CN118479898A - Method for preparing silicon carbide ceramic by pressureless sintering - Google Patents
Method for preparing silicon carbide ceramic by pressureless sintering Download PDFInfo
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- CN118479898A CN118479898A CN202410946779.XA CN202410946779A CN118479898A CN 118479898 A CN118479898 A CN 118479898A CN 202410946779 A CN202410946779 A CN 202410946779A CN 118479898 A CN118479898 A CN 118479898A
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- Prior art keywords
- silicon carbide
- stirring
- solution
- coated particles
- placing
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- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 title claims abstract description 144
- 229910010271 silicon carbide Inorganic materials 0.000 title claims abstract description 138
- 239000000919 ceramic Substances 0.000 title claims abstract description 47
- 238000000034 method Methods 0.000 title claims abstract description 22
- 238000001272 pressureless sintering Methods 0.000 title claims abstract description 20
- 239000002245 particle Substances 0.000 claims abstract description 106
- 238000003756 stirring Methods 0.000 claims abstract description 99
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 81
- 229920000049 Carbon (fiber) Polymers 0.000 claims abstract description 53
- 239000004917 carbon fiber Substances 0.000 claims abstract description 53
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims abstract description 39
- 238000001035 drying Methods 0.000 claims abstract description 37
- 238000005406 washing Methods 0.000 claims abstract description 32
- 238000010438 heat treatment Methods 0.000 claims abstract description 31
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims abstract description 26
- 238000012986 modification Methods 0.000 claims abstract description 26
- 230000004048 modification Effects 0.000 claims abstract description 26
- 239000002002 slurry Substances 0.000 claims abstract description 24
- 238000006243 chemical reaction Methods 0.000 claims abstract description 18
- 238000005245 sintering Methods 0.000 claims abstract description 14
- 238000000576 coating method Methods 0.000 claims abstract description 13
- 229920001661 Chitosan Polymers 0.000 claims abstract description 12
- 239000011248 coating agent Substances 0.000 claims abstract description 12
- 238000002360 preparation method Methods 0.000 claims abstract description 11
- BRLQWZUYTZBJKN-UHFFFAOYSA-N Epichlorohydrin Chemical compound ClCC1CO1 BRLQWZUYTZBJKN-UHFFFAOYSA-N 0.000 claims abstract description 7
- 238000005576 amination reaction Methods 0.000 claims abstract description 5
- 238000000465 moulding Methods 0.000 claims abstract description 4
- 239000000243 solution Substances 0.000 claims description 121
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 88
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 62
- 235000019441 ethanol Nutrition 0.000 claims description 27
- 238000000498 ball milling Methods 0.000 claims description 25
- 239000008367 deionised water Substances 0.000 claims description 25
- 229910021641 deionized water Inorganic materials 0.000 claims description 25
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 25
- 239000011259 mixed solution Substances 0.000 claims description 24
- 239000002253 acid Substances 0.000 claims description 22
- 238000001914 filtration Methods 0.000 claims description 20
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 15
- 229910017604 nitric acid Inorganic materials 0.000 claims description 15
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 15
- VBICKXHEKHSIBG-UHFFFAOYSA-N 1-monostearoylglycerol Chemical compound CCCCCCCCCCCCCCCCCC(=O)OCC(O)CO VBICKXHEKHSIBG-UHFFFAOYSA-N 0.000 claims description 14
- 238000002791 soaking Methods 0.000 claims description 14
- VILCJCGEZXAXTO-UHFFFAOYSA-N 2,2,2-tetramine Chemical compound NCCNCCNCCN VILCJCGEZXAXTO-UHFFFAOYSA-N 0.000 claims description 12
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 12
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 12
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 claims description 12
- 229960001124 trientine Drugs 0.000 claims description 12
- 238000001354 calcination Methods 0.000 claims description 11
- 238000009210 therapy by ultrasound Methods 0.000 claims description 11
- 238000001132 ultrasonic dispersion Methods 0.000 claims description 11
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 10
- 239000007921 spray Substances 0.000 claims description 10
- 238000009777 vacuum freeze-drying Methods 0.000 claims description 10
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 claims description 9
- 235000014113 dietary fatty acids Nutrition 0.000 claims description 9
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- 229930195729 fatty acid Natural products 0.000 claims description 9
- 150000004665 fatty acids Chemical class 0.000 claims description 9
- 239000005011 phenolic resin Substances 0.000 claims description 9
- 229920001568 phenolic resin Polymers 0.000 claims description 9
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 9
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 9
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 9
- QOSSAOTZNIDXMA-UHFFFAOYSA-N Dicylcohexylcarbodiimide Chemical compound C1CCCCC1N=C=NC1CCCCC1 QOSSAOTZNIDXMA-UHFFFAOYSA-N 0.000 claims description 7
- 235000021355 Stearic acid Nutrition 0.000 claims description 7
- FEWJPZIEWOKRBE-UHFFFAOYSA-N Tartaric acid Natural products [H+].[H+].[O-]C(=O)C(O)C(O)C([O-])=O FEWJPZIEWOKRBE-UHFFFAOYSA-N 0.000 claims description 7
- YDEXUEFDPVHGHE-GGMCWBHBSA-L disodium;(2r)-3-(2-hydroxy-3-methoxyphenyl)-2-[2-methoxy-4-(3-sulfonatopropyl)phenoxy]propane-1-sulfonate Chemical compound [Na+].[Na+].COC1=CC=CC(C[C@H](CS([O-])(=O)=O)OC=2C(=CC(CCCS([O-])(=O)=O)=CC=2)OC)=C1O YDEXUEFDPVHGHE-GGMCWBHBSA-L 0.000 claims description 7
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 claims description 7
- 229940075507 glyceryl monostearate Drugs 0.000 claims description 7
- 239000001788 mono and diglycerides of fatty acids Substances 0.000 claims description 7
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims description 7
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 claims description 7
- 229940057847 polyethylene glycol 600 Drugs 0.000 claims description 7
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 claims description 7
- PNGBYKXZVCIZRN-UHFFFAOYSA-M sodium;hexadecane-1-sulfonate Chemical compound [Na+].CCCCCCCCCCCCCCCCS([O-])(=O)=O PNGBYKXZVCIZRN-UHFFFAOYSA-M 0.000 claims description 7
- 239000008117 stearic acid Substances 0.000 claims description 7
- 235000002906 tartaric acid Nutrition 0.000 claims description 7
- 239000011975 tartaric acid Substances 0.000 claims description 7
- 239000000203 mixture Substances 0.000 claims description 6
- 229910000831 Steel Inorganic materials 0.000 claims description 5
- -1 carbon fiber amide Chemical class 0.000 claims description 5
- 235000019864 coconut oil Nutrition 0.000 claims description 5
- 239000003240 coconut oil Substances 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 5
- 238000005469 granulation Methods 0.000 claims description 5
- 230000003179 granulation Effects 0.000 claims description 5
- 239000000463 material Substances 0.000 claims description 5
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 5
- 238000010992 reflux Methods 0.000 claims description 5
- 239000010959 steel Substances 0.000 claims description 5
- 235000013162 Cocos nucifera Nutrition 0.000 claims description 4
- 244000060011 Cocos nucifera Species 0.000 claims description 4
- 238000002386 leaching Methods 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 3
- FEWJPZIEWOKRBE-JCYAYHJZSA-N Dextrotartaric acid Chemical compound OC(=O)[C@H](O)[C@@H](O)C(O)=O FEWJPZIEWOKRBE-JCYAYHJZSA-N 0.000 claims description 2
- 150000001721 carbon Chemical class 0.000 claims 1
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 claims 1
- 238000005452 bending Methods 0.000 abstract description 11
- 238000006735 epoxidation reaction Methods 0.000 abstract description 4
- 230000014759 maintenance of location Effects 0.000 abstract description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 24
- 239000000377 silicon dioxide Substances 0.000 description 12
- 235000012239 silicon dioxide Nutrition 0.000 description 12
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 9
- 229910010293 ceramic material Inorganic materials 0.000 description 7
- 230000000052 comparative effect Effects 0.000 description 7
- 125000003277 amino group Chemical group 0.000 description 6
- 239000000835 fiber Substances 0.000 description 6
- 239000002131 composite material Substances 0.000 description 5
- 229910021389 graphene Inorganic materials 0.000 description 5
- 230000003014 reinforcing effect Effects 0.000 description 5
- 230000002776 aggregation Effects 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 239000011159 matrix material Substances 0.000 description 4
- 238000004321 preservation Methods 0.000 description 4
- 238000007493 shaping process Methods 0.000 description 4
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 2
- 230000004913 activation Effects 0.000 description 2
- 238000005054 agglomeration Methods 0.000 description 2
- 238000004220 aggregation Methods 0.000 description 2
- 239000012752 auxiliary agent Substances 0.000 description 2
- 238000000151 deposition Methods 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 125000003700 epoxy group Chemical group 0.000 description 2
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 2
- 230000003335 steric effect Effects 0.000 description 2
- LRWZZZWJMFNZIK-UHFFFAOYSA-N 2-chloro-3-methyloxirane Chemical compound CC1OC1Cl LRWZZZWJMFNZIK-UHFFFAOYSA-N 0.000 description 1
- 229920000663 Hydroxyethyl cellulose Polymers 0.000 description 1
- 239000004354 Hydroxyethyl cellulose Substances 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 229920002125 Sokalan® Polymers 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910000019 calcium carbonate Inorganic materials 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000002041 carbon nanotube Substances 0.000 description 1
- 229910021393 carbon nanotube Inorganic materials 0.000 description 1
- 238000005234 chemical deposition Methods 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000001723 curing Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 235000019447 hydroxyethyl cellulose Nutrition 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000004377 microelectronic Methods 0.000 description 1
- 238000005065 mining Methods 0.000 description 1
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- 238000011160 research Methods 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 239000011863 silicon-based powder Substances 0.000 description 1
- 230000000087 stabilizing effect Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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- 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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Abstract
The invention provides a method for preparing silicon carbide ceramics by pressureless sintering, which belongs to the technical field of silicon carbide ceramics; the method comprises the steps of pretreatment of silicon carbide, coating, modification of coated particles, amination of carbon fibers, preparation of slurry, molding and sintering; the secondary modification is carried out, the primary modified coated particles are placed in an acetone solution, after being stirred uniformly, epichlorohydrin and a sodium hydroxide solution are added for stirring reaction, and the epoxidized coated particles are prepared after washing and drying; introducing acetic acid solution into a closed container, then adding chitosan, stirring for 1.8-2.2h, adding the epoxidation coated particles after stirring, heating to 60-64 ℃ after stirring uniformly, stirring for 3.4-3.6h, washing and drying to obtain secondary modified coated particles; the silicon carbide ceramic prepared by the method has high fracture toughness and strength, and has high retention rate of toughness and bending strength after low-temperature treatment.
Description
Technical Field
The invention belongs to the technical field of silicon carbide ceramics, and particularly relates to a method for preparing silicon carbide ceramics by pressureless sintering.
Background
The silicon carbide ceramic is ceramic taking silicon carbide as a main component, has good normal-temperature mechanical properties such as bending strength, corrosion resistance, wear resistance and the like, is optimal in the known ceramic materials, and has wide application in the fields of petroleum, chemical industry, microelectronics, automobiles, aerospace, mining industry and laser.
However, silicon carbide ceramics have large brittleness, low fracture toughness, strong crack strength sensitivity and poor sintering performance, and limit the application and development of the silicon carbide ceramics.
At present, in order to improve fracture toughness and sintering performance, carbon fiber, alumina fiber and the like are generally adopted as reinforcing phases to prepare complex-phase ceramic taking silicon carbide as a matrix, but the fiber has poor wettability, low reaction activity and poor interface performance with the silicon carbide matrix, and poor compatibility, and finally the wear resistance and the bending resistance of the silicon carbide ceramic are influenced;
Therefore, modifying the fiber to improve the wettability and reactivity of the fiber, so as to improve the interface performance with the silicon carbide matrix, and enhancing the comprehensive performance of the silicon carbide ceramic becomes a new research direction.
In this regard, the prior art discloses the following methods:
CN113698221a discloses a preparation method of a modified carbon fiber toughened silicon carbide ceramic material and a modified carbon fiber toughened silicon carbide ceramic material, specifically discloses a preparation method of a modified carbon fiber toughened silicon carbide ceramic material, which comprises the steps of firstly grafting graphene oxide on the surface of a carbon fiber, then depositing alumina on the surface of the graphene oxide modified carbon fiber to form a graphene oxide modified carbon fiber coated with alumina, finally depositing a silicon carbide layer on the surface of the graphene oxide modified carbon fiber by a chemical deposition method to prepare a modified carbon fiber, mixing the modified carbon fiber with silicon carbide powder, a sintering aid, phenolic resin, graphite powder and deionized water, and performing dry press molding, curing and calcination to prepare the modified carbon fiber toughened silicon carbide ceramic material;
The patent improves the oxidation resistance of the carbon fiber, thereby improving the toughness and the bending strength of the silicon carbide ceramic material, but the ceramic material prepared by the patent has poor stability, and has more loss of toughness and bending strength after low-temperature treatment, and seriously affects the service performance.
CN118047621a discloses a fiber reinforced silicon carbide composite material and a preparation method thereof, and specifically discloses a raw material composition comprising modified silicon carbide powder, silicon powder, modified carbon fiber, phenolic resin, graphite powder, stabilizing auxiliary agent and sintering auxiliary agent; wherein, the modified silicon carbide powder is prepared by coating and modifying the surface of the silicon carbide powder by using dispersant hydroxyethyl cellulose, calcium carbonate and polyacrylic acid; the modified carbon fiber is a modified carbon fiber which is coated with a graphene oxide layer, a silicon carbide layer and a carbon nano tube layer in sequence from inside to outside;
The silicon carbide powder is modified, so that the problems of easy agglomeration and the like of the silicon carbide powder are solved, the sintering performance of the composite material is improved, the fracture toughness and the bending strength of the composite material are improved, and the mass loss at high temperature is reduced;
However, the silicon carbide ceramic composite material prepared by the patent has poor wear resistance, and has low retention rate of toughness and bending strength after low-temperature treatment, thereby limiting the application of the composite material.
Disclosure of Invention
In order to solve the technical problems in the prior art, the invention provides a method for preparing silicon carbide ceramics by pressureless sintering, which improves the toughness, enhances the bending strength and has good stability and high strength retention performance after low-temperature treatment.
Aiming at the technical problems, the invention adopts the following technical scheme:
the method for preparing the silicon carbide ceramic by pressureless sintering comprises the steps of pretreatment of silicon carbide, coating, modification of coated particles, amination of carbon fiber, preparation of slurry, molding and sintering, and comprises the following specific operations:
1. Silicon carbide pretreatment
Placing silicon carbide in a closed container, introducing sodium hydroxide solution for soaking for 2.2-2.4h at 105-108 ℃, washing after soaking to obtain alkali-soaked silicon carbide, placing the alkali-soaked silicon carbide in absolute ethyl alcohol, adding coconut fatty acid diethanolamide and polyvinylpyrrolidone for ultrasonic treatment for 20-25min, wherein the ultrasonic power is 112-117W, the ultrasonic frequency is 43-48kHz, and drying after ultrasonic treatment to obtain pretreated silicon carbide;
The particle size of the silicon carbide is 135-145nm;
the mass concentration of the sodium hydroxide solution is 8.5-8.9%;
The mass ratio of the silicon carbide to the sodium hydroxide solution is 28-32:145-154;
the mass ratio of the silicon carbide, the absolute ethyl alcohol, the coconut oil fatty acid diethanolamide and the polyvinylpyrrolidone after alkaline leaching is 18-22:63-67:1.0-1.2:0.7-1.0.
2. Coating
Placing pretreated silicon carbide into a first mixed solution, performing ultrasonic dispersion for 14-16min, wherein ultrasonic power is 204-215W, ultrasonic frequency is 25-29kHz, adding ammonia water and a second mixed solution at the same time after ultrasonic dispersion is finished, stirring for 6.8-7.2h, stirring at 215-224rpm, filtering and washing after stirring is finished, placing into a vacuum freeze dryer for vacuum freeze drying, wherein cold trap temperature is-48 to-44 ℃, drying time is 11-13h, vacuum degree is 92-96Pa, and naturally recovering to room temperature after vacuum freeze drying is finished to obtain coated particles;
The mass volume ratio of the pretreated silicon carbide to the first mixed solution, the ammonia water to the second mixed solution is 16-18g:494-505mL:9.7-10.2mL:56-60mL;
the first mixed solution consists of ethanol and deionized water, and the volume ratio of the ethanol to the deionized water is 1.5-1.7:0.3;
The mass fraction of the ammonia water is 24-26%;
the second mixed solution is an ethanol solution of ethyl orthosilicate, and the mass fraction of the ethyl orthosilicate is 24-27%.
3. Modified coated particles
(1) One-time modification
Placing the coated particles in a muffle furnace, heating to 376-384 ℃ at a speed of 4.7-5.3 ℃/min, calcining for 3.3-3.7h at 376-384 ℃, naturally recovering to room temperature after calcining, then placing in an ethanol solution, adding tartaric acid and sodium dodecyl benzene sulfonate for ball milling treatment, wherein the ball milling time is 33-37min, the ball milling rotating speed is 122-126rpm, the ball milling temperature is 67-69 ℃, the ball material ratio is 4-6:1, and filtering and drying after ball milling is finished to obtain primary modified coated particles;
The mass ratio of the coated particles to the ethanol solution to the tartaric acid to the sodium dodecyl benzene sulfonate is 12-14:76-80:0.6-0.8:1.1-1.3;
the mass concentration of the ethanol solution is 36-40%;
(2) Secondary modification
Placing the primary modified coated particles in an acetone solution, uniformly stirring, adding epoxy chloropropane and a sodium hydroxide solution, stirring for reaction, controlling the stirring speed to be 200-210rpm, the stirring time to be 2.8-3.2h, and the stirring temperature to be 52-54 ℃, and washing and drying to obtain the epoxidized coated particles; introducing acetic acid solution into a closed container, adding chitosan into the closed container, stirring for 1.8-2.2h at 312-326rpm, adding the epoxidation coated particles after stirring, heating to 60-64 ℃ at a speed of 1.7-2.3 ℃/min after stirring uniformly, stirring for 3.4-3.6h, washing and drying to obtain secondary modified coated particles;
The mass ratio of the primary modified coated particles to the acetone solution to the epichlorohydrin to the sodium hydroxide solution is 8-12:90-98:64-68:73-77;
the volume-mass ratio of the acetic acid solution to the chitosan to the epoxidized coated particles is 485-494mL, 9.7-10.3g and 2.2-2.4g;
the mass concentration of the acetone solution is 30-34%;
The mass concentration of the sodium hydroxide solution is 26-29%;
The mass concentration of the acetic acid solution is 2.6-2.8%.
4. Aminated carbon fiber
Placing carbon fiber in deionized water, adding glyceryl monostearate and sodium hexadecyl sulfonate, stirring uniformly, then carrying out microwave treatment for 8-12min, wherein the microwave power is 104-115W, the microwave frequency is 17-23kHz, adding an acid solution for stirring after the microwave is finished, the stirring temperature is 62-64 ℃, the stirring time is 2.9-3.1h, filtering, washing and drying after the stirring is finished to obtain acid-treated carbon fiber, placing the acid-treated carbon fiber in a closed container, then introducing triethylene tetramine solution, dropwise adding dicyclohexylcarbodiimide, controlling the pressure to be 0.11-0.14MPa, heating to 112-116 ℃ at a speed of 1.3-1.7 ℃/min, carrying out reflux reaction at 112-116 ℃ for 13-15h, and filtering, washing and drying after the reaction is finished to obtain amino carbon fiber;
The mass ratio of the carbon fiber to the deionized water to the glyceryl monostearate to the sodium hexadecyl sulfonate to the acid solution to the triethylene tetramine solution to the dicyclohexyl carbodiimide is 9-11g, 33-37g, 0.4-0.6g, 0.7-0.9g, 177-184g, 495-504mL, and 10.2-10.4g;
The diameter of the carbon fiber is 195-210nm, and the length is 0.02-0.04 mm;
The acid solution is a mixture of a concentrated nitric acid solution and a concentrated sulfuric acid solution, and the mass ratio of the concentrated nitric acid solution to the concentrated sulfuric acid solution is 1.2-1.5:1.0;
the mass concentration of the concentrated nitric acid solution is 70-74%; the mass concentration of the concentrated sulfuric acid solution is 78-82%;
the mass concentration of the triethylene tetramine solution is 11-13%.
5. Preparation of the slurry
Mixing silicon carbide, secondary modified coated particles, carbon amination fibers, aluminum nitride, phenolic resin, sodium lignin sulfonate, polyethylene glycol 600, stearic acid and deionized water, stirring at 743-755rpm for 1.4-1.6h at 28-32 ℃, and obtaining slurry after stirring;
The mass ratio of the silicon carbide to the secondary modified coated particles to the aminated carbon fiber to the aluminum nitride to the phenolic resin to the sodium lignin sulfonate to the polyethylene glycol 600 to the stearic acid to the deionized water is 86-90:6.3-6.5:4.2-4.4:1.2-1.6:1.5-1.9:1.1-1.3:1.1-1.4:0.8-1.2:96-100;
The particle size of the silicon carbide particles is 0.3-0.5 mu m;
the grain diameter of the aluminum nitride is 0.7-0.9 mu m.
6. Shaping
And (3) placing the slurry in a spray dryer for spray granulation, then placing the slurry in a steel mould, and maintaining the pressure for 92-96s under 33-35MPa to obtain a green body.
7. Sintering
Placing the green body in a pressureless sintering furnace, heating to 664-675 ℃ at the speed of 4.8-5.2 ℃/min under the nitrogen atmosphere, preserving heat for 13-17min at 664-675 ℃, heating to 1250-1360 ℃ at the speed of 3.2-3.8 ℃/min, preserving heat for 18-22min at 1250-1360 ℃, heating to 2010-2050 ℃ at the speed of 1.8-2.2 ℃/min, preserving heat for 1.4-1.6h at 2010-2050 ℃, and naturally cooling to room temperature after the heat preservation is finished, thus obtaining the silicon carbide ceramic.
Compared with the prior art, the invention has the following beneficial effects:
1. According to the invention, the silicon carbide is pretreated by adopting the sodium hydroxide solution, so that the activation performance of the silicon carbide particles is improved, and the attractive force among the silicon carbide particles can be weakened by the treatment of coconut fatty acid diethanolamide and polyvinylpyrrolidone, so that a good dispersing effect is achieved, and a good steric effect is formed; then the silicon carbide particles are coated by silicon dioxide, the compatibility between the silicon carbide and the silicon dioxide is enhanced, the surface dispersion performance of the coated particles is improved by primary modification, the aggregation among the coated particles is reduced, in the secondary modification step, firstly, performing epoxidation treatment, and then adding chitosan to combine amino groups of the chitosan with epoxy groups on the surfaces of the coated particles to obtain modified coated particles, so that the reinforcing property of silicon dioxide on silicon carbide particles is fully exerted; the carbon fiber is aminated, so that the surface of the carbon fiber is rich in amino groups, and the amino groups can be bonded with hydroxyl groups on the surface of the modified coated particles, so that the carbon fiber is tightly combined with the modified coated particles, the connection is firm, the tight combination property among silicon carbide, silicon dioxide and the carbon fiber is finally realized, the reinforcing property of the silicon dioxide and the carbon fiber to the silicon carbide particles is fully exerted, the strength properties of fracture toughness, bending strength and the like of the silicon carbide ceramic are improved, the stability of the silicon carbide ceramic is ensured, and the silicon carbide ceramic can still maintain higher strength property after being processed at low temperature;
2. The silicon carbide ceramic prepared by the method has the tensile strength of 279-283MPa, the fracture toughness of 8.14-8.29 MPa-m 1/2, the bending strength of 482-490MPa and the tensile strength of 338-348MPa;
3. The silicon carbide ceramic prepared by the method is cooled to the temperature of minus 20 ℃ at the speed of 2.0 ℃/min, is kept stand for 12 hours at the temperature of minus 20 ℃, is cooled to the temperature of minus 40 ℃ at the speed of 1.0 ℃/min, is kept stand for 24 hours at the temperature of minus 40 ℃, is cooled to the temperature of minus 50 ℃ at the speed of 0.5 ℃/min, is kept stand for 144 hours at the temperature of minus 50 ℃ and is naturally restored to the room temperature, and the tensile strength of 271-276MPa, the fracture toughness of 7.96-8.17MPa m 1/2, the flexural strength of 466-478MPa and the tensile strength of 324-337MPa are measured again.
Detailed Description
For a clearer understanding of the technical features, objects and effects of the present invention, specific embodiments of the present invention will be described.
Example 1
1. Silicon carbide pretreatment
Placing 30g of silicon carbide in a closed container, introducing 150g of sodium hydroxide solution for soaking for 2.3h at the soaking temperature of 107 ℃, washing after the soaking is finished to obtain alkali-soaked silicon carbide, placing 20g of alkali-soaked silicon carbide in 70g of absolute ethyl alcohol, adding 1.1g of coconut oil fatty acid diethanolamide and 0.8g of polyvinylpyrrolidone for ultrasonic treatment, wherein the ultrasonic time is 23min, the ultrasonic power is 115W, the ultrasonic frequency is 45kHz, and drying after the ultrasonic treatment is finished to obtain pretreated silicon carbide;
the particle size of the silicon carbide is 140nm;
the mass concentration of the sodium hydroxide solution is 8.7%.
2. Coating
Placing 17g of pretreated silicon carbide into 500mL of mixed solution I, performing ultrasonic dispersion, wherein the ultrasonic time is 15min, the ultrasonic power is 210W, the ultrasonic frequency is 27kHz, 10mL of ammonia water and 58mL of mixed solution II are simultaneously added after the ultrasonic dispersion is finished, stirring is performed for 7h, the stirring rotation speed is 220rpm, after the stirring is finished, filtering and washing are performed, and then the obtained product is placed into a vacuum freeze dryer for vacuum freeze drying, wherein the cold trap temperature is-46 ℃, the drying time is 12h, the vacuum degree is 94Pa, and the product is naturally restored to room temperature after the vacuum freeze drying is finished, so as to obtain coated particles;
The first mixed solution consists of ethanol and deionized water, and the volume ratio of the ethanol to the deionized water is 1.6:0.3;
The mass fraction of the ammonia water is 25%;
The second mixed solution is an ethanol solution of ethyl orthosilicate, and the mass fraction of the ethyl orthosilicate is 25%.
3. Modified coated particles
(1) One-time modification
Placing 13g of coated particles in a muffle furnace, heating to 380 ℃ at a speed of 5.0 ℃/min, calcining for 3.5 hours at 380 ℃, naturally recovering to room temperature after calcining, then placing in 78g of ethanol solution, adding 0.7g of tartaric acid and 1.2g of sodium dodecyl benzene sulfonate for ball milling treatment, wherein the ball milling time is 35min, the ball milling rotating speed is 124rpm, the ball milling temperature is 68 ℃, the ball-to-material ratio is 5:1, and filtering and drying after ball milling is finished to obtain primary modified coated particles;
the mass concentration of the ethanol solution is 38%;
(2) Secondary modification
Placing 10g of primary modified coated particles into 95g of acetone solution, uniformly stirring, adding 66g of epichlorohydrin and 75g of sodium hydroxide solution, stirring for reaction, controlling the stirring rotation speed to be 204rpm, stirring for 3.0h at 53 ℃, and washing and drying to obtain epoxidized coated particles; introducing 490mL of acetic acid solution into a closed container, adding 10g of chitosan, stirring for 2.0h at a stirring speed of 320rpm, adding 2.3g of the epoxidized coated particles after stirring, heating to 62 ℃ at a speed of 2.0 ℃/min after stirring uniformly, stirring for 3.5h, washing and drying to obtain secondary modified coated particles;
The mass concentration of the acetone solution is 32%;
The mass concentration of the sodium hydroxide solution is 28%;
the mass concentration of the acetic acid solution is 2.7%.
4. Aminated carbon fiber
Placing 10g of carbon fiber into 35g of deionized water, adding 0.5g of glyceryl monostearate and 0.8g of sodium hexadecyl sulfonate, uniformly stirring, then carrying out microwave treatment, wherein the microwave time is 10min, the microwave power is 110W, the microwave frequency is 20kHz, after the microwave is finished, adding 180g of acid solution, stirring, the stirring temperature is 63 ℃, the stirring time is 3.0h, after the stirring is finished, filtering, washing and drying to obtain acid-treated carbon fiber, placing the acid-treated carbon fiber into a closed container, then introducing 500mL of triethylene tetramine solution, dropwise adding 10.3g of dicyclohexylcarbodiimide, controlling the pressure to be 0.12MPa, heating to 114 ℃ at a speed of 1.5 ℃/min, carrying out reflux reaction for 14h at 114 ℃, and after the reaction is finished, filtering, washing and drying to obtain the amino carbon fiber;
the diameter of the carbon fiber is 200nm, and the length is 0.03 mm;
The acid solution is a mixture of a concentrated nitric acid solution and a concentrated sulfuric acid solution, and the mass ratio of the concentrated nitric acid solution to the concentrated sulfuric acid solution is 1.3:1.0;
the mass concentration of the concentrated nitric acid solution is 72%; the mass concentration of the concentrated sulfuric acid solution is 80%;
The mass concentration of the triethylene tetramine solution is 12%.
5. Preparation of the slurry
88G of silicon carbide, 6.4g of secondary modified coated particles, 4.3g of carbon fiber, 1.4g of aluminum nitride, 1.7g of phenolic resin, 1.2g of sodium lignin sulfonate, 1.3g of polyethylene glycol 600, 1.0g of stearic acid and 98g of deionized water are mixed, and then are stirred at 750rpm for 1.5 hours at 30 ℃ to prepare slurry after stirring is finished;
the particle size of the silicon carbide particles is 0.4 mu m;
The grain size of the aluminum nitride is 0.8 μm.
6. Shaping
And (3) placing the slurry in a spray dryer for spray granulation, then placing the slurry in a steel mould, and maintaining the pressure for 94s under 34MPa to obtain a green body.
7. Sintering
And (3) placing the green body in a pressureless sintering furnace, heating to 670 ℃ at a speed of 5.0 ℃/min under nitrogen atmosphere, preserving heat for 15min at 670 ℃, heating to 1300 ℃ at a speed of 3.5 ℃/min, preserving heat for 20min at 1300 ℃, heating to 2030 ℃ at a speed of 2.0 ℃/min, preserving heat for 1.5h at 2030 ℃, and naturally cooling to room temperature after the heat preservation is finished to obtain the silicon carbide ceramic.
Example 2
1. Silicon carbide pretreatment
Putting 28g of silicon carbide into a closed container, introducing 145g of sodium hydroxide solution for soaking for 2.2 hours at the soaking temperature of 105 ℃, washing after the soaking is finished to obtain alkali-soaked silicon carbide, putting 18g of alkali-soaked silicon carbide into 67g of absolute ethyl alcohol, adding 1.0g of coconut oil fatty acid diethanolamide and 0.7g of polyvinylpyrrolidone for ultrasonic treatment, wherein the ultrasonic time is 20 minutes, the ultrasonic power is 112W, the ultrasonic frequency is 43kHz, and drying after the ultrasonic treatment is finished to obtain pretreated silicon carbide;
the particle size of the silicon carbide is 135nm;
the mass concentration of the sodium hydroxide solution is 8.5%.
2. Coating
Placing 16g of pretreated silicon carbide into 494mL of mixed solution I, performing ultrasonic dispersion, wherein the ultrasonic time is 14min, the ultrasonic power is 204W, the ultrasonic frequency is 25kHz, 9.7mL of ammonia water and 56mL of mixed solution II are simultaneously added after the ultrasonic dispersion is finished, stirring is performed for 6.8h, the stirring rotating speed is 215rpm, after the stirring is finished, filtering and washing, placing into a vacuum freeze dryer for vacuum freeze drying, wherein the cold trap temperature is-48 ℃, the drying time is 11h, the vacuum degree is 92Pa, and naturally recovering to room temperature after the vacuum freeze drying is finished, thus obtaining coated particles;
The first mixed solution consists of ethanol and deionized water, and the volume ratio of the ethanol to the deionized water is 1.5:0.3;
the mass fraction of the ammonia water is 24%;
The second mixed solution is an ethanol solution of ethyl orthosilicate, and the mass fraction of the ethyl orthosilicate is 24%.
3. Modified coated particles
(1) One-time modification
Placing 12g of coated particles in a muffle furnace, heating to 376 ℃ at a speed of 4.7 ℃/min, calcining for 3.3 hours at 376 ℃, naturally recovering to room temperature after calcining, then placing in 76g of ethanol solution, adding 0.6g of tartaric acid and 1.1g of sodium dodecyl benzene sulfonate for ball milling treatment, wherein the ball milling time is 33min, the ball milling rotating speed is 122rpm, the ball milling temperature is 67 ℃, the ball-material ratio is 4:1, and filtering and drying after ball milling is finished to obtain primary modified coated particles;
the mass concentration of the ethanol solution is 36%;
(2) Secondary modification
Placing 8g of primary modified coated particles into 90g of acetone solution, uniformly stirring, adding 64g of epichlorohydrin and 73g of sodium hydroxide solution, stirring for reaction, controlling the stirring speed to be 200rpm, stirring for 2.8h at the temperature of 52 ℃, and washing and drying to obtain epoxidized coated particles; introducing 485mL of acetic acid solution into a closed container, adding 9.7g of chitosan, stirring for 1.8h at a stirring speed of 312rpm, adding 2.2g of epoxidized coated particles after stirring, heating to 60 ℃ at a speed of 1.7 ℃/min after stirring uniformly, stirring for 3.4h, washing and drying to obtain secondary modified coated particles;
the mass concentration of the acetone solution is 30%;
the mass concentration of the sodium hydroxide solution is 26%;
the mass concentration of the acetic acid solution is 2.6%.
4. Aminated carbon fiber
Placing 9g of carbon fiber into 33g of deionized water, adding 0.4g of glyceryl monostearate and 0.7g of sodium hexadecyl sulfonate, uniformly stirring, then carrying out microwave treatment, wherein the microwave time is 8min, the microwave power is 104W, the microwave frequency is 17kHz, after the microwave is finished, adding 177g of acid solution, stirring, the stirring temperature is 62 ℃, the stirring time is 2.9h, after the stirring is finished, filtering, washing and drying to obtain acid-treated carbon fiber, placing the acid-treated carbon fiber into a closed container, then introducing 495mL of triethylene tetramine solution, dropwise adding 10.2g of dicyclohexylcarbodiimide, controlling the pressure to be 0.11MPa, heating to 112 ℃ at a speed of 1.3 ℃/min, carrying out reflux reaction for 13h at 112 ℃, and after the reaction is finished, filtering, washing and drying to obtain the amino carbon fiber;
the diameter of the carbon fiber is 195nm, and the length is 0.02 mm;
The acid solution is a mixture of a concentrated nitric acid solution and a concentrated sulfuric acid solution, and the mass ratio of the concentrated nitric acid solution to the concentrated sulfuric acid solution is 1.2:1.0;
the mass concentration of the concentrated nitric acid solution is 70%; the mass concentration of the concentrated sulfuric acid solution is 78%;
the mass concentration of the triethylene tetramine solution is 11%.
5. Preparation of the slurry
86G of silicon carbide, 6.3g of secondary modified coated particles, 4.2g of carbon fiber, 1.2g of aluminum nitride, 1.5g of phenolic resin, 1.1g of sodium lignin sulfonate, 1.1g of polyethylene glycol 600, 0.8g of stearic acid and 96g of deionized water are mixed, and then are stirred at 743rpm for 1.4 hours at 28 ℃ to prepare slurry after stirring is finished;
the particle size of the silicon carbide particles is 0.3 mu m;
The grain size of the aluminum nitride is 0.7 μm.
6. Shaping
And (3) placing the slurry in a spray dryer for spray granulation, then placing the slurry in a steel mould, and maintaining the pressure for 92s under 33MPa to obtain a green body.
7. Sintering
Placing the green body in a pressureless sintering furnace, heating to 664 ℃ at a speed of 4.8 ℃/min under nitrogen atmosphere, preserving heat for 13min at 664 ℃, heating to 1250 ℃ at a speed of 3.2 ℃/min, preserving heat for 18min at 1250 ℃, heating to 2010 ℃ at a speed of 1.8 ℃/min, preserving heat for 1.4h at 2010 ℃, and naturally cooling to room temperature after the heat preservation is finished to obtain the silicon carbide ceramic.
Example 3
1. Silicon carbide pretreatment
Placing 32g of silicon carbide in a closed container, introducing 154g of sodium hydroxide solution for soaking for 2.4h at the soaking temperature of 108 ℃, washing after the soaking is finished to obtain alkaline-soaked silicon carbide, placing 22g of alkaline-soaked silicon carbide in 73g of absolute ethyl alcohol, adding 1.2g of coconut oil fatty acid diethanolamide and 1.0g of polyvinylpyrrolidone for ultrasonic treatment, wherein the ultrasonic time is 25min, the ultrasonic power is 117W, the ultrasonic frequency is 48kHz, and drying after the ultrasonic treatment is finished to obtain pretreated silicon carbide;
the particle size of the silicon carbide is 145nm;
the mass concentration of the sodium hydroxide solution is 8.9%.
2. Coating
Placing 18g of pretreated silicon carbide into 505mL of mixed solution I, performing ultrasonic dispersion, wherein the ultrasonic time is 16min, the ultrasonic power is 215W, the ultrasonic frequency is 29kHz, 10.2mL of ammonia water and 60mL of mixed solution II are simultaneously added after the ultrasonic dispersion is finished, stirring is performed for 7.2h, the stirring rotating speed is 224rpm, after the stirring is finished, filtering and washing, placing into a vacuum freeze dryer for vacuum freeze drying, wherein the cold trap temperature is-44 ℃, the drying time is 13h, the vacuum degree is 96Pa, and naturally recovering to room temperature after the vacuum freeze drying is finished, thus obtaining coated particles;
The first mixed solution consists of ethanol and deionized water, and the volume ratio of the ethanol to the deionized water is 1.7:0.3;
the mass fraction of the ammonia water is 26%;
The second mixed solution is an ethanol solution of ethyl orthosilicate, and the mass fraction of the ethyl orthosilicate is 27%.
3. Modified coated particles
(1) One-time modification
Placing 14g of coated particles in a muffle furnace, heating to 384 ℃ at a speed of 5.3 ℃/min, calcining for 3.7h at 384 ℃, naturally recovering to room temperature after calcining, then placing in 80g of ethanol solution, adding 0.8g of tartaric acid and 1.3g of sodium dodecyl benzene sulfonate for ball milling treatment, wherein the ball milling time is 37min, the ball milling rotating speed is 126rpm, the ball milling temperature is 69 ℃, the ball-material ratio is 6:1, and filtering and drying after ball milling is finished to obtain primary modified coated particles;
The mass concentration of the ethanol solution is 40%;
(2) Secondary modification
Placing 12g of primary modified coated particles into 98g of acetone solution, uniformly stirring, adding 68g of epichlorohydrin and 77g of sodium hydroxide solution, stirring for reaction, controlling the stirring rotation speed to be 210rpm, stirring for 3.2h at 54 ℃, and washing and drying to obtain epoxidized coated particles; introducing 494mL of acetic acid solution into a closed container, adding 10.3g of chitosan, stirring for 2.2h at a stirring speed of 326rpm, adding 2.4g of epoxidized coated particles after stirring, heating to 64 ℃ at a speed of 2.3 ℃/min after stirring uniformly, stirring for 3.6h, washing and drying to obtain secondary modified coated particles;
the mass concentration of the acetone solution is 34%;
The mass concentration of the sodium hydroxide solution is 29%;
the mass concentration of the acetic acid solution is 2.8%.
4. Aminated carbon fiber
Placing 11g of carbon fiber in 37g of deionized water, adding 0.6g of glyceryl monostearate and 0.9g of sodium hexadecyl sulfonate, uniformly stirring, then carrying out microwave treatment, wherein the microwave time is 12min, the microwave power is 115W, the microwave frequency is 23kHz, after the microwave is finished, adding 184g of acid solution, stirring, the stirring temperature is 64 ℃, the stirring time is 3.1h, after the stirring is finished, filtering, washing and drying to obtain acid-treated carbon fiber, placing the acid-treated carbon fiber in a closed container, then introducing 504mL of triethylene tetramine solution, dropwise adding 10.4g of dicyclohexylcarbodiimide, controlling the pressure to be 0.14MPa, heating to 116 ℃ at a speed of 1.7 ℃/min, carrying out reflux reaction for 15h at 116 ℃, and after the reaction is finished, filtering, washing and drying to obtain the amino carbon fiber;
The diameter of the carbon fiber is 210nm, and the length is 0.04 mm;
The acid solution is a mixture of a concentrated nitric acid solution and a concentrated sulfuric acid solution, and the mass ratio of the concentrated nitric acid solution to the concentrated sulfuric acid solution is 1.5:1.0;
The mass concentration of the concentrated nitric acid solution is 74%; the mass concentration of the concentrated sulfuric acid solution is 82%;
the mass concentration of the triethylene tetramine solution is 13%.
5. Preparation of the slurry
90G of silicon carbide, 6.5g of secondary modified coated particles, 4.4g of carbon fiber, 1.6g of aluminum nitride, 1.9g of phenolic resin, 1.3g of sodium lignin sulfonate, 1.4g of polyethylene glycol 600, 1.2g of stearic acid and 100g of deionized water are mixed, and then are stirred at 755rpm for 1.6h at 32 ℃ to prepare slurry after stirring is finished;
The particle size of the silicon carbide particles is 0.5 mu m;
The grain size of the aluminum nitride is 0.9 μm.
6. Shaping
And (3) placing the slurry in a spray dryer for spray granulation, then placing the slurry in a steel mould, and maintaining the pressure for 96s at 35MPa to obtain a green body.
7. Sintering
And (3) placing the green body in a pressureless sintering furnace, heating to 675 ℃ at a speed of 5.2 ℃/min under nitrogen atmosphere, preserving heat for 17min at 675 ℃, heating to 1360 ℃ at a speed of 3.8 ℃/min, preserving heat for 22min at 1360 ℃, heating to 2050 ℃ at a speed of 2.2 ℃/min, preserving heat for 1.6h at 2050 ℃, and naturally cooling to room temperature after the heat preservation is finished to obtain the silicon carbide ceramic.
Comparative example 1
Based on example 1, the modification was that,
(1) Omitting a silicon carbide pretreatment step, and in the coating step, replacing pretreated silicon carbide with silicon carbide which is not subjected to any treatment in an equivalent manner, wherein the particle size of the silicon carbide is 140nm;
(2) Omitting the secondary modification step of the modified coated particles, and in the step of preparing the slurry, replacing the secondary modified coated particles with primary modified coated particles in an equivalent manner;
the rest of the operations are the same.
Comparative example 2
The modification of example 1 was that the step of aminated carbon fiber was omitted, and in the step of preparing slurry, the same amount of aminated carbon fiber was replaced with carbon fiber which was not subjected to any treatment, the diameter of the carbon fiber was 200nm, and the length was 0.03 mm;
the rest of the operations are the same.
Test example 1
The silicon carbide ceramics prepared in examples 1-3 and comparative examples 1-2 were subjected to performance tests, and the test results are as follows:
test example 2
The silicon carbide ceramics prepared in examples 1 to 3 and comparative examples 1 to 2 were cooled to-20℃at a rate of 2.0℃per minute, allowed to stand at-20℃for 12 hours, cooled to-40℃at a rate of 1.0℃per minute, allowed to stand at-40℃for 24 hours, cooled to-50℃at a rate of 0.5℃per minute, allowed to stand at-50℃for 144 hours, and then naturally returned to room temperature, and the tensile strength, fracture toughness, flexural strength and tensile strength of the silicon carbide ceramics were again tested as follows:
According to the invention, the silicon carbide is pretreated by adopting the sodium hydroxide solution, so that the activation performance of the silicon carbide particles is improved, and the attractive force among the silicon carbide particles can be weakened by the treatment of coconut fatty acid diethanolamide and polyvinylpyrrolidone, so that a good dispersing effect is achieved, and a good steric effect is formed; then the silicon carbide particles are coated by silicon dioxide, the compatibility between the silicon carbide and the silicon dioxide is enhanced, the surface dispersion performance of the coated particles is improved by primary modification, the aggregation among the coated particles is reduced, in the secondary modification step, firstly, performing epoxidation treatment, and then adding chitosan to combine amino groups of the chitosan with epoxy groups on the surfaces of the coated particles to obtain modified coated particles, so that the reinforcing property of silicon dioxide on silicon carbide particles is fully exerted; the carbon fiber is aminated, so that the surface of the carbon fiber is rich in amino groups, and the amino groups can be bonded with hydroxyl groups on the surface of the modified coated particles, so that the carbon fiber is tightly combined with the modified coated particles, the connection is firm, the tight combination property among silicon carbide, silicon dioxide and the carbon fiber is finally realized, the reinforcing property of the silicon dioxide and the carbon fiber to the silicon carbide particles is fully exerted, the strength properties of fracture toughness, bending strength and the like of the silicon carbide ceramic are improved, the stability of the silicon carbide ceramic is ensured, and the silicon carbide ceramic can still maintain higher strength property after being processed at low temperature.
The pretreatment step of silicon carbide is omitted in comparative example 1, silicon dioxide is adopted to coat the silicon carbide particles which are not subjected to any treatment, the silicon carbide particles are in an agglomeration state, in the coating process, the coating is uneven, the dispersibility of the silicon carbide and the silicon dioxide is poor, the secondary modification step of the modified coated particles is omitted in comparative example 1, the prepared primary modified coated particles have poor compatibility with other components, the uniformity of slurry is poor, the strength performance and the stability performance of the silicon carbide ceramic are affected after sintering, and the service life of the ceramic is shortened;
Comparative example 2 omits the amination step for the carbon fiber, the untreated carbon fiber has poor compatibility with components such as secondary modified coated particles, and the like, and the carbon fiber cannot be uniformly dispersed in the silicon carbide ceramic matrix, so that the enhancement performance for silicon carbide is affected, and the fracture toughness of the silicon carbide ceramic is still lower, the strength performance is still poorer, and the low-temperature resistance performance is poor.
The percentages used in the present invention are mass percentages unless otherwise indicated.
Finally, it should be noted that: the foregoing description is only a preferred embodiment of the present invention, and the present invention is not limited thereto, but it is to be understood that modifications and equivalents of some of the technical features described in the foregoing embodiments may be made by those skilled in the art, although the present invention has been described in detail with reference to the foregoing embodiments. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (9)
1. A method for preparing silicon carbide ceramics by pressureless sintering is characterized in that,
The method for preparing the silicon carbide ceramic comprises the steps of silicon carbide pretreatment, coating, modifying coated particles, aminated carbon fibers, preparing slurry, forming and sintering;
the pretreatment of the silicon carbide comprises the steps of placing the silicon carbide in a closed container, introducing sodium hydroxide solution for soaking for 2.2-2.4 hours, wherein the soaking temperature is 105-108 ℃, washing after the soaking is finished to obtain the silicon carbide subjected to alkaline leaching, placing the silicon carbide subjected to alkaline leaching in absolute ethyl alcohol, adding coconut fatty acid diethanolamide and polyvinylpyrrolidone for ultrasonic treatment, and drying after the ultrasonic treatment is finished to obtain the pretreated silicon carbide;
The coating step comprises the steps of placing pretreated silicon carbide in a first mixed solution, performing ultrasonic dispersion, adding ammonia water and a second mixed solution at the same time after ultrasonic dispersion is finished, stirring, filtering and washing after stirring is finished, placing in a vacuum freeze dryer for vacuum freeze drying, wherein the cold trap temperature is-48 to-44 ℃, the drying time is 11-13h, the vacuum degree is 92-96Pa, and naturally recovering to room temperature after vacuum freeze drying is finished to obtain coated particles;
the modified coated particles comprise a primary modification step and a secondary modification step;
The secondary modification comprises the steps of placing the primary modified coated particles in an acetone solution, uniformly stirring, adding epichlorohydrin and sodium hydroxide solution, performing primary stirring reaction, and washing and drying to obtain epoxidized coated particles; introducing acetic acid solution into a closed container, then adding chitosan for secondary stirring, adding the epoxidized coated particles after stirring, heating to 60-64 ℃ at a speed of 1.7-2.3 ℃/min after stirring uniformly, stirring for reacting for 3.4-3.6h, washing and drying to obtain secondary modified coated particles;
The preparation method comprises the steps of placing carbon fibers in deionized water, adding glyceryl monostearate and sodium hexadecyl sulfonate, stirring uniformly, performing microwave treatment, adding an acid solution, stirring after the microwave is finished, filtering, washing and drying to obtain acid-treated carbon fibers, placing the acid-treated carbon fibers in a closed container, introducing triethylene tetramine solution, dropwise adding dicyclohexylcarbodiimide, controlling the pressure to be 0.11-0.14MPa, heating to 112-116 ℃ at a speed of 1.3-1.7 ℃/min, performing reflux reaction for 13-15h at 112-116 ℃, filtering, washing and drying after the reaction is finished, and obtaining the amino carbon fibers.
2. A method for preparing silicon carbide ceramic by pressureless sintering according to claim 1,
In the step of pretreatment of the silicon carbide, the particle size of the silicon carbide is 135-145nm;
the mass concentration of the sodium hydroxide solution is 8.5-8.9%;
The mass ratio of the silicon carbide to the sodium hydroxide solution is 28-32:145-154;
The mass ratio of the silicon carbide, the absolute ethyl alcohol, the coconut oil fatty acid diethanolamide and the polyvinylpyrrolidone after alkaline leaching is 18-22:63-67:1.0-1.2:0.7-1.0;
The ultrasonic treatment is carried out for 20-25min, the ultrasonic power is 112-117W, and the ultrasonic frequency is 43-48kHz.
3. A method for preparing silicon carbide ceramic by pressureless sintering according to claim 1,
In the coating step, the mass volume ratio of the pretreated silicon carbide to the first mixed solution, the ammonia water and the second mixed solution is 16-18g:494-505mL:9.7-10.2mL:56-60mL;
the first mixed solution consists of ethanol and deionized water, and the volume ratio of the ethanol to the deionized water is 1.5-1.7:0.3;
The mass fraction of the ammonia water is 24-26%;
The second mixed solution is an ethanol solution of ethyl orthosilicate, and the mass fraction of the ethyl orthosilicate is 24-27%;
The ultrasonic dispersion is carried out for 14-16min, the ultrasonic power is 204-215W, and the ultrasonic frequency is 25-29kHz;
the stirring time is 6.8-7.2h, and the stirring speed is 215-224rpm.
4. A method for preparing silicon carbide ceramic by pressureless sintering according to claim 1,
The primary modification comprises the steps of placing coated particles in a muffle furnace, heating to 376-384 ℃ at the speed of 4.7-5.3 ℃/min, calcining for 3.3-3.7h at 376-384 ℃, naturally recovering to room temperature after calcining, then placing in an ethanol solution, adding tartaric acid and sodium dodecyl benzene sulfonate for ball milling treatment, wherein the ball milling time is 33-37min, the ball milling rotating speed is 122-126rpm, the ball milling temperature is 67-69 ℃, the ball material ratio is 4-6:1, and filtering and drying after ball milling is finished to obtain primary modified coated particles;
The mass ratio of the coated particles to the ethanol solution to the tartaric acid to the sodium dodecyl benzene sulfonate is 12-14:76-80:0.6-0.8:1.1-1.3;
The mass concentration of the ethanol solution is 36-40%.
5. A method for preparing silicon carbide ceramic by pressureless sintering according to claim 1,
In the step of secondary modification, the mass ratio of the primary modified coated particles to the acetone solution to the epichlorohydrin to the sodium hydroxide solution is 8-12:90-98:64-68:73-77;
the volume-mass ratio of the acetic acid solution to the chitosan to the epoxidized coated particles is 485-494mL, 9.7-10.3g and 2.2-2.4g;
the mass concentration of the acetone solution is 30-34%;
The mass concentration of the sodium hydroxide solution is 26-29%;
The mass concentration of the acetic acid solution is 2.6-2.8%;
the primary stirring reaction is carried out, the stirring rotation speed is 200-210rpm, the stirring time is 2.8-3.2h, and the stirring temperature is 52-54 ℃;
the secondary stirring is carried out for 1.8-2.2h, and the stirring speed is 312-326rpm.
6. A method for preparing silicon carbide ceramic by pressureless sintering according to claim 1,
In the step of the amination carbon fiber, the mass ratio of the carbon fiber, deionized water, glyceryl monostearate, sodium hexadecyl sulfonate, acid solution, triethylene tetramine solution and dicyclohexylcarbodiimide is 9-11g:33-37g:0.4-0.6g:0.7-0.9g:177-184g:495-504mL:10.2-10.4g;
The diameter of the carbon fiber is 195-210nm, and the length is 0.02-0.04 mm;
The acid solution is a mixture of a concentrated nitric acid solution and a concentrated sulfuric acid solution, and the mass ratio of the concentrated nitric acid solution to the concentrated sulfuric acid solution is 1.2-1.5:1.0;
the mass concentration of the concentrated nitric acid solution is 70-74%; the mass concentration of the concentrated sulfuric acid solution is 78-82%;
The mass concentration of the triethylene tetramine solution is 11-13%;
The microwave treatment is carried out for 8-12min, the microwave power is 104-115W, and the microwave frequency is 17-23kHz;
The stirring is carried out at the temperature of 62-64 ℃ for 2.9-3.1h.
7. A method for preparing silicon carbide ceramic by pressureless sintering according to claim 1,
The preparation method comprises the steps of mixing silicon carbide, secondary modified coated particles, carbon fiber amide, aluminum nitride, phenolic resin, sodium lignin sulfonate, polyethylene glycol 600, stearic acid and deionized water, stirring at 743-755rpm for 1.4-1.6h, at 28-32 ℃, and obtaining the slurry after stirring;
The mass ratio of the silicon carbide to the secondary modified coated particles to the aminated carbon fiber to the aluminum nitride to the phenolic resin to the sodium lignin sulfonate to the polyethylene glycol 600 to the stearic acid to the deionized water is 86-90:6.3-6.5:4.2-4.4:1.2-1.6:1.5-1.9:1.1-1.3:1.1-1.4:0.8-1.2:96-100;
The particle size of the silicon carbide particles is 0.3-0.5 mu m;
the grain diameter of the aluminum nitride is 0.7-0.9 mu m.
8. A method for preparing silicon carbide ceramic by pressureless sintering according to claim 1,
The molding step is that the slurry is placed in a spray dryer for spray granulation, then placed in a steel mould, and the pressure is maintained for 92-96 seconds under 33-35MPa, so that the green body is prepared.
9. A method for preparing silicon carbide ceramic by pressureless sintering according to claim 1,
The sintering process includes the steps of setting green body inside pressureless sintering furnace, heating to 664-675 deg.c in nitrogen atmosphere at the speed of 4.8-5.2 deg.c/min, maintaining at 664-675 deg.c for 13-17min, heating to 1250-1360 deg.c at the speed of 3.2-3.8 deg.c/min, maintaining at 1250-1360 deg.c for 18-22min, heating to 2010-2050 deg.c at the speed of 1.8-2.2 deg.c/min, maintaining at 2010-2050 deg.c for 1.4-1.6 hr, and cooling naturally to room temperature to obtain silicon carbide ceramic.
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