CN103553583A - 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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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.Relate in particular 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, separated with film, water purifier, biological ceramics and lagging material etc.Mullite has low thermal expansivity, good thermal shock resistance and excellent mechanical property and chemical stability; Silicon carbide has high physical strength, high hard wear-resisting and chemical stability; Meanwhile, mullite and silicon carbide have close thermal expansivity and good chemical compatibility; This is more and more subject to people's attention the development of porous mullite-silicon carbide compound pottery.
The at present existing certain progress of research about porous mullite-silicon carbide composite ceramic materials, but mainly concentrate on take silicon carbide as principal crystalline phase, take mullite in the material in conjunction with phase, as porous mullite silicon carbide pottery (Liu Shifeng, Zeng Yuping, the east of a river is bright. in-situ oxidation reaction preparation and the performance thereof of porous silicon carbide ceramic. and silicate journal, 2008,36(5): be 597-601) to adopt particle packing hole forming method, take the silicon carbide of specified particle size as 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 be prepared 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 to adopt silicon carbide (d
0.5=37 μ m), aluminium hydroxide (d
0.5=4.5 μ m), 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 μ m) and content seldom (16.7wt%), easy reaction sintering, contribution to pore volume is very little, therefore the method still be take particle packing hole forming method as main, cause the void content very low (only up to 31.5%) of sample, and exist particular particle size can cause the higher problem of raw materials cost simultaneously; " in-situ reaction is prepared the carborundum porous ceramics of mullite bonded " (CN200510029152.5) patented technology and for example, take graphite as pore-forming material, prepared that to take the mullite that silicon carbide reaction in－situ generates be the carborundum porous ceramics in conjunction with phase, although obtained higher void content, after the burning of graphite pore-forming material, produce CO
2, caused secondary pollution, be unfavorable for environment protection; For another example strengthen foam silicon carbide ceramics (Ji Xiaoli, Xu Fei, power its people etc. On In-situ Synthesis of Mullite Whisker And strengthens foam silicon carbide ceramics. Chinese powder technology, 2011,17(3): 33-36) take silicon carbide, aluminum oxide and kaolin as main raw material, adopt foam impregnation legal system standby foam silicon carbide ceramics base substrate, but the method complicated process of preparation, is difficult to obtain the air hole structure of micropore level and even aperture distribution.
In sum, there is four problems in the current preparation about porous mullite-silicon carbide composite ceramic materials: the void content that (1) particle packing port-creating method makes is lower; (2) take particular size material as raw material, increased raw material cost of manufacture; (3) pore-forming material burning produces after pore, the CO of generation
2can cause secondary pollution; (4) foam impregnation method or template complex process, and be difficult to obtain the air hole structure of micropore level and even aperture distribution; (5) mainly take silicon carbide as principal crystalline phase, take mullite as 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 porous mullite-silicon carbide composite ceramic materials of preparing by the method, anti-erosion medium resistance ability is strong and high-temperature behavior good, and environmental friendliness, phase form and pattern is controlled, pore size and volume content controlled.
For achieving the above object, the technical solution used in the present invention is: take the aluminium hydroxide fine powder, 14 ~ 18% silica fine powder, the fine silica powder of 1 ~ 3wt% of 60 ~ 80wt%, the magnesiumcarbonate fine powder of the carbon dust of the silica flour of 1 ~ 12wt%, 0.8 ~ 5wt% and 0.2 ~ 3wt% is raw material, the silicon sol of additional described raw material 4 ~ 6wt%, stir, mechanical pressing, the base substrate after moulding is incubated 12 ~ 36 hours under 110 ℃ of conditions; Then under reducing atmosphere, be warming up to 1200 ~ 1250 ℃, be incubated 1 ~ 3 hour, then under reducing atmosphere, temperature is warming up to 1400 ~ 1500 ℃ by 1200 ~ 1250 ℃, be incubated 3 ~ 8 hours, obtain porous mullite-silicon carbide composite ceramic materials.
In technique scheme:
The Al of described aluminium hydroxide fine powder (OH)
3content is greater than 98wt%, and particle diameter is less than 88 μ m.
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 μ m.
The Si content of described silica flour is greater than 90wt%, and particle diameter is 3 ~ 100 μ m.
The C content of described carbon dust is greater than 90wt%, and particle diameter is less than 88 μ m.
The MgCO of described magnesiumcarbonate fine powder
3content is greater than 97wt%, and particle diameter is less than 88 μ m.
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 self to decompose original position and produces micron order pore, raw material reaction in－situ after decomposition generates mullite, formed the microvoid structure of mullite and even air hole distribution, meanwhile, at micropore situ, form the silicon carbide whisker being evenly distributed, not only strengthened the intensity of mullite microvoid structure, and stopped up part opening micropore, obtained 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 phase forms and pattern is controlled, pore size and volume content is 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, not the restriction to its protection domain.
For avoiding repetition, first the raw material in this embodiment and silicon sol unification are described below, in embodiment, repeat no more:
The Al of described aluminium hydroxide fine powder (OH)
3content is greater than 98wt%, and particle diameter is less than 88 μ m;
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 μ m;
The Si content of described silica flour is greater than 90wt%, and particle diameter is 3 ~ 100 μ m;
The C content of described carbon dust is greater than 90wt%, and particle diameter is less than 88 μ m;
The MgCO of described magnesiumcarbonate fine powder
3content is greater than 97wt%, and particle diameter is less than 88 μ m;
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: take the aluminium hydroxide fine powder, 15 ~ 18% silica fine powder, the fine silica powder of 1 ~ 2wt% of 75 ~ 80wt%, the magnesiumcarbonate fine powder of the carbon dust of the silica flour of 1 ~ 4wt%, 0.8 ~ 1.5wt% and 2.2 ~ 3wt% is raw material, the silicon sol of additional described raw material 4 ~ 6wt%, stir, mechanical pressing under 30 ~ 60MPa pressure, the base substrate after moulding is incubated 24 ~ 36 hours under 110 ℃ of conditions; Then under reducing atmosphere, be warming up to 1200 ~ 1250 ℃, be incubated 1 ~ 2 hour, then under reducing atmosphere, temperature is warming up to 1400 ~ 1450 ℃ by 1200 ~ 1250 ℃, be incubated 3 ~ 5 hours, obtain porous mullite-silicon carbide composite ceramic materials.
Porous mullite-silicon carbide composite ceramic materials that the present embodiment is prepared: apparent porosity is 50 ~ 65%; Volume density is 1.36 ~ 1.65g/cm
3; Mean pore size is 1 ~ 10 μ m; Compressive strength is 15 ~ 40 MPa.
embodiment 2
A kind of porous mullite-silicon carbide composite ceramic materials and preparation method thereof: take the aluminium hydroxide fine powder, 14 ~ 16% silica fine powder, the fine silica powder of 1 ~ 2wt% of 70 ~ 75wt%, the magnesiumcarbonate fine powder of the carbon dust of the silica flour of 5 ~ 8wt%, 1.2 ~ 2.5wt% and 1.8 ~ 2.5wt% is raw material, the silicon sol of additional described raw material 4 ~ 6wt%, stir, mechanical pressing under 50 ~ 80MPa pressure, the base substrate after moulding is incubated 12 ~ 24 hours under 110 ℃ of conditions; Then under reducing atmosphere, be warming up to 1200 ~ 1250 ℃, be incubated 2 ~ 3 hours, then under reducing atmosphere, temperature is warming up to 1450 ~ 1500 ℃ by 1200 ~ 1250 ℃, be incubated 3 ~ 5 hours, obtain porous mullite-silicon carbide composite ceramic materials.
Porous mullite-silicon carbide composite ceramic materials that the present embodiment is prepared: apparent porosity is 45 ~ 55%; Volume density is 1.50 ~ 1.89g/cm
3; Mean pore size is 2 ~ 15 μ m; Compressive strength is 30 ~ 50 MPa.
embodiment 3
A kind of porous mullite-silicon carbide composite ceramic materials and preparation method thereof: take the aluminium hydroxide fine powder, 14 ~ 16% silica fine powder, the fine silica powder of 2 ~ 3wt% of 65 ~ 70wt%, the magnesiumcarbonate fine powder of the carbon dust of the silica flour of 6 ~ 10wt%, 2.5 ~ 4.0wt% and 1.2 ~ 2.0wt% is raw material, the silicon sol of additional described raw material 4 ~ 6wt%, stir, mechanical pressing under 40 ~ 70MPa pressure, the base substrate after moulding is incubated 16 ~ 30 hours under 110 ℃ of conditions; Then under reducing atmosphere, be warming up to 1200 ~ 1250 ℃, be incubated 1 ~ 2 hour, then under reducing atmosphere, temperature is warming up to 1400 ~ 1450 ℃ by 1200 ~ 1250 ℃, be incubated 5 ~ 8 hours, obtain porous mullite-silicon carbide composite ceramic materials.
Porous mullite-silicon carbide composite ceramic materials that the present embodiment is prepared: apparent porosity is 48 ~ 60%; Volume density is 1.40 ~ 1.83g/cm
3; Mean pore size is 5 ~ 25 μ m; Compressive strength is 25 ~ 46 MPa.
embodiment 4
A kind of porous mullite-silicon carbide composite ceramic materials and preparation method thereof: take the aluminium hydroxide fine powder, 14 ~ 18% silica fine powder, the fine silica powder of 1 ~ 3wt% of 60 ~ 65wt%, the magnesiumcarbonate fine powder of the carbon dust of the silica flour of 9 ~ 12wt%, 3.5 ~ 5.0wt% and 0.2 ~ 2.0wt% is raw material, the silicon sol of additional described raw material 4 ~ 6wt%, stir, mechanical pressing under 60 ~ 100MPa pressure, the base substrate after moulding is incubated 24 ~ 36 hours under 110 ℃ of conditions; Then under reducing atmosphere, be warming up to 1200 ~ 1250 ℃, be incubated 1 ~ 2 hour, then under reducing atmosphere, temperature is warming up to 1450 ~ 1500 ℃ by 1200 ~ 1250 ℃, be incubated 4 ~ 8 hours, obtain porous mullite-silicon carbide composite ceramic materials.
Porous mullite-silicon carbide composite ceramic materials that the present embodiment is prepared: apparent porosity is 36 ~ 50%; Volume density is 1.62 ~ 1.98g/cm
3; Mean pore size is 5 ~ 30 μ m; Compressive strength is 40 ~ 80 MPa.
This embodiment is utilized raw material self to decompose original position and is produced micron order pore, raw material reaction in－situ after decomposition generates mullite, formed the microvoid structure of mullite and even air hole distribution, simultaneously, at micropore situ, formed the silicon carbide whisker being evenly distributed, not only strengthen the intensity of mullite microvoid structure, and stopped up part opening micropore, obtained 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 phase forms and pattern is controlled, pore size and volume content is 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 (10)
1. the preparation method of a porous mullite-silicon carbide composite ceramic materials, it is characterized in that take that the aluminium hydroxide fine powder, 14 ~ 18% silica fine powder, the fine silica powder of 1 ~ 3wt% of 60 ~ 80wt% are, the magnesiumcarbonate fine powder of the carbon dust of the silica flour of 1 ~ 12wt%, 0.8 ~ 5wt% and 0.2 ~ 3wt% is raw material, the silicon sol of additional described raw material 4 ~ 6wt%, stir, mechanical pressing, the base substrate after moulding is incubated 12 ~ 36 hours under 110 ℃ of conditions; Then under reducing atmosphere, be warming up to 1200 ~ 1250 ℃, be incubated 1 ~ 3 hour, then under reducing atmosphere, temperature is warming up to 1400 ~ 1500 ℃ by 1200 ~ 1250 ℃, be incubated 3 ~ 8 hours, obtain porous mullite-silicon carbide composite ceramic materials.
2. the preparation method of porous mullite-silicon carbide composite ceramic materials according to claim 1, is characterized in that the Al (OH) of described aluminium hydroxide fine powder
3content is greater than 98wt%, and particle diameter is less than 88 μ m.
3. the preparation method of porous mullite-silicon carbide composite ceramic materials according to claim 1, is characterized in that the SiO of described silica fine powder
2content is greater than 96wt%, and particle diameter is less than 74mm.
4. the preparation method of porous mullite-silicon carbide composite ceramic materials according to claim 1, is characterized in that the SiO of described fine silica powder
2content is greater than 93wt%, and particle diameter is less than 4 μ m.
5. the preparation method of porous mullite-silicon carbide composite ceramic materials according to claim 1, is characterized in that the Si content of described silica flour is greater than 90wt%, and particle diameter is 3 ~ 100 μ m.
6. the preparation method of porous mullite-silicon carbide composite ceramic materials according to claim 1, is characterized in that the C content of described carbon dust is greater than 90wt%, and particle diameter is less than 88 μ m.
7. the preparation method of porous mullite-silicon carbide composite ceramic materials according to claim 1, is characterized in that the MgCO of described magnesiumcarbonate fine powder
3content is greater than 97wt%, and particle diameter is less than 88 μ m.
8. the preparation method of porous mullite-silicon carbide composite ceramic materials according to claim 1, the concentration that it is characterized in that described silicon sol is 20 ~ 40wt%.
9. the preparation method of porous mullite-silicon carbide composite ceramic materials according to claim 1, the pressure that it is characterized in that described mechanical pressing is 30 ~ 100MPa.
10. porous mullite-silicon carbide composite ceramic materials, is characterized in that described porous mullite-silicon carbide composite ceramic materials is according to the prepared porous mullite-silicon carbide composite ceramic materials of preparation method of the porous mullite-silicon carbide composite ceramic materials described in any one in claim 1 ~ 9.
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| CN104529411A (en) * | 2014-12-20 | 2015-04-22 | 佛山铭乾科技有限公司 | Micro-porous ceramic membrane and preparation method thereof |
| CN105541333A (en) * | 2015-12-10 | 2016-05-04 | 江西理工大学 | Preparation method for mullite in-situ reinforced silicon carbide porous ceramic sintered at low temperature |
| 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 |
| CN107266097A (en) * | 2017-07-28 | 2017-10-20 | 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 |
| CN115724684A (en) * | 2022-11-21 | 2023-03-03 | 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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| CN104529411A (en) * | 2014-12-20 | 2015-04-22 | 佛山铭乾科技有限公司 | Micro-porous ceramic membrane and preparation method thereof |
| CN105541333A (en) * | 2015-12-10 | 2016-05-04 | 江西理工大学 | Preparation method for mullite in-situ reinforced silicon carbide porous ceramic sintered at low temperature |
| 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 |
| CN107266097A (en) * | 2017-07-28 | 2017-10-20 | 武汉科技大学 | A kind of light weight mullite refractory and preparation method thereof |
| 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 |
| CN115724684A (en) * | 2022-11-21 | 2023-03-03 | 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 |
| 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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