CN117800763A - Method for preparing silicon carbide material by in-situ solidification of precursor and silicon carbide material - Google Patents
Method for preparing silicon carbide material by in-situ solidification of precursor and silicon carbide material Download PDFInfo
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- CN117800763A CN117800763A CN202311848170.0A CN202311848170A CN117800763A CN 117800763 A CN117800763 A CN 117800763A CN 202311848170 A CN202311848170 A CN 202311848170A CN 117800763 A CN117800763 A CN 117800763A
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- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 title claims abstract description 105
- 239000002243 precursor Substances 0.000 title claims abstract description 103
- 229910010271 silicon carbide Inorganic materials 0.000 title claims abstract description 58
- 238000000034 method Methods 0.000 title claims abstract description 46
- 239000000463 material Substances 0.000 title claims abstract description 38
- 238000011065 in-situ storage Methods 0.000 title claims abstract description 31
- 238000007711 solidification Methods 0.000 title abstract description 10
- 230000008023 solidification Effects 0.000 title abstract description 10
- 229910021426 porous silicon Inorganic materials 0.000 claims abstract description 47
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 38
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 38
- 238000005470 impregnation Methods 0.000 claims abstract description 26
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 18
- 239000002904 solvent Substances 0.000 claims abstract description 16
- 238000004140 cleaning Methods 0.000 claims abstract description 6
- 239000002131 composite material Substances 0.000 claims abstract description 6
- 239000007787 solid Substances 0.000 claims abstract description 6
- 238000012216 screening Methods 0.000 claims abstract description 5
- 238000010000 carbonizing Methods 0.000 claims abstract description 4
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 24
- XPFVYQJUAUNWIW-UHFFFAOYSA-N furfuryl alcohol Chemical compound OCC1=CC=CO1 XPFVYQJUAUNWIW-UHFFFAOYSA-N 0.000 claims description 24
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 19
- 239000003112 inhibitor Substances 0.000 claims description 10
- 238000006116 polymerization reaction Methods 0.000 claims description 10
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 9
- 238000007865 diluting Methods 0.000 claims description 8
- 235000006408 oxalic acid Nutrition 0.000 claims description 8
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 7
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 7
- 238000004519 manufacturing process Methods 0.000 claims description 7
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 6
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 6
- 239000000654 additive Substances 0.000 claims description 6
- 230000000996 additive effect Effects 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 6
- 238000000465 moulding Methods 0.000 claims description 4
- 239000012713 reactive precursor Substances 0.000 claims description 4
- WIEXMPDBTYDSQF-UHFFFAOYSA-N 1,3-bis(furan-2-yl)propan-2-one Chemical compound C=1C=COC=1CC(=O)CC1=CC=CO1 WIEXMPDBTYDSQF-UHFFFAOYSA-N 0.000 claims description 3
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 claims description 3
- JJLJMEJHUUYSSY-UHFFFAOYSA-L Copper hydroxide Chemical compound [OH-].[OH-].[Cu+2] JJLJMEJHUUYSSY-UHFFFAOYSA-L 0.000 claims description 3
- 239000005750 Copper hydroxide Substances 0.000 claims description 3
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 3
- 238000005266 casting Methods 0.000 claims description 3
- 229910001956 copper hydroxide Inorganic materials 0.000 claims description 3
- 239000008367 deionised water Substances 0.000 claims description 3
- 229910021641 deionized water Inorganic materials 0.000 claims description 3
- 229960004887 ferric hydroxide Drugs 0.000 claims description 3
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims description 3
- IEECXTSVVFWGSE-UHFFFAOYSA-M iron(3+);oxygen(2-);hydroxide Chemical compound [OH-].[O-2].[Fe+3] IEECXTSVVFWGSE-UHFFFAOYSA-M 0.000 claims description 3
- 239000005011 phenolic resin Substances 0.000 claims description 3
- 229920001568 phenolic resin Polymers 0.000 claims description 3
- 229920005989 resin Polymers 0.000 claims description 3
- 239000011347 resin Substances 0.000 claims description 3
- 238000002791 soaking Methods 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- 239000003085 diluting agent Substances 0.000 claims description 2
- 238000002360 preparation method Methods 0.000 abstract description 13
- 230000008569 process Effects 0.000 abstract description 9
- 239000000919 ceramic Substances 0.000 abstract description 4
- 238000001035 drying Methods 0.000 abstract description 3
- 239000000243 solution Substances 0.000 description 39
- 238000001723 curing Methods 0.000 description 26
- 238000005245 sintering Methods 0.000 description 14
- 238000005336 cracking Methods 0.000 description 12
- 238000006243 chemical reaction Methods 0.000 description 10
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 7
- 229910052710 silicon Inorganic materials 0.000 description 7
- 239000010703 silicon Substances 0.000 description 7
- 238000007598 dipping method Methods 0.000 description 5
- 235000019441 ethanol Nutrition 0.000 description 5
- 238000003756 stirring Methods 0.000 description 5
- 238000009826 distribution Methods 0.000 description 4
- 230000005484 gravity Effects 0.000 description 4
- 238000013461 design Methods 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000000178 monomer Substances 0.000 description 2
- 238000000016 photochemical curing Methods 0.000 description 2
- 238000004321 preservation Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000009827 uniform distribution Methods 0.000 description 2
- 238000002835 absorbance Methods 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 239000007833 carbon precursor Substances 0.000 description 1
- 238000003763 carbonization Methods 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000005238 degreasing Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 238000001746 injection moulding Methods 0.000 description 1
- 239000012705 liquid precursor Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 150000002894 organic compounds Chemical class 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000000197 pyrolysis Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
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Abstract
The invention relates to the technical field of preparation of silicon carbide ceramics, and particularly provides a method for preparing a silicon carbide material by in-situ solidification of a precursor and the silicon carbide material, wherein the method comprises the following steps: s1, screening active precursors; s2: preparing a precursor solution from the active precursor and a composite solvent, wherein the mass fraction of the active precursor is more than 30%; s3: placing the porous silicon carbide preform in a precursor solution of carbon for full impregnation; s4: adding a curing agent with the mass fraction of 1% -10%; s5: when the silicon carbide is completely converted into solid, taking out the porous silicon carbide preform for cleaning; s6: carbonizing the cleaned porous silicon carbide preform, and converting the active precursor into cracked carbon in the porous silicon carbide preform to prepare a silicon carbide material; the method of the invention modifies large-size silicon carbide by in-situ solidification of the precursor, omits a drying and solidifying process and shortens the preparation period.
Description
Technical Field
The invention relates to the technical field of preparation of silicon carbide ceramics, and particularly provides a method for preparing a silicon carbide material by in-situ solidification of a precursor and the silicon carbide material.
Background
The reaction sintering silicon carbide has the advantages of low preparation cost and short process period, and is a main candidate material for the large-size space optical reflector. The preparation process comprises the following steps: mixing silicon carbide powder and organic matters to form a silicon carbide preform with a specific structure, sintering at high temperature to obtain a porous silicon carbide preform containing cracked carbon, impregnating liquid silicon into the porous silicon carbide preform, reacting part of silicon with carbon to form beta-prepared SiC, filling the pores with the rest of silicon, and finally obtaining the compact reaction sintering silicon carbide ceramic material. However, the strength, modulus, etc. properties of silicon are much lower than those of silicon carbide, and therefore, reducing the residual silicon content is an effective way to produce high performance reaction sintered silicon carbide.
Patent CN 106478105B discloses that adding carbon during the forming process converts the carbon into silicon carbide through reaction sintering, and has a certain effect of reducing the amount of residual silicon. However, this method is not universal, particularly for photo-curing additive manufacturing of silicon carbide, where the absorbance of carbon is extremely high during photo-curing, and the addition of carbon reduces the molding accuracy. The carbon source precursor impregnation cracking treatment is a method commonly used at present for improving the performance of the reaction sintering silicon carbide. The method is characterized in that a porous silicon carbide preform is impregnated with a precursor solution of carbon, the precursor of the carbon is converted into cracked carbon after high temperature, and finally, the part of carbon is converted into beta-SiC through reaction sintering, so that the method is a simple and effective way for reducing residual silicon. The method has the advantages of easy operation, low cost and short period, and has universality. Patent CN 110734287a shows that the method is capable of modifying cold isostatic pressed silicon carbide. Patent CN 116332652A shows that the method is suitable for improving the performance of silicon carbide molded by additive manufacturing. The precursor solution is immersed into the porous silicon carbide preform under the action of capillary force, and the impregnated precursor solution is shown in fig. 1; the disclosures of these patents show that the precursor solution needs to be cured under heating, but after the preform is taken out of the solution, the precursor solution flows out of the porous silicon carbide preform along the gravity direction during drying and curing because the precursor solution is influenced by the gravity of the solution, so that the precursor solution is unevenly distributed, as shown in fig. 2; after pyrolysis, the cracked carbon is unevenly distributed as shown in fig. 3; on one hand, the reaction sintering silicon carbide microstructure is uneven, particularly in the field of high-end equipment manufacturing, when a temperature field, a pressure field and the like are changed due to the uneven microstructure, stress is generated in the material, and the service performance of the equipment is affected; on the other hand, the liquid precursor flows out of the porous preform, so that the process efficiency of the precursor dipping treatment is reduced; therefore, it is necessary to find new preparation methods to improve the homogeneity of the silicon carbide ceramic structure.
Disclosure of Invention
Aiming at the problem of uneven microstructure caused by precursor dipping treatment, the invention provides a method for preparing a silicon carbide material by precursor in-situ curing. Specifically, through screening the precursor solution and designing the components, the in-situ solidification/cracking of the carbon precursor in the porous silicon carbide preform is realized, the cracked carbon is promoted to be uniformly dispersed and distributed in the porous silicon carbide preform, and finally the preparation of the homogeneous high-performance reaction sintering silicon carbide ceramic is completed.
The invention provides a method for preparing a silicon carbide material by in-situ curing of a precursor, which comprises the following steps:
s1, screening active precursors;
s2: preparing a precursor solution from the active precursor and a composite solvent, wherein the mass fraction of the precursor solution is 100%, and the mass fraction of the active precursor is more than 30%;
s3: placing the porous silicon carbide preform in a precursor solution of carbon, and fully soaking;
s4: adding a curing agent into the precursor solution, wherein the mass fraction of the added curing agent is 1-10% based on the mass fraction of the active precursor as 100%;
s5: when the precursor solution is completely converted into solid from liquid, taking out the porous silicon carbide preform, and cleaning the porous silicon carbide preform;
s6: and carbonizing the cleaned porous silicon carbide preform, and converting the active precursor into cracked carbon in the porous silicon carbide preform to prepare the silicon carbide material.
Preferably, the reactive precursor is selected from at least one of furfuryl alcohol containing an unsaturated bond, furfuryl ketone resin, or phenolic resin.
Preferably, the complex solvent includes a polymerization inhibitor and a diluting solvent.
Preferably, the polymerization inhibitor is selected from one or more of ammonia water, copper hydroxide or ferric hydroxide; the diluting solvent is selected from one or more of ethanol, glycol or deionized water.
Preferably, the mass ratio relationship among the active precursor, the polymerization inhibitor, the curing agent and the diluting solvent is (30% -70%): (1% -6%): (1% -10%): (17% -66%).
Preferably, the time for the sufficient impregnation is 3 hours or more.
Preferably, the sufficient impregnation mode is selected from any one of vacuum impregnation, normal pressure impregnation, air pressure impregnation or mechanical pressure impregnation.
Preferably, the curing agent is selected from any one of acetic acid, phosphoric acid or oxalic acid; the mass ratio of the curing agent to the precursor solution is (1:100) - (10:100).
Preferably, the porous silicon carbide preform is obtained by additive manufacturing molding or gel casting.
The invention also provides a silicon carbide material which is prepared by the method for preparing the silicon carbide material by in-situ curing of the precursor.
Compared with the prior art, the invention has the following beneficial effects:
the invention provides a method for preparing a silicon carbide material by in-situ solidification of a precursor, which can control the content of green body silicon carbide after final reaction sintering by adjusting the components of the precursor solution, so that the preparation of high-performance reaction sintering silicon carbide can be realized; on the basis of the traditional impregnation treatment method, the carbon source precursor component design is carried out, so that the uniform distribution of the impregnated porous preform carbon is ensured, and the defect of low efficiency of the traditional impregnation treatment is overcome; the in-situ solidification cracking method can realize the directional design of the content and distribution of the cracked carbon in the porous prefabricated body; compared with the traditional dipping treatment, the method provided by the invention does not need treatment processes such as drying, heating and curing, and the like, so that the process preparation period is shortened; and the forming mode of the porous silicon carbide preform is not limited.
Drawings
FIG. 1 is a schematic representation of precursor impregnation (without curative) in the prior art;
FIG. 2 is a schematic diagram of a prior art precursor dry cure;
FIG. 3 is a schematic diagram of the distribution of cracked carbon in a preform after cracking of a precursor according to the prior art;
FIG. 4 is a schematic illustration of precursor solution impregnation with reactive precursors and curing agents, etc. in accordance with an embodiment of the present invention;
FIG. 5 is a schematic illustration of in situ curing of reactive precursors according to an embodiment of the invention;
FIG. 6 is a schematic representation of the uniform distribution of cracked carbon after cracking of an in situ cured organic compound according to an embodiment of the present invention.
Detailed Description
Hereinafter, embodiments of the present invention will be described with reference to the accompanying drawings. In the following description, like modules are denoted by like reference numerals. In the case of the same reference numerals, their names and functions are also the same. Therefore, a detailed description thereof will not be repeated.
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention will be further described in detail with reference to the accompanying drawings and specific embodiments. It should be understood that the specific embodiments described herein are for purposes of illustration only and are not to be construed as limiting the invention.
In a specific embodiment, the invention provides a method for preparing a silicon carbide material by in-situ curing a precursor, which comprises the following steps:
s1, screening active precursors; the active precursor is selected from at least one of furfuryl alcohol, furfuryl ketone resin or phenolic resin containing unsaturated bond.
S2: preparing a precursor solution from the active precursor and a composite solvent, wherein the mass fraction of the precursor solution is 100%, and the mass fraction of the active precursor is more than 30%; in a preferred embodiment, the composite solvent comprises a polymerization inhibitor and a diluting solvent, so that the viscosity rise caused by self-crosslinking of the active precursor is prevented, and the viscosity of the precursor solution is controlled to be lower than 3 Pa.S, thereby being beneficial to improving the impregnation efficiency; specifically, the polymerization inhibitor can be one or more selected from ammonia water, copper hydroxide or ferric hydroxide; the diluting solvent can be one or more selected from ethanol, glycol or deionized water.
In the method for preparing the silicon carbide material by in-situ solidification of the precursor, the design scheme of the precursor solution components is mainly provided, the precursor is self-solidified in the precursor solution by regulating and controlling the precursor components and the proportion, and the phenomenon of uneven distribution of cracked carbon caused by directional flow of the precursor solution due to gravity after the precursor is taken out from the precursor solution in the traditional method is avoided.
S3: placing the porous silicon carbide preform in a precursor solution of carbon, and fully impregnating, as shown in fig. 4; specifically, the porous silicon carbide preform is obtained through additive manufacturing molding or gel injection molding; the time for the sufficient impregnation is 3 hours or more. The fully impregnating mode is selected from any one of vacuum impregnation, normal pressure impregnation, air pressure impregnation or mechanical pressurization impregnation.
S4: adding a curing agent into the precursor solution, wherein the mass fraction of the added curing agent is 1-10% based on the mass fraction of the active precursor as 100%; the curing agent is any one of acetic acid, phosphoric acid or oxalic acid; the mass ratio of the curing agent to the precursor solution is (1:100) - (10:100). Specifically, stirring is carried out for 2 minutes by adopting a spiral stirrer, the stirring speed is 140 revolutions per minute, and when the temperature of the solution rises to more than 35 ℃ from room temperature, the solidification process is started, and at the moment, the stirring head, the thermometer and the like are taken out.
In a specific embodiment, the mass ratio relationship among the active precursor, the polymerization inhibitor, the curing agent and the diluting solvent is (30% -70%): (1% -6%): (1% -10%): (17% -66%), the mass sum is 100%; with this preferred ratio, it is ensured that the precursor solution has a sufficiently low viscosity to meet the requirements for adequate impregnation of the preform, while having sufficient carbon for cracking of the preform.
S5: when the precursor solution is completely converted into solid from liquid, taking out the porous silicon carbide preform, and cleaning the porous silicon carbide preform; specifically, when the precursor solution is completely converted from a liquid state to a solid state, the curing is completed, and at the moment, the precursor organic matters are in a solid state without fluidity, so that the precursor in-situ curing is realized, as shown in fig. 5; the problem of cracking carbon distribution caused by the directional flow of liquid state due to gravity in the prior art can be avoided; specifically, the porous silicon carbide preform is cleaned, and a saw blade or a flat file can be used for cleaning cured organic matters on the surface of the porous silicon carbide preform.
S6: and (3) carbonizing the cleaned porous silicon carbide preform, wherein the active precursor is converted into cracking carbon in the porous silicon carbide preform, and the cracking carbon is uniformly distributed as shown in fig. 6, so as to prepare the silicon carbide material.
The invention also provides a silicon carbide material which is prepared by the method for preparing the silicon carbide material by in-situ curing of the precursor.
Further description will be provided below in connection with specific embodiments.
Example 1
1) Preparation of porous silicon carbide preform
And (3) forming a silicon carbide preform by gel casting, and performing high-temperature degreasing and glue discharging treatment on the preform to obtain the porous silicon carbide preform.
2) Preparation of carbon source precursor solution
a. The raw materials are prepared according to the following proportion:
furfuryl alcohol 50%; 3% of ammonia water; ethanol 40%; oxalic acid 7%; the above proportions are volume ratios, and the sum of the percentages is 100%. Sequentially adding ammonia water and furfuryl alcohol monomer into absolute ethyl alcohol, and fully stirring at room temperature to prepare a solution; wherein furfuryl alcohol is an active precursor, ammonia water is a polymerization inhibitor, ethanol is a diluent, and oxalic acid is a curing agent;
b. adding a porous silicon carbide preform, and soaking for 3 hours at room temperature;
c. adding the prepared oxalic acid, and standing for 0.5h. The carbon source precursor solution is fully impregnated in the porous silicon carbide preform and in-situ curing is completed.
3) And taking out the impregnated porous silicon carbide preform, and cleaning the surface-cured carbon source precursor.
4) Placing the solidified porous silicon carbide preform into a vacuum sintering furnace for carbonization treatment, wherein the sintering process is 1000 ℃ heat preservation treatment for 1h; obtaining the silicon carbide material with evenly distributed cracking carbon.
Example 2
Substantially the same as in example 1, except that:
step 1) preparation of porous silicon carbide preform
Preparing a porous silicon carbide preform by adopting an additive manufacturing process.
Step 2) preparing a carbon source precursor solution,
a. the raw materials are prepared according to the following proportion: furfuryl alcohol 45%; the method comprises the steps of carrying out a first treatment on the surface of the Ammonia 1%; ethanol 50%; oxalic acid 4%; the above proportions are volume ratios, and the sum of the percentages is 100%. Sequentially adding ammonia water and furfuryl alcohol monomer into absolute ethyl alcohol, and fully stirring at room temperature to prepare a solution;
b. adding a porous silicon carbide preform, and carrying out room-temperature dipping treatment for 3 hours;
c. adding the prepared oxalic acid, and standing for 0.5h; the carbon source precursor solution is fully impregnated in the porous silicon carbide preform and in-situ curing is completed.
Step 4), the sintering process is heat preservation treatment at 1000 ℃ for 2 hours; obtaining the silicon carbide material with evenly distributed cracking carbon.
Measurement of the Density of the porous silicon carbide preform produced by the present inventionThe degree, in particular to 5 sample strips along the thickness direction, and the measurement result shows that the density of the porous silicon carbide preform is 1.71+/-0.002 g/cm after the precursor dipping in-situ curing method is adopted 3 The density of the porous silicon carbide preform prepared by the traditional impregnation method is 1.67+/-0.03 g/cm 3 The porous silicon carbide preform prepared by the method has higher density, fully shows that the in-situ curing method improves the impregnation efficiency, and has small error, and shows that the preparation method improves the uniformity of the porous silicon carbide preform; and finally, the silicon carbide material with evenly distributed cracking carbon obtained by sintering has better performance.
While embodiments of the present invention have been illustrated and described above, it will be appreciated that the above described embodiments are illustrative and should not be construed as limiting the invention. Variations, modifications, alternatives and variations of the above-described embodiments may be made by those of ordinary skill in the art within the scope of the present invention.
The above embodiments of the present invention do not limit the scope of the present invention. Any other corresponding changes and modifications made in accordance with the technical idea of the present invention shall be included in the scope of the claims of the present invention.
Claims (10)
1. The method for preparing the silicon carbide material by in-situ curing of the precursor is characterized by comprising the following steps of:
s1, screening active precursors;
s2: preparing a precursor solution from the active precursor and a composite solvent, wherein the mass fraction of the precursor solution is 100%, and the mass fraction of the active precursor is more than 30%;
s3: placing the porous silicon carbide preform in a precursor solution of carbon, and fully soaking;
s4: adding a curing agent into the precursor solution, wherein the mass fraction of the added curing agent is 1-10% based on the mass fraction of the active precursor as 100%;
s5: when the precursor solution is completely converted into solid from liquid, taking out the porous silicon carbide preform, and cleaning the porous silicon carbide preform;
s6: and carbonizing the cleaned porous silicon carbide preform, and converting the active precursor into cracked carbon in the porous silicon carbide preform to prepare the silicon carbide material.
2. The method of preparing a silicon carbide material by in situ curing of a precursor according to claim 1, wherein the reactive precursor is selected from at least one of furfuryl alcohol containing an unsaturated bond, furfuryl ketone resin, and phenolic resin.
3. The method of preparing a silicon carbide material by in situ curing of a precursor according to claim 1, wherein the composite solvent comprises a polymerization inhibitor and a diluent solvent.
4. A method for preparing a silicon carbide material by in situ curing of a precursor according to claim 3, wherein the polymerization inhibitor is selected from one or more of ammonia water, copper hydroxide or ferric hydroxide;
the diluting solvent is selected from one or more of ethanol, glycol or deionized water.
5. A method for preparing a silicon carbide material by in situ curing of a precursor according to claim 3, wherein the mass ratio relationship among the active precursor, the polymerization inhibitor, the curing agent and the diluting solvent is (30% -70%): (1% -6%): (3% -7%): (17% -66%).
6. The method of preparing a silicon carbide material by in situ curing a precursor according to claim 1, wherein the time for sufficient impregnation is 3 hours or more.
7. The method of preparing a silicon carbide material by in situ curing of a precursor according to claim 6, wherein the substantially impregnating means is selected from any one of vacuum impregnation, atmospheric impregnation, pneumatic impregnation or mechanical pressurization impregnation.
8. The method for preparing silicon carbide material by in situ curing of a precursor according to claim 1, wherein the curing agent is selected from any one of acetic acid, phosphoric acid or oxalic acid; the mass ratio of the curing agent to the precursor solution is (1:100) - (10:100).
9. The method of preparing a silicon carbide material by in situ curing of a precursor according to claim 1, wherein the porous silicon carbide preform is obtained by additive manufacturing molding or gel casting.
10. A silicon carbide material, characterized in that the silicon carbide material is prepared by the method for preparing the silicon carbide material by in-situ curing the precursor according to any one of claims 1 to 9.
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| CN202311848170.0A CN117800763A (en) | 2023-12-29 | 2023-12-29 | Method for preparing silicon carbide material by in-situ solidification of precursor and silicon carbide material |
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