CN102976758B - Preparation method of macroporous interconnection SiC ceramics - Google Patents
Preparation method of macroporous interconnection SiC ceramics Download PDFInfo
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- CN102976758B CN102976758B CN201210556026.5A CN201210556026A CN102976758B CN 102976758 B CN102976758 B CN 102976758B CN 201210556026 A CN201210556026 A CN 201210556026A CN 102976758 B CN102976758 B CN 102976758B
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Abstract
The invention relates to the technical field of ceramic materials, particularly a preparation method of macroporous interconnection SiC ceramics, which comprises the following steps: uniformly mixing SiC powder and boron carbide powder to form a SiC mixture; mixing the SiC mixture, a cationic surfactant and a binding agent polyvinyl alcohol water solution to form a uniform slurry, and manually oscillating or mechanically stirring the slurry to introduce bubbles; putting the uniform slurry subjected to bubble introduction in a closed container, and carrying out a controlled pressure reduction technique; freezing the expanded slurry along with the container at -17 DEG C for 4-12 hours; extracting in absolute ethanol or industrial ethanol under the condition of room temperature or freezing; immersing in a 7 wt% phenol formaldehyde resin ethanol solution, drying the sample at 50-120 DEG C for 4 hours; and in an inert atmosphere, keeping the temperature of 1950-2100 DEG C for 0.5-2 hours to complete sintering. The invention adopts the pressure reduction technique to increase the pore size of the SiC ceramic from submillimeter level to millimeter level, and has the advantages of low production cost and simplified technique.
Description
Technical field
The present invention relates to technical field of ceramic material, be specifically related to the preparation method of the interconnected SiC ceramic of a kind of macropore.
Background technology
Large hole silicon carbide has the characteristics such as high temperature resistant, corrosion-resistant, resistance to molten metal washes away, high strength, high passband, bigger serface, is used for filtering and stable molten metal liquid and gas in metallurgical casting field, and the support of the catalyst under can be used as severe condition.
For the preparation of wide aperture carborundum porous ceramics, research both domestic and external mainly concentrates on hard template method, namely by using presoma, as polymeric particles, organic foam and inorganic salt etc. mix with ceramic material powder as template, then in preparation process, removing template and forming porous ceramics.As: by being mixed by a certain percentage with silicon carbide powder by carbon dust, through pressing mold, high temperature sintering, then carbon granule is removed in air combustion, can prepare wide-aperture carborundum porous ceramics; Use polymer microsphere as template, as utilize starch gel sponge, polyurethane sponge (Yao Xiumin etc., secondary hanging viscosity on the impact of mesh structural porous silicon carbide ceramics performance, Ceram.Inter.32 (2006), 137, use MgO-Al
2o
3-SiO
2as agglutinant low-temperature sintering mesh structural porous silicon carbide ceramics J. Mater. Sci 42 (2007) 4960), carbon sponge (Guo Quangui etc., nanometer AIN content prepares the impact of porous silicon carbide silicon microstructure and mechanical property to sic foam, J. Eur. Ceram. Soc.30 (2010) 113, foam porous silicon carbide is prepared from mesoporous pitch and nanometer silicon carbide mixture silicification reaction, Mater. Sci. Eng. A 488 (2008) 514) etc. as template, macropore silicon carbide ceramics can be prepared by hanging, drying and follow-up sintering; In addition, the timber with macroporous structure also can be adopted to have biomimetic features macropore silicon carbide ceramics as carbon source preparation.
But mainly rely on hard mould agent for preparing large hole silicon carbide at present or have the preparation method of macropore framework material, its shortcoming is also apparent: first aperture and pass will rely on aperture and the pass of template, cannot carry out adjustment remodeling; Secondly, synthesis step is comparatively loaded down with trivial details, and except the sintering step of pottery, what have also relates to Template preparation and pre-treatment, comprises the step such as pore-forming, carbonization; Particularly utilize various cavernous body as template, easy generation cinclides (staying after sponge skeletal disintegration) (Yao Xiumin etc., secondary hanging viscosity is on the impact of mesh structural porous silicon carbide ceramics performance, Ceram. Inter.32 (2006) 137), this is disadvantageous for improving the rear ceramic mechanical property of sintering.Therefore all to there is complex process, cost high and containing the shortcomings such as hole of holding one's breath for these methods, and use is subject to certain restrictions.The method of the macropore carbofrax material that the preparation structure studying a kind of low cost can design and regulate has important using value.
In the applicant granted patent (patent No.: 201010580712.7), we talk of a kind of cold method causing gel property and prepare the interconnected silicon carbide of macropore by means of polyvinyl alcohol, aperture is between 0.1 ~ 0.4mm, and at melted metal filtering etc., some need more wide-aperture application is not had advantage to this material.The preparation method of research and development one more wide aperture (0.5 ~ 2mm) interconnected SiC ceramic has significant application value.
Summary of the invention
For deficiency of the prior art, the invention provides that a kind of production cost is low, work simplification and the preparation method of the interconnected SiC ceramic of the macropore of hole diameter enlargement.
The preparation method of the interconnected SiC ceramic of a kind of macropore of the present invention, comprises the following steps:
(1) SiC powder and boron carbide powder are mixed composition SiC compound, by weight percentage containing SiC powder 98.92% in SiC compound, containing boron carbide powder 1.08%;
(2) by SiC compound, cats product and binding agent polyvinyl alcohol water solution by weight being (7 ~ 17): (0 ~ 3 × 10
-3): 44 mix, and form uniform sizing material, hand vibration or mechanical stirring slurry, introduce bubble; Putting into airtight container by drawing the uniform sizing material after bubble, carrying out controlling decompression art breading;
(3) after slurry expand into 2 ~ 4 times of original volume, in company with container at-17 DEG C of temperature after freezing 4 ~ 12h, in dehydrated alcohol or industrial alcohol, 4 ~ 24h is extracted under room temperature or-17 DEG C of freezing conditions, repeat 1 ~ 3 time, then the resol ethanolic soln that massfraction is 7% is immersed, sample is dry 4h at 50 ~ 120 DEG C of temperature, in an inert atmosphere, is incubated 0.5 ~ 2h and completes sintering at 1950 ~ 2100 DEG C of temperature.
Wherein, the mean particle size of the SiC powder described in step (1) is 1.0 μm, and the mean particle size of boron carbide powder is 4.1 μm;
Binding agent polyvinyl alcohol water solution described in step (2) is the polymerization degree of polyvinyl alcohol is 2000, and alcoholysis degree is 99%, and strength of solution is the polymerization degree of 6.5 ~ 7.0wt% or polyvinyl alcohol is 1700, and alcoholysis degree is 99%, and strength of solution is 7.0 ~ 8.0wt%;
Cats product described in step (2) is sodium lauryl sulphate;
The bubble that draws described in step (2) is by hand vibration or mechanical stirring mode introducing air bubble;
Decompression technique described in step (2) expands drawing the uniform sizing material after bubble through decompression in encloses container, thus increase the size of bubble;
Resol described in step (3) is Resole type, and molecular weight is 600, is mainly used for drawing carbon.
Feature of the present invention and beneficial effect are:
L () the present invention adopts decompression technique that bubble is expanded through decompression in encloses container, thus increase the size of bubble, aperture is significantly increased on the basis of the size of granted patent report, is namely increased to grade from submillimeter level;
(2) the present invention adopts polyvinyl alcohol as binding agent, and the bubble of vibration introducing is had to the stabilization of long period, its freezing gel characteristic has played effect in fixing bubble, makes need not to realize gel by very harsh freezing conditions;
(3) can be facilitated by the use of micro-tensio-active agent and effectively regulate the pass of macroporous SiC ceramic, aperture, porosity and UNICOM's degree;
(4) adopt ethanol to sample extraction, therefore without the need to using expensive freeze drying equipment and the maintenance of pore structure and the drying of sample can being realized longer time of drying, make the inventive method easily organize production, and extraction after ethanol and water mixture can through simply distillation after re-use;
(5) because polyvinyl alcohol is easy to obtain, and except sintering process and preparation path, do not relate to the use of the template of complicated chemical reaction and sacrificial, make the present invention easily organize production, cost is lower.
Accompanying drawing explanation
Fig. 1 is slurry puffing pore-forming schematic diagram;
Fig. 2 is (b) optical microscope photograph after (a) and sintering before the obtained macropore silicon carbide ceramic body sintering of embodiment 1, and (c) be the stereoscan photograph after (b) figure circled is amplified, and (d) is the graph of pore diameter distribution after sintering;
Fig. 3 is the graph of pore diameter distribution (c) after the optical microscope photograph of (b) after (a) and sintering before the obtained macropore silicon carbide ceramics sintering of embodiment 2 and sintering;
Fig. 4 is optical microscope photograph (a) after the obtained macropore silicon carbide ceramic body sintering of embodiment 3 and graph of pore diameter distribution (b);
Fig. 5 is optical microscope photograph (a) after the obtained macropore silicon carbide ceramic body sintering of embodiment 4 and graph of pore diameter distribution (b);
Fig. 6 is optical microscope photograph (a) after the obtained macropore silicon carbide ceramic body sintering of embodiment 5 and graph of pore diameter distribution (b).
Embodiment
Below in conjunction with embodiment, the present invention will be further described.
The microscope model that the present embodiment uses is USB Digital microscope, and scanning electron microscope model is S3400N type scanning electron microscope.
Embodiment 1
(1) SiC powder and boron carbide powder are mixed composition SiC compound, wherein the mean particle size of SiC powder is 1.0 μm, and the mean particle size of boron carbide powder is 4.1 μm; By weight percentage containing SiC powder 98.92% in SiC compound, containing boron carbide powder 1.08%;
(2) adopt concentration be the polyvinyl alcohol water solution 20-99 of 6.75wt% as binding agent, SiC compound and binding agent polyvinyl alcohol water solution are mixed by weight for 7.58:44, form uniform sizing material, mechanical stirring slurry, introducing bubble; Putting into airtight container by drawing the uniform sizing material after bubble, carrying out controlling decompression art breading, making slurry even inflation to three times of original volume;
(3) slurry after expanding in company with container at-17 DEG C of temperature after freezing 9h, sample after freezing is directly transferred in industrial alcohol and extracts 5 hours, repeat 1 ~ 3 time, then immerse the resol ethanolic soln that massfraction is 7%, sample is dry 4h at 80 DEG C of temperature; In an inert atmosphere, be incubated 0.5h and complete sintering at 2000 DEG C of temperature, temperature rise rate is 5 DEG C/min.
Fig. 2 is the graph of pore diameter distribution (d) before the obtained macropore silicon carbide ceramic body sintering of the present embodiment after (a) and sintering after (b) optical microscope photograph and sintering after the stereoscan photograph (c) of hole wall and sintering.The aperture of the present embodiment gained macropore silicon carbide ceramic body is 0.6 ± 0.2mm, and mean pore size is 0.6mm, be about before this patent report (patent No.: the 201010580712.7) twice in aperture, between macropore by communicating aperture be connected.Stereoscan photograph display after sintering, SiC particle is interconnected by sintering.
Embodiment 2
(1) SiC powder and boron carbide powder are mixed composition SiC compound, wherein the mean particle size of SiC powder is 1.0 μm, and the mean particle size of boron carbide powder is 4.1 μm; By weight percentage containing SiC powder 98.92% in SiC compound, containing boron carbide powder 1.08%;
(2) adopt concentration be the polyvinyl alcohol water solution 20-99 of 6.75wt% as binding agent, SiC compound and binding agent polyvinyl alcohol water solution are mixed by weight for 14.19:44, form uniform sizing material, mechanical stirring slurry, introducing bubble; Putting into airtight container by drawing the uniform sizing material after bubble, carrying out controlling decompression art breading, making slurry even inflation to three times of original volume;
(3) slurry after expanding in company with container at-17 DEG C of temperature after freezing 9h, sample after freezing is directly transferred in industrial alcohol and extracts 5 hours, repeat 1 ~ 3 time, then immerse the resol ethanolic soln that massfraction is 7%, sample is dry 4h at 80 DEG C of temperature; In an inert atmosphere, be incubated 0.5h and complete sintering at 2000 DEG C of temperature, temperature rise rate is 5 DEG C/min.
Fig. 3 is the graph of pore diameter distribution (c) after the optical microscope photograph of (b) after (a) and sintering before the obtained macropore silicon carbide ceramics sintering of the present embodiment and sintering.The present embodiment is compared with embodiment 1, and do not change other conditions and increase the mass ratio of SiC composite granule and PVA solution, obviously can increase the size of macropore, macropore size about 1.2 ± 0.4mm, mean pore size is about 1.0mm.Be connected by communicating aperture between macropore, aperture is 0.05 ~ 0.2mm about, and hole wall has thickening phenomenon simultaneously.Clearly, by the present invention, grade can be brought up to further in the aperture of three-dimensional interconnected large hole silicon carbide.
Embodiment 3
(1) SiC powder and boron carbide powder are mixed composition SiC compound, wherein the mean particle size of SiC powder is 1.0 μm, and the mean particle size of boron carbide powder is 4.1 μm; By weight percentage containing SiC powder 98.92% in SiC compound, containing boron carbide powder 1.08%;
(2) adopt concentration be the polyvinyl alcohol water solution 20-99 of 6.75wt% as binding agent, by SiC compound, sodium lauryl sulphate and binding agent polyvinyl alcohol water solution by weight being 14.19:2 × 10
-3: 44 mix, and form uniform sizing material, mechanical stirring slurry, introduce bubble; Putting into airtight container by drawing the uniform sizing material after bubble, carrying out controlling decompression art breading, making slurry even inflation to three times of original volume;
(3) slurry after expanding in company with container at-17 DEG C of temperature after freezing 9h, sample after freezing is directly transferred in industrial alcohol and extracts 5 hours, repeat 1 ~ 3 time, then immerse the resol ethanolic soln that massfraction is 7%, sample is dry 4h at 80 DEG C of temperature; In an inert atmosphere, be incubated 0.5h and complete sintering at 2000 DEG C of temperature, temperature rise rate is 5 DEG C/min.
Fig. 4 be the present embodiment obtain macropore silicon carbide ceramic body sintering after optical microscope photograph (a) and graph of pore diameter distribution (b).The present embodiment, compared with embodiment 2, does not change other conditions, adds micro-surfactant SDS, and large hole silicon carbide aperture about 0.8 ± 0.4mm and homogeneity are improved, and the connectivity between macropore is also significantly improved, and linked hole size is at 0.2 ± 0.1mm.This and the granted patent (patent No.: the action principle of the tensio-active agent (OP-10) 201010580712.7) is similar.
Embodiment 4
(1) SiC powder and boron carbide powder are mixed composition SiC compound, wherein the mean particle size of SiC powder is 1.0 μm, and the mean particle size of boron carbide powder is 4.1 μm; By weight percentage containing SiC powder 98.92% in SiC compound, containing boron carbide powder 1.08%;
(2) adopt concentration be the polyvinyl alcohol water solution 20-99 of 6.75wt% as binding agent, SiC compound and binding agent polyvinyl alcohol water solution are mixed by weight for 14.19:44, form uniform sizing material, mechanical stirring slurry, introducing bubble; Putting into airtight container by drawing the uniform sizing material after bubble, carrying out controlling decompression art breading, making slurry even inflation to the twice of original volume;
(3) slurry after expanding in company with container at-17 DEG C of temperature after freezing 9h, sample after freezing is directly transferred in industrial alcohol and extracts 5 hours, repeat 1 ~ 3 time, then immerse the resol ethanolic soln that massfraction is 7%, sample is dry 4h at 80 DEG C of temperature; In an inert atmosphere, be incubated 0.5h and complete sintering at 2000 DEG C of temperature, temperature rise rate is 5 DEG C/min.
Fig. 5 be the present embodiment obtain macropore silicon carbide ceramic body sintering after optical microscope photograph (a) and graph of pore diameter distribution (b).The present embodiment, compared with embodiment 2, does not change other conditions, and reduce the volume expanded, can reduce the size of macropore, macropore size drops to about 0.4 ± 0.2mm from about 1.2 ± 0.3mm, and be connected by communicating aperture between macropore, aperture is 0.05 ~ 0.1mm about.
Embodiment 5
(1) SiC powder and boron carbide powder are mixed composition SiC compound, wherein the mean particle size of SiC powder is 1.0 μm, and the mean particle size of boron carbide powder is 4.1 μm; By weight percentage containing SiC powder 98.92% in SiC compound, containing boron carbide powder 1.08%;
(2) adopt concentration be the polyvinyl alcohol water solution 20-99 of 6.75wt% as binding agent, SiC compound and binding agent polyvinyl alcohol water solution are mixed by weight for 14.19:44, form uniform sizing material, mechanical stirring slurry, introducing bubble; Putting into airtight container by drawing the uniform sizing material after bubble, carrying out controlling decompression art breading, making slurry even inflation to four times of original volume;
(3) slurry after expanding in company with container at-17 DEG C of temperature after freezing 9h, sample after freezing is directly transferred in industrial alcohol and extracts 5 hours, repeat 1 ~ 3 time, then immerse the resol ethanolic soln that massfraction is 7%, sample is dry 4h at 80 DEG C of temperature; In an inert atmosphere, be incubated 0.5h and complete sintering at 2000 DEG C of temperature, temperature rise rate is 5 DEG C/min.
Fig. 6 be the present embodiment obtain macropore silicon carbide ceramic body sintering after optical microscope photograph (a) and graph of pore diameter distribution (b).The present embodiment, compared with embodiment 4, does not change other conditions, and increase the volume expanded, can increase the size of macropore, macropore size is increased to about 0.8 ± 0.3mm from about 0.4 ± 0.2mm, and be connected by communicating aperture between macropore, aperture is 0.05 ~ 0.3mm about.
Embodiment 6
(1) SiC powder and boron carbide powder are mixed composition SiC compound, wherein the mean particle size of SiC powder is 1.0 μm, and the mean particle size of boron carbide powder is 4.1 μm; By weight percentage containing SiC powder 98.92% in SiC compound, containing boron carbide powder 1.08%;
(2) adopt concentration be the polyvinyl alcohol water solution 17-99 of 8.0wt% as binding agent, by SiC compound, sodium lauryl sulphate and binding agent polyvinyl alcohol water solution by weight being 17:3 × 10
-3: 44 mix, and form uniform sizing material, hand vibration slurry, introduce bubble; Putting into airtight container by drawing the uniform sizing material after bubble, carrying out controlling decompression art breading, making slurry even inflation to three times of original volume;
(3) slurry after expanding in company with container at-17 DEG C of temperature after freezing 4h, sample after freezing is put to room temperature, is transferred in dehydrated alcohol and extracts 4 hours, repeat 1 ~ 3 time, then immerse the resol ethanolic soln that massfraction is 7%, sample is dry 4h at 50 DEG C of temperature; In an inert atmosphere, be incubated 2h and complete sintering at 1950 DEG C of temperature, temperature rise rate is 5 DEG C/min.
Embodiment 7
(1) SiC powder and boron carbide powder are mixed composition SiC compound, wherein the mean particle size of SiC powder is 1.0 μm, and the mean particle size of boron carbide powder is 4.1 μm; By weight percentage containing SiC powder 98.92% in SiC compound, containing boron carbide powder 1.08%;
(2) adopt concentration be the polyvinyl alcohol water solution 20-99 of 7.0wt% as binding agent, SiC compound and binding agent polyvinyl alcohol water solution are mixed by weight for 7:44, form uniform sizing material, mechanical stirring slurry, introducing bubble; Putting into airtight container by drawing the uniform sizing material after bubble, carrying out controlling decompression art breading, making slurry even inflation to four times of original volume;
(3) slurry after expanding in company with container at-17 DEG C of temperature after freezing 12h, sample after freezing is put to room temperature, is transferred in dehydrated alcohol and extracts 12 hours, repeat 1 ~ 3 time, then immerse the resol ethanolic soln that massfraction is 7%, sample is dry 4h at 120 DEG C of temperature; In an inert atmosphere, be incubated 0.5h and complete sintering at 2100 DEG C of temperature, temperature rise rate is 5 DEG C/min.
Embodiment 8
(1) SiC powder and boron carbide powder are mixed composition SiC compound, wherein the mean particle size of SiC powder is 1.0 μm, and the mean particle size of boron carbide powder is 4.1 μm; By weight percentage containing SiC powder 98.92% in SiC compound, containing boron carbide powder 1.08%;
(2) adopt concentration be the polyvinyl alcohol water solution 20-99 of 6.5wt% as binding agent, SiC compound and binding agent polyvinyl alcohol water solution are mixed by weight for 10:44, form uniform sizing material, hand vibration slurry, introducing bubble; Putting into airtight container by drawing the uniform sizing material after bubble, carrying out controlling decompression art breading, making slurry even inflation to four times of original volume;
(3) slurry after expanding in company with container at-17 DEG C of temperature after freezing 12h, sample after freezing is put to room temperature, is transferred in dehydrated alcohol and extracts 24 hours, repeat 1 ~ 3 time, then immerse the resol ethanolic soln that massfraction is 7%, sample is dry 4h at 120 DEG C of temperature; In an inert atmosphere, be incubated 0.5h and complete sintering at 2100 DEG C of temperature, temperature rise rate is 5 DEG C/min.
Embodiment 9
(1) SiC powder and boron carbide powder are mixed composition SiC compound, wherein the mean particle size of SiC powder is 1.0 μm, and the mean particle size of boron carbide powder is 4.1 μm; By weight percentage containing SiC powder 98.92% in SiC compound, containing boron carbide powder 1.08%;
(2) adopt concentration be the polyvinyl alcohol water solution 17-99 of 7.0wt% as binding agent, SiC compound and binding agent polyvinyl alcohol water solution are mixed by weight for 7:44, form uniform sizing material, mechanical stirring slurry, introducing bubble; Putting into airtight container by drawing the uniform sizing material after bubble, carrying out controlling decompression art breading, making slurry even inflation to two times of original volume;
(3) slurry after expanding in company with container at-17 DEG C of temperature after freezing 12h, sample after freezing is put to room temperature, is transferred in dehydrated alcohol and extracts 5 hours, repeat 1 ~ 3 time, then immerse the resol ethanolic soln that massfraction is 7%, sample is dry 4h at 120 DEG C of temperature; In an inert atmosphere, be incubated 0.5h and complete sintering at 2100 DEG C of temperature, temperature rise rate is 5 DEG C/min.
Claims (1)
1. a preparation method for the interconnected SiC ceramic of macropore, comprises the following steps:
(1) SiC powder and boron carbide powder are mixed composition SiC compound, by weight percentage containing SiC powder 98.92% in SiC compound, containing boron carbide powder 1.08%; The mean particle size of described SiC powder is 1.0 μm, and the mean particle size of boron carbide powder is 4.1 μm;
(2) adopt concentration be the polyvinyl alcohol water solution 20-99 of 6.75wt% as binding agent, SiC compound and binding agent polyvinyl alcohol water solution are mixed by weight for 14.19:44, form uniform sizing material, mechanical stirring slurry, introducing bubble; Putting into airtight container by drawing the uniform sizing material after bubble, carrying out controlling decompression art breading;
It is characterized in that:
(3) after slurry expand into 3 times of original volume, in company with container at-17 DEG C of temperature after freezing 9h, in industrial alcohol, 5h is extracted under room temperature or-17 DEG C of freezing conditions, repeat 1 ~ 3 time, then the resol ethanolic soln that massfraction is 7% is immersed, sample is dry 4h at 80 DEG C of temperature, in an inert atmosphere, is incubated 0.5h and completes sintering at 2000 DEG C of temperature; Described resol is Resole type, and molecular weight is 600, is mainly used for drawing carbon;
Macropore size 1.2 ± the 0.4mm of the interconnected SiC ceramic of described macropore, mean pore size 1.0mm, be connected by communicating aperture between macropore, aperture 0.05 ~ 0.2mm, and hole wall has thickening phenomenon simultaneously.
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| CN103396123B (en) * | 2013-07-30 | 2014-07-16 | 东北大学 | Method for preparing large-aperture three-dimensional network SiC ceramic material |
| CN107188610B (en) * | 2017-06-01 | 2020-10-30 | 洛阳师范学院 | Preparation method of porous silicon carbide ceramic |
| CN107365887A (en) * | 2017-06-07 | 2017-11-21 | 常州豫春化工有限公司 | A kind of preparation method of fluxing type slagging agent |
| CN109180195A (en) * | 2018-09-30 | 2019-01-11 | 威海威林特电控科技有限公司 | One kind is based on adding obdurability porous ceramic composite and its preparation process made of infiltrated metal method |
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