CN105272350A - Preparation method of high-porosity porous alumina ceramic - Google Patents
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Abstract
The invention discloses a preparation method of high-porosity porous alumina ceramic, relates to a preparation method of porous alumina ceramic and aims to solve the problem of low porosity of the porous alumina ceramic prepared with an existing method. The method comprises steps as follows: 1), preparation of slurry of alumina ceramic; 2), preparation of a porous alumina ceramic body with a freezing injection molding method; 3), drying and sintering. Accordingly, the high-porosity porous alumina ceramic is obtained. On the premise that an inside three-dimensional net structure is not changed, the porosity of the porous ceramic is increased. The prepared porous alumina ceramic not only has higher pore-forming porosity, lower volume density, higher filtration and adsorption performance and higher mechanical strength, and the mechanical performance is remarkably improved. The preparation method is used for the field of porous ceramic materials.
Description
Technical field
The present invention relates to the preparation method of a method of porous alumina ceramics.
Background technology
Porous ceramics normally with refractory raw material if oxide powder is for aggregate, add the admixture stupalith that high temperature sintering obtains after certain technological forming, its structural performance is that inside has a large amount of through or fine pores of partly passing through, and aperture is controlled.Except having high temperature resistant, high pressure, outside the characteristics such as acid-alkali-corrosive-resisting, also there is uniform pore diameter, ventilation property high, therefore filtration, separation, Bu Qi and noise reduction field can be widely used in, as liquid-solid, gas solid separation in petroleum chemical industry, the sterile purification process of meticulous brewing industry, the high-temperature flue gas purification etc. in environmental protection industry (epi).
Compared with other ceramic materials, aluminum oxide has as filtration porous ceramic film material that porosity is high, resistance to acids and bases good, physical strength is high, high temperature resistant, self-cleaning good, the advantages such as long service life, become the ideal structure material forming filtration high porosity porous ceramics.
The preparation of current porous ceramics is mainly based on techniques such as pore-forming material method, foaming, template duplicating method, granulation mass area method, above method or there is the problems such as even air hole distribution is poor, porosity is low, or to raw material and equipment requirements higher, be difficult to obtain that structure is homogeneous, the porous ceramic articles of even aperture distribution.
Summary of the invention
The present invention will solve the lower problem of the porosity of alumina porous ceramic prepared by existing method, provides
a kind of preparation method of high-porosity alumina porous ceramics.
The preparation method of high-porosity alumina porous ceramics of the present invention, carries out according to the following steps:
One, the preparation of alumina-ceramic slurry:
By alumina powder jointed, 3013 additives, carbon dust and amphene mixing, adopt constant temperature ball-grinding machine ball milling 6 ~ 10h at 60 DEG C, speed setting 60 ~ 100r/min, obtains alumina-ceramic slurry; Wherein amphene is as solvent, and alumina powder jointed is (1 ~ 2.5) with the mass ratio of the solid content of amphene: (7.5 ~ 9), and 3013 additives account for 1% ~ 3% of slurry total mass, and carbon dust accounts for 1% ~ 2% of slurry total mass;
Two, freezing injection molding prepares alumina porous ceramic base substrate
The alumina-ceramic slurry obtained through step one is poured in freeze forming mould fast, one layer of heat preservation material is covered at mould upper surface after slurry injects, adopt cooled with liquid nitrogen, liquid nitrogen injection rate is not higher than mold base, freezing time is 10 ~ 15min, then be transferred in the refrigerator of-10 DEG C by mould, freezing time is 15 ~ 30min, the then demoulding; Wherein said lagging material is that any extraneous air that can completely cut off is by mould upper opening and the inner lagging material producing heat exchange;
Three, dry and sintering
After the base substrate demoulding is taken out, be placed on the corundum load bearing board of surfacing, be placed on vacuum freezing drying oven inner drying 24h, 1100 DEG C are warming up to the speed of 1 DEG C/min after drying, insulation 5h, then be warming up to 1450 DEG C with the speed of 3 DEG C/min, insulation 2h, namely obtains high-porosity alumina porous ceramics.
Wherein said amphene is bought from Aldrich (95%); Described alumina powder jointed purchase is from Japanese Showa electrician L43; 3013 additives described in step one are Texaphor963, are the dispersing auxiliary of solvent-thinned paint and ink, buy from Shenzhen Hai Chuan chemical industry.
Alumina powder jointedly in step one should to dry before use; Amphene should finally add to prevent it from room temperature volatilizing; And the slurry prepared to expose the time in atmosphere unsuitable long, closure ball grinding jar should carry out ball milling as early as possible.In step one, mechanical milling process adopts aluminum oxide abrading-ball, and ratio of grinding media to material is 2:1.
Before forming experiment starts, need in step 2 that mould is put into baking oven be preheated to 60 DEG C; To vacuumize in vacuum drying oven before in step 2, mould poured into by slurry; The time that slurry injects mould should shorten as far as possible.
Forming mould is divided into two portions: the base contacted with molding blank lower surface is 304 stainless steels, middle place mat one deck graphite paper, and the part contacted with green body side is PTFE material, and place mat one deck template on the contact surface.Base substrate after shaping is right cylinder.
Beneficial effect of the present invention:
The present invention prepares on the Process ba-sis of amphene base alumina porous ceramic at freezing injection molding, add carbon dust as composite pore-forming agent, carbon dust is got rid of by heating, the region that former carbon dust is existed produces pore, UNICOM's effect is played to the pore that amphene dendritic growth produces, thus increases porosity and the interior bone rate of alumina porous ceramic goods.Due to the filter of porous ceramic film material
reason is mainif filter and retain, require that material not only has higher through-hole rate, also should have certain physical strength and erosion resistance.The alumina porous ceramic utilizing the method to obtain not only has higher through-hole rate, makes that it is permeable, permeability obviously promotes, and has certain physical strength, and the characteristic of its material itself also makes the corrosion resisting property of product significantly improve.
(1) the present invention is not only applicable to filtration alumina porous ceramic preparation field, and is widely used in the porous ceramics production field that has higher requirements to porosity and through-hole rate, and this preparation technology's flow process is simple, and the cycle is short, and environment affinity is better.
(2) alumina porous ceramic utilizing the inventive method to obtain has higher porosity and through-hole rate, with do not add compared with carbon dust, porosity improves 10%-15%, makes it in the field higher to strainability requirement, have good filterability, and then can ensure its use properties.
(3) when the alumina porous ceramic material that prepared by the present invention is on active service in gas or liquid medium, the specific surface area contacted with medium is relatively high, and alumina porous ceramic has higher physical strength, and its Practical Performance is significantly improved.
(4) the present invention can ensure, alumina porous ceramic material keeps good use properties in long service, and cleans porous ceramics by modes such as cleaning, blowback, burnings, and this material can be recycled within the specific limits.
Accompanying drawing explanation
fig. 1for not adding the alumina porous ceramic sample SEM picture of carbon dust in embodiment 1;
fig. 2for adding the alumina porous ceramic sample SEM picture of carbon dust in embodiment 1;
fig. 3for the alumina porous ceramic base substrate macro morphology of diameter 100mm in embodiment 1;
fig. 4for adding the alumina porous ceramic SEM picture of carbon dust in embodiment 1;
fig. 5for not adding carbon dust in embodiment 1, the alumina porous ceramic SEM picture that other conditions are identical.
Embodiment
Technical solution of the present invention is not limited to following cited embodiment, also comprises the arbitrary combination between each embodiment.
Embodiment one: the preparation method of present embodiment high-porosity alumina porous ceramics, carry out according to the following steps:
One, the preparation of alumina-ceramic slurry:
By alumina powder jointed, 3013 additives, carbon dust and amphene mixing, adopt constant temperature ball-grinding machine ball milling 6 ~ 10h at 60 DEG C, speed setting 60 ~ 100r/min, obtains alumina-ceramic slurry;
Two, freezing injection molding prepares alumina porous ceramic base substrate
The alumina-ceramic slurry obtained through step one is poured in freeze forming mould, one layer of heat preservation material is covered at mould upper surface after slurry injects, adopt cooled with liquid nitrogen, freezing time is 10 ~ 15min, then mould is transferred in the refrigerator of-10 DEG C, freezing time is 15 ~ 30min, the then demoulding;
Three, dry and sintering
After the base substrate demoulding is taken out, be placed on the corundum load bearing board of surfacing, be placed on vacuum freezing drying oven inner drying 24h, 1100 DEG C are warming up to the speed of 1 DEG C/min after drying, insulation 5h, then be warming up to 1450 DEG C with the speed of 3 DEG C/min, insulation 2h, namely obtains high-porosity alumina porous ceramics.
Wherein said amphene is bought from Aldrich (95%); Described alumina powder jointed purchase is from Japanese Showa electrician L43; 3013 additives described in step one are Texaphor963, are the dispersing auxiliary of solvent-thinned paint and ink, buy from Shenzhen Hai Chuan chemical industry.
Alumina powder jointedly in step one should to dry before use; Amphene should finally add to prevent it from room temperature volatilizing; And the slurry prepared to expose the time in atmosphere unsuitable long, closure ball grinding jar should carry out ball milling as early as possible.
Before forming experiment starts, need in step 2 that mould is put into baking oven be preheated to 60 DEG C; The time that slurry injects mould should shorten as far as possible.
Present embodiment take high purity alumina powder as raw material, adopt amphene solvent with
gacpowder pore-forming material compound prepares ceramic size, prepares alumina porous ceramic base substrate through freezing molding process is shaping, obtains alumina porous ceramic, under the prerequisite not changing interior three-dimensional network structure, improve porous ceramic articles ventilate rate after dry, sintering.The alumina porous ceramic of preparation not only has higher open-cell porosity and lower volume density, makes it show higher filtration, absorption property, and has higher physical strength, its mechanical property is significantly improved.
Embodiment two: present embodiment and embodiment one unlike: alumina powder jointed in step one is (1 ~ 2.5) with the mass ratio of the solid content of amphene: (7.5 ~ 9).Other is identical with embodiment one.
Embodiment three: present embodiment and embodiment one or two unlike: in step one, 3013 additives account for 1% ~ 3% of slurry total mass.Other is identical with embodiment one or two.
Embodiment four: present embodiment and embodiment one or two unlike: in step one, 3013 additives account for 2% of slurry total mass.Other is identical with embodiment one or two.
Embodiment five: one of present embodiment and embodiment one to four unlike: in step one, carbon dust accounts for 1% ~ 2% of slurry total mass.Other is identical with one of embodiment one to four.
Embodiment six: one of present embodiment and embodiment one to five unlike: in step one, mechanical milling process adopts aluminum oxide abrading-ball, and ratio of grinding media to material is 2:1.Other is identical with one of embodiment one to five.
Embodiment seven: one of present embodiment and embodiment one to six unlike: to vacuumize in vacuum drying oven before in step 2, mould poured into by slurry.Other is identical with one of embodiment one to six.
Embodiment eight: one of present embodiment and embodiment one to seven unlike: lagging material described in step 2 is insulating foam.Other is identical with one of embodiment one to seven.
For verifying that beneficial effect of the present invention carries out following test:
Embodiment 1: the alumina porous ceramic sample preparing diameter 100mm
One, configure two groups of each 200mL amphene base alumina-ceramic slurries, wherein one group of salic 78.8g, amphene 159.4g, 3013 additive 7.15g, another organizes salic 78.8g, amphene 159.4g, 3013 additive 7.15g, carbon dust 4.75g;
Above-mentioned raw materials is put into 304 stainless steel jar mill respectively, and adds 500g aluminum oxide abrading-ball wherein, be installed on constant temperature ball-grinding machine after ball grinder is properly closed, heating and ball-milling 6h at 60 DEG C, speed setting 100r/min;
Two, assemble shaping mould therefor in advance, and be placed in baking oven and be preheated to 60 DEG C;
After slurry ball milling, mould is taken out and is placed in a large container, pour slurry into fast wherein, after this process, cover one layer of heat preservation foam at mould upper surface;
Rapid dumps liquid nitrogen in large container, is no more than mold bottom upper surface with liquid level and is advisable, and after freezing 15min, the base substrate of preliminary condensation is put into refrigerator together with mould, temperature is set to quick-frozen shelves, freezing 15min;
Three, after said process, to mold releasability, take out the alumina-ceramic base substrate for preparing, be placed on the smooth load bearing board of one piece of clean surface, base substrate is together put into vacuum freezing drying oven together with load bearing board, and time of drying is set to 24h;
Sintered by establishing following system by dried base substrate: be warming up to 1100 DEG C with the speed of 1 DEG C/min, insulation 5h, is then warming up to 1450 DEG C with the speed of 3 DEG C/min, insulation 2h; Obtain the alumina porous ceramic base substrate that diameter is 100mm, its macro morphology
as Fig. 3.
Alumina porous ceramic sample after sintering is after the flow processs such as cutting, polishing, cleaning, oven dry, carry out scanning electron microscope test and porosity test, compared with the sample not adding carbon dust, hole showed increased, and can internally observe the three-dimensional net structure be interconnected.
According to GB GB/T1966-1996 Porosity of Porous Ceramics, Capacity Test Method, test two groups of sample apparent porosities, it is 79.21% that carbon dust sample gas porosity is added in result display, and not adding carbon dust sample gas porosity is 70.15%.The structure and morphology of sample
as Fig. 1 and 2shown in,
fig. 1for not adding carbon dust sample,
fig. 2for adding carbon dust sample, by
fig. 1 and 2the visible specimen surface not adding carbon dust has dense structure, there is hole hardly, and after adding carbon dust, occur the hole of some amount in the surface compact layer of sample, this effectively improves the porosity of alumina-ceramic.
fig. 4for the present embodiment adds the alumina porous ceramic SEM picture of carbon dust,
fig. 5for the present embodiment does not add the alumina porous ceramic SEM picture of carbon dust.
fig. 4and
fig. 5be respectively two kinds of sample interior schematic enlarged-scale view sheets, by
figureknown, after adding carbon dust, sample interior porosity significantly promotes, hole wall is thinning, Kong Jian UNICOM leads raising, this makes alumina porous ceramic under long-term filtration Service Environment, keeps higher flow rate, improves its use properties and active time, the build-in attributes such as the solidity to corrosion of simultaneous oxidation aluminium stupalith, physical strength are high make it can be cleaned porous ceramics by modes such as cleaning, blowback, burnings, and this material can be recycled within the specific limits.
Embodiment 2: prepare diameter 80mm alumina porous ceramic sample
One, configure two groups of each 200mL amphene base alumina-ceramic slurries, wherein one group of salic 76.9g, amphene 147.3g, 3013 additive 6.72g, another organizes salic 76.9g, amphene 147.3g, 3013 additive 6.72g, carbon dust 4.49g;
Above-mentioned raw materials is put into 304 stainless steel jar mill respectively, and adds 450g aluminum oxide abrading-ball wherein, be installed on constant temperature ball-grinding machine after ball grinder is properly closed, heating and ball-milling 6h at 60 DEG C, speed setting 100r/min;
Two, assemble shaping mould therefor in advance, and be placed in baking oven and be preheated to 60 DEG C;
After slurry ball milling, mould is taken out and is placed in a large container, pour slurry into fast wherein, after this process, cover one layer of heat preservation foam at mould upper surface;
Rapid dumps liquid nitrogen in large container, is no more than mold bottom upper surface with liquid level and is advisable, and after freezing 15min, the base substrate of preliminary condensation is put into refrigerator together with mould, temperature is set to quick-frozen shelves, freezing 20min;
Three, after said process, to mold releasability, take out the alumina-ceramic base substrate for preparing, be placed on the smooth load bearing board of one piece of clean surface, base substrate is together put into vacuum freezing drying oven together with load bearing board, and time of drying is set to 24h;
Sintered by establishing following system by dried base substrate: be warming up to 1100 DEG C with the speed of 1 DEG C/min, insulation 5h, is then warming up to 1450 DEG C with the speed of 3 DEG C/min, insulation 2h;
Alumina porous ceramic sample after sintering is after the flow processs such as cutting, polishing, cleaning, oven dry, carry out scanning electron microscope test and porosity test, compared with the sample not adding carbon dust, hole showed increased, and can internally observe the three-dimensional net structure be interconnected.
According to GB GB/T1966-1996 Porosity of Porous Ceramics, Capacity Test Method, test two groups of sample apparent porosities, it is 81.15% that carbon dust sample gas porosity is added in result display, not adding carbon dust sample gas porosity is 73.21%, illustrates that adding of carbon dust serves keying action to the increase of alumina porous ceramic void content.
Embodiment 3: prepare diameter 120mm alumina porous ceramic sample
One, configure two groups of each 300mL amphene base alumina-ceramic slurries, wherein one group of salic 97.9g, amphene 201.2g, 3013 additive 8.97g, another organizes salic 97.9g, amphene 201.2g, 3013 additive 8.97g, carbon dust 5.98g;
Above-mentioned raw materials is put into 304 stainless steel jar mill respectively, and adds 600g aluminum oxide abrading-ball wherein, be installed on constant temperature ball-grinding machine after ball grinder is properly closed, heating and ball-milling 6h at 60 DEG C, speed setting 100r/min;
Two, assemble shaping mould therefor in advance, and be placed in baking oven and be preheated to 60 DEG C;
After slurry ball milling, mould is taken out and is placed in a large container, pour slurry into fast wherein, after this process, cover one layer of heat preservation foam at mould upper surface;
Rapid dumps liquid nitrogen in large container, is no more than mold bottom upper surface with liquid level and is advisable, and after freezing 15min, the base substrate of preliminary condensation is put into refrigerator together with mould, temperature is set to quick-frozen shelves, freezing 20min;
Three, after said process, to mold releasability, take out the alumina-ceramic base substrate prepared, be placed on one piece
tableon the clean smooth load bearing board in face, base substrate is together put into vacuum freezing drying oven together with load bearing board, and time of drying is set to 24h;
Sintered by establishing following system by dried base substrate: be warming up to 1100 DEG C with the speed of 1 DEG C/min, insulation 5h, is then warming up to 1450 DEG C with the speed of 3 DEG C/min, insulation 2h;
Alumina porous ceramic sample after sintering is after the flow processs such as cutting, polishing, cleaning, oven dry, carry out scanning electron microscope test and porosity test, compared with the sample not adding carbon dust, hole showed increased, and can internally observe the three-dimensional net structure be interconnected.
According to GB GB/T1966-1996 Porosity of Porous Ceramics, Capacity Test Method, test two groups of sample apparent porosities, it is 77.93% that carbon dust sample gas porosity is added in result display, not adding carbon dust sample gas porosity is 69.87%, illustrates that adding of carbon dust serves keying action to the increase of alumina porous ceramic void content.
Claims (7)
1. a preparation method for high-porosity alumina porous ceramics, is characterized in that the method is carried out according to the following steps:
One, the preparation of alumina-ceramic slurry:
By alumina powder jointed, 3013 additives, carbon dust and amphene mixing, adopt constant temperature ball-grinding machine ball milling 6 ~ 10h at 60 DEG C, speed setting 60 ~ 100r/min, obtains alumina-ceramic slurry;
Two, freezing injection molding prepares alumina porous ceramic base substrate
The alumina-ceramic slurry obtained through step one is poured in freeze forming mould, one layer of heat preservation material is covered at mould upper surface after slurry injects, adopt cooled with liquid nitrogen, freezing time is 10 ~ 15min, then mould is transferred in the refrigerator of-10 DEG C, freezing time is 15 ~ 30min, the then demoulding;
Three, dry and sintering
After the base substrate demoulding is taken out, be placed on the corundum load bearing board of surfacing, be placed on vacuum freezing drying oven inner drying 24h, 1100 DEG C are warming up to the speed of 1 DEG C/min after drying, insulation 5h, then be warming up to 1450 DEG C with the speed of 3 DEG C/min, insulation 2h, namely obtains high-porosity alumina porous ceramics.
2. the preparation method of a kind of high-porosity alumina porous ceramics according to claim 1, is characterized in that alumina powder jointed in step one is (1 ~ 2.5) with the mass ratio of the solid content of amphene: (7.5 ~ 9).
3. the preparation method of a kind of high-porosity alumina porous ceramics according to claim 1, is characterized in that in step one, 3013 additives account for 1% ~ 3% of slurry total mass.
4. the preparation method of a kind of high-porosity alumina porous ceramics according to claim 1, is characterized in that in step one, 3013 additives account for 2% of slurry total mass.
5. the preparation method of a kind of high-porosity alumina porous ceramics according to claim 1, is characterized in that in step one, carbon dust accounts for 1% ~ 2% of slurry total mass.
6. the preparation method of a kind of high-porosity alumina porous ceramics according to claim 1, it is characterized in that in step one, mechanical milling process adopts aluminum oxide abrading-ball, ratio of grinding media to material is 2:1.
7. the preparation method of a kind of high-porosity alumina porous ceramics according to claim 1, is characterized in that to vacuumize in vacuum drying oven before in step 2, mould poured into by slurry.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106588090A (en) * | 2016-11-23 | 2017-04-26 | 湖南仁海科技材料发展有限公司 | Preparation method for ceramic aluminum oxide load-bearing board with multiple slotted holes in surface |
| CN108503343A (en) * | 2018-04-10 | 2018-09-07 | 北京英华高科技有限公司 | A kind of novel porous ceramic gas distributor and preparation method thereof |
| CN115894066A (en) * | 2022-12-23 | 2023-04-04 | 中山大学·深圳 | High-porosity porous ceramic material and preparation method and application thereof |
| CN116639981A (en) * | 2023-07-27 | 2023-08-25 | 山东金鸿新材料股份有限公司 | Preparation method of pressureless boron carbide ceramic |
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| US20110256203A1 (en) * | 2010-04-16 | 2011-10-20 | Hyoun-Ee Kim | Porous ceramic scaffold having an organic/inorganic hybrid coating layer containing bioactive factor and method thereof |
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| CN101698605A (en) * | 2009-11-17 | 2010-04-28 | 哈尔滨工业大学 | Preparation method of gradient porous alumina ceramics |
| US20110256203A1 (en) * | 2010-04-16 | 2011-10-20 | Hyoun-Ee Kim | Porous ceramic scaffold having an organic/inorganic hybrid coating layer containing bioactive factor and method thereof |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106588090A (en) * | 2016-11-23 | 2017-04-26 | 湖南仁海科技材料发展有限公司 | Preparation method for ceramic aluminum oxide load-bearing board with multiple slotted holes in surface |
| CN108503343A (en) * | 2018-04-10 | 2018-09-07 | 北京英华高科技有限公司 | A kind of novel porous ceramic gas distributor and preparation method thereof |
| CN115894066A (en) * | 2022-12-23 | 2023-04-04 | 中山大学·深圳 | High-porosity porous ceramic material and preparation method and application thereof |
| CN115894066B (en) * | 2022-12-23 | 2023-09-12 | 中山大学·深圳 | High-porosity porous ceramic material and preparation method and application thereof |
| CN116639981A (en) * | 2023-07-27 | 2023-08-25 | 山东金鸿新材料股份有限公司 | Preparation method of pressureless boron carbide ceramic |
| CN116639981B (en) * | 2023-07-27 | 2023-10-13 | 山东金鸿新材料股份有限公司 | Preparation method of pressureless boron carbide ceramic |
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Application publication date: 20160127 |