CN1234641C - Preparing method for Ti3 SiC2 material without TiC impurity - Google Patents
Preparing method for Ti3 SiC2 material without TiC impurity Download PDFInfo
- Publication number
- CN1234641C CN1234641C CN 03133510 CN03133510A CN1234641C CN 1234641 C CN1234641 C CN 1234641C CN 03133510 CN03133510 CN 03133510 CN 03133510 A CN03133510 A CN 03133510A CN 1234641 C CN1234641 C CN 1234641C
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- China
- Prior art keywords
- tic
- sintering
- sic
- sic2
- impurity
- Prior art date
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- 239000012535 impurity Substances 0.000 title claims abstract description 20
- 239000000463 material Substances 0.000 title abstract description 18
- 238000000034 method Methods 0.000 title abstract description 7
- 238000005245 sintering Methods 0.000 claims abstract description 31
- 238000002360 preparation method Methods 0.000 claims abstract description 13
- 239000002994 raw material Substances 0.000 claims abstract description 6
- 229910052751 metal Inorganic materials 0.000 claims abstract description 5
- 239000002184 metal Substances 0.000 claims abstract description 5
- 229910052782 aluminium Inorganic materials 0.000 claims description 16
- 239000004411 aluminium Substances 0.000 claims description 10
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 10
- 238000002156 mixing Methods 0.000 claims description 9
- 238000001513 hot isostatic pressing Methods 0.000 abstract 2
- 229910009816 Ti3Si Inorganic materials 0.000 abstract 1
- 230000003026 anti-oxygenic effect Effects 0.000 abstract 1
- 229910010293 ceramic material Inorganic materials 0.000 abstract 1
- 238000002050 diffraction method Methods 0.000 description 6
- 230000003647 oxidation Effects 0.000 description 6
- 238000007254 oxidation reaction Methods 0.000 description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 4
- 229910002804 graphite Inorganic materials 0.000 description 4
- 239000010439 graphite Substances 0.000 description 4
- 239000000919 ceramic Substances 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 230000004584 weight gain Effects 0.000 description 3
- 235000019786 weight gain Nutrition 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 239000000956 alloy Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 230000008030 elimination Effects 0.000 description 1
- 238000003379 elimination reaction Methods 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 238000007731 hot pressing Methods 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
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Abstract
The present invention relates to a preparative technique of a Ti3 SiC2 material without TiC impurities, more specifically a preparation method of a Ti3 SiC2 material without TiC impurities. A metal Al is added in a raw material for preparing the Ti3 SiC2 ceramic material, and after the metal Al is uniformly mixed with the raw material, hot pressed sintering or hot isostatic pressing sintering is carried out, the sintering temperature is from 1350 to 1650 DEG C, the sintering time is from 0.5 to 2 hours, and Ti3Si<1-x>Al<x>C2 sosoloid is formed, wherein x=0.02 to 0.2. The present invention has the advantages that homogeneous and compact material of a Ti3 SiC2 body in which a small quantity of Al is doped under the condition of hot pressed sintering or hot isostatic pressing sintering at the temperature of 1350 to 1650 DEG C for 0.5 to 2 hours and no containing of TiC; the intensity and the hardness are equivalent to the intensity and the hardness of Ti3 SiC2 in which the Al is not doped, but high-temperature antioxygenic performance is greatly enhanced.
Description
Technical field
What the present invention relates to not have TiC impurity contains aluminium Ti
3SiC
2The technology of preparing of material is specially a kind of by mixing Al elimination TiC impurity raising Ti
3SiC
2The method of body material purity.
Background technology
Ti
3SiC
2It is a kind of novel tertiary stratiform processable ceramic, it integrates the conduction, heat conduction of high temperature resistant, high strength, high-modulus, low-gravity and the metal of pottery, easily processing and thermal shock resistance, therefore has a wide range of applications in fields such as Aeronautics and Astronautics, boats and ships, nuclear industry.Yet, the preparation method who adopts comprises reaction hot-pressing sintering (U.S.'s ceramics meeting magazine at present, J Am Ceram Soc 79:1953,1996), solid-liquid phase reaction original position densification (investigation of materials innovation, Mater Res Innovat 2:142,1998) spread fine pressure (solid ion, Solid State Inonics 59:101,1997 such as synthetic after heat, certainly; Material wall bulletin, Mater Lett22:163,1995) etc. technology synthetic Ti
3SiC
2All contain TiC impurity phase in the body material.Existing research work shows that the existence of impurity TiC makes Ti
3SiC
2High-temperature oxidation resistance reduce, the therefore essential impurity TiC that eliminates is to improve Ti
3SiC
2Purity and high-temperature oxidation resistance.
Though done a lot of improvement in research in the past or the invention in the adjustment of material composition and preparation method, the impurity of TiC is difficult to all eliminate that (U.S.'s ceramics is understood magazine, J Am Ceram Soc 78:667,1995; The material proceedings, Mater Trans JIM 41:606,2000; Alloy and compound magazine, J Alloy Comp 285:85,1999).
Summary of the invention
The invention provides a kind of by mixing a small amount of Al raising Ti
3SiC
2The no TiC impurity of purity preparation contain aluminium Ti
3SiC
2The method of material.
Technical scheme of the present invention is:
A kind of TiC of nothing impurity contain aluminium Ti
3SiC
2Preparation methods is at Ti
3SiC
2Add metal A l in the preparation raw material of stupalith, behind the uniform mixing, carry out hot pressed sintering or HIP sintering, sintering temperature is 1350-1650 ℃, and sintering time is 0.5-2 hour, forms Ti
3Si
1-xAl
xC
2Sosoloid, x=0.02-0.2 wherein, promptly the atomic ratio of Al and Si is 1: 49-1: 4.
Sintering atmosphere is an Ar gas.
Described hot pressed sintering pressure is 25-40MPa.
Described HIP sintering pressure is 30-70MPa.
Ti of the present invention
3SiC
2The starting material of material preparation are Ti, Si, Al and powdered graphite.
The invention has the beneficial effects as follows:
1, the present invention makes Ti by mix a small amount of Al in raw material
3SiC
2Purity increase substantially, contain aluminium Ti with what hot pressed sintering or HIP sintering method had been prepared no TiC impurity
3SiC
2The body material, Ti
3SiC
2The body material is even, fine and close.
2, method of the present invention is simple, and adopting Ti, Si, Al and powdered graphite is raw material, and under 1350-1650 ℃, 0.5-2 hour, hot pressed sintering or HIP sintering get final product.
3, the no TiC impurity of the present invention preparation contains aluminium Ti
3SiC
2The body material, its intensity and hardness and do not mix the Ti of Al
3SiC
2Quite, but have extraordinary high-temperature oxidation resistance.
Description of drawings
Fig. 1 is that the Al content of embodiment 1 is to Ti
3SiC
2In the TiC foreign matter content influence X-line diffraction analysis curve.
Fig. 2 is not for containing the Ti of Al
3SiC
2And contain 10at%Al Ti
3SiC
2The oxidation weight gain curve of body material.
Embodiment
With Ti, Si, Al and powdered graphite uniform mixing 12 hours in the ball mill mixing machine, wherein to account for the atomic percent of Si content be 1at%, 3at%, 5at%, 7at%, 9at%, 10at% to the content of Al.Under Ar gas atmosphere, 1500 ℃ of hot pressed sinterings 1 hour, pressure is 30MPa.With the add-on of X-line diffraction analysis Al to Ti
3SiC
2In the influence (Fig. 1) of TiC content, as can be seen from the figure the content along with the increase TiC of Al content reduces gradually, TiC was thoroughly eliminated when the atomic percent that accounts for Si content when the content of Al was 5at%, 7at%, 9at%, 10at%.
With Ti, Si, Al and powdered graphite uniform mixing 12 hours in the ball mill mixing machine, wherein to account for the atomic percent of Si content be 10at% to the content of Al.Under Ar gas atmosphere, 1550 ℃ of HIP sintering 0.5 hour, pressure is 50MPa.Prepared material does not contain TiC impurity.Fig. 2 does not contain the Ti of Al when containing 10at%Al
3SiC
21100 ℃ oxidation weight gain experimental result, owing to mixing Al and having eliminated TiC impurity antioxidant property is obviously improved as can be seen, oxidation weight gain is from 0.082kg/m
2Reduce to 0.003kg/m
2
Difference from Example 1 is:
1450 ℃ of hot pressed sinterings 2 hours, pressure was 40MPa, formed sosoloid, and wherein to account for the atomic percent of Si content be 12% to the content of Al, and TiC is thoroughly eliminated with X-line diffraction analysis.
Difference from Example 1 is:
1600 ℃ of HIP sintering 0.5 hour, pressure was 60MPa, formed sosoloid, and wherein to account for the atomic percent of Si content be 25% to the content of Al, and TiC is thoroughly eliminated with X-line diffraction analysis.
Difference from Example 1 is:
1550 ℃ of hot pressed sinterings 1.5 hours, pressure was 25MPa, formed sosoloid, and wherein to account for the atomic percent of Si content be 15% to the content of Al, and TiC is thoroughly eliminated with X-line diffraction analysis.
Difference from Example 1 is:
1650 ℃ of hot pressed sinterings 1 hour, pressure was 40MPa, formed sosoloid, and wherein to account for the atomic percent of Si content be 20% to the content of Al, and TiC is thoroughly eliminated with X-line diffraction analysis.
Claims (4)
1, a kind of TiC of nothing impurity contains aluminium Ti
3SiC
2Preparation methods is characterized in that: at Ti
3SiC
2Add metal A l in the preparation raw material of stupalith, behind the uniform mixing, carry out hot pressed sintering or HIP sintering, sintering temperature is 1350-1650 ℃, and sintering time is 0.5-2 hour, forms Ti
3Si
1-xAl
xC
2Sosoloid, wherein x=0.02-0.2.
2, contain aluminium Ti according to the described no TiC impurity of claim 1
3SiC
2Preparation methods is characterized in that: sintering atmosphere is an Ar gas.
3, contain aluminium Ti according to the described no TiC impurity of claim 1
3SiC
2Preparation methods is characterized in that: described hot pressed sintering pressure is 25-40MPa.
4, contain aluminium Ti according to the described no TiC impurity of claim 1
3SiC
2Preparation methods is characterized in that: described HIP sintering pressure is 30-70MPa.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 03133510 CN1234641C (en) | 2003-05-28 | 2003-05-28 | Preparing method for Ti3 SiC2 material without TiC impurity |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 03133510 CN1234641C (en) | 2003-05-28 | 2003-05-28 | Preparing method for Ti3 SiC2 material without TiC impurity |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1552662A CN1552662A (en) | 2004-12-08 |
| CN1234641C true CN1234641C (en) | 2006-01-04 |
Family
ID=34323060
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 03133510 Expired - Fee Related CN1234641C (en) | 2003-05-28 | 2003-05-28 | Preparing method for Ti3 SiC2 material without TiC impurity |
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| Country | Link |
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Families Citing this family (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100364928C (en) * | 2006-01-12 | 2008-01-30 | 上海大学 | Ceramet Ti3SiC2 powder preparation method |
| CN100422109C (en) * | 2006-05-12 | 2008-10-01 | 中国科学院金属研究所 | Aluminium oxide silicon titanium carbonate/aluminium oxide lamina composite material and preparing method |
| CN100422113C (en) * | 2006-05-12 | 2008-10-01 | 中国科学院金属研究所 | Silicon-aluminium titanium carbonate solid-solution material and preparing method |
| US8877099B2 (en) * | 2011-01-26 | 2014-11-04 | Ngk Insulators, Ltd. | Ti3SiC2 based material, electrode, spark plug and manufacturing method thereof |
| CN102659407B (en) * | 2012-04-05 | 2014-04-23 | 中国科学院金属研究所 | Method for preparing Lu4Si2O7N2 ceramic material by in-situ reaction |
| CN103351164A (en) * | 2013-05-23 | 2013-10-16 | 安泰科技股份有限公司 | High-purity and high-performance titanium silicon carbide ceramic block material and preparation method thereof |
| CN106966749B (en) * | 2016-06-03 | 2018-05-29 | 北京航空航天大学 | It is a kind of to use Ti3Si(Al)C2The method of modified thermostructural composite |
| CN110128145A (en) * | 2019-06-26 | 2019-08-16 | 辽宁工业大学 | A kind of synthesis high-purity Ti3SiC2Method |
| CN116178020A (en) * | 2023-03-03 | 2023-05-30 | 青岛大学 | Ceramic connector material of solid oxide fuel cell and preparation method thereof |
| CN116178021A (en) * | 2023-03-03 | 2023-05-30 | 青岛大学 | Ceramic connector material of solid oxide fuel cell |
-
2003
- 2003-05-28 CN CN 03133510 patent/CN1234641C/en not_active Expired - Fee Related
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| Publication number | Publication date |
|---|---|
| CN1552662A (en) | 2004-12-08 |
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