite Powder 99 in the original proportioning.
4. according to the described TaC-SiC ceramic composite of claim 1, it is characterized in that: the tantalum powder of described adding, silica flour and Graphite Powder 99 size range are 200~600 orders.
5. according to the described TaC-SiC ceramic composite of claim 1, it is characterized in that: ball milling under the drying conditions in resin container.
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CN110818420B (en) * | 2019-11-25 | 2021-08-17 | 武汉科技大学 | SiC-doped TaxHf1-xC ceramic and preparation method thereof |
CN115521151A (en) * | 2022-09-28 | 2022-12-27 | 中国科学院上海硅酸盐研究所 | Discharge plasma sintering method of silicon carbide/tantalum carbide toughened ceramic |
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CN101024575A (en) * | 2006-02-17 | 2007-08-29 | 中国科学院金属研究所 | Method for preparing tantalum-aluminium-carbon ceramic by in-situ heat-pressing/solid-liquid phase reaction |
CN101033134A (en) * | 2006-03-10 | 2007-09-12 | 中国科学院金属研究所 | Original position reaction hot pressing synthesis TiB2-NbC-SiC refractory ceramics composite material and preparing method thereof |
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CN101024575A (en) * | 2006-02-17 | 2007-08-29 | 中国科学院金属研究所 | Method for preparing tantalum-aluminium-carbon ceramic by in-situ heat-pressing/solid-liquid phase reaction |
CN101033134A (en) * | 2006-03-10 | 2007-09-12 | 中国科学院金属研究所 | Original position reaction hot pressing synthesis TiB2-NbC-SiC refractory ceramics composite material and preparing method thereof |
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