CN1120816C - 一种钛碳化硅粉末的制备方法 - Google Patents
一种钛碳化硅粉末的制备方法 Download PDFInfo
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- CN1120816C CN1120816C CN98114247A CN98114247A CN1120816C CN 1120816 C CN1120816 C CN 1120816C CN 98114247 A CN98114247 A CN 98114247A CN 98114247 A CN98114247 A CN 98114247A CN 1120816 C CN1120816 C CN 1120816C
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- CN
- China
- Prior art keywords
- silicon carbide
- naf
- powder
- sic
- carbide powder
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- 238000004519 manufacturing process Methods 0.000 title abstract description 4
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 title abstract 2
- 229910009817 Ti3SiC2 Inorganic materials 0.000 claims abstract description 10
- 238000000034 method Methods 0.000 claims abstract description 10
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 10
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 10
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000002994 raw material Substances 0.000 claims abstract description 8
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 3
- 239000010936 titanium Substances 0.000 claims description 15
- 239000000843 powder Substances 0.000 claims description 8
- UGACIEPFGXRWCH-UHFFFAOYSA-N [Si].[Ti] Chemical compound [Si].[Ti] UGACIEPFGXRWCH-UHFFFAOYSA-N 0.000 claims description 6
- 238000006243 chemical reaction Methods 0.000 claims description 6
- 229910010271 silicon carbide Inorganic materials 0.000 claims description 5
- KLZUFWVZNOTSEM-UHFFFAOYSA-K Aluminum fluoride Inorganic materials F[Al](F)F KLZUFWVZNOTSEM-UHFFFAOYSA-K 0.000 claims description 3
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 claims description 3
- 239000012300 argon atmosphere Substances 0.000 claims description 2
- 239000012298 atmosphere Substances 0.000 abstract description 2
- 150000002222 fluorine compounds Chemical class 0.000 abstract description 2
- 239000007791 liquid phase Substances 0.000 description 6
- 239000000919 ceramic Substances 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- 239000006229 carbon black Substances 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 239000011863 silicon-based powder Substances 0.000 description 2
- 229910003910 SiCl4 Inorganic materials 0.000 description 1
- 229910009871 Ti5Si3 Inorganic materials 0.000 description 1
- 229910003074 TiCl4 Inorganic materials 0.000 description 1
- 229910008479 TiSi2 Inorganic materials 0.000 description 1
- 238000000137 annealing Methods 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 244000309464 bull Species 0.000 description 1
- VZGDMQKNWNREIO-UHFFFAOYSA-N carbon tetrachloride Substances ClC(Cl)(Cl)Cl VZGDMQKNWNREIO-UHFFFAOYSA-N 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 238000010574 gas phase reaction Methods 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- FDNAPBUWERUEDA-UHFFFAOYSA-N silicon tetrachloride Chemical compound Cl[Si](Cl)(Cl)Cl FDNAPBUWERUEDA-UHFFFAOYSA-N 0.000 description 1
- 238000003746 solid phase reaction Methods 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 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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- Carbon And Carbon Compounds (AREA)
Abstract
一种钛碳化硅粉末的制备方法，其特征在于：以Si、Ti、石墨粉及NaF或AlF3·NaF为原料，氟化物加入量为2～10wt%，Si、Ti、C以原子比3∶1∶2的化学计量加入，在氩气气氛下1200～1300℃，保温1～4小时反应生成Ti3SiC2。本发明简便易行，产率高，纯度高，适合于工业规模生产。
Description
本发明涉及功能陶瓷技术，特别提供了一种钛碳化硅陶瓷的固液相反应合成方法。
钛碳化硅(Ti3SiC2)是一种杰出的结构/功能陶瓷材料，它综合了金属的塑性、导电、导热、可加工和陶瓷的耐高温、高强度等特点，但是Ti3SiC2的合成却很难。文献1 Monatash Chem.98(1967)329利用TiH2、Si和石墨为原料，在2000℃反应合成Ti3SiC2。文献2 J.Less-Common Met.，26(1972)283和文献3 Matev.Res.Bull.，22(1987)1195用SiCl4、TiCl4、CCl4和H2做原料，通过气相沉积法制备Ti3SiC2。文献4 Matev.Lett.，22(1995)163是选择Ti、Si和碳黑为原料，用自慢延反应方法合成Ti3SiC2。文献5 J.Am.Cercom.Soc 78(1995)667是以Ti、Si和碳黑为原料，用电弧熔化法和后退火处理制备块状材料，但是所有这些方法合成的Ti3SiC2中都含有TiC或Ti5Si3、TiSi2等杂质，并且气相法、电弧熔化法等不适于工业化规模。
本发明的目的在于提供一种钛碳化硅粉末的制备方法，其简便易行，产率高，纯度高，适合于工业规模生产。
本发明提供了一种钛碳化硅粉末的制备方法，其特征在于：以Si、Ti、石墨粉及NaF或AlF3·NaF为原料，氟化物加入量为2～10wt％，Si、Ti、C以原子比3∶1∶2的化学计量加入，在氩气气氛下1200～1300℃，保温1～4小时反应生成Ti3SiC2。
本发明的实质是利用一种固液相的反应方法合成Ti3SiC2粉末，采用的原材料为Si、Ti和石墨粉末，液相生成剂是NaF或AlF3·NaF，由于氟化物在高温熔融成液相，Ti、Si和石墨粉溶入液相中反应生成Ti3SiC2粉末，再沉淀出来。由于熔融氟化物的存在，该方法称为固-液相反应法，以区别气相和固相反应。该方法可以描述为
本发明的产物中Ti3SiC2含量高，在普通的高温炉，保护气氛中即可进行，适合于工业规模生产，合成的Ti3SiC2颗粒呈棒状。
下面通过实施例详述本发明。
实施例1
Ti粉：72g，Si粉：14g，石墨粉：12g，加入NaF 4.9g，放入管式电炉中，通入动态Ar气保护，反应温度为1250℃，保温3hr，经清洗后，得到的Ti3SiC2的产率为93％。
实施例2
Ti粉：72g，Si粉：14g，石墨粉：12g，加入AlF3·NaF 10.8g，放入管式炉中，通入Ar气保护，反应温度为1210℃，保温时间4hr，经清洗得Ti3SiC2的产率为95％。
Claims (1)
1.一种钛碳化硅粉末的制备方法，其特征在于：以Si、Ti、石墨粉及NaF或AlF3·NaF为原料，氟化物加入量为2～10wt％，Si、Ti、C以原子比3∶1∶2的化学计量加入，在氩气气氛下1200～1300℃，保温1～4小时反应生成Ti3SiC2。
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN98114247A CN1120816C (zh) | 1998-08-19 | 1998-08-19 | 一种钛碳化硅粉末的制备方法 |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN98114247A CN1120816C (zh) | 1998-08-19 | 1998-08-19 | 一种钛碳化硅粉末的制备方法 |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1245155A CN1245155A (zh) | 2000-02-23 |
| CN1120816C true CN1120816C (zh) | 2003-09-10 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN98114247A Expired - Fee Related CN1120816C (zh) | 1998-08-19 | 1998-08-19 | 一种钛碳化硅粉末的制备方法 |
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Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| SE521882C2 (sv) * | 2001-06-21 | 2003-12-16 | Sandvik Ab | Förfarande för framställning av en enfassammansättning innefattande metall |
| JP6182082B2 (ja) * | 2013-03-15 | 2017-08-16 | 日本碍子株式会社 | 緻密質複合材料、その製法及び半導体製造装置用部材 |
| CN107319948A (zh) * | 2017-08-09 | 2017-11-07 | 泾县信达工贸有限公司 | 一种不粘无毒电饭煲内胆涂层 |
| CN108358205B (zh) * | 2018-03-07 | 2020-03-10 | 中南大学 | 一种Ti3SiC2粉体的合成方法 |
| CN110349839B (zh) * | 2019-06-21 | 2021-03-12 | 全球能源互联网研究院有限公司 | 一种p/n型碳化硅欧姆接触的制备方法 |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS63274665A (ja) * | 1987-04-30 | 1988-11-11 | Toshio Hirai | 多結晶質セラミックス |
| JPH01197374A (ja) * | 1987-12-24 | 1989-08-09 | Kernforschungsanlage Juelich Gmbh | 炭化珪素成形物を炭化珪素又は金属の他の成形物と接合する方法 |
| FR2675141A1 (fr) * | 1991-04-09 | 1992-10-16 | Europ Propulsion | Materiau composite a matrice ceramique avec interphase lamellaire entre fibres de renfort refractaires et matrice, et procede pour sa fabrication. |
-
1998
- 1998-08-19 CN CN98114247A patent/CN1120816C/zh not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS63274665A (ja) * | 1987-04-30 | 1988-11-11 | Toshio Hirai | 多結晶質セラミックス |
| JPH01197374A (ja) * | 1987-12-24 | 1989-08-09 | Kernforschungsanlage Juelich Gmbh | 炭化珪素成形物を炭化珪素又は金属の他の成形物と接合する方法 |
| 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 (fr) * | 1991-04-09 | 1992-10-16 | Europ Propulsion | Materiau composite a matrice ceramique avec interphase lamellaire entre fibres de renfort refractaires et matrice, et procede pour sa fabrication. |
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| Publication number | Publication date |
|---|---|
| CN1245155A (zh) | 2000-02-23 |
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