CN1587203A - High toughness high hardness silicon carbide ceramic lqiuid phase sintering method - Google Patents
High toughness high hardness silicon carbide ceramic lqiuid phase sintering method Download PDFInfo
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- CN1587203A CN1587203A CN 200410062956 CN200410062956A CN1587203A CN 1587203 A CN1587203 A CN 1587203A CN 200410062956 CN200410062956 CN 200410062956 CN 200410062956 A CN200410062956 A CN 200410062956A CN 1587203 A CN1587203 A CN 1587203A
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Abstract
The liquid phase sintering process of high toughness and high hardness silicon carbide ceramic features adopting RE oxide and aluminum nitride as co-sintering agent. The present invention can obtain high performance SiC ceramic at relatively lower temperature of 1800-1900 deg.c, and the SiC ceramic has toughness of 6-8 MPa.m1/2 and other obviously raised performance.
Description
Technical Field
The invention relates to the field of manufacturing processes of inorganic solid materials, belongs to the manufacturing technology of silicon carbide ceramics, and particularly relates to a high-toughness and high-hardness silicon carbide ceramic liquid-phase sintering method.
Background
Silicon carbideThe normal pressure sintering method of the ceramic has two types: one is a solid phase sintering process and the other is a liquid phase sintering process. Silicon carbide is a strong covalent compound and is difficult to sinter and densify, and S.Prochazka in the last seventies[1]Firstly, a small amount of boron (B) and carbon (C) are used as additives, and a SiC-B-C system is densified by solid phase sintering at the temperature of more than 2100 ℃. The solid-phase sintered SiC ceramic has high hardness but high fracture toughness (3MPa. m)1/2) And the strength (200-300 MPa) is low, and the sintering temperature is too high.
The liquid phase sintering method overcomes many of the disadvantages of the solid phase sintering method, and the most typical liquid phase sintering method which is being used most is SiC-Al2O3-Y2O3System of[2]With Al2O3And Y2O3Densification was achieved above 1900 ℃ for the sintering aid, a disadvantage of this system is:
(1) al in the system2O3And Y2O3With SiO present on the SiC surface2The eutectic temperature is too low, only 1360 ℃, liquid phase appears too early, and the mass is easy to lose in the high-temperature sintering process.
(2) Thermochemical reaction at high temperature:
the above decomposition reactions lead to mass loss (high ignition loss) and also tend to roughen the surface, so that a powder bed (powder burying) is often required to reduce the mass loss.
Using AlN instead of Al2O3And rare earth oxide is added as sintering aid to overcome Al2O3-Y2O3The defect of sintering aid. AlN-based sintering aids have been successfully used for Si3N4Atmospheric liquid phase sintering of ceramics[3]However, only hot pressing and high nitrogen pressure sintering reports have been reported for SiC ceramics[4，5]The invention is to first convert AlN-Re into2O3(Re is a rare earth element) and is successfully used for the SiC atmospheric pressure liquid phase sintering.
Disclosure of Invention
The invention aims to overcome the defects of the existing solid-liquid phase sintering method and provide the silicon carbide ceramic normal-pressure liquid-phase sintering method with high toughness and high hardness.
The purpose of the invention is realized according to the following scheme:
a high-toughness and-hardness silicon carbide ceramic normal-pressure liquid-phase sintering method features that rare-earth oxide and aluminium nitride are used as sintering aid.
The mixing weight percentage of the silicon carbide, the rare earth oxide and the aluminum nitride sintering aid is respectively 60-98% and 40-2% or wider;
the rare earth oxide is lanthanide rare earth oxide or mixed rare earth oxide;
the rare earth oxide is lanthanide La2O3To Lu2O3Any one of 15 rare earth oxides;
the rare earth oxide is lanthanide La2O3To Lu2O3Any two or more rare earth oxides of 15 rare earth oxides;
the above rare earth oxide is Y2O3And from La2O3To Lu2O3Any one of 15 rare earth oxides;
the rare earth oxide is yttrium oxide (Y)2O3)。
The invention can be sintered at lower temperature to obtain high-performance SiC ceramic, the indentation hardness can reach more than 20GPa, and the toughness can reach 6-8MPa1/2The sintering temperature is reduced to 1800-1900 ℃.
Detailed Description
The invention relates to liquid phase sintering SiC ceramic under normal pressure argon or nitrogen atmosphere.
(1) SiC is β -SiC or α -SiC, one or two of mixed powder is adopted as the raw material, and the sintering aid is AlN with the purity of more than 99.5 percent (Beijing steel research)Total institute product) and rare earth oxide (baotou rare earth materials institute product), the proportion (wt%) of SiC and sintering aid is AlN: 60-98%, Re2O3：40-2％。
(2) Mixing raw materials: the above mixture is treated with Si in anhydrous alcohol3N4Or SiC pellets are used as grinding media, after mixed grinding, the media pellets are filtered out, the slurry is dried and sieved to obtain mixed powder.
(3) Molding: by dry or cold static pressure (2-3T/cm)2) And (5) molding.
(4) And (3) sintering: the formed powder blank is placed in a graphite tongs pan paved with Boron Nitride (BN) powder, the temperature is raised to about 1800 ℃ or higher in a graphite tube furnace filled with atmospheric pressure argon or nitrogen, the sintering is carried out for 2 to 3 hours or longer, and the sintering system can be adjusted according to the requirements of microstructures.
(5) Hot-pressing and sintering: the mixed powder is directly put into a graphite pressing die and is hot-pressed for 1 to 3 hours in a hot-pressing furnace at the temperature of 1800-1900 ℃ under the atmospheric pressure argon or nitrogen atmosphere.
After sintering, the SiC ceramic can be obtained by annealing treatment or direct cooling.
Reference documents:
[1]Prochazka，S.，“The role of boron and carbon in the sintering of siliconcarbide”In“Special Ceramics”(Vol.6)，ed.P.Popper.Br.Ceram.Res.Assoc.，Stoke on Trent，1975，pp.171-181
[2]Omori，M.and Takei，H.，“Pressureless sintering of SiC”，J.Am.Ceram.Soc.，1982，65，C-92
[3]Zhen-Kun Huang，Anatoly Rosenflanz，and I-Wei Chen“PressurelessSintering of Si3N4Ceramics Using AlN and Rare-Earth Oxides”，J.Am.Ceram.Soc.，80(5)1256-1262(1997)
[4]You Zhou，Kiyoshi Hirao，Yukihiko Yamauchi，Shuzo Kanzaki“Tailoringthe mechanical properties of silicon carbide ceramics by modification of theintergranular phase chemistry and microstructure”J.Euro.Ceram.Soc.，22(2002)2689-2696
[5]Georg Rixecker，Koushik Biswas，Arno Rosinus，Siddharth Sharma，IngoWiedmann，Fritz Aldinger“Fracture properties of SiC ceramics withoxynitride additives”J.Euro.Ceram.Soc.22(2002)2669-2675
Claims (7)
1. a liquid-phase sintering method for high-toughness and-hardness silicon carbide ceramics features that rare-earth oxide and aluminium nitride are used as sintering aid.
2. The liquid phase sintering process of claim 1 wherein the silicon carbide is mixed with the rare earth oxide and the aluminum nitride sintering aid in amounts of 60-98% and 40-2% by weight, respectively.
3. The liquid phase sintering method of high toughness, high hardness silicon carbide ceramic according to claim 1, wherein said rare earth oxide is a lanthanoid rare earth oxide or a lanthanoid mixed rare earth oxide.
4. The liquid phase sintering method of claim 1, wherein the rare earth oxide is yttria (Y)2O3)。
5. The liquid phase sintering method of high toughness, high hardness silicon carbide ceramic according to claim 1 wherein said rare earth oxide is La2O3To Lu2O3Any one of fifteen rare earth oxides.
6. The liquid phase sintering method of high toughness, high hardness silicon carbide ceramic according to claim 1 wherein said rare earth oxide is La2O3To Lu2O3Any two or more rare earth oxides of fifteen rare earth oxides.
7. The liquid phase sintering method of high toughness, high hardness silicon carbide ceramic according to claim 1 wherein said rare earth oxide is Y2O3And La2O3To Lu2O3Any one of the fifteen rare earth oxides of (a).
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100363303C (en) * | 2005-10-28 | 2008-01-23 | 浙江大学 | Silicon carbide base multiphase composite ceramic and its preparation method |
| CN100465132C (en) * | 2007-02-15 | 2009-03-04 | 浙江大学 | Preparation method of carborundum composite-phase ceramic |
| CN109592983A (en) * | 2017-09-30 | 2019-04-09 | 中国科学院上海硅酸盐研究所 | A kind of highly thermally conductive liquid phase sintering silicon carbide ceramic and preparation method thereof |
| CN114516756A (en) * | 2022-03-14 | 2022-05-20 | 台州学院 | Silicon carbide composite ceramic material and preparation method and application thereof |
-
2004
- 2004-07-01 CN CN 200410062956 patent/CN1587203A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100363303C (en) * | 2005-10-28 | 2008-01-23 | 浙江大学 | Silicon carbide base multiphase composite ceramic and its preparation method |
| CN100465132C (en) * | 2007-02-15 | 2009-03-04 | 浙江大学 | Preparation method of carborundum composite-phase ceramic |
| CN109592983A (en) * | 2017-09-30 | 2019-04-09 | 中国科学院上海硅酸盐研究所 | A kind of highly thermally conductive liquid phase sintering silicon carbide ceramic and preparation method thereof |
| CN109592983B (en) * | 2017-09-30 | 2021-07-13 | 中国科学院上海硅酸盐研究所 | High-thermal-conductivity liquid-phase sintered silicon carbide ceramic and preparation method thereof |
| CN114516756A (en) * | 2022-03-14 | 2022-05-20 | 台州学院 | Silicon carbide composite ceramic material and preparation method and application thereof |
| CN114516756B (en) * | 2022-03-14 | 2022-10-18 | 台州学院 | Silicon carbide composite ceramic material and preparation method and application thereof |
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