CN113788683A - Preparation method of SiC ceramic powder - Google Patents
Preparation method of SiC ceramic powder Download PDFInfo
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- CN113788683A CN113788683A CN202111155379.XA CN202111155379A CN113788683A CN 113788683 A CN113788683 A CN 113788683A CN 202111155379 A CN202111155379 A CN 202111155379A CN 113788683 A CN113788683 A CN 113788683A
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- 239000000843 powder Substances 0.000 title claims abstract description 57
- 239000000919 ceramic Substances 0.000 title claims abstract description 40
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims abstract description 129
- 229910010271 silicon carbide Inorganic materials 0.000 claims abstract description 126
- 239000002245 particle Substances 0.000 claims abstract description 35
- 238000003756 stirring Methods 0.000 claims abstract description 35
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 29
- 239000002202 Polyethylene glycol Substances 0.000 claims abstract description 25
- 229920001223 polyethylene glycol Polymers 0.000 claims abstract description 25
- 238000001035 drying Methods 0.000 claims abstract description 12
- 238000010438 heat treatment Methods 0.000 claims abstract description 12
- 238000005245 sintering Methods 0.000 claims abstract description 12
- 239000011259 mixed solution Substances 0.000 claims abstract description 9
- 238000001816 cooling Methods 0.000 claims abstract description 5
- 238000002156 mixing Methods 0.000 claims abstract description 5
- 238000007789 sealing Methods 0.000 claims abstract description 5
- 239000000203 mixture Substances 0.000 claims description 16
- 239000011812 mixed powder Substances 0.000 claims description 14
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 12
- 239000008187 granular material Substances 0.000 claims description 10
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 8
- 239000007864 aqueous solution Substances 0.000 claims description 8
- 238000000034 method Methods 0.000 claims description 8
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 4
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 4
- 229960000583 acetic acid Drugs 0.000 claims description 4
- 150000001875 compounds Chemical class 0.000 claims description 4
- 235000019441 ethanol Nutrition 0.000 claims description 4
- 239000012362 glacial acetic acid Substances 0.000 claims description 4
- 238000005469 granulation Methods 0.000 claims description 4
- 230000003179 granulation Effects 0.000 claims description 4
- 238000003760 magnetic stirring Methods 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 claims description 4
- 239000002105 nanoparticle Substances 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- 238000005303 weighing Methods 0.000 claims description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 2
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 claims description 2
- 229910052786 argon Inorganic materials 0.000 claims description 2
- 229910052799 carbon Inorganic materials 0.000 claims description 2
- 238000005260 corrosion Methods 0.000 claims description 2
- 230000007797 corrosion Effects 0.000 claims description 2
- 230000007123 defense Effects 0.000 claims description 2
- 239000008103 glucose Substances 0.000 claims description 2
- 229910052757 nitrogen Inorganic materials 0.000 claims description 2
- 229940093429 polyethylene glycol 6000 Drugs 0.000 claims description 2
- 239000007795 chemical reaction product Substances 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 5
- 229910052681 coesite Inorganic materials 0.000 abstract description 4
- 229910052906 cristobalite Inorganic materials 0.000 abstract description 4
- 239000000377 silicon dioxide Substances 0.000 abstract description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 abstract description 4
- 229910052682 stishovite Inorganic materials 0.000 abstract description 4
- 229910052905 tridymite Inorganic materials 0.000 abstract description 4
- 239000007769 metal material Substances 0.000 abstract description 2
- 239000002114 nanocomposite Substances 0.000 abstract description 2
- 239000000243 solution Substances 0.000 abstract description 2
- 239000002699 waste material Substances 0.000 abstract description 2
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 abstract 1
- 239000000654 additive Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 229910010293 ceramic material Inorganic materials 0.000 description 2
- 238000000465 moulding Methods 0.000 description 2
- 238000007796 conventional method Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
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- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/56—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides
- C04B35/565—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on silicon carbide
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- C—CHEMISTRY; METALLURGY
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- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/62605—Treating the starting powders individually or as mixtures
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/50—Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
- C04B2235/54—Particle size related information
- C04B2235/5418—Particle size related information expressed by the size of the particles or aggregates thereof
- C04B2235/5436—Particle size related information expressed by the size of the particles or aggregates thereof micrometer sized, i.e. from 1 to 100 micron
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/50—Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
- C04B2235/54—Particle size related information
- C04B2235/5418—Particle size related information expressed by the size of the particles or aggregates thereof
- C04B2235/5445—Particle size related information expressed by the size of the particles or aggregates thereof submicron sized, i.e. from 0,1 to 1 micron
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Abstract
The invention provides a preparation method of SiC ceramic powder, belonging to the field of inorganic non-metallic materials and nano composite materials. The preparation method comprises the following steps: adding silicon carbide micro powder into an ethanol water solution, and ultrasonically stirring for 1-2 hours; preparing SiO in the mixed solution2Sol and drying to obtain nanometer coated silicon carbide particles; adding polyethylene glycol 10000 into absolute ethyl alcohol, ultrasonically stirring for 0.5-1 h, adding the treated silicon carbide particles, magnetically stirring for 1-2 h, drying, adding PVA, uniformly mixing, sealing, standing, granulating, drying, performing heat treatment on the SiC particles at 1200-1500 ℃ for 2-3 h in vacuum, cooling to room temperature, and performing non-pressure heat treatment at 500-600 ℃ for 2-3 h to obtain the SiC ceramic powder with reconstructed particle size. The invention adds SiO2The sintering temperature is greatly reduced by adopting the sol and polyethylene glycol 10000 modes, the ceramic powder after granularity reconstruction has high purity and excellent service performance, and the waste is well solvedThe problem of utilizing silicon carbide powder in the aspect of ceramics is solved.
Description
Technical Field
The invention belongs to the field of inorganic non-metallic materials and nano composite materials, and particularly relates to a preparation method of SiC ceramic powder.
Background
Silicon carbide ceramic as a novel structural ceramic material has properties incomparable with structural materials such as a plurality of metals and the like: the high-temperature-resistant high-strength wear-resistant high-temperature-resistant high-hardness high-wear-resistant high-corrosion-resistance high-hardness high-wear-resistant high-corrosion-resistance high-hardness high-creep-resistance high-wear-resistance high-corrosion-resistance high-hardness high-creep-resistance high-wear-resistance high-corrosion-resistance high-wear-resistance high-hardness high-wear-resistance high-corrosion-resistance high-hardness high-creep-resistance high-wear-resistance high-corrosion-resistance high-hardness high-creep-resistance high-toughness high-creep-resistance high-corrosion-resistance high-hardness high-resistance high-creep-resistance high-corrosion-resistance high-hardness high-resistance high-wear-resistance high-hardness high-resistance high-creep-resistance high-corrosion-resistance high-hardness high-creep-corrosion-resistance high-hardness high-corrosion-resistance high-wear-resistance high-hardness high-corrosion-resistance high-hardness high-resistance high-creep-resistance high-hardness high-creep-hardness high-resistance creep-wear-resistance high-hardness high-resistance high-hardness high-resistance creep-resistance high-creep-resistance high-hardness high-resistance high-hardness high-wear-resistance high-toughness high-resistance high-hardness high-resistance high-hardness high-.
The grain size of silicon carbide has a very important influence on its own applications. The application of silicon carbide in ceramics is common, the silicon carbide ceramics has good performance but is difficult to sinter and densify, and if the granularity of the silicon carbide micro powder used in the preparation of the ceramics is small, the silicon carbide micro powder is not beneficial to molding and the usability of the sintered product is not good. In the preparation process of silicon carbide, a plurality of superfine silicon carbide micro-powders are often generated, and the silicon carbide micro-powders cannot be effectively utilized due to the excessively fine particle size, so that the production cost is increased and certain environmental pollution is caused. The silicon carbide powder with ultra-fine granularity can meet the basic granularity requirement of the ceramic material through granularity reconstruction, thereby more effectively utilizing resources and reducing production cost.
Disclosure of Invention
In order to solve the problems in the production and application of silicon carbide, the invention uses SiO2The sol, the polyethylene glycol and the PVA are used as additives, and the preparation method of the SiC ceramic powder is provided.
Specifically, the preparation method of the SiC ceramic powder provided by the invention is implemented according to the following steps:
s1: weighing a certain amount of silicon carbide micro powder, adding the silicon carbide micro powder in S2 into an ethanol aqueous solution under the condition of ultrasonic stirring, continuously stirring for 1-2 hours until the silicon carbide micro powder is fully dispersed, wherein the volume ratio of absolute ethanol to water in the absolute ethanol aqueous solution is 1-3: 1, taking the mass ratio of the volume of the absolute ethyl alcohol to the silicon carbide micro powder as 0.2-1 ml: 1g of a compound;
s2: preparing nano-coated silicon carbide particles;
s21: adding tetraethoxysilane into the SiC mixed solution of S1 under the condition of ultrasonic stirring, wherein SiO contained in the tetraethoxysilane2The mass ratio of the amount of the silicon carbide to the silicon carbide in S1 is 3-10%, continuously stirring, adding glacial acetic acid to adjust the pH value to 1-3, fully reacting for 2-6 h, and drying at 80-120 ℃ for 4-8 h to obtain nano-coated silicon carbide particles;
s3: adding polyethylene glycol 10000 into 10-15 ml of absolute ethyl alcohol under the condition of ultrasonic stirring, wherein the molar ratio of the C content in the polyethylene glycol 10000 to the Si content in ethyl orthosilicate in S21 is 1.2-2, and continuously stirring for 0.5-1 h until the mixture is fully dispersed;
s4, adding the silicon carbide particles coated with the nano particles in the S21 into a mixed solution of S3 polyethylene glycol 10000 under the condition of magnetic stirring, continuously and magnetically stirring for 1-2 hours until the silicon carbide particles are fully dispersed, and drying the mixture for 3-5 hours at 100-150 ℃ to obtain silicon carbide mixed powder;
s5: adding PVA into the silicon carbide mixed powder of S4, wherein the mass percentage of the PVA to the silicon carbide mixed powder of S4 is 3-5%, mechanically stirring for 1-2 h, sealing and standing for 5-10 h after uniform mixing to obtain a SiC micropowder mixture;
s6: pouring the uniformly mixed powder in the S5 into a granulator for granulation to obtain SiC granules with uniform size and granularity ranging from 10 to 200 mu m, and drying the SiC granules at the temperature of 90 to 100 ℃ for 1 to 2 hours to obtain SiC granules with proper humidity;
s7: and (3) putting the silicon carbide particles treated in the step (S6) into a high-temperature vacuum atmosphere furnace for sintering, carrying out heat treatment for 2-3 h at 1300-1500 ℃, cooling to room temperature, putting into a muffle furnace for carrying out heat treatment for 2-3 h at 500-600 ℃, and then obtaining SiC ceramic powder with reconstructed particle size.
Preferably, the particle size of the SiC micropowder used in S1 is 0.5-3 μm.
Preferably, SiO contained in the tetraethoxysilane used in S212The mass ratio of the amount of the silicon carbide to the silicon carbide in the S1 is 3% -10%.
Preferably, the molar ratio of the content of C in polyethylene glycol 10000 used in S3 to the content of Si in tetraethoxysilane used in S21 is 1.2-2, and the organic carbon source polyethylene glycol 10000 can be replaced by polyethylene glycol 2000, polyethylene glycol 6000, polyethylene glycol 20000, glucose and the like.
Preferably, the sintering temperature of the SiC particles in S7 is 1300-1500 ℃, and the sintering atmosphere can be vacuum argon protection and vacuum nitrogen protection; the temperature of the secondary heat treatment is 500-600 ℃.
The silicon carbide ceramic powder with reconstructed granularity prepared by the method has high purity, low porosity and excellent use performance.
The silicon carbide ceramic powder with the reconstructed granularity prepared by the method is widely applied, in particular to the application in the fields of high-temperature corrosion resistance, national defense and military industry, special ceramics and the like.
The technical scheme of the invention has the following beneficial effects:
the invention firstly provides a preparation method of SiC ceramic powder, which utilizes polyethylene glycol 10000 and SiO2The sol and PVA are used as additives, and the problem that the silicon carbide micro powder cannot be utilized due to the excessively fine granularity is solved. Nano SiO2The addition of the sol and the polyethylene glycol 10000 reduces the sintering temperature, and the ceramic powder after particle size reconstruction has high purity, low porosity and excellent service performance, thereby well solving the problem of recycling the waste silicon carbide powder in the aspect of ceramics. The preparation method of the SiC ceramic powder provided by the invention can be well applied to other types of ceramic micro powder, and has good practicability.
Detailed Description
The present invention is further described with reference to the following specific examples, which should be construed by those skilled in the art as being illustrative and not limiting.
All technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art. In the following examples, unless otherwise specified, the methods used were all conventional methods, and the starting materials used were all commercially available analytical pure materials. Without limiting the invention thereto, one skilled in the art can, in light of the present disclosure and knowledge of the prior art, use similar methods, apparatus, materials to practice the invention repeatedly.
The following specifically exemplifies the technical solution of the present invention.
Example 1
A preparation method of SiC ceramic powder comprises the following specific steps:
s1: weighing 30g of silicon carbide micro powder, adding the silicon carbide micro powder in S2 into 30ml of ethanol aqueous solution under the condition of ultrasonic stirring, and continuously stirring for 2h until the silicon carbide micro powder is fully dispersed, wherein the volume ratio of absolute ethanol to water in the absolute ethanol aqueous solution is 1.5: 1, taking the mass ratio of the volume of the absolute ethyl alcohol to the silicon carbide micro powder as 1 ml: 1g of a compound;
s2: preparing nano-coated silicon carbide particles;
s21: adding tetraethoxysilane into the SiC mixed solution of S1 under the condition of ultrasonic stirring, wherein SiO contained in the tetraethoxysilane2The mass ratio of the amount of the silicon carbide to the silicon carbide in S1 is 5%, the stirring is continued, glacial acetic acid is added to adjust the PH value to 2, the mixture is fully reacted for 6 hours, and the mixture is dried for 8 hours at 80 ℃ to obtain nano-coated silicon carbide particles;
s3: adding polyethylene glycol 10000 into 15ml of absolute ethyl alcohol under the condition of ultrasonic stirring, wherein the molar ratio of the C content in the polyethylene glycol 10000 to the Si content in the tetraethoxysilane in S21 is 1.5, and continuously stirring for 1h until the mixture is fully dispersed;
s4, adding the silicon carbide particles coated with the nano particles in the S21 into a mixed solution of S3 polyethylene glycol 10000 under the condition of magnetic stirring, continuously and magnetically stirring for 2 hours until the silicon carbide particles are fully dispersed, and drying the mixture for 5 hours at 100 ℃ to obtain silicon carbide mixed powder;
s5: adding PVA into the silicon carbide mixed powder of S4, wherein the mass percentage of the PVA to the silicon carbide mixed powder of S4 is 5%, mechanically stirring for 1h, uniformly mixing, sealing and standing for 10h to obtain a SiC micro powder mixture;
s6: pouring the powder uniformly mixed in the S5 into a granulator for granulation to obtain SiC granules with uniform size and granularity of 15 mu m, and drying at 90 ℃ for 1h to obtain SiC granules with proper humidity;
s7: and (3) putting the silicon carbide particles treated in the step (S6) into a high-temperature vacuum atmosphere furnace for sintering, carrying out heat treatment for 3h at 1450 ℃, cooling to room temperature, putting into a muffle furnace for carrying out heat treatment for 2h at 500 ℃, and then obtaining SiC ceramic powder with reconstructed particle size.
Example 2
A preparation method of SiC ceramic powder comprises the following specific steps:
s1: weighing 30g of silicon carbide micro powder, adding the silicon carbide micro powder in S2 into 20ml of ethanol aqueous solution under the condition of ultrasonic stirring, and continuously stirring for 2h until the silicon carbide micro powder is fully dispersed, wherein the volume ratio of absolute ethanol to water in the absolute ethanol aqueous solution is 2: 1, taking the mass ratio of the volume of the absolute ethyl alcohol to the silicon carbide micro powder as 1 ml: 1g of a compound;
s2: preparing nano-coated silicon carbide particles;
s21: adding tetraethoxysilane into the SiC mixed solution of S1 under the condition of ultrasonic stirring, wherein SiO contained in the tetraethoxysilane2The mass ratio of the amount of the silicon carbide to the silicon carbide in S1 is 7%, the stirring is continued, glacial acetic acid is added to adjust the PH value to 3, the mixture is dried for 8 hours at 80 ℃ after the full reaction for 6 hours, and the nano-coated silicon carbide particles are obtained;
s3: adding polyethylene glycol 10000 into 15ml of absolute ethyl alcohol under the condition of ultrasonic stirring, wherein the molar ratio of the C content in the polyethylene glycol 10000 to the Si content in the tetraethoxysilane in S21 is 1.5, and continuously stirring for 1h until the mixture is fully dispersed;
s4, adding the silicon carbide particles coated with the nano particles in the S21 into a mixed solution of S3 polyethylene glycol 10000 under the condition of magnetic stirring, continuously and magnetically stirring for 1h until the silicon carbide particles are fully dispersed, and drying the mixture for 5h at 100 ℃ to obtain silicon carbide mixed powder;
s5: adding PVA into the silicon carbide mixed powder of S4, wherein the mass percentage of the PVA to the silicon carbide mixed powder of S4 is 5%, mechanically stirring for 1h, uniformly mixing, sealing and standing for 10h to obtain a SiC micro powder mixture;
s6: pouring the powder uniformly mixed in the S5 into a granulator for granulation to obtain SiC granules with uniform size and granularity of 20 mu m, and drying at 90 ℃ for 1h to obtain SiC granules with proper humidity;
s7: and (3) putting the silicon carbide particles treated in the step (S6) into a high-temperature vacuum atmosphere furnace for sintering, carrying out heat treatment for 3h at 1450 ℃, cooling to room temperature, putting into a muffle furnace for carrying out heat treatment for 2h at 500 ℃, and then obtaining SiC ceramic powder with reconstructed particle size.
The SiC ceramic powder prepared in the embodiment 1 and the embodiment 2 has the advantages of stable process, reliable quality and excellent performance. For example, SiC ceramic is prepared by selecting SiC particles with the particle sizes of 15 μm and 20 μm prepared in the example 1 and the example 2, and compared with SiC ceramic prepared by SiC powder with the same particle size in the market, the sintering temperature is low; the sintering temperature of the SiC ceramics prepared in the embodiment 1 and the embodiment 2 is respectively reduced by 50 ℃ and 40 ℃, and the strength is respectively improved by 2 percent and 3 percent; the ceramic powder prepared by the invention has good molding fluidity and higher density.
The above-mentioned embodiments are merely preferred embodiments for fully illustrating the present invention, and the scope of protection is not limited thereto. The equivalents and modifications of the present invention which may occur to those skilled in the art are within the scope of the present invention as defined by the appended claims.
Claims (7)
1. The preparation method of the SiC ceramic powder is characterized by comprising the following specific implementation steps:
s1: weighing a certain amount of silicon carbide micro powder, adding the silicon carbide micro powder in S2 into an ethanol aqueous solution under the condition of ultrasonic stirring, continuously stirring for 1-2 hours until the silicon carbide micro powder is fully dispersed, wherein the volume ratio of absolute ethanol to water in the absolute ethanol aqueous solution is 1-3: 1, taking the mass ratio of the volume of the absolute ethyl alcohol to the silicon carbide micro powder as 0.2-1 ml: 1g of a compound;
s2: preparing nano-coated silicon carbide particles;
s21: adding tetraethoxysilane into the SiC mixed solution of S1 under the condition of ultrasonic stirring, wherein SiO contained in the tetraethoxysilane2The mass ratio of the amount of the silicon carbide to the amount of the silicon carbide in S1 is 3-10%, the stirring is continued, glacial acetic acid is added to adjust the pH value to 1-3, the mixture is fully reacted for 2-6 h, and the reaction product is dried for 4-8 h at 80-120 ℃ to obtain nano-coated silicon carbide particlesGranulating;
s3: adding polyethylene glycol 10000 into 10-15 ml of absolute ethyl alcohol under the condition of ultrasonic stirring, wherein the molar ratio of the C content in the polyethylene glycol 10000 to the Si content in ethyl orthosilicate in S21 is 1.2-2, and continuously stirring for 0.5-1 h until the mixture is fully dispersed;
s4, adding the silicon carbide particles coated with the nano particles in the S21 into a mixed solution of S3 polyethylene glycol 10000 under the condition of magnetic stirring, continuously and magnetically stirring for 1-2 hours until the silicon carbide particles are fully dispersed, and drying the mixture for 3-5 hours at 100-150 ℃ to obtain silicon carbide mixed powder;
s5: adding PVA into the silicon carbide mixed powder of S4, wherein the mass percentage of the PVA to the silicon carbide mixed powder of S4 is 3-5%, mechanically stirring for 1-2 h, sealing and standing for 5-10 h after uniform mixing to obtain a SiC micropowder mixture;
s6: pouring the uniformly mixed powder in the S5 into a granulator for granulation to obtain SiC granules with uniform size and granularity ranging from 10 to 200 mu m, and drying the SiC granules at the temperature of 90 to 100 ℃ for 1 to 2 hours to obtain SiC granules with proper humidity;
s7: and (3) putting the silicon carbide particles treated in the step (S6) into a high-temperature vacuum atmosphere furnace for sintering, carrying out heat treatment for 2-3 h at 1300-1500 ℃, cooling to room temperature, putting into a muffle furnace for carrying out heat treatment for 2-3 h at 500-600 ℃, and then obtaining SiC ceramic powder with reconstructed particle size.
2. The method for preparing SiC ceramic powder according to claim 1, wherein the SiC fine powder used in S1 has a particle size of 0.5 to 3 μm.
3. The method for producing SiC ceramic powder according to claim 1, wherein SiO contained in tetraethoxysilane used in S212The mass ratio of the amount of the silicon carbide to the silicon carbide in the S1 is 3% -10%.
4. The method for preparing SiC ceramic powder according to claim 1, wherein the molar ratio of the C content of polyethylene glycol 10000 used in S3 to the Si content of tetraethoxysilane used in S21 is 1.2-2, and the organic carbon source polyethylene glycol 10000 can be replaced by polyethylene glycol 2000, polyethylene glycol 6000, polyethylene glycol 20000, glucose and the like.
5. The preparation method of the SiC ceramic powder according to claim 1, wherein the sintering temperature of the SiC particles in S7 is 1300-1500 ℃, and the sintering atmosphere can be vacuum argon protection or vacuum nitrogen protection; the temperature of the secondary heat treatment is 500-600 ℃.
6. A SiC ceramic powder characterized by being produced by the method according to any one of claims 1 to 5.
7. The SiC ceramic powder of claim 6, which can be used in the fields of high temperature corrosion resistance, national defense and military industry, special ceramics, etc.
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| CN113912399A (en) * | 2021-12-15 | 2022-01-11 | 山东金鸿新材料股份有限公司 | Preparation method of high-density pressureless sintered silicon carbide ceramic |
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| CN113912399A (en) * | 2021-12-15 | 2022-01-11 | 山东金鸿新材料股份有限公司 | Preparation method of high-density pressureless sintered silicon carbide ceramic |
| CN113912399B (en) * | 2021-12-15 | 2022-02-25 | 山东金鸿新材料股份有限公司 | Preparation method of high-density pressureless sintered silicon carbide ceramic |
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