CN108467281A - The preparation method of zircite porous ceramic - Google Patents

The preparation method of zircite porous ceramic Download PDF

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Publication number
CN108467281A
CN108467281A CN201810253041.XA CN201810253041A CN108467281A CN 108467281 A CN108467281 A CN 108467281A CN 201810253041 A CN201810253041 A CN 201810253041A CN 108467281 A CN108467281 A CN 108467281A
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porous ceramic
preparation
zircite
zircite porous
carbon fiber
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CN108467281B (en
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聂向军
周光辉
陈宏裕
王文利
孙亮
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Dongguan CSG Ceramics Technology Co Ltd
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Dongguan CSG Ceramics Technology Co Ltd
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Abstract

The present invention relates to a kind of preparation methods of zircite porous ceramic, include the following steps:Step 1:By in Zirconium powder and carbon fiber input container, suitable quantity of water is added, is stirred, foaming agent and foam stabilizer are put into whipping process, until being bubbled uniformly, then puts into binder, obtains mixed material;Step 2:Mixed material is poured into molding die, naturally dry molding obtains green compact;Step 3:Closed box is put the green body into, is vacuumized, butane and oxygen to normal pressure is then charged with and stands, after 1.5~3 hours, electronics fire, which is lighted, makes During Combustion of Butane, all burnt, obtains the green body of trepanning;Step 4:By the green body high temperature sintering of trepanning, zircite porous ceramic is obtained.Carbon fiber intersection connects to forming network skeleton, is Zirconium powder and other materials with firm support, increases the toughness and intensity of ceramics;Foam stabilizer is introduced, to control the opportunity of lather collapse, acquisition uniform pore diameter, arrangement are closely porous, and preparation process is environmentally protective.

Description

The preparation method of zircite porous ceramic
Technical field
The present invention relates to ceramic technical fields, more particularly to the preparation method of zircite porous ceramic.
Background technology
The application of porous ceramics starts from 19 century 70s, is merely used as uranium purification material and bacteriological filter material at that time Material.With the continuous expansion of porous ceramics use scope, application field is also gradually expanded, gradual by fields such as filtering, thermal technologies Expand to heat-insulated, sound-absorbing, electronics, photoelectricity, sensing, environmental organism and chemical field.
From structure, porous ceramics is the porous ceramic bodies of the high porosity with three dimensions grid structure, is made Cavernous body of the type like the foamed plastics of tempering or porcelain.Due to it have porosity height, large specific surface area, anti-thermal shock, High temperature resistant, resistant to chemical etching and good mechanical strength and filtering absorption property, can be widely applied to heat exchange material, gas distribution material Molten metal is filtered in material, vehicle exhaust device, purification metallurgical industry, and thermal energy recycles, light industry spraying industry, at trade effluent Reason, thermal and sound insulating materials are used as chemical catalysis agent carrier, electrolyte membrane and separation dispersive element etc..
Therefore, porous ceramics is widened and developed to the porous ceramic bodies for preparing high intensity, uniform pore diameter at home in every profession and trade Application, it is undoubtedly very necessary.
Invention content
Based on this, the present invention provides a kind of preparation method of zircite porous ceramic, and preparation process non-poisonous material generates, green Colour circle is protected, and manufactured zircite porous ceramic uniform pore diameter, toughness and intensity are good.
A kind of preparation method of zircite porous ceramic, includes the following steps:
Step 1:By in Zirconium powder and carbon fiber input container, suitable quantity of water is added, is stirred, in whipping process Foaming agent and foam stabilizer are put into, until being bubbled uniformly, binder is then put into, obtains mixed material;
Step 2:Mixed material is poured into molding die, naturally dry molding obtains green compact;
Step 3:Closed box is put the green body into, is vacuumized, butane and oxygen is then charged with to normal pressure, stands 1.5~3 hours Afterwards, electronics fire, which is lighted, makes During Combustion of Butane, and all burnt obtains the green body of trepanning;
Step 4:By the green body high temperature sintering of trepanning, zircite porous ceramic is obtained.
The preparation method of above-mentioned zircite porous ceramic, the light specific gravity of carbon fiber can invest foam outer wall, and intersection connects Formation network skeleton is Zirconium powder and other materials with firm support, increases the toughness and intensity of ceramics, makes porous pottery Porcelain stable structure is firm;Foam stabilizer is introduced in the reaction system, to control the opportunity of lather collapse, after foaming agent foam, is made Foam is not easily broken before the forming, and acquisition uniform pore diameter, arrangement are closely porous after drying molding and opening step;And it prepares Process non-poisonous material generates, environmentally protective.
Zirconium powder, carbon fiber, foaming agent, foam stabilizer, binder mass ratio are in one of the embodiments,: 100:15~40:5~10:0.1~1.5:6~12.
A diameter of 6~20 μm of carbon fiber in one of the embodiments, length are 3~12mm.
The granularity of Zirconium powder is 0.2~1 μm in one of the embodiments,.
In one of the embodiments, in Zirconium powder zirconium oxide mass content >=90%.
Foaming agent is anion surfactant in one of the embodiments,.
In one of the embodiments, foaming agent be sodium n-alkylbenzenesulfonate, alkylsulfonate, alpha-olefin sodium sulfonate, Alpha-sulfo monocarboxylic acid and its derivative, aliphatic acid sulfoalkyl ester or aliphatic acid sulfoalkyl amide.
Foam stabilizer is silicones polyethers lotion in one of the embodiments,.
Binder is polyvinyl alcohol in one of the embodiments,.
High temperature sintering is in one of the embodiments,:First 500 DEG C are warming up to the rate of 0.5 DEG C/min~2 DEG C/min ~750 DEG C, and keep the temperature 1~2h, then 1400 DEG C~1600 DEG C are warming up to the rate of 2 DEG C/min~3 DEG C/min, and keep 2~ 4h。
Specific implementation mode
It to facilitate the understanding of the present invention, below will be to invention is more fully described.But the present invention can be to be permitted Mostly different form is realized, however it is not limited to embodiment described herein.Make on the contrary, purpose of providing these embodiments is It is more thorough and comprehensive to the understanding of the disclosure.
Unless otherwise defined, all of technologies and scientific terms used here by the article and belong to the technical field of the present invention The normally understood meaning of technical staff is identical.Used term is intended merely to description tool in the description of the invention herein The purpose of the embodiment of body, it is not intended that in the limitation present invention.
The present invention provides a kind of preparation method of zircite porous ceramic, includes the following steps:
Step 1:Zirconium powder, carbon fiber, foaming agent, foam stabilizer, binder, water are provided.
For example, each component is provided in mass ratio, Zirconium powder:Carbon fiber:Foaming agent:Foam stabilizer:Binder=100: 15~40:5~10:0.1~1.5:6~12.
Step 2:By in Zirconium powder and carbon fiber input container, suitable quantity of water is added, the dosage of water is to soak zirconium oxide It subject to powder and carbon fiber, is stirred, foaming agent and foam stabilizer is put into whipping process, until being bubbled uniformly, then put into Binder obtains mixed material.
The light specific gravity of carbon fiber, can invest foam outer wall, and intersection connects to forming network skeleton, be Zirconium powder and its Its material is increased the toughness and intensity of ceramics, so that porous ceramic structure is stablized firm with firm support.More preferably, carbon fiber Diameter be selected as 6~20 μm, length is selected as 3~12mm.Carbon fiber, which is shorter than 3mm or is longer than 12mm, is unfavorable for carbon fiber in foam The absorption of outer wall, may be formed it is too short and can not form interconnection or long and outsourcing foam outer wall be unfavorable for it is adjacent The formation of foam causes foam interval excessive, the low problem of one-tenth porosity.
Zirconium powder selects the Zirconium powder of the tetragonal phase crystalline structure of stabilized with yttrium oxide, is aoxidized in Zirconium powder Mass content >=90% of zirconium obtains the ceramic of better mechanical property to ensure that intercrystalline is tightly combined.Granularity is It 0.2~1 μm, can meticulously insert in the network skeleton that carbon fiber is made into, and do not destroy the formation of foam, Zirconium powder When granularity is more than 1 μm, it is unfavorable for forming foam since it is more coarse.
Foaming agent selects anion surfactant, contains moisture content in this reaction system, anion surfactant is in water After middle dissociation, hydrophobicity anion is generated, there is surface-active, form foam in stirring.More preferably, foaming agent selects straight chain Anion surfactant is easy to be degraded by microorganisms, more environmentally friendly, such as sodium n-alkylbenzenesulfonate, alkylsulfonate, α- Alkene sulfonic acid sodium, alpha-sulfo monocarboxylic acid and its derivative, aliphatic acid sulfoalkyl ester or aliphatic acid sulfoalkyl amide.
To make foam that can stablize into bubble before porous ceramic shaping, it is added into foam stabilizer.Certainly, foam stabilizer is not to get over It is much better, if foam does not rupture, it will be unable to form the porous of connection in ceramics, so needing to control by controlling the amount of foam stabilizer The rupture opportunity of foam processed or the thickness of foam.It is 5~10 that the present invention, which selects the mass ratio of foaming agent and foam stabilizer,:0.1~ 1.5, make foam that can be stabilized in stirring, when drying molding, because of the reduction of moisture content, the molecule of foaming agent is received Pore is presented with molecular contraction for the relatively thin side wall of contracting, foam or the thickness of side wall is thinned, then, can in During Combustion of Butane Wash the thin-walled of pore open with the impulse force using flame, opening is porous, and because of the network structure of carbon fiber, and porous ceramics will not produce The problem of raw rupture.
Preferably, foam stabilizer select silicones polyethers lotion, by change Blowing agent molecules internal arrangement sequence, make bubble with Arrangement is close neat between bubble, to form fine and close inner layer film so that anti-pressure ability is especially strong, can control air bubble liquid-membrane Structural stability makes Blowing agent molecules in the Methodistic distribution of the liquid film of bubble, assigns the good elasticity of foam and review one's lessons by oneself reactivation Power, to reach especially desirable foam stabilizing effect.
It is 2.5wt% that binder, which selects polyvinyl alcohol, polyvinyl alcohol water solution mass concentration, is carried for the molding of porous ceramics For good cohesive force, and it is easy to exclude in dumping.
Step:3:Mixed material is poured into molding die, naturally dry molding obtains green compact.Molding die can the side of being The mold of shape or circle or other irregular shapes, material to be mixed dry molding, you can take out, the process for carrying out next step.
Step 4:Closed box is put the green body into, is vacuumized, is then charged with butane and oxygen to normal pressure (generally 1atm).Fourth Alkane and oxygen are to be filled in closed box together after mixing, avoid butane and oxygen mix uneven, caused by burning it is non-uniform Problem.It is 5~10L/min that gas, which is filled with flow, allows air-flow that there is certain impulse force to be filled in the pore of green compact, and one Retain certain mobility in the fixed time, keeps gas mixing uniform.It keeps standing 1.5~3 hours after being filled with gas, makes butane It is uniformly filled in the pore of green compact with oxygen gas, electronics fire, which is lighted, makes During Combustion of Butane, and the temperature of During Combustion of Butane is up to 800~1000 DEG C, flame alters burning in pore, and discharge part binder, foaming agent and foam stabilizer make pore open, and penetrate through certain orientation Pore keeps trepanning uniform.All burnt naturally cools to 50~100 DEG C, obtains the green body of trepanning.
Step 5:By the green body high temperature sintering of trepanning, first with the rate of 0.5 DEG C/min~2 DEG C/min be warming up to 500 DEG C~ 750 DEG C, and keep the temperature 1~2h makes temperature slowly penetrate into pore to heat up at a slow speed, the inner wall of Even Sintering pore;Again with 2 DEG C/ The rate of min~3 DEG C/min is warming up to 1400 DEG C~1600 DEG C, and keeps 2~4h, keeps blank sintering fine and close.High temperature sintering is complete Finish, obtains zircite porous ceramic.
The preparation method of zircite porous ceramic of the present invention introduces carbon fiber in the reaction system, forms network skeleton, is Porous ceramics provides firm support, increases the intensity and toughness of porous ceramics, performance is made to stablize, and after foaming agent foam, uses Foam stabilizer makes foam be not easily broken before the forming, and acquisition uniform pore diameter, arrangement are closely more after drying molding and opening step Hole.
It is specific embodiment explanation below.
Embodiment 1
A kind of preparation method of zircite porous ceramic of the present embodiment, includes the following steps:
Step 1:Following parts by weight of component is provided:100 parts of Zirconium powder, 15 parts of carbon fiber, 6 parts of foaming agent, foam stabilizer 0.5 part, 10 parts of binder, suitable quantity of water.
A diameter of 6~12 μm of carbon fiber, length is selected as 3~8mm.
Zirconium powder selects the Zirconium powder of the tetragonal phase crystalline structure of stabilized with yttrium oxide, is aoxidized in Zirconium powder The mass content of zirconium is 95%, and granularity is 0.2~0.6 μm.
Foaming agent selects sodium n-alkylbenzenesulfonate.
Foam stabilizer selects silicones polyethers lotion.
It is 2.5wt% that binder, which selects polyvinyl alcohol, polyvinyl alcohol water solution mass concentration,.
Step 2:By in Zirconium powder and carbon fiber input container, suitable quantity of water is added, is stirred, in whipping process Foaming agent and foam stabilizer are put into, until being bubbled uniformly, binder is then put into, obtains mixed material.
Step 3:Mixed material is poured into molding die, naturally dry molding obtains green compact.
Step 4:Closed box is put the green body into, is vacuumized, is then charged with butane and oxygen to normal pressure, butane and oxygen are mixed It is filled in closed box together after conjunction, it is 5L/min that gas, which is filled with flow, keeps standing 2 hours after being filled with gas.All burnt, from 100 DEG C so are cooled to, obtains the green body of trepanning.
Step 5:By the green body high temperature sintering of trepanning, 600 DEG C first are warming up to the rate of 0.5 DEG C/min, and keep the temperature 1.5h, 1500 DEG C are warming up to the rate of 2 DEG C/min again, and keeps 2h.High temperature sintering finishes, and obtains zircite porous ceramic.
After testing, the porosity of the Zirconium oxide foamed ceramic is 72%, bending strength 96MPa.
Embodiment 2
A kind of preparation method of zircite porous ceramic of the present embodiment, includes the following steps:
Step 1:Following parts by weight of component is provided:100 parts of Zirconium powder, 20 parts of carbon fiber, 5 parts of foaming agent, foam stabilizer 0.2 part, 8 parts of binder, suitable quantity of water.
The diameter of carbon fiber is selected as 8~10 μm, and length is selected as 5~8mm.
Zirconium powder selects the Zirconium powder of the tetragonal phase crystalline structure of stabilized with yttrium oxide, is aoxidized in Zirconium powder The mass content of zirconium is 98%, and granularity is 0.4~0.8 μm.
Foaming agent selects alkylsulfonate.
Foam stabilizer selects silicones polyethers lotion.
It is 2.5wt% that binder, which selects polyvinyl alcohol, polyvinyl alcohol water solution mass concentration,.
Step 2:By in Zirconium powder and carbon fiber input container, suitable quantity of water is added, is stirred, in whipping process Foaming agent and foam stabilizer are put into, until being bubbled uniformly, binder is then put into, obtains mixed material.
Step:3:Mixed material is poured into molding die, naturally dry molding obtains green compact.
Step 4:Closed box is put the green body into, is vacuumized, is then charged with butane and oxygen to normal pressure, butane and oxygen are mixed It is filled in closed box together after conjunction, it is 6L/min that gas, which is filled with flow, keeps standing 1.5 hours after being filled with gas.All burnt, 90 DEG C are naturally cooled to, the green body of trepanning is obtained.
Step 5:By the green body high temperature sintering of trepanning, 500 DEG C first are warming up to the rate of 1 DEG C/min, and keep the temperature 2h, then with The rate of 2 DEG C/min is warming up to 1400 DEG C, and keeps 3h, and high temperature sintering finishes, and obtains zircite porous ceramic.
After testing, the porosity of the Zirconium oxide foamed ceramic is 78%, bending strength 105MPa.
Embodiment 3
A kind of preparation method of zircite porous ceramic of the present embodiment, includes the following steps:
Step 1:Following parts by weight of component is provided:100 parts of Zirconium powder, 25 parts of carbon fiber, 8 parts of foaming agent, foam stabilizer 0.8 part, 10 parts of binder, suitable quantity of water.
The diameter of carbon fiber is selected as 10~20 μm, and length is selected as 3~8mm.
Zirconium powder selects the Zirconium powder of the tetragonal phase crystalline structure of stabilized with yttrium oxide, is aoxidized in Zirconium powder The mass content of zirconium is 98%, and granularity is 0.3~0.8 μm.
Foaming agent selected fatty acid sulfoalkyl amide.
Foam stabilizer selects silicones polyethers lotion.
It is 2.5wt% that binder, which selects polyvinyl alcohol, polyvinyl alcohol water solution mass concentration,.
Step 2:By in Zirconium powder and carbon fiber input container, suitable quantity of water is added, is stirred, in whipping process Foaming agent and foam stabilizer are put into, until being bubbled uniformly, binder is then put into, obtains mixed material.
Step:3:Mixed material is poured into molding die, naturally dry molding obtains green compact.
Step 4:Closed box is put the green body into, is vacuumized, is then charged with butane and oxygen to normal pressure, butane and oxygen are mixed It is filled in closed box together after conjunction, it is 7L/min that gas, which is filled with flow, keeps standing 2 hours after being filled with gas.All burnt, from 80 DEG C so are cooled to, obtains the green body of trepanning.
Step 5:By the green body high temperature sintering of trepanning, 500 DEG C first are warming up to the rate of 2 DEG C/min, and keep the temperature 2h, then with The rate of 2 DEG C/min is warming up to 1600 DEG C, and keeps 2h, and high temperature sintering finishes, and obtains zircite porous ceramic.
After testing, the porosity of the Zirconium oxide foamed ceramic is 80%, bending strength 107MPa.
Embodiment 4
A kind of preparation method of zircite porous ceramic of the present embodiment, includes the following steps:
Step 1:Following parts by weight of component is provided:100 parts of Zirconium powder, 35 parts of carbon fiber, 9 parts of foaming agent, foam stabilizer 1 Part, 11 parts of binder, suitable quantity of water.
The diameter of carbon fiber is selected as 8~15 μm, and length is selected as 6~10mm.
Zirconium powder selects the Zirconium powder of the tetragonal phase crystalline structure of stabilized with yttrium oxide, is aoxidized in Zirconium powder The mass content of zirconium is 95%, and granularity is 0.5~1 μm.
Foaming agent selects alpha-olefin sodium sulfonate.
Foam stabilizer selects silicones polyethers lotion.
It is 2.5wt% that binder, which selects polyvinyl alcohol, polyvinyl alcohol water solution mass concentration,.
Step 2:By in Zirconium powder and carbon fiber input container, suitable quantity of water is added, is stirred, in whipping process Foaming agent and foam stabilizer are put into, until being bubbled uniformly, binder is then put into, obtains mixed material.
Step:3:Mixed material is poured into molding die, naturally dry molding obtains green compact.
Step 4:Closed box is put the green body into, is vacuumized, butane and oxygen to normal pressure is then charged with and stands, butane and oxygen To be filled in closed box together after mixing, it is 10L/min that gas, which is filled with flow, keeps standing 2.5 hours after being filled with gas.Burning It finishes, naturally cools to 70 DEG C, obtain the green body of trepanning.
Step 5:By the green body high temperature sintering of trepanning, 600 DEG C first are warming up to the rate of 1.2 DEG C/min, and keep the temperature 1h, then 1600 DEG C are warming up to the rate of 3 DEG C/min, and keeps 2h, high temperature sintering finishes, and obtains zircite porous ceramic.
After testing, the porosity of the Zirconium oxide foamed ceramic is 79%, bending strength 102MPa.
Embodiment 5
A kind of preparation method of zircite porous ceramic of the present embodiment, includes the following steps:
Step 1:Following parts by weight of component is provided:100 parts of Zirconium powder, 40 parts of carbon fiber, 9 parts of foaming agent, foam stabilizer 1.5 parts, 12 parts of binder, suitable quantity of water.
The diameter of carbon fiber is selected as 12~20 μm, and length is selected as 7~12mm.
Zirconium powder selects the Zirconium powder of the tetragonal phase crystalline structure of stabilized with yttrium oxide, is aoxidized in Zirconium powder The mass content of zirconium is 98%, and granularity is 0.6~1 μm.
Foaming agent selects sodium n-alkylbenzenesulfonate.
Foam stabilizer selects silicones polyethers lotion.
It is 2.5wt% that binder, which selects polyvinyl alcohol, polyvinyl alcohol water solution mass concentration,.
Step 2:By in Zirconium powder and carbon fiber input container, suitable quantity of water is added, is stirred, in whipping process Foaming agent and foam stabilizer are put into, until being bubbled uniformly, binder is then put into, obtains mixed material.
Step:3:Mixed material is poured into molding die, naturally dry molding obtains green compact.
Step 4:Closed box is put the green body into, is vacuumized, is then charged with butane and oxygen to normal pressure, butane and oxygen are mixed It is filled in closed box together after conjunction, it is 10L/min that gas, which is filled with flow, keeps standing 3 hours after being filled with gas.All burnt, 50 DEG C are naturally cooled to, the green body of trepanning is obtained.
Step 5:By the green body high temperature sintering of trepanning, 750 DEG C first are warming up to the rate of 1 DEG C/min, and keep the temperature 1h, then with The rate of 2 DEG C/min is warming up to 1400 DEG C, and keeps 2h, and high temperature sintering finishes, and obtains zircite porous ceramic.
After testing, the porosity of the Zirconium oxide foamed ceramic is 77%, bending strength 99MPa.
By the case of embodiment 1 to 5 it is found that the zirconium oxide prepared using the preparation method of zircite porous ceramic of the present invention The porous ceramics porosity is up to 70% or more, and bending strength is more than 90MPa, and via hole diameter measures, and aperture is more uniform, and crack-free is existing As.
Each technical characteristic of embodiment described above can be combined arbitrarily, to keep description succinct, not to above-mentioned reality It applies all possible combination of each technical characteristic in example to be all described, as long as however, the combination of these technical characteristics is not deposited In contradiction, it is all considered to be the range of this specification record.
Several embodiments of the invention above described embodiment only expresses, the description thereof is more specific and detailed, but simultaneously It cannot therefore be construed as limiting the scope of the patent.It should be pointed out that coming for those of ordinary skill in the art It says, without departing from the inventive concept of the premise, various modifications and improvements can be made, these belong to the protection of the present invention Range.Therefore, the protection domain of patent of the present invention should be determined by the appended claims.

Claims (10)

1. a kind of preparation method of zircite porous ceramic, which is characterized in that include the following steps:
Step 1:By in Zirconium powder and carbon fiber input container, suitable quantity of water is added, is stirred, is put into whipping process Then foaming agent and foam stabilizer put into binder until being bubbled uniformly, obtain mixed material;
Step 2:The mixed material is poured into molding die, naturally dry molding obtains green compact;
Step 3:The green compact are put into closed box, are vacuumized, butane and oxygen is then charged with to normal pressure, stands 1.5~3 hours Afterwards, electronics fire, which is lighted, makes During Combustion of Butane, and all burnt obtains the green body of trepanning;
Step 4:By the green body high temperature sintering of the trepanning, zircite porous ceramic is obtained.
2. the preparation method of zircite porous ceramic according to claim 1, which is characterized in that the Zirconium powder, Carbon fiber, foaming agent, foam stabilizer, binder mass ratio are:100:15~40:5~10:0.1~1.5:6~12.
3. the preparation method of zircite porous ceramic according to claim 1, which is characterized in that the diameter of the carbon fiber It it is 6~20 μm, length is 3~12mm.
4. the preparation method of zircite porous ceramic according to claim 1, which is characterized in that the Zirconium powder Granularity is 0.2~1 μm.
5. the preparation method of zircite porous ceramic according to claim 1, which is characterized in that in the Zirconium powder Mass content >=90% of zirconium oxide.
6. the preparation method of zircite porous ceramic according to claim 1, which is characterized in that the foaming agent be it is cloudy from Sub- surfactant.
7. the preparation method of zircite porous ceramic according to claim 1, which is characterized in that the foaming agent is straight chain Sodium alkyl benzene sulfonate, alkylsulfonate, alpha-olefin sodium sulfonate, alpha-sulfo monocarboxylic acid and its derivative, aliphatic acid sulfoalkyl ester or Aliphatic acid sulfoalkyl amide.
8. the preparation method of zircite porous ceramic according to claim 1, which is characterized in that the foam stabilizer is silicon tree Fat polyethers lotion.
9. the preparation method of zircite porous ceramic according to claim 1, which is characterized in that the binder is poly- second Enol.
10. the preparation method of zircite porous ceramic according to claim 1, which is characterized in that the high temperature sintering is: First be warming up to 500 DEG C~750 DEG C with the rate of 0.5 DEG C/min~2 DEG C/min, and keep the temperature 1~2h, then with 2 DEG C/min~3 DEG C/ The rate of min is warming up to 1400 DEG C~1600 DEG C, and keeps 2~4h.
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