CN104649709A - Method for manufacturing porous silicon carbide ceramic - Google Patents
Method for manufacturing porous silicon carbide ceramic Download PDFInfo
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- CN104649709A CN104649709A CN201310601354.7A CN201310601354A CN104649709A CN 104649709 A CN104649709 A CN 104649709A CN 201310601354 A CN201310601354 A CN 201310601354A CN 104649709 A CN104649709 A CN 104649709A
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Abstract
The invention discloses a method for manufacturing a porous silicon carbide ceramic. The porous silicon carbide ceramic manufactured by using the method overcomes the defect that silicon carbide is difficult to sinter, has an intercommunicated open pore structure, and can realize near size sintering. The method is implemented through the following technical scheme: silicon carbide and aluminum oxide are used as main raw materials, the ratio of the silicon carbide to the aluminum oxide is 5:3, graphite is used as a pore forming agent, and the content of the pore forming agent is controlled to be 15-30wt%. Alcohol is used as a dispersion medium, a proper amount of phenolic resin is added as an adhesive, and dispersed slurry is obtained in a ball milling manner, wherein the mass ratio of powder to milling balls is 1:2. The solvent is removed from the slurry by adopting a rotary evaporator to obtain dried powder. The dried powder is pressed into a green body by a cold press under the pressure of 30-90MPa, the obtained green body is heated to the sintering temperature of 1400-1550 DEG C in a quick heating furnace, natural cooling is carried out after the sintering temperature is kept for 1-4 hours, and the rate from room temperature to the sintering temperature and from cooling after sintering to room temperature is about 5 DEG C per minute in the sintering process.
Description
Technical field
The present invention relates to the manufacture method of thyrite, is a kind of method preparing porous silicon carbide ceramic specifically.
Background technology
Porous silicon carbide ceramic is the new function material having a lot of hole in a kind of internal structure.Owing to having feature such as low density, high strength, high porosity, hypertonicity, specific surface area large, anticorrosive, anti-oxidant, good thermal insulation, shock resistance and high thermal resistance etc., make it obtain in general industry field and high-tech area and apply more and more widely.Such as: high temperature gas cleaning device, the solid particle filter of diesel emission, filter for molten metal, heat exchanger, sensor, insulation and sound-proof material can be made, the support of the catalyst etc. of vehicle exhaust.In addition, they also have potential application prospect in bio-medical field.At present, carborundum porous ceramics, because of the performance of its excellence, is more and more subject to people's attention.Its application is throughout multiple fields such as metallurgy, chemical industry, electronics, the energy, aviation, environmental protection, biologies.The range of application of carborundum porous ceramics is in continuous expansion, and application level is improving constantly, and its technology of preparing is also at development.The preparation of porous silicon carbide ceramic has kinds of processes method.As added pore-forming material technique, foam process, Foam dipping method, sol gel process, template duplicating method etc.Wherein adding pore-forming material is in sintering process, and pore-forming material volatilization or decomposition are left matrix and left pore to prepare the processing method of porous ceramics.Pore-forming material kind has inorganic and organic two kinds.According to combination between silicon-carbide particle; the preparation method of carborundum porous ceramics mostly is direct synthesis technique; this method realizes sintering with the direct combination between silicon-carbide particle; the carborundum porous ceramics that this method obtains has excellent mechanical property; but sintering temperature is high; need protection of inert gas, thus improve the preparation cost of carborundum porous ceramics.
Summary of the invention
The object of the invention is the shortcoming overcoming prior art, a kind of method of the manufacture porous silicon carbide ceramic improved is provided.Utilize present method can realize the nearly size sintering of porous silicon carbide ceramic, thus overcome the defect that silicon carbide is difficult to sinter.The porous silicon carbide ceramic utilizing this method to produce, to prepare complicated shape goods, has cost low, the advantage that product performance are moderate.
The present invention is achieved by following technical proposals: with silicon carbide and aluminum oxide for starting raw material, using graphite as pore-forming material, silicon carbide and aluminum oxide are mixed according to 5: 3 mass ratios, graphite quality percentage ranges controls at 1530wt%, stir after taking three kinds of raw materials respectively, obtain ceramic powder; Be dispersion solvent with alcohol, the resol adding 1 ~ 10wt% is binding agent, resol and alcohol is mixed according to 1: 10 volume ratio, obtains batch mixing solution; Ceramic powder is mixed with batch mixing solution, adopts silicon carbide mill ball, be 1: 2 according to powder and mill ball mass ratio, by above-mentioned ceramic powder and batch mixing solution tetrafluoroethylene ball grinder, be placed in ball milling on planetary ball mill, obtain ceramic slurry; By gained slip, dry 2 ~ 4 hours (object is to get rid of solvent) under Rotary Evaporators 70 ~ 80 DEG C of conditions, grinds after being dried by powder, and crosses 120 mesh sieves, obtain dry powder; Powder is pressed in chilling press rectangle examination bar, the size of described base substrate is controlled by die size in coldmoulding, and forming pressure is 30 ~ 90MPa; The biscuit body of gained is risen to sintering temperature 1400 ~ 1550 DEG C being rapidly heated in stove, sintering temperature keeps naturally cooling after 1 ~ 4 hour, obtain porous silicon carbide ceramic, risen to by room temperature in sintering procedure and be cooled to room temperature process medium-rate after sintering temperature and sintering complete and be about 5 DEG C/min.
The difference of the present invention and other manufacture method: (1) with silicon carbide and aluminum oxide for starting raw material, using graphite as pore-forming material, combined by a large amount of oxidations and mullitization product between silicon-carbide particle, ensureing that carborundum porous ceramics has higher intensity. ceramic powder and batch mixing solution are first stirred 30min by (2) on magnetic stirring apparatus, be placed in ball milling on planetary ball mill again, drum's speed of rotation is 120 ~ 360r/min, Ball-milling Time 1 ~ 4 hour.(3) adopt Rotary Evaporators to carry out drying, prevent the sedimentation layering of slip powder in drying process.
(4) risen to by room temperature in sintering procedure and be cooled to room temperature process medium-rate after sintering temperature and sintering complete and be about 5 DEG C/min.
The present invention is with silicon carbide and aluminum oxide for starting raw material, and graphite is pore-forming material, has prepared carborundum porous ceramics by reaction in－situ combined process.Graphite is thermosetting material, and can not liquefy during oxidation in atmosphere, and oxidizing temperature is high, thermal analyses shows: the oxidation of graphite is from 600 DEG C, until 800 DEG C complete.The oxidation of silicon-carbide particle occurs in more than 750 DEG C, and therefore before Oxidation of SiC, graphite can not by complete burn off, and before 800 DEG C, base substrate can by not having the graphite granule of complete burn off to support, thus make base substrate remain intact.After 800 DEG C, in sintering process, silicon carbide is oxidized to unformed silicon-dioxide, can set up support frame.In whole process, base substrate can remain intact.Along with the rising of temperature, at 1100 DEG C, amorphous silica is converted into cristobalite, and reacts with aluminum oxide gradually, generates mullite at silicon-carbide particle surface in situ, thus the reaction in－situ achieving porous silicon carbide ceramic combines.Mullite has good normal temperature and hot strength, thus substantially increases the mechanical property of porous ceramics.
In the present invention: silicon carbide micro-powder purity 99.4%, d50=10 μm; Alumina powder, the content of α phase is greater than 95%, d50=0.6 μm; Graphite purity is 99.9%, d50=5 ~ 20 μm.
Technique effect
Gained porous silicon carbide ceramic property indices of the present invention is as follows: X-ray diffraction analysis, and the principal phase of porous ceramics is silicon carbide, in conjunction with being mullite and cristobalite mutually; Electron microscopic observation: porous ceramics has the open-celled structure be interconnected, pore mean diameter is 2 ~ 8 μm; Measure open porosity and volume density by drainage, open porosity is 43 ~ 57%, and volume density is 1.4 ~ 1.72g/cm3; Linear shrinkage ratio is tested, and porous silicon carbide ceramic has very little dimensional change in sintering process, and linear shrinkage ratio is in ± 1.5%; Porous silicon carbide ceramic in 1450 DEG C of insulations preparation in 4 hours carries out resistance to acids and bases test, constantly little 1200 DEG C of insulations 10, and record sample weightening finish and be only 0.2%, bending strength declines 6.1%.Acid resistance, sample is in the 20wt% sulphuric acid soln boiled, and keep 1h, sample is moderate is 1.3%, and bending strength declines 13.3%; Alkaline resistance properties, sample is placed in the 1wt% sulphuric acid soln boiled, and keep 1h, sample is moderate is 5.5%, and bending strength declines 53.6%.Therefore the porous silicon carbide ceramic adopting the present invention to prepare has the open-celled structure be interconnected, and achieve nearly size sintering, sintering temperature is low, and moderate performance, show good ventilation property, high temperature oxidation resistance and acid-resistant corrosion in addition.
In sum, the present invention has prepared porous silicon carbide ceramic by reaction in－situ combined process, overcomes the defect that silicon carbide is difficult to sinter, and achieves the nearly size sintering of porous silicon carbide ceramic, can prepare complex-shaped goods.
Embodiment
Below in conjunction with specific embodiment, the invention will be further described.
In following examples: silicon carbide micro-powder refers to the particle of purity 99.4%, d50=10 μm; Alumina powder refers to that the content of α phase is greater than the micro mist of 95%, d50=0.6 μm.
Embodiment 1:
1) preparation of porous ceramics powder
Take 106.25g silicon carbide respectively, 63.75g aluminum oxide, 30g median size be stir after 5 μm of graphite, obtain ceramic powder.
2) batch mixing
Be dispersion solvent with alcohol, adding 6g resol is binding agent, resol and alcohol is mixed according to 1: 10 volume ratio, obtains batch mixing solution; Mixed with premixed liquid by ceramic powder, adopt silicon carbide mill ball, be 1: 2 according to powder and mill ball mass ratio, the planetary ball mill 2h in tetrafluoroethylene ball grinder by above-mentioned ceramic powder and batch mixing solution, obtains ceramic slurry.
3) dry
By step 2) gained slip, pour pear shape bottle into, dry 2 hours (object is to get rid of solvent) under Rotary Evaporators 80 DEG C of conditions, grinds after being dried by powder, and crosses 120 mesh sieves, obtain dry powder.
4) shaping
Powder is pressed in chilling press rectangle examination bar, the size of described base substrate is controlled by die size in coldmoulding, and forming pressure is 30MPa.
5) sinter
By step 4) the biscuit body of gained rises to sintering temperature 1450 DEG C, sintered heat insulating 4h being rapidly heated in stove.Gained carborundum porous ceramics indices is as follows: X-ray diffraction analysis, and the principal phase of porous ceramics is silicon carbide, in conjunction with being mullite and cristobalite mutually; Electron microscopic observation: porous ceramics has the open-celled structure be interconnected, pore mean diameter is 2 μm; Measure open porosity and volume density by drainage, open porosity is 50%, and volume density is 1.59g/cm3; Linear shrinkage ratio is tested, carborundum porous ceramics-1.0%.
Embodiment 2:
1) preparation of porous ceramics powder
Take 87.5g silicon carbide respectively, 52.5g aluminum oxide, 60g median size be stir after 5 μm of graphite, obtain ceramic powder.
2) batch mixing
Be dispersion solvent with alcohol, adding 6g resol is binding agent, resol and alcohol is mixed according to 1: 10 volume ratio, obtains batch mixing solution; Mixed with premixed liquid by ceramic powder, adopt silicon carbide mill ball, be 1: 2 according to powder and mill ball mass ratio, the planetary ball mill 2h in tetrafluoroethylene ball grinder by above-mentioned ceramic powder and batch mixing solution, obtains ceramic slurry.
3) dry
By step 2) gained slip, pouring pear shape bottle into, dry 2h (object is to get rid of solvent) under Rotary Evaporators 80 DEG C of conditions, grinding after powder is dried, and crossing 120 mesh sieves, obtaining dry powder.
4) shaping
Powder is pressed in chilling press rectangle examination bar, the size of described base substrate is controlled by die size in coldmoulding, and forming pressure is 30MPa.
5) sinter
By step 4) the biscuit body of gained rises to sintering temperature 1450 DEG C, sintered heat insulating 4h being rapidly heated in stove.Gained carborundum porous ceramics indices is as follows: X-ray diffraction analysis, and the principal phase of porous ceramics is silicon carbide, in conjunction with being mullite and cristobalite mutually; Electron microscopic observation: porous ceramics has the open-celled structure be interconnected, pore mean diameter is 2 μm; Measure open porosity and volume density by drainage, open porosity is 57%, and volume density is 1.4g/cm3; Linear shrinkage ratio is tested, carborundum porous ceramics+0.6%.
Embodiment 3:
1) preparation of porous ceramics powder
Take 105.26g silicon carbide respectively, 63.75g aluminum oxide, 30g median size be stir after 5 μm of graphite, obtain ceramic powder.
2) batch mixing
Be dispersion solvent with alcohol, the resol adding 6g is binding agent, resol and alcohol is mixed according to 1: 10 volume ratio, obtains batch mixing solution; Mixed with premixed liquid by ceramic powder, adopting silicon carbide mill ball, is 1: 2 according to powder and mill ball mass ratio, by above-mentioned ceramic powder and batch mixing solution planetary ball mill 2 hours in tetrafluoroethylene ball grinder, obtains ceramic slurry.
3) dry
By step 2) gained slip, pouring pear shape bottle into, dry 2h (object is to get rid of solvent) under Rotary Evaporators 80 DEG C of conditions, grinding after powder is dried, and crossing 120 mesh sieves, obtaining dry powder.
4) shaping
Powder is pressed in chilling press rectangle examination bar, the size of described base substrate is controlled by die size in coldmoulding, and forming pressure is 70MPa.
5) sinter
By step 4) the biscuit body of gained rises to sintering temperature 1450 DEG C, sintered heat insulating 4h being rapidly heated in stove.Gained carborundum porous ceramics indices is as follows: X-ray diffraction analysis, and the principal phase of porous ceramics is silicon carbide, in conjunction with being mullite and cristobalite mutually; Electron microscopic observation: porous ceramics has the open-celled structure be interconnected, pore mean diameter is 2 μm; Measure open porosity and volume density by drainage, open porosity is 46.5%, and volume density is 1.69g/cm3; Linear shrinkage ratio is tested, carborundum porous ceramics-1.2%.
Comparative example 1:
By step 5 in embodiment 1) described in sintering temperature change 1550 DEG C into; All the other are as follows with embodiment 1. gained carborundum porous ceramics indices: gained carborundum porous ceramics indices is as follows: X-ray diffraction analysis, and the principal phase of porous ceramics is silicon carbide, in conjunction with being mullite and cristobalite mutually; Electron microscopic observation: porous ceramics has the open-celled structure be interconnected, pore mean diameter is 2 μm; Measure open porosity and volume density by drainage, open porosity is 43%, and volume density is 1.68g/cm3; Linear shrinkage ratio is tested, carborundum porous ceramics-0.7%;
Comparative example 2:
By step 1 in embodiment 1) described in graphite median size change 20 μm into; All the other are as follows with embodiment 1. gained carborundum porous ceramics indices: X-ray diffraction analysis, and the principal phase of porous ceramics is silicon carbide, in conjunction with being mullite and cristobalite mutually; Electron microscopic observation: porous ceramics has the open-celled structure be interconnected, pore mean diameter is 8 μm, and the pore size distribution of porous ceramics presents bimodal distribution.
Claims (6)
1. a manufacture method for porous silicon carbide ceramic, is characterized in that, it comprises the following steps:
(1) prepare burden: with silicon carbide and aluminum oxide for starting raw material, using graphite as pore-forming material; Silicon carbide and aluminum oxide are mixed according to 5: 3 mass ratios, graphite quality percentage ranges controls at 15 ~ 30wt%, stirs, obtain ceramic powder after taking three kinds of raw materials respectively;
(2) batch mixing: be dispersion medium with alcohol, the resol adding 1 ~ 10wt% is binding agent, resol and alcohol is mixed according to 1: 10 volume ratio, obtains batch mixing solution; Mixed with batch mixing solution by ceramic powder, adopting silicon carbide mill ball, is 1: 2 according to powder and mill ball mass ratio, by above-mentioned ceramic powder and batch mixing solution in tetrafluoroethylene ball grinder, is placed in ball milling on planetary ball mill, obtains ceramic slurry;
(3) dry: by step 2) gained slip, drying 2 ~ 4 hours under Rotary Evaporators 70 ~ 80 DEG C of conditions, grinds after being dried by powder, and crosses 120 mesh sieves, obtain dry powder;
(4) shaping: powder is pressed in chilling press rectangle examination bar, the size of described base substrate is controlled by die size in coldmoulding, and forming pressure is 30 ~ 90MPa;
(5) sintering: by step 4) base substrate of gained rises to sintering temperature 1400 ~ 1550 DEG C, sintered heat insulating 1 ~ 4 hour being rapidly heated in stove.Risen to by room temperature in sintering procedure and be cooled to room temperature process medium-rate after sintering temperature and sintering complete and be about 5 DEG C/min.
2. the manufacture method of porous silicon carbide ceramic according to claim 1, is characterized in that: with silicon carbide and aluminum oxide for starting raw material, using graphite as pore-forming material; Silicon carbide and aluminum oxide are mixed according to 5: 3 mass ratios, graphite quality percentage ranges controls at 15 ~ 30wt%.
3. the manufacture method of porous silicon carbide ceramic according to claim 1, is characterized in that: be dispersion medium with alcohol, and the resol adding 1 ~ 10wt% is binding agent, resol and alcohol is mixed according to 1: 10 volume ratio, obtains batch mixing solution; Mixed with batch mixing solution by ceramic powder, adopting silicon carbide mill ball, is 1: 2 according to powder and mill ball mass ratio, by above-mentioned ceramic powder and batch mixing solution in tetrafluoroethylene ball grinder, be placed in ball milling on planetary ball mill, drum's speed of rotation is 120 ~ 360r/min, and Ball-milling Time 1 ~ 4 is little
Time, obtain ceramic slurry.
4. the manufacture method of porous silicon carbide ceramic according to claim 1, is characterized in that: by slip under Rotary Evaporators 70 ~ 80 DEG C of conditions dry 2 ~ 4 hours, grind, and cross 120 mesh sieves, make dry powder after being dried by powder.
5. the manufacture method of porous silicon carbide ceramic according to claim 1, is characterized in that: powder is pressed in chilling press rectangle examination bar, the size of described base substrate is controlled by die size in coldmoulding, and forming pressure is 30 ~ 90MPa.
6. the manufacture method of porous silicon carbide ceramic according to claim 1, is characterized in that: base substrate is risen to sintering temperature 1400 ~ 1550 DEG C, sintered heat insulating 1 ~ 4 hour being rapidly heated in stove.Risen to by room temperature in sintering procedure that to be cooled to room temperature process medium-rate after sintering temperature and sintering complete be 5 DEG C/min.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105130445A (en) * | 2015-09-15 | 2015-12-09 | 哈尔滨工业大学 | Method of co-sintering joined silicon-carbide-based composite ceramic green bodies |
| CN107673481A (en) * | 2017-09-29 | 2018-02-09 | 乔银娣 | A kind of water body purification of aquaculture agent and preparation method thereof |
| CN108558406A (en) * | 2018-05-03 | 2018-09-21 | 苏州卫优知识产权运营有限公司 | A kind of preparation process of silicon carbide ceramics grinding bead |
| CN110526713A (en) * | 2019-08-27 | 2019-12-03 | 广东工业大学 | A kind of porous silicon carbide ceramic and its preparation method and application |
| WO2021134811A1 (en) * | 2020-01-03 | 2021-07-08 | 南京工业大学 | Method for preparing silicon carbide catalytic film by means of co-sintering |
| CN113292344A (en) * | 2021-05-27 | 2021-08-24 | 山东大学 | Preparation method of mullite whisker reinforced silicon carbide ceramic matrix composite material with in-situ growth |
| CN114988903A (en) * | 2022-05-24 | 2022-09-02 | 北京科技大学广州新材料研究院 | High-strength low-shrinkage porous ceramic and preparation method thereof |
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2013
- 2013-11-17 CN CN201310601354.7A patent/CN104649709A/en active Pending
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105130445A (en) * | 2015-09-15 | 2015-12-09 | 哈尔滨工业大学 | Method of co-sintering joined silicon-carbide-based composite ceramic green bodies |
| CN107673481A (en) * | 2017-09-29 | 2018-02-09 | 乔银娣 | A kind of water body purification of aquaculture agent and preparation method thereof |
| CN108558406A (en) * | 2018-05-03 | 2018-09-21 | 苏州卫优知识产权运营有限公司 | A kind of preparation process of silicon carbide ceramics grinding bead |
| CN110526713A (en) * | 2019-08-27 | 2019-12-03 | 广东工业大学 | A kind of porous silicon carbide ceramic and its preparation method and application |
| WO2021134811A1 (en) * | 2020-01-03 | 2021-07-08 | 南京工业大学 | Method for preparing silicon carbide catalytic film by means of co-sintering |
| CN113292344A (en) * | 2021-05-27 | 2021-08-24 | 山东大学 | Preparation method of mullite whisker reinforced silicon carbide ceramic matrix composite material with in-situ growth |
| CN114988903A (en) * | 2022-05-24 | 2022-09-02 | 北京科技大学广州新材料研究院 | High-strength low-shrinkage porous ceramic and preparation method thereof |
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