CN105753501A - ZrSiO4-SiC porous ceramics and preparation method thereof - Google Patents
ZrSiO4-SiC porous ceramics and preparation method thereof Download PDFInfo
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Abstract
The invention relates to ZrSiO4-SiC porous ceramics and a preparation method thereof. The technical scheme is that the method comprises the following steps: fine SiC powder and a Ni-containing liquid in the mass ratio being 1:2 are fed into a ball mill for mixed milling for 0.5-6 h, and mixed slurry is obtained; the mixed slurry is drained and dried at the temperature of 110 DEG C for 24 h, mixed material blocks are obtained and subjected to ball milling until the particle size ranges from 1 mu m to 100 mu m, and mixed powder is obtained; 70wt%-95wt% of the mixed powder and 5wt%-30wt% of polyethylene glycol particles are mixed uniformly and pressed, and a blank is prepared; the pressed blank is subjected to heat preservation at the temperature of 1,000-1,800 DEG C for 1-6 h and cooled, and the ZrSiO4-SiC porous ceramics are obtained. The ZrSiO4-SiC porous ceramics have high high-temperature strength, good oxidation resistance, corrosion resistance, high thermal shock resistance and low specific gravity, cannot be oxidized at a high temperature and cannot have crystal transformation in a process from the room temperature to the temperature of 1,676 DEG C.
Description
Technical field
The invention belongs to high-temperature ceramic techniques field.Particularly relate to a kind of ZrSiO4-SiC porous ceramics and preparation method thereof.
Background technology
Porous ceramics is that one is burnt till through high temperature, and internal have communicate with each other in a large number pore or the ceramic material of Guan Bi pore.Its development starts from 19 century 70s, and due to the performance that it is excellent, porous ceramics is the most gradually applied to multiple fields such as metallurgy, chemical industry, environmental protection, the energy and biology.Utilize the uniform permeability of porous ceramics, various filter, separator, fluid distribution component, hybrid element can be manufactured, ooze out element and restricting element etc.;Utilize the feature of porous ceramics high-specific surface area, porous electrode, catalyst carrier, heat exchanger, gas sensor etc. can be made into;Utilize porous ceramics to absorb the performance of energy, can serve as various sound-absorbing material, vibration-absorptive material etc.;Utilize the density that porous ceramics is low, low heat-conductive characteristic, various insulation material and lightweight structural material etc. can be made.
At present, the carborundum porous ceramics that can use under the high temperature conditions has that elevated temperature strength is high, antioxygenic property is good, erosion resistant and thermal shock resistance is high, proportion is little, higher thermal conductivity and the feature such as microwave absorption capacity is strong, has a wide range of applications in the industry.The preparation method of carborundum porous ceramics mainly has: add pore creating material method, foaming, Polymeric sponge method and sol-gel process etc..The carborundum porous ceramics material using said method to prepare typically suffers from preferably applying in different occasions.
But carborundum porous ceramics is when high temperature is applied, its surface can generate SiO due to the oxidation of SiC2, although SiO2It is wrapped in SiC particulate surface, the internal effect not oxidized for SiC of protection can be played, but, in the change procedure of temperature, the SiO on silicon-carbide particle surface2(quartzy) can occur crystal transfer, and the bulk effect that its crystal transfer produces can reduce the structural strength of carborundum porous ceramics and a series of calorifics and optical property, and the application to carborundum porous ceramics material has a negative impact.
Summary of the invention
It is contemplated that overcome prior art not enough, it is therefore an objective to provide a kind of ZrSiO4The preparation method of-SiC porous ceramics, prepared ZrSiO4-SiC porous ceramics elevated temperature strength is high, antioxygenic property is good, erosion resistant and thermal shock resistance is high and proportion is little, carborundum can not only be protected the most not oxidized, it is to avoid surface of SiC in use forms SiO2The negative consequence brought, and can be all without there being crystal transfer during room temperature to 1676 DEG C.
For achieving the above object, the technical solution adopted in the present invention is: first carbide fine powder and nickeliferous mixed liquor that mass ratio is 1: 2 is placed in ball mill, mix grinding 0.5 ~ 6 hour, obtains mixed slurry;Being filtered dry by mixed slurry, be dried 24 hours, obtain mixture block under the conditions of 110 DEG C, described mixture block is milled to granularity is 1 ~ 100 μm, obtains mixed powder;Then by mixed powder and the polyethylene glycol particle mixing of 5 ~ 30wt% of 70 ~ 95wt%, it is pressed into base substrate;Finally the base substrate suppressed is incubated 1 ~ 6 hour under the conditions of 1000 ~ 1800 DEG C, cooling, obtain ZrSiO4-SiC porous ceramics.
The preparation method of described nickeliferous mixed liquor is: be first 1: 1 by the atomic molar ratio of Si and Zr, silicon tetrachloride and four n-butoxy zirconium solutions is mixed, obtains mixed solution;It is 1 by the mass ratio of mixed solution Yu nickel nitrate again: (0.001 ~ 0.02), in mixed solution, adds nickel nitrate, mixing, obtain nickeliferous mixed liquor.
SiC content >=97wt% in described carbide fine powder;Particle diameter is 1 ~ 500 μm.
Ni (NO) in described nickel nitrate3·6H2O content >=97wt%;Particle diameter is 1 ~ 500 μm.
The particle diameter of described polyethylene glycol particle is 0.1 ~ 2mm.
Owing to using technique scheme, the present invention compared with prior art has a following good effect:
The present invention is in high temperature preparation process, and silicon-carbide particle surface can form ZrSiO4(silicon tetrachloride and the four n-butoxy zirconiums that are wrapped in SiC particulate surface react under the effect of nickel-base catalyst and generate ZrSiO4), i.e. SiC particulate surface will parcel a thin layer ZrSiO4, ZrSiO4The existence of layer, not only can protect carborundum not oxidized, it is to avoid surface of SiC in use forms SiO2The negative consequence brought, and occur all without the problem having crystal transfer from room temperature to 1676 DEG C synthetic material.ZrSiO prepared by the present invention4-SiC porous ceramics can use in the environment of maximum temperature is 1676 DEG C, and the temperature range of use has exceeded the temperature limiting that the most common silicon carbide ceramics is used, and can change, with bearing temperature, the damage brought;Elevated temperature strength is high, antioxygenic property is good, erosion resistant and thermal shock resistance high.
ZrSiO prepared by the present invention4-SiC porous ceramics is after testing: SiC content >=96wt%;The porosity >=30%.Can be as materials such as filtering material, catalyst carrier, thermodynamic material, sound-absorbing material and composite skeletons.
Therefore, the ZrSiO that prepared by the present invention4-SiC porous ceramics elevated temperature strength is high, antioxygenic property is good, erosion resistant and thermal shock resistance is high and proportion is little, carborundum can not only be protected the most not oxidized, it is to avoid surface of SiC in use forms SiO2The negative consequence brought, and can be all without there being crystal transfer during room temperature to 1676 DEG C.
Detailed description of the invention
Below in conjunction with detailed description of the invention, the present invention will be further described, not the restriction to its protection domain.
For avoiding repeating, existing by as follows for the technical parameter Unify legislation involved by this detailed description of the invention, embodiment repeats no more:
The preparation method of described nickeliferous mixed liquor is: be first 1: 1 by the atomic molar ratio of Si and Zr, silicon tetrachloride and four n-butoxy zirconium solutions is mixed, obtains mixed solution;It is 1 by the mass ratio of mixed solution Yu nickel nitrate again: (0.001 ~ 0.02), in mixed solution, adds nickel nitrate, mixing, obtain nickeliferous mixed liquor.
SiC content >=97wt% in described carbide fine powder;Particle diameter is 1 ~ 500 μm.
Ni (NO) in described nickel nitrate3·6H2O content >=97wt%;Particle diameter is 1 ~ 500 μm.
The particle diameter of described polyethylene glycol particle is 0.1 ~ 2mm.
Embodiment
1
A kind of ZrSiO4-SiC porous ceramics and preparation method thereof, its technical scheme is: first carbide fine powder and nickeliferous mixed liquor that mass ratio is 1: 2 is placed in ball mill, mix grinding 0.5 ~ 1 hour, obtains mixed slurry;Being filtered dry by mixed slurry, be dried 24 hours, obtain mixture block under the conditions of 110 DEG C, described mixture block is milled to granularity is 1 ~ 100 μm, obtains mixed powder;Then by mixed powder and the polyethylene glycol particle mixing of 20 ~ 30wt% of 70 ~ 80wt%, it is pressed into base substrate;Finally the base substrate suppressed is incubated 1 ~ 2 hour under the conditions of 1000 ~ 1200 DEG C, cooling, obtain ZrSiO4-SiC porous ceramics.
ZrSiO prepared by the present embodiment4-SiC porous ceramics is after testing: SiC content >=96wt%;The porosity >=45%.
Embodiment
2
A kind of ZrSiO4-SiC porous ceramics and preparation method thereof, its technical scheme is: first carbide fine powder and nickeliferous mixed liquor that mass ratio is 1: 2 is placed in ball mill, mix grinding 1 ~ 3 hour, obtains mixed slurry;Being filtered dry by mixed slurry, be dried 24 hours, obtain mixture block under the conditions of 110 DEG C, described mixture block is milled to granularity is 1 ~ 100 μm, obtains mixed powder;Then by mixed powder and the polyethylene glycol particle mixing of 10 ~ 20wt% of 80 ~ 90wt%, it is pressed into base substrate;Finally the base substrate suppressed is incubated 2 ~ 4 hours under the conditions of 1200 ~ 1500 DEG C, cooling, obtain ZrSiO4-SiC porous ceramics.
ZrSiO prepared by the present embodiment4-SiC porous ceramics is after testing: SiC content >=96.5wt%;The porosity >=40%.
Embodiment
3
A kind of ZrSiO4-SiC porous ceramics and preparation method thereof, its technical scheme is: first carbide fine powder and nickeliferous mixed liquor that mass ratio is 1: 2 is placed in ball mill, mix grinding 3 ~ 6 hours, obtains mixed slurry;Being filtered dry by mixed slurry, be dried 24 hours, obtain mixture block under the conditions of 110 DEG C, described mixture block is milled to granularity is 1 ~ 100 μm, obtains mixed powder;Then by mixed powder and the polyethylene glycol particle mixing of 5 ~ 10wt% of 90 ~ 95wt%, it is pressed into base substrate;Finally the base substrate suppressed is incubated 4 ~ 6 hours under the conditions of 1500 ~ 1800 DEG C, cooling, obtain ZrSiO4-SiC porous ceramics.
ZrSiO prepared by the present embodiment4-SiC porous ceramics is after testing: SiC content >=97wt%;The porosity >=30%.
This detailed description of the invention compared with prior art has a following good effect:
This detailed description of the invention is in high temperature preparation process, and silicon-carbide particle surface can form ZrSiO4(silicon tetrachloride and the four n-butoxy zirconiums that are wrapped in SiC particulate surface react under the effect of nickel-base catalyst and generate ZrSiO4), i.e. SiC particulate surface will parcel a thin layer ZrSiO4, ZrSiO4The existence of layer, not only can protect carborundum not oxidized, it is to avoid surface of SiC in use forms SiO2The negative consequence brought, and occur all without the problem having crystal transfer from room temperature to 1676 DEG C synthetic material.ZrSiO prepared by this detailed description of the invention4-SiC porous ceramics can use in the environment of maximum temperature is 1676 DEG C, and the temperature range of use has exceeded the temperature limiting that the most common silicon carbide ceramics is used, and can change, with bearing temperature, the damage brought;Elevated temperature strength is high, antioxygenic property is good, erosion resistant and thermal shock resistance high.
ZrSiO prepared by this detailed description of the invention4-SiC porous ceramics is after testing: SiC content >=96wt%;The porosity >=30%.Can be as materials such as filtering material, catalyst carrier, thermodynamic material, sound-absorbing material and composite skeletons.
Therefore, the ZrSiO that prepared by this detailed description of the invention4-SiC porous ceramics elevated temperature strength is high, antioxygenic property is good, erosion resistant and thermal shock resistance is high and proportion is little, carborundum can not only be protected the most not oxidized, it is to avoid surface of SiC in use forms SiO2The negative consequence brought, and can be all without there being crystal transfer during room temperature to 1676 DEG C.
Claims (5)
1. a ZrSiO4The preparation method of-SiC porous ceramics, its technical scheme is: be first the carbon of 1: 2 by mass ratio
SiClx fine powder and nickeliferous mixed liquor are placed in ball mill, mix grinding 0.5~6 hours, obtain mixed slurry;Again mixed slurry is filtered
Dry, it is dried 24 hours under the conditions of 110 DEG C, obtains mixture block, described mixture block is milled to granularity is
1~100 μm, obtain mixed powder;Then the mixed powder of 70~95wt% and the polyethylene glycol particle of 5~30wt% are mixed,
It is pressed into base substrate;Finally the base substrate suppressed is incubated 1~6 hour under the conditions of 1000~1800 DEG C, cooling, to obtain final product
ZrSiO4-SiC porous ceramics;
The preparation method of described nickeliferous mixed liquor is: be first 1: 1 by the atomic molar ratio of Si and Zr, by silicon tetrachloride and
Four n-butoxy zirconium solution mixing, obtain mixed solution;It is 1 by the mass ratio of mixed solution Yu nickel nitrate again:
(0.001~0.02), adds nickel nitrate, mixing in mixed solution, obtains nickeliferous mixed liquor.
ZrSiO the most according to claim 14The preparation method of-SiC porous ceramics, it is characterised in that described carbonization
SiC content >=97wt% in silica fine powder;Particle diameter is 1~500 μm.
ZrSiO the most according to claim 14The preparation method of-SiC porous ceramics, it is characterised in that described nitric acid
Ni (NO) in nickel3·6H2O content >=97wt%;Particle diameter is 1~500 μm.
ZrSiO the most according to claim 14The preparation method of-SiC porous ceramics, it is characterised in that described poly-second
The particle diameter of glycol particle is 0.1~2mm.
5. a ZrSiO4-SiC porous ceramics, it is characterised in that described ZrSiO4-SiC porous ceramics is to want according to right
Seek the ZrSiO according to any one of 1~44ZrSiO prepared by the preparation method of-SiC porous ceramics4-SiC porous is made pottery
Porcelain.
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Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
DE2045808A1 (en) * | 1970-09-16 | 1972-03-23 | Anna Werk Gmbh | Silicon carbide refractory - produced by firing with tialite |
US4777152A (en) * | 1984-05-29 | 1988-10-11 | Ibiden Kabushiki Kaisha | Porous silicon carbide sinter and its production |
CN103896593A (en) * | 2014-03-05 | 2014-07-02 | 武汉科技大学 | Silicon nitride combined silicon carbide complex-phase high-temperature-resistant material and preparation method thereof |
CN104529507A (en) * | 2015-01-19 | 2015-04-22 | 武汉科技大学 | Porous silicon nitride/silicon carbide composite ceramic material and preparation method thereof |
CN105384450A (en) * | 2015-11-10 | 2016-03-09 | 安吉科灵磁性材料有限公司 | Production method of aluminum silicon sol reinforced silicon carbide kiln furniture |
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2016
- 2016-03-17 CN CN201610152356.6A patent/CN105753501B/en not_active Expired - Fee Related
Patent Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
DE2045808A1 (en) * | 1970-09-16 | 1972-03-23 | Anna Werk Gmbh | Silicon carbide refractory - produced by firing with tialite |
US4777152A (en) * | 1984-05-29 | 1988-10-11 | Ibiden Kabushiki Kaisha | Porous silicon carbide sinter and its production |
CN103896593A (en) * | 2014-03-05 | 2014-07-02 | 武汉科技大学 | Silicon nitride combined silicon carbide complex-phase high-temperature-resistant material and preparation method thereof |
CN104529507A (en) * | 2015-01-19 | 2015-04-22 | 武汉科技大学 | Porous silicon nitride/silicon carbide composite ceramic material and preparation method thereof |
CN105384450A (en) * | 2015-11-10 | 2016-03-09 | 安吉科灵磁性材料有限公司 | Production method of aluminum silicon sol reinforced silicon carbide kiln furniture |
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