CN102115330A - Preparation method of solid phase sintering silicon carbide ceramics taking phenolic resin as carbon source - Google Patents
Preparation method of solid phase sintering silicon carbide ceramics taking phenolic resin as carbon source Download PDFInfo
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- CN102115330A CN102115330A CN2009102478657A CN200910247865A CN102115330A CN 102115330 A CN102115330 A CN 102115330A CN 2009102478657 A CN2009102478657 A CN 2009102478657A CN 200910247865 A CN200910247865 A CN 200910247865A CN 102115330 A CN102115330 A CN 102115330A
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Abstract
The invention provides a preparation method of solid phase sintering silicon carbide ceramics taking phenolic resin as carbon source, belonging to the field of silicon carbide ceramics. The method comprises the steps of: taking SiC powder, B4C powder and phenolic resin as raw materials, wherein the weight percentage of the B4C powder to the total weight is 0.1-1wt%, and the weight percentage of the phenolic resin to the total weight is 5-30wt%; and taking the water as dissolvent, preparing the raw materials to be 40-45wt% of sizing agent, taking SiC balls as mill balls, mixing, drying, smashing, screening, forming by means of dry pressing and/or isostatic pressing, unsticking, and sintering under the Ar atmosphere. The density of the solid phase sintering silicon carbide ceramics prepared by the method is 3.10-3.16g/cm<3>, and the bending strength of the solid phase sintering silicon carbide ceramics is 300-500MPa.
Description
Technical field
The present invention relates to the preparation method that resol is the solid-phase sintered silicon carbide ceramics of carbon source, belong to the SiC ceramic field.
Background technology
The SiC pottery is with its excellent high-temperature stability, wear resistance, high thermal conductivity and be widely used in the industrial production.Wherein the SiC of solid state sintering pottery is because sintering aid content is very low, and the crystal boundary place can residual more low-melting material, and its physical and chemical performance has high-temperature stability, so the SiC pottery of solid state sintering has special using value.Solid State Sintered SiC Ceramics is a sintering aid with C and B mainly, and in the former research, sintering aid C introduces with resol simultaneously so that C is black, and it is unfavorable for that industry produces, so this patent adds B simultaneously by introducing the C source with resol fully
4C is as sintering aid, and this method can reduce the black add-on of C, increases the consumption of resol simultaneously, and it helps the moulding of SiC pottery.Can obtain the SiC pottery of various grain sizes and pattern in addition by adjusting C content and temperature, processing for the optics of SiC pottery provides experiment and theoretical basis.
Summary of the invention
The object of the invention is to reduce the quantity of additive, and sintering aid C is uniformly mixed, and its preparation method is as follows:
(1) SiC powder, B
4C powder and resol are raw material; B
4The C powder accounts for 0.1～1wt% of total amount, and resol accounts for the 5-30wt% of total amount;
Described SiC powder and B
4The preferred median size of C powder is 0.1～1 μ m;
It is 40-60wt% that the residual C of the preferred cracking of described resol leads,
(2) with water be solvent, raw material is made into the slurry of 40-45wt%,, mix as mill ball with the SiC ball, oven dry is pulverized, sieve, and dry-pressing and/or isostatic pressing, after the unsticking, sintering under Ar gas atmosphere;
Described raw material: SiC ball mass ratio is 1: 1～5;
Described dry-pressing pressure is 20MPa-100MPa, and described hydrostatic pressure is 100MP～500MPa;
Described sintering temperature is 1900-2300 ℃, and soaking time is 30-90min.
The present invention is 2200 ℃-1h under same sintering schedule, by adding different content resol, has obtained the SiC pottery of different densities and mechanical property, and density reaches as high as 3.15gcm
-3, the bending strength maximum can be about 431.4MPa.
Table 1 is the SiC pottery mechanical property of different phenolic resin contents, Fig. 1 is the XRD curve of the SiC sintered compact of the different phenolic resin contents of interpolation, be mainly the 6H crystal formation of α-SiC from scheming SiC powder as can be seen, behind 2200 ℃ high temperature sintering, have part 6H to be converted into the 4H crystal formation, 4H is the high-temperature stable phase mutually.Fig. 2 is the microtexture optical photograph of the SiC pottery of different phenolic resin contents, and as can be seen from the figure along with the increase of phenolic resin content, the grain-size size of SiC pottery has the trend that reduces.SiC pottery for adding 10wt% resol by different sintering temperatures, can obtain the SiC pottery (Fig. 3) of various grain sizes and mechanical property.
Table 2 is the mechanical property under the different sintering schedules of 10wt% phenolic resin content SiC pottery under the room temperature.
Table 1
Table 2
In sum, the present invention prepares the solid State Sintered SiC Ceramics that the SiC pottery can be prepared the better and different grain morphology sizes of mechanical property with resol for the C source.
Description of drawings
The SiC pottery XRD curve a-10wt% of the different phenolic resin contents of Fig. 1, b-13.3wt%, c-16.7wt%, d-20wt%, e-23.3wt%.
Optical photograph under the different phenolic resin contents of Fig. 2 behind the SiC ceramic surface corrosion, a-10wt%, b-13.3wt%, c-16.7wt%, d-20wt%, e-23.3wt%.
Optical photograph under the different sintering temperatures of Fig. 3 behind the SiC ceramic surface corrosion of resol 10wt% content: a-2200 ℃/1h, b-2100 ℃/1h, c-2050/3h.
Embodiment
Further specify characteristics of the present invention below by specific embodiment, but the present invention is confined to embodiment by no means.
Embodiment 1
SiC, sintering aid B
4C (0.5wt%) and resol (10wt%) is 100g altogether, is solvent with water, and three kinds of powders are made into the slurry that solid content is 45wt%, is ball-milling medium with SiC ball 200g, mixes 24h, then in thermostat container till 80 ℃ of oven dry.Grind then, through after the 100 purpose sieve, the powder that obtains is the 16MPa pressure forming on vulcanizing press again, then at the inferior static pressure of 200MPa pressure.After the unsticking under normal pressure Ar gas atmosphere sintering, sintering temperature is 2200 ℃, soaking time is 1h, the SiC ceramic density that obtains is 3.14gcm
-3, bending strength is 304.9MPa.
Embodiment 2
SiC, sintering aid B
4C (0.6wt%) and resol (20wt%) is 100g altogether, is solvent with water, and three kinds of powders are made into the slurry that solid content is 40wt%, is ball-milling medium with SiC ball 200g, mixes 24h, then in thermostat container till 80 ℃ of oven dry.Grind then, through after the 100 purpose sieve, the powder that obtains is the 16Mpa pressure forming on vulcanizing press again, then at the inferior static pressure of 200MPa pressure.After the unsticking under normal pressure Ar gas atmosphere sintering, sintering temperature is 2200 ℃, soaking time is 1h, the SiC ceramic density that obtains is 3.13gcm
-3, bending strength is 431.4MPa.
Claims (7)
1. resol is the preparation method of the solid-phase sintered silicon carbide ceramics of carbon source, it is characterized in that comprising the steps:
(1) SiC powder, B
4C powder and resol are raw material; B
4The C powder accounts for 0.1～1wt% of total amount, and resol accounts for the 5-30wt% of total amount;
(2) with water be solvent, raw material is made into the slurry of 40-45wt%,, mix as mill ball with the SiC ball, oven dry is pulverized, sieve, and dry-pressing and/or isostatic pressing, after the unsticking, sintering under Ar gas atmosphere.
2. by the described preparation method of claim 1, it is characterized in that described SiC powder and B
4C powder median size is 0.1～1 μ m.
3. by claim 1 or 2 described preparation methods, it is characterized in that it is 40-60wt% that the residual C of described resol cracking leads,
4. by claim 1 or 2 described preparation methods, it is characterized in that described raw material: SiC ball mass ratio is 1: 1～5;
5. by claim 1 or 2 described preparation methods, it is characterized in that described dry-pressing pressure is 20MPa～100MPa.
6. by claim 1 or 2 described preparation methods, it is characterized in that described hydrostatic pressure is 100MP～500MPa;
7. by claim 1 or 2 described preparation methods, it is characterized in that described sintering temperature is 1900-2300 ℃, soaking time is 30-90min.
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Cited By (12)
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|---|---|---|---|---|
| CN102617149A (en) * | 2012-03-29 | 2012-08-01 | 温州东迅密封科技有限公司 | Pressureless sintering silicon carbide and preparation process thereof |
| CN104276823A (en) * | 2013-07-12 | 2015-01-14 | 中国科学院上海硅酸盐研究所 | High-insulation silicon carbide/boron nitride ceramic material and preparation method thereof |
| CN104291827A (en) * | 2014-10-14 | 2015-01-21 | 中国钢研科技集团有限公司 | Process for preparing silicon carbide ceramic in complicated shape from phenolic resin serving as carbon source by adopting solid phase sintering |
| CN105645961A (en) * | 2015-12-30 | 2016-06-08 | 中国科学院上海硅酸盐研究所 | Negative-temperature-coefficient (NTC) SiC (silicon carbide) thermal sensitive ceramic and preparation method thereof |
| CN106045520A (en) * | 2016-05-30 | 2016-10-26 | 中国科学院上海硅酸盐研究所 | Low-resistivity linear-resistance silicon carbide and graphite composite and preparation method thereof |
| CN107399971A (en) * | 2017-07-25 | 2017-11-28 | 苏州纳朴材料科技有限公司 | A kind of boron carbide ceramics method for preparing microsphere |
| CN107417280A (en) * | 2017-07-25 | 2017-12-01 | 苏州纳朴材料科技有限公司 | A kind of normal pressure-sintered boron carbide ceramics preparation method |
| CN108218462A (en) * | 2016-12-22 | 2018-06-29 | 中国科学院上海硅酸盐研究所 | Resin based sizing and SiC ceramic reaction forming method |
| CN109180195A (en) * | 2018-09-30 | 2019-01-11 | 威海威林特电控科技有限公司 | One kind is based on adding obdurability porous ceramic composite and its preparation process made of infiltrated metal method |
| CN109809822A (en) * | 2019-04-10 | 2019-05-28 | 南通三责精密陶瓷有限公司 | A kind of high-strength and high ductility silicon carbide ceramics load plate, manufacturing method and application |
| CN112794719A (en) * | 2021-01-05 | 2021-05-14 | 中国科学院上海硅酸盐研究所 | Normal pressure sintered anti-irradiation silicon carbide ceramic material and preparation method thereof |
| CN113416076A (en) * | 2021-08-16 | 2021-09-21 | 东北大学 | Preparation method of self-reinforced silicon carbide ceramic material |
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Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102617149A (en) * | 2012-03-29 | 2012-08-01 | 温州东迅密封科技有限公司 | Pressureless sintering silicon carbide and preparation process thereof |
| CN104276823A (en) * | 2013-07-12 | 2015-01-14 | 中国科学院上海硅酸盐研究所 | High-insulation silicon carbide/boron nitride ceramic material and preparation method thereof |
| CN104276823B (en) * | 2013-07-12 | 2016-03-23 | 中国科学院上海硅酸盐研究所 | High insulating silicon carbide/boron nitride ceramic material and preparation method thereof |
| CN104291827A (en) * | 2014-10-14 | 2015-01-21 | 中国钢研科技集团有限公司 | Process for preparing silicon carbide ceramic in complicated shape from phenolic resin serving as carbon source by adopting solid phase sintering |
| CN104291827B (en) * | 2014-10-14 | 2016-05-25 | 中国钢研科技集团有限公司 | Phenolic resins is that carbon source solid-phase sintering is prepared complicated shape silicon carbide ceramic process |
| CN105645961A (en) * | 2015-12-30 | 2016-06-08 | 中国科学院上海硅酸盐研究所 | Negative-temperature-coefficient (NTC) SiC (silicon carbide) thermal sensitive ceramic and preparation method thereof |
| CN106045520A (en) * | 2016-05-30 | 2016-10-26 | 中国科学院上海硅酸盐研究所 | Low-resistivity linear-resistance silicon carbide and graphite composite and preparation method thereof |
| CN106045520B (en) * | 2016-05-30 | 2018-06-22 | 中国科学院上海硅酸盐研究所 | A kind of silicon carbide/graphite composite material with low-resistivity, linear resistance property and preparation method thereof |
| CN108218462A (en) * | 2016-12-22 | 2018-06-29 | 中国科学院上海硅酸盐研究所 | Resin based sizing and SiC ceramic reaction forming method |
| CN107399971A (en) * | 2017-07-25 | 2017-11-28 | 苏州纳朴材料科技有限公司 | A kind of boron carbide ceramics method for preparing microsphere |
| CN107417280A (en) * | 2017-07-25 | 2017-12-01 | 苏州纳朴材料科技有限公司 | A kind of normal pressure-sintered boron carbide ceramics preparation method |
| CN109180195A (en) * | 2018-09-30 | 2019-01-11 | 威海威林特电控科技有限公司 | One kind is based on adding obdurability porous ceramic composite and its preparation process made of infiltrated metal method |
| CN109809822A (en) * | 2019-04-10 | 2019-05-28 | 南通三责精密陶瓷有限公司 | A kind of high-strength and high ductility silicon carbide ceramics load plate, manufacturing method and application |
| CN112794719A (en) * | 2021-01-05 | 2021-05-14 | 中国科学院上海硅酸盐研究所 | Normal pressure sintered anti-irradiation silicon carbide ceramic material and preparation method thereof |
| CN113416076A (en) * | 2021-08-16 | 2021-09-21 | 东北大学 | Preparation method of self-reinforced silicon carbide ceramic material |
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