CN102503533B - Method for preparing silicon carbide honeycomb ceramics - Google Patents
Method for preparing silicon carbide honeycomb ceramics Download PDFInfo
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Abstract
The invention discloses a method for preparing silicon carbide honeycomb ceramics. The method comprises the following steps of: 1) mixing bamboo charcoal micro-powder, silica sol, aluminum oxide, yttrium oxide and organic matter starch at a weight ratio of 70: 20: (1-5): (1-5): (1-8), so as to obtain honeycomb ceramics powder; 2) mixing and pugging: mixing water, polyvinyl alcohol and polyhydroxy ethanol according to a weight ratio of 70: (10-20): (10-20), and uniformly stirring the components to obtain a solution; and mixing the solution with the honeycomb ceramics powder according to a weight ratio of 100: (65-80), fully mixing the mixture in a mixing machine at a normal pressure and temperature for 0.5-1 hour, and then aging the mixture at the normal pressure and temperature for 2-3 hours, so as to obtain slurry material; 3) carrying out extrusion molding; 4) drying; and 5) sintering. The silicon carbide honeycomb ceramics produced by the preparation method disclosed by the invention has the characteristics of controllable holes, high specific surface area, intensity meeting requirements, and the like.
Description
Technical field
The present invention relates to a kind of preparation method of silicon carbide honeycomb ceramics, specifically, is that bamboo charcoal micropowder and commercial silicon dioxide colloidal sol are the preparation method of the silicon carbide honeycomb ceramics of aggregate.
Background technology
Ceramic honey comb is a kind of porous functional materials, healthy and free from worry (Corning) company of just rising by the U.S. as far back as 20 century 70s begins trial-production, just use ceramic honey comb to carry out the test of compact car tail gas clean-up, and obtained good effect the said firm in 1975.Ceramic honey comb has high specific surface area and good physical and chemical stability, also have in addition low density, high permeability, good energy absorption and high temperature resistant, corrosion-resistant, chemical stability and dimensional stability high, be easy to the various features such as regeneration.
In recent years, along with the development of ceramic honey comb technology of preparing, also in continuous expansion, application level improves constantly its range of application more really.Ceramic honey comb more and more is subject to people's attention as a kind of type material.Compare with traditional particulate state ceramic monolith, the vesicular honeycomb ceramic carrier has that Pressure Drop is little, geometric jacquard patterning unit surface is large, extended range is short, be conducive to the discharge with resultant of entering of reactant, and the advantages such as volume that can dwindle reactor, make ceramic honey comb use also comparatively extensive.
The material of preparation honeycomb ceramic carrier is except present widely used trichroite, also have aluminium titanates, aluminum oxide, silicon carbide, zircon, triphane, mullite etc., although wherein its thermal expansivity of carbofrax material is relatively higher, but can satisfy to a certain extent the requirement of performance, have also simultaneously that intensity is high, high temperature resistant, corrosion-resistant, wear-resistant, high-specific surface area, high than the series of advantages such as strong.Because the preparation technology of silicon carbide in recent years is day by day ripe, its synthetic method is varied, and is cheap, is easy to make the research of silicon carbide honeycomb ceramics and use increasingly extensive.
Conventional silicon carbide honeycomb ceramics all adopts the mode of pore-creating to prepare, the high cost that causes of temperature of reaction rises, be unfavorable for realizing production, cause thus the purifying vehicle exhaust dynamics inadequate, atmospheric pollution can not effectively be controlled, and also has simultaneously the contradiction between sintering character and vesicular structure, still insufficient strength as many in the material hole, can not provide high specific surface area again under the prerequisite that intensity guarantees, become its new research direction so select new raw material and technique to prepare silicon carbide honeycomb ceramics.
The preparation method of existing a kind of silicon carbide honeycomb ceramics adopts the binding agent Walocel MT 20.000PV, softening agent glycerine by 12%～15%: 7%～10% and water 81%～75% mix, mix with ceramic powder 70%～75% again, old, extrude after impurity screening and burning till more than 2200 ℃.Not only temperature of reaction is high, and hole is relatively low.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of preparation method of silicon carbide honeycomb ceramics, and it is controlled that the silicon carbide honeycomb ceramics produced of method has hole thus, and specific surface area is high, the intensity characteristics such as meet the demands.
In order to solve the problems of the technologies described above, the invention provides a kind of preparation method of silicon carbide honeycomb ceramics, comprise the following steps:
1), the preparation of ceramic honey comb powder:
Take bamboo charcoal micropowder and silicon dioxide gel as aggregate, take aluminum oxide and yttrium oxide as sintering aid, take organism starch as pore-forming material;
Bamboo charcoal micropowder, silicon dioxide gel, aluminum oxide, yttrium oxide and organism starch are mixed according to 70: 20: 1～5: 1～5: 1～8 weight ratio, get the ceramic honey comb powder;
2), mix pugging:
Water, polyvinyl alcohol and poly-hydroxyl ethanol are mixed according to 70: 10～20: 10～20 weight ratio, and uniform stirring gets solution;
Solution is mixed according to 100: 65～80 weight ratio with the ceramic honey comb powder, then fully mixed in mixing roll 0.5～1 hour at normal temperatures and pressures, then old 2～3 hours at normal temperatures and pressures; Get pug;
3), extrusion moulding:
Pug is extruded biscuit by extrusion equipment, and the size and dimension of this biscuit is controlled by the mould in extrusion equipment;
4), drying:
Biscuit is first adopted microwave heating (purpose is in order to discharge moisture), then in 0.5～1 hour (purpose is in order to get rid of aluminum oxide, yttrium oxide and organism starch) of 120～130 ℃ of heating;
5) burn till:
With step 4) dry after the product of gained fired 1～4 hour in 1600 ℃～1800 ℃ under normal pressure, then 1000～1200 ℃ of insulations 1～2 hour.
Improvement as the preparation method of silicon carbide honeycomb ceramics of the present invention: bamboo charcoal micropowder refers to that particle diameter is that 10～100 microns, specific surface area are 200～300m
2The bamboo charcoal of/g.
Further improvement as the preparation method of silicon carbide honeycomb ceramics of the present invention: organism starch is plant amylum, is for example potato starch.
Further improvement as the preparation method of silicon carbide honeycomb ceramics of the present invention: be step 3): first pug is carried out filtration, purification and process that (purpose is that pug causes the product plug-hole when preventing extrusion moulding, isolate and deformation defect), and then extrude biscuit by extrusion equipment.
Further improvement as the preparation method of silicon carbide honeycomb ceramics of the present invention: step 4): biscuit is adopted 450～490 watts of microwave heatings 12～15 minutes.
Further improvement as the preparation method of silicon carbide honeycomb ceramics of the present invention: step 5): sintering procedure is when 500～600 ℃ of being begun by room temperature to rise to as low temperature, and heat-up rate is 20～30 ℃/h.Purpose is in order to prevent as the too fast blank cracking that easily causes that heats up.
The present invention a kind ofly prepares the method for silicon carbide honeycomb ceramics take bamboo charcoal and commercial silicon dioxide colloidal sol as aggregate, the bamboo charcoal vesicular can produce hole after synthetic with commercial silicon dioxide colloidal sol original position.
To be bamboo wood fire under high temperature, few oxygen condition bamboo charcoal a kind ofly has a natural materials that enriches pore passage structure.Common bamboo charcoal specific surface area is 200～300m
2/ g, after secondary charing and activation treatment, the specific surface area of bamboo charcoal can be up to 700m
2/ g has high reactive behavior, suitable carbon source as SiC synthesis.Silicon dioxide gel is optional uses industrial silicon dioxide gel, and commercial silicon dioxide colloidal sol is due to uniform particles, and impurity is few, and higher specific surface area is more suitable for the silicon source as the preparation of silicon carbide honeycomb ceramics carrier.Adopting bamboo charcoal micropowder and silicon sol to prepare silicon carbide honeycomb ceramics is an innovation, can significantly reduce the synthesis temperature of silicon carbide honeycomb ceramics carrier, and the organism pyrolytic decomposition can increase small hole, increasing specific surface area.
In the present invention:
The silicon dioxide gel that commercial silicon dioxide colloidal sol for example can be produced available from Tianjin company of Nuo Bang Science and Technology Ltd. is (as 6SiO
2.3H
2O, foreign matter content are 1%～5%; Meet GB);
The particle diameter of aluminum oxide and yttrium oxide is 20～200mm.
In limited range value of the present invention, by changing sintering temperature, sintering aid content and Content of Pore-forming Agents can be controlled specific surface area and intensity level.Generally speaking: increase sintering aid content and can reduce sintering temperature, thereby reduce production costs, help to realize industrialization; Increase Content of Pore-forming Agents and can increase specific surface area, improve detergent power.
The present invention is that the contriver obtains through conscientiously studying, testing.Bamboo charcoal micropowder and commercial silicon dioxide colloidal sol are aggregate, and aluminum oxide and yttrium oxide are sintering aid, and organism starch is that the honeycomb ceramic carrier hole of pore-forming material preparation is controlled, and specific surface area is high, and intensity is good.The properties of this ceramic honey comb is as follows: the gained sample is pressed the mercury test, and the void content that records is 50%～75%, and the pore mean diameter is 10～15 microns, and volume density is 1.6～2.0g/cm
3There is small hole in electron microscopic observation in product, increasing specific surface area greatly, and intensity meets the requirements, ultimate compression strength 〉=35MPa.
In sum, the present invention not only can improve temperature condition, thereby reduces sintering temperature; Thereby the micropore increasing specific surface area that produces when burning till in addition simultaneously again can the proof strength requirement.
Embodiment
In following examples:
Bamboo charcoal micropowder refers to that particle diameter is that 10～100 microns, specific surface area are 200～300m
2The bamboo charcoal of/g;
Silicon dioxide gel is selected commercial silicon dioxide colloidal sol;
The particle diameter of aluminum oxide and yttrium oxide is 20～200mm.
The preparation method of embodiment 1, a kind of silicon carbide honeycomb ceramics, carry out following steps successively:
1), the preparation of ceramic honey comb powder:
Take bamboo charcoal micropowder and commercial silicon dioxide colloidal sol as aggregate, take aluminum oxide and yttrium oxide as sintering aid, take potato starch as pore-forming material;
Bamboo charcoal micropowder, commercial silicon dioxide colloidal sol, aluminum oxide, yttrium oxide and potato starch were pressed 70: 20: 3: the weight ratio of 3: 4 is mixed; Get the ceramic honey comb powder;
2) mix pugging:
Water, polyvinyl alcohol and poly-hydroxyl ethanol are mixed according to the weight ratio of 70: 15: 15, and uniform stirring gets solution;
Solution is mixed according to the weight ratio of 100: 75 with the ceramic honey comb powder, then fully mixed in mixing roll 40 minutes at normal temperatures and pressures, under similarity condition (being under normal temperature and pressure) old 2.5 hours; Get pug;
3), extrusion moulding:
First pug is carried out filtration, purification and process (pug is crossed 60 mesh sieves), thereby when preventing extrusion moulding, pug causes the product plug-hole, isolate and the defective such as distortion.
Pug after filtration, purification is processed is extruded biscuit by extrusion equipment, and the geomery size of biscuit is controlled (this is routine techniques) by the mould in extrusion equipment.
4), drying:
First adopt 450 watts of microwave heatings 12 minutes discharging moisture biscuit, then in 120 ℃ of heating 0.5 hour to get rid of aluminum oxide, yttrium oxide and potato starch etc.;
5) burn till:
With step 4) dry after the product of gained fired 2 hours in 1750 ℃ under normal pressure, then 1000 ℃ of insulations 1 hour, get silicon carbide honeycomb ceramics.
Sintering procedure is when 500～600 ℃ of being begun by room temperature to rise to as low temperature, and heat-up rate is 20 ℃/h, as the too fast blank cracking that easily causes that heats up.
The silicon carbide honeycomb ceramics of gained can be as catalyst carrier for automobile tail gas purifier, and its property indices is as follows:
The gained sample is pressed the mercury test, and the void content that records is 60%, and the pore mean diameter is 12 microns, and volume density is 1.8g/cm
3, there is small hole in electron microscopic observation in product, increasing specific surface area greatly, ultimate compression strength 〉=35MPa.
The preparation method of embodiment 2, a kind of silicon carbide honeycomb ceramics, carry out following steps successively:
1), the preparation of ceramic honey comb powder:
Take bamboo charcoal micropowder and commercial silicon dioxide colloidal sol as aggregate, take aluminum oxide and yttrium oxide as sintering aid, take potato starch as pore-forming material;
Bamboo charcoal micropowder, commercial silicon dioxide colloidal sol, aluminum oxide, yttrium oxide and potato starch were pressed 70: 20: 2: the weight ratio of 2: 6 is mixed; Get the ceramic honey comb powder;
2) mix pugging:
Water, polyvinyl alcohol and poly-hydroxyl ethanol are mixed according to the weight ratio of 70: 10: 20, and uniform stirring gets solution;
Solution is mixed according to the weight ratio of 100: 70 with the ceramic honey comb powder, then fully mixed in mixing roll 0.5 hour at normal temperatures and pressures, under similarity condition (being under normal temperature and pressure) old 2 hours; Get pug;
3), extrusion moulding:
First pug is carried out filtration, purification and process (pug is crossed 60 mesh sieves), thereby when preventing extrusion moulding, pug causes the product plug-hole, isolate and the defective such as distortion.
Pug after filtration, purification is processed is extruded biscuit by extrusion equipment, and the geomery size of biscuit is controlled (this is routine techniques) by the mould in extrusion equipment.
4), drying:
First adopt 460 watts of microwave heatings 12 minutes discharging moisture biscuit, then in 125 ℃ of heating 40 minutes to get rid of aluminum oxide, yttrium oxide and potato starch etc.;
5) burn till:
With step 4) dry after the product of gained fired 1.5 hours in 1800 ℃ under normal pressure, then 1100 ℃ of insulations 1 hour, get silicon carbide honeycomb ceramics.
Sintering procedure is when 500～600 ℃ of being begun by room temperature to rise to as low temperature, and heat-up rate is 25 ℃/h, as the too fast blank cracking that easily causes that heats up.
The silicon carbide honeycomb ceramics of gained can be as catalyst carrier for automobile tail gas purifier, and its property indices is as follows:
The gained sample is pressed the mercury test, and the void content that records is 75%, and the pore mean diameter is 13 microns, and volume density is 1.65g/cm
3, there is small hole in electron microscopic observation in product, increasing specific surface area greatly, ultimate compression strength 〉=35MPa.
The preparation method of embodiment 3, a kind of silicon carbide honeycomb ceramics, carry out following steps successively:
1), the preparation of ceramic honey comb powder:
Take bamboo charcoal micropowder and commercial silicon dioxide colloidal sol as aggregate, take aluminum oxide and yttrium oxide as sintering aid, take potato starch as pore-forming material;
Bamboo charcoal micropowder, commercial silicon dioxide colloidal sol, aluminum oxide, yttrium oxide and potato starch were pressed 70: 20: 4: the weight ratio of 4: 2 is mixed; Get the ceramic honey comb powder;
2) mix pugging:
Water, polyvinyl alcohol and poly-hydroxyl ethanol are mixed according to the weight ratio of 70: 14: 16, and uniform stirring gets solution;
Solution is mixed according to the weight ratio of 100: 78 with the ceramic honey comb powder, then fully mixed in mixing roll 45 minutes at normal temperatures and pressures, under similarity condition (being under normal temperature and pressure) old 3 hours; Get pug;
3), extrusion moulding:
First pug is carried out filtration, purification and process (pug is crossed 60 mesh sieves), thereby when preventing extrusion moulding, pug causes the product plug-hole, isolate and the defective such as distortion.
Pug after filtration, purification is processed is extruded biscuit by extrusion equipment, and the geomery size of biscuit is controlled (this is routine techniques) by the mould in extrusion equipment.
4), drying:
First adopt 460 watts of microwave heatings 12 minutes discharging moisture biscuit, then in 125 ℃ of heating 40 minutes to get rid of aluminum oxide, yttrium oxide and potato starch etc.;
5) burn till:
With step 4) dry after the product of gained fired 2 hours in 1600 ℃ under normal pressure, then 1000 ℃ of insulations 2 hours, get silicon carbide honeycomb ceramics.
Sintering procedure is when 500～600 ℃ of being begun by room temperature to rise to as low temperature, and heat-up rate is 25 ℃/h, as the too fast blank cracking that easily causes that heats up.
The silicon carbide honeycomb ceramics of gained can be as catalyst carrier for automobile tail gas purifier, and its property indices is as follows:
The gained sample is pressed the mercury test, and the void content that records is 55%, and the pore mean diameter is 13 microns, and volume density is 1.9g/cm
3, there is small hole in electron microscopic observation in product, increasing specific surface area greatly, ultimate compression strength 〉=35MPa.
Comparative Examples 1,
With embodiment 1 step 2) in solution make into: water, Walocel MT 20.000PV and glycerine mix according to the weight ratio of 70: 15: 15, and uniform stirring gets solution; All the other are with embodiment 1.
The silicon carbide honeycomb ceramics property indices of gained is as follows:
The gained sample is pressed the mercury test, and the void content that records is 45%, and the pore mean diameter is 10 microns, and volume density is 2.3g/cm
3
Comparative Examples 2,
The step 1 that replaces embodiment 1 with the ceramic powder of routine) the ceramic honey comb powder in is with step 5) firing temperature make 2200 ℃ into, all the other are with embodiment 1.
The silicon carbide honeycomb ceramics property indices of gained is as follows:
The gained sample is pressed the mercury test, and the void content that records is 40%, and the pore mean diameter is 8 microns, and volume density is 2.4g/cm
3
At last, it is also to be noted that, what more than enumerate is only several specific embodiments of the present invention.Obviously, the invention is not restricted to above embodiment, many distortion can also be arranged.All distortion that those of ordinary skill in the art can directly derive or associate from content disclosed by the invention all should be thought protection scope of the present invention.
Claims (6)
1. the preparation method of silicon carbide honeycomb ceramics is characterized in that comprising the following steps:
1), the preparation of ceramic honey comb powder:
Take bamboo charcoal micropowder and silicon dioxide gel as aggregate, take aluminum oxide and yttrium oxide as sintering aid, take organism starch as pore-forming material;
Bamboo charcoal micropowder, silicon dioxide gel, aluminum oxide, yttrium oxide and organism starch are mixed according to the weight ratio of 70:20:1 ~ 5:1 ~ 5:1 ~ 8, get the ceramic honey comb powder;
Described bamboo charcoal micropowder refers to that particle diameter is that 10 ~ 100 microns, specific surface area are 200～300 m
2The bamboo charcoal of/g;
2), mix pugging:
Water, polyvinyl alcohol and poly-hydroxyl ethanol are mixed according to the weight ratio of 70:10 ~ 20:10 ~ 20, and uniform stirring gets solution;
Described solution is mixed according to the weight ratio of 100:65 ~ 80 with the ceramic honey comb powder, then fully mixed in mixing roll 0.5 ~ 1 hour at normal temperatures and pressures, then old 2 ~ 3 hours at normal temperatures and pressures; Get pug;
3), extrusion moulding:
Pug is extruded biscuit by extrusion equipment, and the size and dimension of described biscuit is controlled by the mould in extrusion equipment;
4), drying:
Biscuit is first adopted microwave heating, then in 120 ~ 130 ℃ of heating 0.5 ~ 1 hour;
5), burn till:
The product of gained after the step 4) drying was fired 1 ~ 4 hour in 1600 ℃ ~ 1800 ℃ under normal pressure, then 1000 ~ 1200 ℃ of insulations 1 ~ 2 hour.
2. the preparation method of silicon carbide honeycomb ceramics according to claim 1, it is characterized in that: described organism starch is plant amylum.
3. the preparation method of silicon carbide honeycomb ceramics according to claim 2, it is characterized in that: described plant amylum is potato starch.
4. the preparation method of according to claim 1 ~ 3 arbitrary described silicon carbide honeycomb ceramics, it is characterized in that: described step 3) is: first pug is carried out filtration, purification and process, and then extrude biscuit by extrusion equipment.
5. the preparation method of silicon carbide honeycomb ceramics according to claim 4, is characterized in that: in described step 4): biscuit is adopted 450 ~ 490 watts of microwave heatings 12 ~ 15 minutes.
6. the preparation method of silicon carbide honeycomb ceramics according to claim 5 is characterized in that: in described step 5):
Sintering procedure is when 500 ~ 600 ℃ of being begun by room temperature to rise to as low temperature, and heat-up rate is 20 ~ 30 ℃/h.
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| CN102850593A (en) * | 2012-09-18 | 2013-01-02 | 蚌埠鑫源石英材料有限公司 | Preparation method of black silicon dioxide powder material |
| CN104072141B (en) * | 2013-03-29 | 2016-06-08 | 北京市理化分析测试中心 | The preparation method of a kind of silicon carbide honeycomb ceramics |
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| CN107698276A (en) * | 2017-09-19 | 2018-02-16 | 常州朋悦纺织品有限公司 | A kind of porous silicon carbide ceramic and preparation method thereof |
| CN107573077A (en) * | 2017-10-18 | 2018-01-12 | 重庆奥福精细陶瓷有限公司 | Recrystallized silicon carbide diesel vehicle soot grain catcher and preparation method thereof |
| CN108610050A (en) * | 2018-04-16 | 2018-10-02 | 长兴科创科技咨询有限公司 | A kind of porous silicon carbide ceramic and preparation method thereof |
| CN110022622B (en) * | 2019-05-16 | 2021-05-04 | 厦门蜂涛陶瓷有限公司 | Alumina honeycomb ceramic heating body and preparation method thereof |
| CN115364580B (en) * | 2021-05-20 | 2023-10-10 | 中国石油化工股份有限公司 | Honeycomb carbon-based filter material and preparation method thereof |
| CN115636414A (en) * | 2022-10-31 | 2023-01-24 | 常州永蓁材料科技有限公司 | Silicon carbide composite particles with high specific surface area, and preparation method and application thereof |
| CN116120069B (en) * | 2022-12-28 | 2024-04-26 | 大莲电瓷（福建）有限公司 | Silicon carbide honeycomb ceramic and preparation method thereof |
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