CN103553583B - Porous mullite-silicon carbide composite ceramic material and preparation method thereof - Google Patents
Porous mullite-silicon carbide composite ceramic material and preparation method thereof Download PDFInfo
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- CN103553583B CN103553583B CN201310471566.8A CN201310471566A CN103553583B CN 103553583 B CN103553583 B CN 103553583B CN 201310471566 A CN201310471566 A CN 201310471566A CN 103553583 B CN103553583 B CN 103553583B
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Abstract
The invention relates to a porous mullite-silicon carbide composite ceramic material and a preparation method thereof. A technical solution is that the porous mullite-silicon carbide composite ceramic material is obtained by using 60-80 wt% of aluminium hydroxide fine powder, 14-18 wt% of silica fine powder, 1-3 wt% of silica micro powder, 0.8-5 wt% of carbon powder and 0.2-3 wt% of magnesium carbonate fine powder as raw materials and through the steps of adding silica gel with an amount of 4-6 wt% that of the raw material; stirring; forming; keeping a temperature for 12-36 hours at a temperature of 110 DEG C; heating to a temperature of 1,200-1,250 DEG C under a reducing atmosphere; keeping the temperature for 1-3 hours; heating to a temperature of 1,400-1,500 DEG C from a temperature of 1,200-1,250 DEG C under the reducing atmosphere; and keeping the temperature for 3-8 hours. The process is simple and environment-friendly. The prepared porous mullite-silicon carbide composite ceramic material is controllable in material phase composition and morphology, controllable pore size and volume content, high in porosity, high in strength, low in heat conductivity coefficient, strong in medium erosion resistance and good high-temperature performance.
Description
Technical field
The invention belongs to porous ceramic film material technical field.Particularly relate to a kind of porous mullite-silicon carbide composite ceramic materials and preparation method thereof.
Background technology
Porous ceramics, owing to having excellent performance, has been widely used in support of the catalyst, filter for molten metal, separation film, water purifier, biological ceramics and lagging material etc.Mullite has mechanical property and the chemical stability of low thermal expansivity, good thermal shock resistance and excellence; Silicon carbide has the firmly wear-resisting and chemical stability of high physical strength, height; Meanwhile, mullite and silicon carbide have close thermal expansivity and good chemical compatibility; This makes the development of porous mullite-carbide composite ceramic more and more be subject to people's attention.
About the progress that the research of porous mullite-silicon carbide composite ceramic materials is existing certain at present, but mainly to concentrate on silicon carbide be principal crystalline phase, with mullite in conjunction with in the material of phase, as porous mullite silicon carbide pottery (Liu Shifeng, Zeng Yuping, the east of a river is bright. the in-situ oxidation reaction preparation of porous silicon carbide ceramic and performance thereof. and silicate journal, 2008,36(5): be 597-601) adopt particle packing hole forming method, with the silicon carbide of specified particle size for aggregate with the Al of specified particle size
2o
3for additive is prepared from, but on the one hand, particle packing hole forming method can not prepare the material of high porosity, and on the other hand, particular particle size can cause raw materials cost higher; And for example high strength silicate in conjunction with SiC composite porous (beautiful. high strength silicate is in conjunction with the composite porous preparation of SiC. master thesis, Wuhan University of Technology, 2008) be adopt silicon carbide (d
0.5=37 μm), aluminium hydroxide (d
0.5=4.5 μm), andaluzite, kyanite, silicon ash and white carbon black be that raw material is prepared from, due to the very little (d of hydroxide particle-size
0.5=4.5 μm) and content is seldom (16.7wt%), easy reaction sintering, very little to the contribution of pore volume, therefore the method is still based on particle packing hole forming method, cause the void content of sample very low (only up to 31.5%), and there is the problem that particular particle size can cause raw materials cost higher simultaneously; And for example " in-situ reaction prepares the carborundum porous ceramics of mullite bonded " (CN200510029152.5) patented technology, take graphite as pore-forming material, prepare with the mullite of silicon carbide reaction in－situ generation for the carborundum porous ceramics in conjunction with phase, although obtain higher void content, after graphite pore former burning, produce CO
2, cause secondary pollution, be unfavorable for environment protection; For another example foam silicon carbide ceramics (Ji Xiaoli is strengthened, Xu Fei, power is national. and On In-situ Synthesis of Mullite Whisker strengthens foam silicon carbide ceramics. Chinese powder technology, 2011,17(3): 33-36) with silicon carbide, aluminum oxide and kaolin for main raw material, Polymeric sponge method is adopted to prepare foam silicon carbide ceramics base substrate, but the method complicated process of preparation, be difficult to obtain micropore level and the air hole structure of even aperture distribution.
In sum, there is four problems about the preparation of porous mullite-silicon carbide composite ceramic materials at present: the void content that (1) particle packing port-creating method obtains is lower; (2) with particular size material for raw material, add raw material cost of manufacture; (3) after pore-forming material burning produces pore, the CO of generation
2secondary pollution can be caused; (4) Polymeric sponge method or template complex process, and be difficult to obtain micropore level and the air hole structure of even aperture distribution; (5) main take silicon carbide as principal crystalline phase, with mullite in conjunction with phase, thermal conductivity is too high.
Summary of the invention
The present invention is intended to overcome prior art defect, object is to provide the preparation method of the simple porous mullite-silicon carbide composite ceramic materials of a kind of preparation technology, not only void content is high, intensity is high, thermal conductivity is low for the porous mullite-silicon carbide composite ceramic materials prepared by the method, anti-erosion medium resistance ability is strong and high-temperature behavior good, and environmental friendliness, thing phase composite and morphology controllable, pore size and volume content are controlled.
For achieving the above object, the technical solution used in the present invention is: with the aluminium hydroxide fine powder of 60 ~ 80wt%, 14 ~ 18% silica fine powder, the fine silica powder of 1 ~ 3wt%, the silica flour of 1 ~ 12wt%, the carbon dust of 0.8 ~ 5wt% and 0.2 ~ 3wt% magnesiumcarbonate fine powder for raw material, the silicon sol of additional described raw material 4 ~ 6wt%, stir, mechanical pressing, the base substrate after shaping is incubated 12 ~ 36 hours under 110 DEG C of conditions; Then be warming up to 1200 ~ 1250 DEG C under reducing atmosphere, be incubated 1 ~ 3 hour, more under reducing atmosphere temperature be warming up to 1400 ~ 1500 DEG C by 1200 ~ 1250 DEG C, be incubated 3 ~ 8 hours, obtain porous mullite-silicon carbide composite ceramic materials.
In technique scheme:
The Al (OH) of described aluminium hydroxide fine powder
3content is greater than 98wt%, and particle diameter is less than 88 μm.
The SiO of described silica fine powder
2content is greater than 96wt%, and particle diameter is less than 74mm.
The SiO of described fine silica powder
2content is greater than 93wt%, and particle diameter is less than 4 μm.
The Si content of described silica flour is greater than 90wt%, and particle diameter is 3 ~ 100 μm.
The C content of described carbon dust is greater than 90wt%, and particle diameter is less than 88 μm.
The MgCO of described magnesiumcarbonate fine powder
3content is greater than 97wt%, and particle diameter is less than 88 μm.
The concentration of described silicon sol is 20 ~ 40wt%.
The pressure of described mechanical pressing is 30 ~ 100MPa.
Owing to adopting technique scheme, the present invention utilizes raw material decompose themselves original position to produce micron order pore, raw material reaction in－situ after decomposition generates mullite, define the microvoid structure of mullite and even air hole distribution, meanwhile, define the silicon carbide whisker be evenly distributed at micropore situ, not only increase the intensity of mullite microvoid structure, and plug outs open micropore, obtain porous mullite-silicon carbide composite ceramic materials.Prepared product has better hot strength and anti-erosion medium resistance performance.
Therefore, simple and the environmental friendliness of preparation technology of the present invention, prepared porous mullite-silicon carbide composite ceramic materials thing phase composite and morphology controllable, pore size and volume content are controlled, void content is high, thermal conductivity is low, intensity is high, anti-erosion medium resistance ability is strong and high-temperature behavior good.
Embodiment
Below in conjunction with embodiment, the invention will be further described, the restriction not to its protection domain.
For avoiding repetition, first by the raw material in this embodiment and silicon sol Unify legislation as follows, repeat no more in embodiment:
The Al (OH) of described aluminium hydroxide fine powder
3content is greater than 98wt%, and particle diameter is less than 88 μm;
The SiO of described silica fine powder
2content is greater than 96wt%, and particle diameter is less than 74mm;
The SiO of described fine silica powder
2content is greater than 93wt%, and particle diameter is less than 4 μm;
The Si content of described silica flour is greater than 90wt%, and particle diameter is 3 ~ 100 μm;
The C content of described carbon dust is greater than 90wt%, and particle diameter is less than 88 μm;
The MgCO of described magnesiumcarbonate fine powder
3content is greater than 97wt%, and particle diameter is less than 88 μm;
The concentration of described silicon sol is 20 ~ 40wt%.
embodiment 1
A kind of porous mullite-silicon carbide composite ceramic materials and preparation method thereof: with the aluminium hydroxide fine powder of 75 ~ 80wt%, 15 ~ 18% silica fine powder, the fine silica powder of 1 ~ 2wt%, the silica flour of 1 ~ 4wt%, the carbon dust of 0.8 ~ 1.5wt% and 2.2 ~ 3wt% magnesiumcarbonate fine powder for raw material, the silicon sol of additional described raw material 4 ~ 6wt%, stir, mechanical pressing under 30 ~ 60MPa pressure, the base substrate after shaping is incubated 24 ~ 36 hours under 110 DEG C of conditions; Then be warming up to 1200 ~ 1250 DEG C under reducing atmosphere, be incubated 1 ~ 2 hour, more under reducing atmosphere temperature be warming up to 1400 ~ 1450 DEG C by 1200 ~ 1250 DEG C, be incubated 3 ~ 5 hours, obtain porous mullite-silicon carbide composite ceramic materials.
Porous mullite-silicon carbide composite ceramic materials prepared by the present embodiment: apparent porosity is 50 ~ 65%; Volume density is 1.36 ~ 1.65g/cm
3; Mean pore size is 1 ~ 10 μm; Compressive strength is 15 ~ 40 MPa.
embodiment 2
A kind of porous mullite-silicon carbide composite ceramic materials and preparation method thereof: with the aluminium hydroxide fine powder of 70 ~ 75wt%, 14 ~ 16% silica fine powder, the fine silica powder of 1 ~ 2wt%, the silica flour of 5 ~ 8wt%, the carbon dust of 1.2 ~ 2.5wt% and 1.8 ~ 2.5wt% magnesiumcarbonate fine powder for raw material, the silicon sol of additional described raw material 4 ~ 6wt%, stir, mechanical pressing under 50 ~ 80MPa pressure, the base substrate after shaping is incubated 12 ~ 24 hours under 110 DEG C of conditions; Then be warming up to 1200 ~ 1250 DEG C under reducing atmosphere, be incubated 2 ~ 3 hours, more under reducing atmosphere temperature be warming up to 1450 ~ 1500 DEG C by 1200 ~ 1250 DEG C, be incubated 3 ~ 5 hours, obtain porous mullite-silicon carbide composite ceramic materials.
Porous mullite-silicon carbide composite ceramic materials prepared by the present embodiment: apparent porosity is 45 ~ 55%; Volume density is 1.50 ~ 1.89g/cm
3; Mean pore size is 2 ~ 15 μm; Compressive strength is 30 ~ 50 MPa.
embodiment 3
A kind of porous mullite-silicon carbide composite ceramic materials and preparation method thereof: with the aluminium hydroxide fine powder of 65 ~ 70wt%, 14 ~ 16% silica fine powder, the fine silica powder of 2 ~ 3wt%, the silica flour of 6 ~ 10wt%, the carbon dust of 2.5 ~ 4.0wt% and 1.2 ~ 2.0wt% magnesiumcarbonate fine powder for raw material, the silicon sol of additional described raw material 4 ~ 6wt%, stir, mechanical pressing under 40 ~ 70MPa pressure, the base substrate after shaping is incubated 16 ~ 30 hours under 110 DEG C of conditions; Then be warming up to 1200 ~ 1250 DEG C under reducing atmosphere, be incubated 1 ~ 2 hour, more under reducing atmosphere temperature be warming up to 1400 ~ 1450 DEG C by 1200 ~ 1250 DEG C, be incubated 5 ~ 8 hours, obtain porous mullite-silicon carbide composite ceramic materials.
Porous mullite-silicon carbide composite ceramic materials prepared by the present embodiment: apparent porosity is 48 ~ 60%; Volume density is 1.40 ~ 1.83g/cm
3; Mean pore size is 5 ~ 25 μm; Compressive strength is 25 ~ 46 MPa.
embodiment 4
A kind of porous mullite-silicon carbide composite ceramic materials and preparation method thereof: with the aluminium hydroxide fine powder of 60 ~ 65wt%, 14 ~ 18% silica fine powder, the fine silica powder of 1 ~ 3wt%, the silica flour of 9 ~ 12wt%, the carbon dust of 3.5 ~ 5.0wt% and 0.2 ~ 2.0wt% magnesiumcarbonate fine powder for raw material, the silicon sol of additional described raw material 4 ~ 6wt%, stir, mechanical pressing under 60 ~ 100MPa pressure, the base substrate after shaping is incubated 24 ~ 36 hours under 110 DEG C of conditions; Then be warming up to 1200 ~ 1250 DEG C under reducing atmosphere, be incubated 1 ~ 2 hour, more under reducing atmosphere temperature be warming up to 1450 ~ 1500 DEG C by 1200 ~ 1250 DEG C, be incubated 4 ~ 8 hours, obtain porous mullite-silicon carbide composite ceramic materials.
Porous mullite-silicon carbide composite ceramic materials prepared by the present embodiment: apparent porosity is 36 ~ 50%; Volume density is 1.62 ~ 1.98g/cm
3; Mean pore size is 5 ~ 30 μm; Compressive strength is 40 ~ 80 MPa.
This embodiment utilizes raw material decompose themselves original position to produce micron order pore, raw material reaction in－situ after decomposition generates mullite, define the microvoid structure of mullite and even air hole distribution, simultaneously, the silicon carbide whisker be evenly distributed is defined at micropore situ, not only increase the intensity of mullite microvoid structure, and plug outs open micropore, obtain porous mullite-silicon carbide composite ceramic materials.Prepared product has better hot strength and anti-erosion medium resistance performance.
Therefore, simple and the environmental friendliness of this embodiment preparation technology, prepared porous mullite-silicon carbide composite ceramic materials thing phase composite and morphology controllable, pore size and volume content are controlled, void content is high, thermal conductivity is low, intensity is high, anti-erosion medium resistance ability is strong and high-temperature behavior good.
Claims (4)
1. the preparation method of porous mullite-silicon carbide composite ceramic materials, it is characterized in that with the aluminium hydroxide fine powder of 60 ~ 80wt%, 14 ~ 18% silica fine powder, the fine silica powder of 1 ~ 3wt%, the silica flour of 1 ~ 12wt%, the carbon dust of 0.8 ~ 5wt% and 0.2 ~ 3wt% magnesiumcarbonate fine powder for raw material, the silicon sol of additional described raw material 4 ~ 6wt%, stir, mechanical pressing, the base substrate after shaping is incubated 12 ~ 36 hours under 110 DEG C of conditions; Then be warming up to 1200 ~ 1250 DEG C under reducing atmosphere, be incubated 1 ~ 3 hour, more under reducing atmosphere temperature be warming up to 1400 ~ 1500 DEG C by 1200 ~ 1250 DEG C, be incubated 3 ~ 8 hours, obtain porous mullite-silicon carbide composite ceramic materials;
The Al (OH) of described aluminium hydroxide fine powder
3content is greater than 98wt%, and particle diameter is less than 88 μm;
The SiO of described silica fine powder
2content is greater than 96wt%, and particle diameter is less than 74 μm;
The SiO of described fine silica powder
2content is greater than 93wt%, and particle diameter is less than 4 μm;
The Si content of described silica flour is greater than 90wt%, and particle diameter is 3 ~ 100 μm;
The C content of described carbon dust is greater than 90wt%, and particle diameter is less than 88 μm;
The MgCO of described magnesiumcarbonate fine powder
3content is greater than 97wt%, and particle diameter is less than 88 μm.
2. the preparation method of porous mullite-silicon carbide composite ceramic materials according to claim 1, is characterized in that the concentration of described silicon sol is 20 ~ 40wt%.
3. the preparation method of porous mullite-silicon carbide composite ceramic materials according to claim 1, is characterized in that the pressure of described mechanical pressing is 30 ~ 100MPa.
4. porous mullite-silicon carbide composite ceramic materials, is characterized in that described porous mullite-silicon carbide composite ceramic materials is the porous mullite-silicon carbide composite ceramic materials prepared by preparation method of the porous mullite-silicon carbide composite ceramic materials according to any one of claim 1 ~ 3.
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| CN104529411B (en) * | 2014-12-20 | 2016-08-24 | 佛山铭乾科技有限公司 | A kind of microporous membrane and preparation method thereof |
| CN105541333B (en) * | 2015-12-10 | 2018-05-01 | 江西理工大学 | A kind of preparation method of low sintering mullite In-sltu reinforcement carborundum porous ceramics |
| CN106747560A (en) * | 2016-12-05 | 2017-05-31 | 郑州丽福爱生物技术有限公司 | A kind of porous thermal insulating composite ceramic material |
| CN107266097B (en) * | 2017-07-28 | 2019-08-20 | 武汉科技大学 | A kind of light weight mullite refractory and preparation method thereof |
| CN108017404A (en) * | 2017-11-22 | 2018-05-11 | 马鞍山科润冶金材料有限公司 | A kind of preparation method of mullite bonded carborundum composite-phase ceramic material |
| CN108218382A (en) * | 2018-02-02 | 2018-06-29 | 付主枝 | The preparation method of degradable magnesium based composite metal bioceramic material |
| CN111233499A (en) * | 2020-03-12 | 2020-06-05 | 巩义市芙豪冶金材料有限公司 | SiC/C homogeneous material, stemming and preparation method thereof |
| CN112537950A (en) * | 2020-11-30 | 2021-03-23 | 中国科学院金属研究所 | High-temperature alloy slag inclusion filter screen and application |
| CN115724684B (en) * | 2022-11-21 | 2023-05-26 | 景德镇陶瓷大学 | Low-temperature in-situ synthesis method of SiC nanofiber coating modified mullite honeycomb ceramic and product prepared by same |
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| CN102432312B (en) * | 2011-09-13 | 2013-06-05 | 武汉科技大学 | Micro-porous mullite-silicon carbide multiphase fire resistant material and preparation method thereof |
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