CN1120817C - In-situ hot pressing solid-liquid phase reaction process to prepare silicon titanium-carbide material - Google Patents
In-situ hot pressing solid-liquid phase reaction process to prepare silicon titanium-carbide material Download PDFInfo
- Publication number
- CN1120817C CN1120817C CN98114365A CN98114365A CN1120817C CN 1120817 C CN1120817 C CN 1120817C CN 98114365 A CN98114365 A CN 98114365A CN 98114365 A CN98114365 A CN 98114365A CN 1120817 C CN1120817 C CN 1120817C
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- China
- Prior art keywords
- hot pressing
- liquid phase
- phase reaction
- silicon titanium
- carbide material
- Prior art date
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- 229910052710 silicon Inorganic materials 0.000 title claims abstract description 14
- 238000006243 chemical reaction Methods 0.000 title claims abstract description 13
- 238000007731 hot pressing Methods 0.000 title claims abstract description 12
- 239000000463 material Substances 0.000 title claims abstract description 11
- 239000007791 liquid phase Substances 0.000 title claims abstract description 10
- 238000011065 in-situ storage Methods 0.000 title claims abstract description 7
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 title abstract description 4
- 239000010703 silicon Substances 0.000 title abstract description 4
- MTPVUVINMAGMJL-UHFFFAOYSA-N trimethyl(1,1,2,2,2-pentafluoroethyl)silane Chemical compound C[Si](C)(C)C(F)(F)C(F)(F)F MTPVUVINMAGMJL-UHFFFAOYSA-N 0.000 title abstract 2
- 238000000034 method Methods 0.000 claims abstract description 12
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 10
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 10
- 238000005245 sintering Methods 0.000 claims abstract description 7
- 239000002994 raw material Substances 0.000 claims abstract description 5
- 239000010936 titanium Substances 0.000 claims description 18
- UGACIEPFGXRWCH-UHFFFAOYSA-N [Si].[Ti] Chemical compound [Si].[Ti] UGACIEPFGXRWCH-UHFFFAOYSA-N 0.000 claims description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 4
- 229910052786 argon Inorganic materials 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- 239000000203 mixture Substances 0.000 abstract description 6
- 229910009817 Ti3SiC2 Inorganic materials 0.000 abstract description 2
- 238000011031 large-scale manufacturing process Methods 0.000 abstract description 2
- 239000011261 inert gas Substances 0.000 abstract 1
- 229910052799 carbon Inorganic materials 0.000 description 6
- 239000013590 bulk material Substances 0.000 description 5
- 229910002804 graphite Inorganic materials 0.000 description 4
- 239000010439 graphite Substances 0.000 description 4
- 238000002844 melting Methods 0.000 description 3
- 230000008018 melting Effects 0.000 description 3
- 229910010293 ceramic material Inorganic materials 0.000 description 2
- 238000001513 hot isostatic pressing Methods 0.000 description 2
- 239000000976 ink Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000013001 point bending Methods 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 229910003074 TiCl4 Inorganic materials 0.000 description 1
- 238000000137 annealing Methods 0.000 description 1
- 238000000498 ball milling Methods 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- VZGDMQKNWNREIO-UHFFFAOYSA-N carbon tetrachloride Substances ClC(Cl)(Cl)Cl VZGDMQKNWNREIO-UHFFFAOYSA-N 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000011812 mixed powder Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 229910010271 silicon carbide Inorganic materials 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229910000048 titanium hydride Inorganic materials 0.000 description 1
- XJDNKRIXUMDJCW-UHFFFAOYSA-J titanium tetrachloride Chemical compound Cl[Ti](Cl)(Cl)Cl XJDNKRIXUMDJCW-UHFFFAOYSA-J 0.000 description 1
- 238000007740 vapor deposition Methods 0.000 description 1
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- Ceramic Products (AREA)
Abstract
The present invention relates to a method for preparing a silicon titanium-carbide material by in-situ hot pressing solid-liquid phase reaction, which is characterized in that Ti, Si and graphite powder are used as raw materials and are mixed by the nonstoichiometry (molar ratio) of Ti: Si: C=(1.5-2.5): 1: (1.7-2), and then hot pressing sintering is carried out to the mixture for 0.2 to 4 hours under inert gas protection; the temperature of the hot pressing sintering is from 1500 to 1650 DEG C, and the pressure of the hot pressing sintering is from 35 to 45MPa. Ti3SiC2 prepared by the method of the present invention has the advantages of high purity and stable mechanical property and is suitable for large-scale production.
Description
The invention relates to the preparation of ceramic materials, and particularly provides a method for preparing a silicon titanium carbide body material by in-situ hot pressing solid-liquid phase reaction.
Silicon titanium carbide (Ti)3SiC2) Is an excellent high-temperature structural/functional material, and isOrganically combines the characteristics of electric conduction, heat conduction, plasticity and easy processing of metal and the characteristics of high temperature resistance, oxidation resistance, high strength, low specific gravity and the like of ceramic materials. However, the synthesis of silicon titanocarbide is difficult, and document (1) describes the use of TiH2Si and graphite powder are reacted at 2000 ℃ to synthesize silicon titanocarbide, but this method can be limited to laboratory level. SiCl for document (2)4、TiCl4、CCl4And H2As a raw material, Ti is prepared by a vapor deposition method3SiC2A film. Document (3) production of Ti by self-mandril reaction plus hot isostatic pressing sintering3SiC2Bulk materials, the raw materials of choice are Ti, Si and carbon inks, but the reaction temperature and chemical composition of this method are difficult to control accurately and the process of hot isostatic pressing is not easy to achieve. Document (4) is a method of preparing Ti from raw powders of Ti, Si and carbon ink by arc melting and post-annealing3SiC2The bulk material, however, has a high content of impurities, and the reaction temperature is not easy to be precisely controlled.
The object of the present invention is to provide aTi3SiC2Method for producing bulk material, Ti produced by the method3SiC2High purity and stable mechanical property, and is suitable for industrial large-scale production.
The invention provides a method for preparing a silicon titanium carbide body material by in-situ hot pressing solid-liquid phase reaction, which is characterized by comprising the following steps: mixing Ti, Si and graphite powder which are used as raw materials according to the components deviating from the stoichiometric ratio (the molar ratio is 1.5-2.5) to 1 (1.7-2), and carrying out hot-pressing sintering for 0.2-4 hours under the protection of argon at the temperature of 1500-1650 ℃ and the pressure of 35-45 MPa.
The essence of the invention is that the Ti is prepared by utilizing a solid-liquid phase reaction in-situ hot pressing3SiC2The bulk material and the liquid phase are generated by high-temperature melting of Si, and Ti and C are dissolved in liquid Si to generate Ti through chemical reaction3SiC2Then precipitating out. The reaction can be described as:
ti in the product of the invention3SiC2High content of Ti obtained3SiC2Bulk material density greater than 99%, bending strength sigmab≥500MPa，KIC≥10MPa·m1/2The superplastic deformation amount reaches 40 percent at 1150 ℃.
The innovation of the invention is that the melting point of Si is 1420 ℃, so that liquid phase Si is generated when the mixed powder of Ti, Si and C is added to the temperature of more than 1420 ℃, and the liquid phase Si can promote Ti3SiC2The synthesis reaction of (2) can also accelerate sintering, so that a compact block material can be obtained.
The present invention is described in detail below by way of examples.
Example 1
Ti, Si and C are 1.8: 1: 1.6 (mol ratio), ball milling is carried out for 10 hours, then dry pressing forming is carried out, the mixture is put into a graphite mould, Ar is introduced for protection, the mixture is put into a graphite resistance furnace, the reaction temperature is 1570 ℃, the temperature is kept for 1 hour, the pressure is 40MPa, the density of the obtained block material is 99.5 percent, and Ti, Si and C are mixed according to the mol ratio3SiC2The content is 96%. Three point bending strength of sigmabMore than or equal to 520MPa and fracture toughness KIC＝10MPa·m1/2。
Example 2
The molar ratio of Ti to Si to C is 19: 1: 1.65, the mixture is ball-milled for 10 hours, then is dry-pressed and molded, and then is put into a graphite die, Ar is introduced for protection, the mixture is heated to 1600 ℃ in a graphite resistance furnace, the temperature is kept for 1 hour, the pressure is 40MPa, the density of the obtained block material is 99.8 percent, and the Ti and Si are mixed together to obtain the bulk material3SiC2The content was 95%. Three point bending strength of sigmabMore than or equal to 540MPa and fracture toughness KIC＝10MPa·m1/2。
Claims (1)
1. A method for preparing a silicon titanium carbide body material by in-situ hot pressing solid-liquid phase reaction is characterized by comprising the following steps: mixing Ti, Si and graphite powder which are used as raw materials according to the components deviating from the stoichiometric ratio (the molar ratio is 1.5-2.5) to 1 (1.7-2), and carrying out hot-pressing sintering for 0.2-4 hours under the protection of argon at the temperature of 1500-1650 ℃ and the pressure of 35-45 MPa.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN98114365A CN1120817C (en) | 1998-10-07 | 1998-10-07 | In-situ hot pressing solid-liquid phase reaction process to prepare silicon titanium-carbide material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN98114365A CN1120817C (en) | 1998-10-07 | 1998-10-07 | In-situ hot pressing solid-liquid phase reaction process to prepare silicon titanium-carbide material |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1250039A CN1250039A (en) | 2000-04-12 |
| CN1120817C true CN1120817C (en) | 2003-09-10 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN98114365A Expired - Fee Related CN1120817C (en) | 1998-10-07 | 1998-10-07 | In-situ hot pressing solid-liquid phase reaction process to prepare silicon titanium-carbide material |
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| Country | Link |
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| CN (1) | CN1120817C (en) |
Families Citing this family (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| SE521882C2 (en) | 2001-06-21 | 2003-12-16 | Sandvik Ab | Process for making a single-phase composition comprising metal |
| CN100455688C (en) * | 2006-08-16 | 2009-01-28 | 中国科学院上海硅酸盐研究所 | Preparation method of titanium carbosilicide based gradient material and in situ reaction |
| CN102992765B (en) * | 2012-11-09 | 2014-03-05 | 航天材料及工艺研究所 | Preparation method of tungsten-doped titanium-silicon-aluminum-carbon ceramic block body material |
| FR3032449B1 (en) | 2015-02-09 | 2017-01-27 | Office Nat D'etudes Et De Rech Aerospatiales (Onera) | CERMET MATERIALS AND PROCESS FOR PRODUCING SUCH MATERIALS |
| CN107319948A (en) * | 2017-08-09 | 2017-11-07 | 泾县信达工贸有限公司 | It is a kind of not glue nontoxic inner container of electric cooker coating |
| CN110128145A (en) * | 2019-06-26 | 2019-08-16 | 辽宁工业大学 | A kind of synthesis high-purity Ti3SiC2Method |
| CN111192707B (en) * | 2020-01-06 | 2020-09-29 | 湖南湘江电缆有限公司 | High-temperature-resistant and aging-resistant power cable |
| CN112331392B (en) * | 2020-11-18 | 2022-06-17 | 湖南华菱线缆股份有限公司 | Impact-resistant oxidation-resistant waterproof cable |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS63274665A (en) * | 1987-04-30 | 1988-11-11 | Toshio Hirai | Polycrystalline ceramics having plastic deformability |
| JPH01197374A (en) * | 1987-12-24 | 1989-08-09 | Kernforschungsanlage Juelich Gmbh | Method for bonding silicon carbide molded body to silicon carbide or metal molded body |
| FR2675141A1 (en) * | 1991-04-09 | 1992-10-16 | Europ Propulsion | Composite material with a ceramic matrix with lamellar interphase between refractory reinforcing fibres and matrix, and process for its manufacture |
-
1998
- 1998-10-07 CN CN98114365A patent/CN1120817C/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS63274665A (en) * | 1987-04-30 | 1988-11-11 | Toshio Hirai | Polycrystalline ceramics having plastic deformability |
| JPH01197374A (en) * | 1987-12-24 | 1989-08-09 | Kernforschungsanlage Juelich Gmbh | Method for bonding silicon carbide molded body to silicon carbide or metal molded body |
| US4961529A (en) * | 1987-12-24 | 1990-10-09 | Kernforschungsanlage Julich Gmbh | Method and components for bonding a silicon carbide molded part to another such part or to a metallic part |
| FR2675141A1 (en) * | 1991-04-09 | 1992-10-16 | Europ Propulsion | Composite material with a ceramic matrix with lamellar interphase between refractory reinforcing fibres and matrix, and process for its manufacture |
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| Publication number | Publication date |
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| CN1250039A (en) | 2000-04-12 |
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