CN100519477C - Method for preparing tantalum-aluminium-carbon ceramic by in-situ heat-pressing/solid-liquid phase reaction - Google Patents
Method for preparing tantalum-aluminium-carbon ceramic by in-situ heat-pressing/solid-liquid phase reaction Download PDFInfo
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- CN100519477C CN100519477C CNB2006100458443A CN200610045844A CN100519477C CN 100519477 C CN100519477 C CN 100519477C CN B2006100458443 A CNB2006100458443 A CN B2006100458443A CN 200610045844 A CN200610045844 A CN 200610045844A CN 100519477 C CN100519477 C CN 100519477C
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- powder
- alc
- solid
- liquid phase
- hot pressing
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- 239000007791 liquid phase Substances 0.000 title claims abstract description 14
- 239000000919 ceramic Substances 0.000 title claims abstract description 9
- 238000006243 chemical reaction Methods 0.000 title claims description 12
- 238000011065 in-situ storage Methods 0.000 title claims description 12
- 238000000034 method Methods 0.000 title claims description 12
- 238000003825 pressing Methods 0.000 title abstract 2
- -1 tantalum-aluminium-carbon Chemical compound 0.000 title abstract 2
- 238000007731 hot pressing Methods 0.000 claims abstract description 24
- 239000000843 powder Substances 0.000 claims abstract description 21
- 239000002994 raw material Substances 0.000 claims abstract description 8
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 6
- 238000000498 ball milling Methods 0.000 claims abstract description 6
- 238000005516 engineering process Methods 0.000 claims abstract description 6
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 6
- 239000010439 graphite Substances 0.000 claims abstract description 6
- 239000012071 phase Substances 0.000 claims description 14
- RQMIWLMVTCKXAQ-UHFFFAOYSA-N [AlH3].[C] Chemical compound [AlH3].[C] RQMIWLMVTCKXAQ-UHFFFAOYSA-N 0.000 claims description 10
- 229910052715 tantalum Inorganic materials 0.000 claims description 10
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 claims description 10
- 239000002131 composite material Substances 0.000 claims description 3
- 238000002360 preparation method Methods 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 2
- 230000001105 regulatory effect Effects 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 12
- 150000001875 compounds Chemical class 0.000 abstract description 9
- 230000007797 corrosion Effects 0.000 abstract description 2
- 238000005260 corrosion Methods 0.000 abstract description 2
- 238000010438 heat treatment Methods 0.000 abstract 1
- 238000004519 manufacturing process Methods 0.000 abstract 1
- 229910052756 noble gas Inorganic materials 0.000 abstract 1
- 239000007789 gas Substances 0.000 description 8
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 6
- 239000007795 chemical reaction product Substances 0.000 description 6
- 230000005540 biological transmission Effects 0.000 description 5
- 238000001228 spectrum Methods 0.000 description 4
- 238000002441 X-ray diffraction Methods 0.000 description 3
- 229910052786 argon Inorganic materials 0.000 description 3
- 238000000280 densification Methods 0.000 description 2
- 238000012856 packing Methods 0.000 description 2
- 239000003963 antioxidant agent Substances 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- 235000006708 antioxidants Nutrition 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 230000006378 damage Effects 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 150000001247 metal acetylides Chemical class 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
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Abstract
The invention relates to a manufacturing technology for processable sill like ceramic. The feature is that it uses Ta powder, Al powder and C powder as raw material, taking ball milling for 5-15 hours, pressing to cake shape under 10-20MPa, encasing into graphite mold, heating to 1100-1600 degree centigrade in hot-pressing furnace at 2-50 degree centigrade per minutes under protection of noble gas, taking home position hot pressing/ solid-liquid phase reacting for 0.5-4 hours, the hot pressing pressure is 20-40MPa. The invention could compound high purity, high intension, and corrosion proof tantalum aluminum carbon block material at low temperature and in short tie. The material could be used in the environment temperature over 1000 degree centigrade.
Description
Technical field
The present invention relates to process ceramic layered technology of preparing, provide a kind of in-situ hot pressing/solid-liquid phase reaction to prepare tantalum aluminium carbon (Ta especially
4AlC
3, Ta
2AlC and two-phase are compound) method of ceramic block material.
Background technology
Tantalum aluminium carbon (Ta
4AlC
3, Ta
2AlC and two-phase are compound) block materials is a kind of novel ternary layered material.It combines the plurality of advantages of pottery and metal, and the high-modulus of existing ceramic aspect is (as Ta
4AlC
3Be 259GPa), anti-oxidant, corrosion-resistant etc.; The performance that metallic substance is arranged again simultaneously, high conductivity, thermal conductivity, stronger destruction tolerance etc.At high-technology fields such as Aeronautics and Astronautics, nuclear industry, fuel cell, electronic information, ultrahigh-temperature structural parts the potential wide application prospect is arranged all.Although tantalum aluminium carbon (Ta
4AlC
3, Ta
2AlC and two-phase are compound) block materials has excellent properties like this, and the difficulty in the preparation has limited the research of its performance and its application.Up to now not about tantalum aluminium carbon (Ta
4AlC
3, Ta
2AlC and two-phase are compound) block materials prepares the report of aspect.Study the Ta-Al-C system in the document 1 (Z.Metallkd. (German Acta Metallurgica Sinica) 71,341 (1980)) at 700 ℃, 1000 ℃ phase equilibrium relationship, they have found Ta
2AlC and Ta
5Al
3Two kinds of double carbides of C, but fail to obtain pure Ta
2AlC does not study its relevant performance yet.Up to now, less than report about body material aspect.
Summary of the invention
The present invention has proposed a kind of in-situ hot pressing/solid-liquid phase reaction first and has prepared tantalum aluminium carbon (Ta
4AlC
3, Ta
2AlC and two-phase are compound) method of ceramic block material.Wherein, Ta
4AlC
3Determined its structure for discovery first and by transmission electron microscope observing and Theoretical Calculation.This method is with the Ta powder, and Al powder and C powder are raw material, at lesser temps, has synthesized high purity, fine and close tantalum aluminium carbon (Ta in the short period of time
4AlC
3, Ta
2AlC and two-phase are compound) block materials.
Technical scheme of the present invention is as follows:
A kind of in-situ hot pressing/solid-liquid phase reaction prepares the method for tantalum aluminium-carbon ceramic, and this method feature is:
1) raw material is formed and composition range:
Ta
2The stoichiometric ratio of AlC (being mol ratio) is respectively Ta:Al:C=4:(0.8-2.5): (1.8-3.5) and Ta:Al:C=2:(0.8-2.5): (0.7-1.5), synthetic Ta
4AlC
3With Ta
2The stoichiometric ratio of AlC two-phase composite material can be regulated between above two ratios.
2) preparation technology:
Raw material is through ball milling 5-15 hour, is cold-pressed into pie with the pressure of 10-20MPa, and in the graphite jig of packing into, (or under the vacuum, vacuum tightness is higher than 10 as protection gas being connected with rare gas element (as argon gas)
-1Pa) (be preferably 5-30 ℃/min) temperature rise rate and rise to 1100 ℃-1600 ℃ (being preferably 1350 ℃-1550 ℃) in-situ hot pressings/solid-liquid phase reaction 0.5-4 hour (being preferably 0.5-2 hour), hot pressing pressure is 20-40MPa (being preferably 30-40MPa) with 2-50 ℃/min in the hot pressing furnace.
Characteristics of the present invention are:
1. selecting for use raw material simple, is respectively Ta powder, Al powder and C powder;
2. utilized the existence of liquid phase to promote the carrying out of mass transfer diffusion process, so can be at low temperature (below 1600 ℃), the short period of time (generally in two hours) is synthetic;
3. by in-situ hot pressing/solid-liquid phase reaction, sintering and densification are carried out simultaneously, obtain the tantalum aluminium carbon (Ta of single-phase densification
4AlC
3, Ta
2AlC and two-phase are compound) block materials.
4. the material environment for use temperature that adopts the inventive method to obtain can be used under greater than 1000 ℃ ultrahigh-temperature in room temperature.
Description of drawings
Fig. 1 Ta
4AlC
3X-ray diffracting spectrum.
The stereoscan photograph of Fig. 2 reaction product.
The transmission electron microscope photo of Fig. 3 reaction product.
Fig. 4 Ta
4AlC
3And Ta
2AlC two-phase compound X-ray diffracting spectrum.
The transmission electron microscope photo of Fig. 5 reaction product.
Embodiment
Below by example in detail the present invention is described in detail.
Embodiment 1.
Ta powder 180.95 grams, Al powder 13.49 grams and C powder 9.00 grams; ball milling 8 hours; under the pressure of 15MPa, be cold-pressed into pie; pack in the graphite jig; rose to 1530 ℃ of in-situ hot pressings/solid-liquid phase reaction 0.5 hour with the temperature rise rate of 10 ℃/min in as the hot pressing furnace of protection gas being connected with rare gas element (argon gas), hot pressing pressure is 30MPa.The principal reaction product that obtains is Ta through the X-ray diffraction analysis
4AlC
3Corresponding X-ray diffracting spectrum, stereoscan photograph, and transmission electron microscope photo is listed in respectively on the accompanying drawing 1-3.
Embodiment 2.
Ta powder 180.95 grams, Al powder 14.84 grams and C powder 6.00 grams; ball milling 12 hours; under the pressure of 10MPa, be cold-pressed into pie; pack in the graphite jig; rose to 1450 ℃ of in-situ hot pressings/solid-liquid phase reaction 1 hour with the temperature rise rate of 20 ℃/min in as the hot pressing furnace of protection gas being connected with argon gas, hot pressing pressure is 35MPa.The principal reaction product that obtains is Ta through the X-ray diffraction analysis
4AlC
3And Ta
2The two-phase composite material of AlC.Corresponding X-ray diffracting spectrum is listed on the accompanying drawing 4.
Embodiment 3.
Ta powder 180.95 grams, Al powder 20.24 grams and C powder 6.00 grams, ball milling 12 hours is cold-pressed into pie under the pressure of 20MPa, and in the graphite jig of packing into, (vacuum tightness is 10 under vacuum
-2Pa) rose to 1350 ℃ of in-situ hot pressings/solid-liquid phase reaction 2 hours with the temperature rise rate of 10 ℃/min in the hot pressing furnace, hot pressing pressure is 40MPa.The principal reaction product that obtains is Ta through the X-ray diffraction analysis
2AlC.Corresponding transmission electron microscope photo is on accompanying drawing 5.
Claims (1)
1, a kind of in-situ hot pressing/solid-liquid phase reaction prepares the method for tantalum aluminium-carbon ceramic, and this method feature is:
1) raw material is formed and composition range:
With the Ta powder, Al powder and C powder are raw material, synthetic single-phase Ta
4AlC
3, Ta
2The stoichiometric ratio of AlC is respectively Ta:Al:C=4:(0.8-2.5): (1.8-3.5) and Ta:Al:C=2:(0.8-2.5): (0.7-1.5), synthetic: Ta
4AlC
3With Ta
2The stoichiometric ratio of AlC two-phase composite material is regulated between above two ratios;
2) preparation technology:
Raw material process ball milling 5-15 hour; pressure with 10-20MPa is cold-pressed into pie; pack in the graphite jig; rose to 1100 ℃ of-1600 ℃ of in-situ hot pressings/solid-liquid phase reaction 0.5-4 hour with the temperature rise rate of 2-50 ℃/min in as the hot pressing furnace under protection gas or the vacuum being connected with rare gas element, hot pressing pressure is 20-40MPa.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006100458443A CN100519477C (en) | 2006-02-17 | 2006-02-17 | Method for preparing tantalum-aluminium-carbon ceramic by in-situ heat-pressing/solid-liquid phase reaction |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006100458443A CN100519477C (en) | 2006-02-17 | 2006-02-17 | Method for preparing tantalum-aluminium-carbon ceramic by in-situ heat-pressing/solid-liquid phase reaction |
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| Publication Number | Publication Date |
|---|---|
| CN101024575A CN101024575A (en) | 2007-08-29 |
| CN100519477C true CN100519477C (en) | 2009-07-29 |
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| CNB2006100458443A Expired - Fee Related CN100519477C (en) | 2006-02-17 | 2006-02-17 | Method for preparing tantalum-aluminium-carbon ceramic by in-situ heat-pressing/solid-liquid phase reaction |
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Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101417878B (en) * | 2007-10-24 | 2011-06-29 | 中国科学院金属研究所 | TaC-SiC ceramic composite material synthesized by hot pressing at in-situ reaction |
| CN101948313A (en) * | 2010-08-20 | 2011-01-19 | 湖北工业大学 | Compact ZrO2/Ti2AlN composite material prepared by in-situ hot pressed sintering process |
| CN104909757A (en) * | 2015-05-22 | 2015-09-16 | 河海大学 | Method for preparing Ta2AlC monolithic ceramics by mechanical activating and hot-pressing |
| CN106800413B (en) * | 2015-11-26 | 2019-10-22 | 中国科学院金属研究所 | A kind of preparation method of yttrium aluminum-carbon ceramic material |
| CN108801492A (en) * | 2018-06-25 | 2018-11-13 | 江苏林大智能科技应用研究院有限公司 | The temperature sensor of high reliability |
| CN109608198A (en) * | 2019-01-17 | 2019-04-12 | 河海大学 | A kind of Ta2AlC-Ta4AlC3The preparation method of composite material |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1352317A (en) * | 2000-11-06 | 2002-06-05 | 中国科学院金属研究所 | Method for preparing titanium aluminium carbon block material by in-situ hot pressing/solid-liquid phase reaction |
| US20050262965A1 (en) * | 2004-05-26 | 2005-12-01 | Honeywell International, Inc. | Ternary carbide and nitride composites having tribological applications and methods of making same |
-
2006
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1352317A (en) * | 2000-11-06 | 2002-06-05 | 中国科学院金属研究所 | Method for preparing titanium aluminium carbon block material by in-situ hot pressing/solid-liquid phase reaction |
| US20050262965A1 (en) * | 2004-05-26 | 2005-12-01 | Honeywell International, Inc. | Ternary carbide and nitride composites having tribological applications and methods of making same |
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