CN105753501B - A kind of ZrSiO4- SiC porous ceramics and preparation method thereof - Google Patents

A kind of ZrSiO4- SiC porous ceramics and preparation method thereof Download PDF

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CN105753501B
CN105753501B CN201610152356.6A CN201610152356A CN105753501B CN 105753501 B CN105753501 B CN 105753501B CN 201610152356 A CN201610152356 A CN 201610152356A CN 105753501 B CN105753501 B CN 105753501B
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porous ceramics
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魏耀武
张争
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Wuhan University of Science and Engineering WUSE
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Abstract

The present invention relates to a kind of ZrSiO4SiC porous ceramics and preparation method thereof.Its technical solution is：First mass ratio is placed in for 1: 2 carbide fine powder and nickeliferous mixed liquor in ball mill, when mix grinding 0.5 ~ 6 is small, obtains mixed slurry；Mixed slurry is filtered dry again, when drying 24 is small under the conditions of 110 DEG C, obtains mixture block, the mixture block is milled to granularity as 1 ~ 100 μm, obtains mixed powder；Then by the polyethylene glycol particle mixing of the mixed powder of 70 ~ 95wt% and 5 ~ 30wt%, it is pressed into green body；Finally the green body suppressed is cooled down when heat preservation 1 ~ 6 is small under the conditions of 1000 ~ 1800 DEG C to get ZrSiO4SiC porous ceramics.ZrSiO prepared by the present invention4SiC porous ceramics elevated temperature strength is high, antioxygenic property is good, erosion resistant and thermal shock resistance is high and proportion is small, can be not oxidized at high temperature, can be from room temperature to not having crystal transfer during 1676 DEG C.

Description

A kind of ZrSiO4- SiC porous ceramics and preparation method thereof
Technical field
The invention belongs to high-temperature ceramic techniques fields.More particularly to a kind of ZrSiO4- SiC porous ceramics and its preparation side Method.
Background technology
Porous ceramics is a kind of through high temperature firing, the ceramic material in vivo with largely communicate with each other stomata or closure stomata Material.Its development starts from 19 century 70s, and due to its excellent performance, porous ceramics is gradually applied to metallurgy, chemical industry, ring The multiple fields such as guarantor, the energy and biology.Using the uniform permeability of porous ceramics, can manufacture various filters, separator, Fluid distribution component, hybrid element, exudation element and restricting element etc.；It the characteristics of using porous ceramics high-specific surface area, can To be made into porous electrode, catalyst carrier, heat exchanger, gas sensor etc.；The property of energy is absorbed using porous ceramics Can, it may be used as various sound-absorbing materials, vibration-absorptive material etc.；Using the low density of porous ceramics, low heat-conductive characteristic, can make Into various thermal insulation materials and lightweight structural material etc..
At present, the carborundum porous ceramics that can be used under the high temperature conditions have elevated temperature strength is high, antioxygenic property is good, The features such as erosion resistant and thermal shock resistance are high, proportion is small, higher thermal conductivity and microwave absorption capacity are strong, has wide in the industry General application.The preparation method of carborundum porous ceramics mainly has：Add pore creating material method, foaming, Polymeric sponge method and Sol-gel method etc..The carborundum porous ceramics material prepared using the above method is generally suffered from preferably in different occasions Application.
But carborundum porous ceramics in high temperature in application, its surface can generate SiO due to the oxidation of SiC2Although SiO2SiC particulate surface is wrapped in, the not oxidized effects of the internal SiC of protection can be played, still, in the change procedure of temperature In, the SiO on silicon-carbide particle surface2（Quartz）Crystal transfer can occur, the bulk effect that crystal transfer generates can reduce carbon The structural strength of SiClx porous ceramics and a series of calorifics and optical property generate the application of carborundum porous ceramics material Adverse effect.
The content of the invention
It it is contemplated that overcomes the shortage of prior art, it is therefore an objective to which a kind of ZrSiO is provided4The preparation side of-SiC porous ceramics Method, prepared ZrSiO4- SiC porous ceramics elevated temperature strength is high, antioxygenic property is good, erosion resistant and thermal shock resistance is high and ratio Weight is small, and carborundum can not only be protected not oxidized at high temperature, surface of SiC is avoided to form SiO in use2It is caused Negative consequence, and can not have crystal transfer in the process from room temperature to 1676 DEG C.
To achieve the above object, the technical solution adopted in the present invention is：First by mass ratio be 1: 2 carbide fine powder and Nickeliferous mixed liquor is placed in ball mill, when mix grinding 0.5 ~ 6 is small, obtains mixed slurry；Mixed slurry is filtered dry again, in 110 DEG C of conditions When lower drying 24 is small, mixture block is obtained, the mixture block is milled to granularity as 1 ~ 100 μm, obtains mixed powder；Then will The mixed powder of 70 ~ 95wt% and the polyethylene glycol particle mixing of 5 ~ 30wt%, are pressed into green body；Finally by the green body suppressed in When heat preservation 1 ~ 6 is small under the conditions of 1000 ~ 1800 DEG C, cool down to get ZrSiO4- SiC porous ceramics.
The preparation method of the nickeliferous mixed liquor is：It is first 1: 1 by the atomic molar ratio of Si and Zr, by silicon tetrachloride and four N-butoxy zirconium solution mixes, and obtains mixed solution；It is again 1 by the mass ratio of mixed solution and nickel nitrate:（0.001~0.02）, to Nickel nitrate is added in mixed solution, is mixed to get nickeliferous mixed liquor.
SiC content >=97wt% in the carbide fine powder；Grain size is 1 ~ 500 μm.
Ni (NO) in the nickel nitrate3·6H2O content >=97wt%；Grain size is 1 ~ 500 μm.
The grain size of the polyethylene glycol particle is 0.1 ~ 2mm.
Due to the adoption of the above technical scheme, the present invention has following good effect compared with prior art：
For the present invention in high temperature preparation process, silicon-carbide particle surface can form ZrSiO4（It is wrapped in SiC particulate surface Silicon tetrachloride and four n-butoxy zirconiums react under the action of nickel-base catalyst and generate ZrSiO4）, i.e. SiC particulate surface It will package a thin layer ZrSiO4, ZrSiO4The presence of layer, can not only protect carborundum not oxidized, surface of SiC is avoided to use SiO is formed in journey2Caused negative consequence, and asking for crystal transfer is not had into 1676 DEG C of synthetic materials from room temperature Topic occurs.ZrSiO prepared by the present invention4- SiC porous ceramics can use in the environment of maximum temperature is 1676 DEG C, use Temperature range has been more than temperature limiting used in common silicon carbide ceramics at present, and caused by being changed with bearing temperature Damage；Elevated temperature strength is high, antioxygenic property is good, erosion resistant and thermal shock resistance are high.
ZrSiO prepared by the present invention4- SiC porous ceramics is after testing：SiC content >=96wt%；The porosity >=30%.It can make For materials such as filtering material, catalyst carrier, thermodynamic material, sound-absorbing material and composite material 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 heat It is high small with proportion to shake stability, carborundum can not only be protected not oxidized at high temperature, avoid surface of SiC shape in use Into SiO2Caused negative consequence, and can not have crystal transfer in the process from room temperature to 1676 DEG C.
Specific embodiment
The present invention will be further described With reference to embodiment, not to the limitation of its protection domain.
It is now that the technical parameter Unify legislation involved by present embodiment is as follows to avoid repeating, in embodiment not It repeats again：
The preparation method of the nickeliferous mixed liquor is：It is first 1: 1 by the atomic molar ratio of Si and Zr, by silicon tetrachloride and four N-butoxy zirconium solution mixes, and obtains mixed solution；It is again 1 by the mass ratio of mixed solution and nickel nitrate:（0.001~0.02）, to Nickel nitrate is added in mixed solution, is mixed to get nickeliferous mixed liquor.
SiC content >=97wt% in the carbide fine powder；Grain size is 1 ~ 500 μm.
Ni (NO) in the nickel nitrate3·6H2O content >=97wt%；Grain size is 1 ~ 500 μm.
The grain size of the polyethylene glycol particle is 0.1 ~ 2mm.
Embodiment 1
A kind of ZrSiO4- SiC porous ceramics and preparation method thereof, technical solution are：First by mass ratio be 1: 2 carbonization Silica fine powder and nickeliferous mixed liquor are placed in ball mill, when mix grinding 0.5 ~ 1 is small, obtain mixed slurry；Mixed slurry is filtered dry again, When drying 24 is small under the conditions of 110 DEG C, mixture block is obtained, the mixture block is milled to granularity as 1 ~ 100 μm, obtains mixed powder Body；Then by the polyethylene glycol particle mixing of the mixed powder of 70 ~ 80wt% and 20 ~ 30wt%, it is pressed into green body；It will finally be pressed The green body of system is cooled down when heat preservation 1 ~ 2 is small under the conditions of 1000 ~ 1200 DEG C to get ZrSiO4- SiC porous ceramics.
ZrSiO manufactured in 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, technical solution are：First by mass ratio be 1: 2 carbonization Silica fine powder and nickeliferous mixed liquor are placed in ball mill, when mix grinding 1 ~ 3 is small, obtain mixed slurry；Mixed slurry is filtered dry again, 110 When drying 24 is small under the conditions of DEG C, mixture block is obtained, the mixture block is milled to granularity as 1 ~ 100 μm, obtains mixed powder； Then by the polyethylene glycol particle mixing of the mixed powder of 80 ~ 90wt% and 10 ~ 20wt%, it is pressed into green body；It will finally be suppressed Green body under the conditions of 1200 ~ 1500 DEG C heat preservation 2 ~ 4 it is small when, cool down to get ZrSiO4- SiC porous ceramics.
ZrSiO manufactured in 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, technical solution are：First by mass ratio be 1: 2 carbonization Silica fine powder and nickeliferous mixed liquor are placed in ball mill, when mix grinding 3 ~ 6 is small, obtain mixed slurry；Mixed slurry is filtered dry again, 110 When drying 24 is small under the conditions of DEG C, mixture block is obtained, the mixture block is milled to granularity as 1 ~ 100 μm, obtains mixed powder； Then by the polyethylene glycol particle mixing of the mixed powder of 90 ~ 95wt% and 5 ~ 10wt%, it is pressed into green body；It will finally be suppressed Green body is cooled down when heat preservation 4 ~ 6 is small under the conditions of 1500 ~ 1800 DEG C to get ZrSiO4- SiC porous ceramics.
ZrSiO manufactured in the present embodiment4- SiC porous ceramics is after testing：SiC content >=97wt%；The porosity >=30%.
Present embodiment has following good effect compared with prior art：
For present embodiment in high temperature preparation process, silicon-carbide particle surface can form ZrSiO4（It is wrapped in SiC The silicon tetrachloride and four n-butoxy zirconiums on grain surface react under the action of nickel-base catalyst and generate ZrSiO4）, i.e. SiC Particle surface will wrap up a thin layer ZrSiO4, ZrSiO4The presence of layer, can not only protect carborundum not oxidized, avoid surface of SiC SiO is formed in use2Caused negative consequence, and from room temperature crystal form is not had into 1676 DEG C of synthetic materials The problem of transformation, occurs.ZrSiO prepared by present embodiment4- SiC porous ceramics can be 1676 DEG C in maximum temperature It is used under environment, the temperature range used has been more than temperature limiting used in common silicon carbide ceramics, and can holding at present By damage caused by temperature change；Elevated temperature strength is high, antioxygenic property is good, erosion resistant and thermal shock resistance are high.
ZrSiO prepared by present embodiment4- SiC porous ceramics is after testing：SiC content >=96wt%；The porosity >= 30%.The materials such as filtering material, catalyst carrier, thermodynamic material, sound-absorbing material and composite material skeleton can be used as.
Therefore, the ZrSiO that prepared by present embodiment4- SiC porous ceramics elevated temperature strength is high, antioxygenic property is good, resistance to Abrasion and thermal shock resistance are high small with proportion, and carborundum can not only be protected not oxidized at high temperature, surface of SiC is avoided to use SiO is formed in the process2Caused negative consequence, and can not have crystal transfer in the process from room temperature to 1676 DEG C.

Claims (5)

1. a kind of ZrSiO4The preparation method of-SiC porous ceramics, technical solution are：It is first that mass ratio is thin for 1: 2 carborundum Powder and nickeliferous mixed liquor are placed in ball mill, when mix grinding 0.5~6 is small, obtain mixed slurry；Mixed slurry is filtered dry again, at 110 DEG C Under the conditions of it is dry 24 it is small when, obtain mixture block, the mixture block be milled to granularity as 1~100 μm, obtains mixed powder； Then by the polyethylene glycol particle mixing of the mixed powder of 70~95wt% and 5~30wt%, it is pressed into green body；It will finally be pressed The green body of system is cooled down when heat preservation 1~6 is small under the conditions of 1000~1800 DEG C to get ZrSiO4- SiC porous ceramics；
The preparation method of the nickeliferous mixed liquor is：It is first 1: 1 by the atomic molar ratio of Si and Zr, by silicon tetrachloride and four positive fourths Oxygroup zirconium solution mixes, and obtains mixed solution；It is again 1 by the mass ratio of mixed solution and nickel nitrate: (0.001~0.02), to mixed It closes in solution and adds in nickel nitrate, mix to get nickeliferous mixed liquor.
2. ZrSiO according to claim 14The preparation method of-SiC porous ceramics, it is characterised in that the carbide fine powder Middle SiC content >=97wt%；Grain size is 1~500 μm.
3. ZrSiO according to claim 14The preparation method of-SiC porous ceramics, it is characterised in that Ni in the nickel nitrate (NO3)2· 6H2O content >=97wt%；Grain size is 1~500 μm.
4. ZrSiO according to claim 14The preparation method of-SiC porous ceramics, it is characterised in that the polyethylene glycol The grain size of grain is 0.1~2mm.
5. a kind of ZrSiO4- SiC porous ceramics, it is characterised in that the ZrSiO4- SiC porous ceramics be according to claim 1~ ZrSiO any one of 44ZrSiO prepared by the preparation method of-SiC porous ceramics4- SiC porous ceramics.
CN201610152356.6A 2016-03-17 2016-03-17 A kind of ZrSiO4- SiC porous ceramics and preparation method thereof Expired - Fee Related CN105753501B (en)

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DE2045808A1 (en) * 1970-09-16 1972-03-23 Anna Werk Gmbh Silicon carbide refractory - produced by firing with tialite
JPS60255671A (en) * 1984-05-29 1985-12-17 イビデン株式会社 High strength porous silicon carbide sintered body and manufacture
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