CN114149274A - Method for preparing directional porous SiC ceramic by using coal slime as pore-forming agent - Google Patents
Method for preparing directional porous SiC ceramic by using coal slime as pore-forming agent Download PDFInfo
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- 239000000919 ceramic Substances 0.000 title claims abstract description 39
- 239000003245 coal Substances 0.000 title claims abstract description 19
- 238000000034 method Methods 0.000 title claims abstract description 17
- 239000003795 chemical substances by application Substances 0.000 title claims abstract description 16
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 18
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 17
- 238000005245 sintering Methods 0.000 claims abstract description 9
- 238000002156 mixing Methods 0.000 claims abstract description 8
- 238000001035 drying Methods 0.000 claims abstract description 7
- 238000003825 pressing Methods 0.000 claims abstract description 7
- 239000000843 powder Substances 0.000 claims abstract description 6
- 238000002360 preparation method Methods 0.000 claims description 7
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 7
- 229910052814 silicon oxide Inorganic materials 0.000 claims description 4
- 239000007864 aqueous solution Substances 0.000 claims description 3
- 239000012300 argon atmosphere Substances 0.000 claims description 3
- 230000003179 granulation Effects 0.000 claims description 3
- 238000005469 granulation Methods 0.000 claims description 3
- 238000000465 moulding Methods 0.000 claims description 3
- 239000002245 particle Substances 0.000 claims description 3
- 230000000630 rising effect Effects 0.000 claims description 3
- 239000002002 slurry Substances 0.000 claims description 3
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 2
- 229910052681 coesite Inorganic materials 0.000 claims description 2
- 238000001816 cooling Methods 0.000 claims description 2
- 229910052593 corundum Inorganic materials 0.000 claims description 2
- 229910052906 cristobalite Inorganic materials 0.000 claims description 2
- 238000000197 pyrolysis Methods 0.000 claims description 2
- 239000000377 silicon dioxide Substances 0.000 claims description 2
- 229910052682 stishovite Inorganic materials 0.000 claims description 2
- 239000000126 substance Substances 0.000 claims description 2
- 229910052905 tridymite Inorganic materials 0.000 claims description 2
- 229910001845 yogo sapphire Inorganic materials 0.000 claims description 2
- 239000003250 coal slurry Substances 0.000 claims 2
- 238000000498 ball milling Methods 0.000 claims 1
- 239000004927 clay Substances 0.000 claims 1
- 229910052500 inorganic mineral Inorganic materials 0.000 claims 1
- 239000011707 mineral Substances 0.000 claims 1
- 239000000203 mixture Substances 0.000 claims 1
- 239000005416 organic matter Substances 0.000 claims 1
- 239000010453 quartz Substances 0.000 claims 1
- 238000009826 distribution Methods 0.000 abstract description 5
- 230000015572 biosynthetic process Effects 0.000 abstract description 3
- 239000002994 raw material Substances 0.000 abstract description 3
- 238000006243 chemical reaction Methods 0.000 abstract description 2
- 238000010438 heat treatment Methods 0.000 abstract 1
- 238000004519 manufacturing process Methods 0.000 abstract 1
- 238000002844 melting Methods 0.000 abstract 1
- 230000008018 melting Effects 0.000 abstract 1
- 239000013589 supplement Substances 0.000 abstract 1
- 238000009740 moulding (composite fabrication) Methods 0.000 description 11
- 239000011148 porous material Substances 0.000 description 7
- 229910052581 Si3N4 Inorganic materials 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005674 electromagnetic induction Effects 0.000 description 1
- 238000001125 extrusion Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 238000004108 freeze drying Methods 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 1
- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Chemical compound [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 description 1
- 239000011863 silicon-based powder Substances 0.000 description 1
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Abstract
The invention discloses a method for preparing directional porous SiC ceramic by using coal slime as a pore-forming agent, belonging to the technical field of porous ceramic. SiC powder is used as a raw material, coal slime with different contents is added as a pore-forming agent, a blank body is obtained by dry pressing after wet mixing, and the directional porous SiC ceramic is obtained after drying and sintering the blank body. According to the invention, the coal slime is used as the pore-forming agent, and in the process of heating to the re-sintering temperature, the porous carbon formed in the coal slime supplements carbon loss caused by other pore-forming agents, so that the improvement of the relative density is promoted. Low melting point volatile species and reaction generated SiC can promote directional porosity formation, forming a smooth columnar structure. The invention has the advantages of easily obtained raw materials, low cost and simple manufacturing process. The prepared porous ceramic has the characteristic of directional distribution of air holes, and has higher relative density and axial rupture strength.
Description
Technical Field
The invention belongs to the technical field of porous ceramics, and particularly relates to a method for preparing directional porous SiC ceramic by using coal slime as a pore-forming agent.
Background
Oriented porous SiC ceramics are widely concerned with due to the special pore oriented distribution characteristics, especially have great significance in the high-tech fields of technical melt filtration, combustion reactors, chips and the like, and the oriented porous ceramics prepared by the traditional oriented porous SiC ceramic preparation methods (such as a freeze drying method, an extrusion molding method, a template method and the like) at present have low relative density and low strength, so that the application of the oriented porous ceramics is greatly limited. In patent CN101323524, SiC, carbon powder, silicon powder and silicon oxide are used as raw materials, directional porous SiC ceramic is prepared by utilizing temperature difference distribution in the furnace along the axial direction, but the porous ceramic prepared by loose accumulation of the particles has lower strength, and SiO is adopted in succession for Liu bright, Liu Bo, and the like2And Si3N4The directional porous SiC ceramic with the directional distribution characteristic of pores is prepared by taking the SiC as a pore-forming agent, and the applicant adopts Fe2O3The oriented porous SiC ceramic with high pore rib density and strength is prepared after dry pressing, forming and sintering as a pore-forming agent, and the pore size is controlled by adjusting the content of the pore-forming agent. However, the gradient distribution of the temperature field causes a large amount of Si to be generated in the high-temperature area at the bottom of the sample2C and SiC2The carbon-carrying pore-forming agent carries a large amount of carbon elements to volatilize, so that the carbon at the bottom is lost, the difference between the pore structures at the bottom and the top of the sample is large, and the application of the material is limited, so that the finding of the pore-forming agent which can provide a carbon source and promote the formation of the directional pore is important.
Disclosure of Invention
In order to solve the problems, the invention provides a method for preparing oriented porous SiC ceramic by using coal slime as a pore-forming agent, which is realized by the following specific technical scheme that on one hand, porous carbon formed by high-temperature pyrolysis of the coal slime is used for providing a carbon source, and on the other hand, a large amount of silicon oxide components in the coal slime are used as the pore-forming agent:
the invention discloses a method for preparing directional porous SiC ceramic by using coal slime as a pore-forming agent, which comprises the following steps:
1) adding 15-35% of coal slime into SiC powder for wet mixing, adding a proper amount of 5% PVB aqueous solution after the slurry is dried, and performing dry pressing molding after granulation to obtain a green body;
2) and drying the green body and then re-sintering to obtain the directional porous SiC ceramic.
Preferably, the grain size after mixing is 320 meshes.
Preferably, the time for wet mixing is 12 h.
Preferably, the pressure for dry pressing is 5 tons.
Preferably, in the step 3), the drying temperature is 120 ℃ and the drying time is 12 h.
Preferably, the sintering is carried out in an argon atmosphere at a furnace pressure of 0.8MPa, wherein the temperature is increased to 2150 ℃ from the room temperature at a temperature rising speed of 100 ℃ per minute, the temperature is kept for 2 hours, and then the sintering is cooled to the room temperature at a temperature reducing speed of 10 ℃ per minute.
The invention also discloses the directional porous SiC ceramic prepared by the method.
Compared with the prior art, the invention has the following beneficial technical effects:
in the method for orienting the porous SiC ceramic, the main component of the coal slime is SiO2And Al2O3And the carbon element with high content is heated to 1000 ℃ and converted into porous carbon, the porous carbon is heated to 1600 ℃ and reacts with silicon oxide to generate SiC, the temperature is raised to 2100 ℃, aluminum oxide and other components are volatilized, and a large amount of fine particle SiC and a large amount of porous carbon are remained. The formation of directional porous can be promoted by volatile substances and SiC generated by reaction, and the relative density can be improved by a large amount of residual porous carbon, so that a carbon source is provided for the bottom of the sample, the loss of a large amount of carbon at the bottom of the sample is prevented, and the consistency of the bottom and top structures of the sample is ensured。
Drawings
FIG. 1 is an axial microstructure of an oriented porous SiC ceramic prepared in example 3 of the present invention.
Detailed Description
The present invention will now be described in further detail with reference to specific examples, which are intended to be illustrative, but not limiting, of the invention. The invention discloses a preparation method of directional porous SiC ceramic, which comprises the following steps:
example 1
1) Adding 15-35% of coal slime into SiC powder for wet mixing, adding a proper amount of 5% PVB aqueous solution after the slurry is dried, and performing dry pressing molding after granulation to obtain a green body;
2) putting the green body into a drying oven, and drying at 120 ℃ for 12 h; and then putting the directional porous SiC ceramic into a medium-frequency electromagnetic induction vacuum high-temperature sintering furnace, increasing the temperature from the room temperature to 2150 ℃ at the temperature rising speed of 100 ℃ per minute under the furnace pressure of 0.8MPa in the argon atmosphere, preserving the temperature for 2h, and cooling to the room temperature at the temperature falling speed of 10 ℃ per minute to obtain the directional porous SiC ceramic. The density of the directional porous SiC ceramic pore ribs prepared by testing is 2.85g/cm3The axial rupture strength was 37.12MPa, and the relative density was 89.6%.
Under the condition that other conditions are not changed, the examples 2-6 which are carried out by changing the mass percentages of the coal slime and the SiC powder are shown in the table 1, and the axial rupture strength and the relative density numerical value of the prepared directional porous SiC ceramic are shown in the table 1.
TABLE 1
As seen from Table 1, the prepared directional porous SiC ceramics had good axial flexural strength and relative density.
Claims (10)
1. A method for preparing directional porous SiC ceramic by using coal slime as a pore-forming agent is characterized by comprising the following steps:
1) adding 15-35% of coal slime into SiC powder for wet mixing, adding a proper amount of 5% PVB aqueous solution after the slurry is dried, and performing dry pressing molding after granulation to obtain a green body;
2) and drying the green body and then re-sintering to obtain the directional porous SiC ceramic.
2. The method of claim 1, wherein the SiC powder has an average particle size of 30 μm and the particle size after mixing is 320 mesh.
3. The preparation method of the directional porous SiC ceramic according to claim 1, wherein the mixture is fully stirred before wet mixing, is sieved by a 20-mesh sieve, and is subjected to wet ball milling for 12 hours.
4. The method for preparing oriented porous SiC ceramic according to claim 1, wherein the main chemical component of the coal slurry in the step 1) is 25.56% SiO2And 21.4% Al2O3The main mineral components are clay and a certain amount of quartz.
5. The preparation method of oriented porous SiC ceramic according to claim 1, wherein the coal slurry in step 1) mainly contains 49.35% of organic matter and 28.49% of carbon.
6. The method of preparing an oriented porous SiC ceramic according to claim 1, characterized in that the pressure of dry pressing is 5 tons.
7. The preparation method of the directional porous SiC ceramic according to claim 1, wherein organic matters in the coal slime are pyrolyzed at a high temperature at about 1000 ℃ to form porous carbon.
8. The preparation method of the directional porous SiC ceramic according to claim 1, wherein porous carbon formed by high-temperature pyrolysis of organic matters in coal slime at about 1600 ℃ reacts with silicon oxide to generate SiC phase.
9. The preparation method of directional porous SiC ceramic according to claim 1, wherein the sintering is carried out in an argon atmosphere at a furnace pressure of 0.8MPa at a temperature rising speed of 100 ℃ per minute from room temperature to 2150 ℃ for 2h, and then cooling to room temperature at a temperature lowering speed of 10 ℃ per minute.
10. The method for preparing oriented porous SiC ceramic according to claim 1, wherein the prepared oriented porous SiC ceramic is free from gradient porosity.
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