CN118619583A - Method for preparing large-size recrystallized silicon carbide board by using gypsum board mold for gel casting - Google Patents
Method for preparing large-size recrystallized silicon carbide board by using gypsum board mold for gel casting Download PDFInfo
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- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 title claims abstract description 90
- 229910010271 silicon carbide Inorganic materials 0.000 title claims abstract description 53
- 238000000034 method Methods 0.000 title claims abstract description 35
- 239000010440 gypsum Substances 0.000 title claims abstract description 29
- 229910052602 gypsum Inorganic materials 0.000 title claims abstract description 29
- 238000005266 casting Methods 0.000 title claims abstract description 22
- 229920000049 Carbon (fiber) Polymers 0.000 claims abstract description 96
- 239000004917 carbon fiber Substances 0.000 claims abstract description 96
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims abstract description 94
- 239000002131 composite material Substances 0.000 claims abstract description 78
- 238000001035 drying Methods 0.000 claims abstract description 72
- 238000002156 mixing Methods 0.000 claims abstract description 51
- 238000003756 stirring Methods 0.000 claims abstract description 43
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 28
- 239000008367 deionised water Substances 0.000 claims abstract description 25
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 25
- 239000002002 slurry Substances 0.000 claims abstract description 24
- 239000002270 dispersing agent Substances 0.000 claims abstract description 15
- 239000003054 catalyst Substances 0.000 claims abstract description 13
- WGTYBPLFGIVFAS-UHFFFAOYSA-M tetramethylammonium hydroxide Chemical compound [OH-].C[N+](C)(C)C WGTYBPLFGIVFAS-UHFFFAOYSA-M 0.000 claims abstract description 12
- 239000003999 initiator Substances 0.000 claims abstract description 11
- 239000000178 monomer Substances 0.000 claims abstract description 10
- 239000003431 cross linking reagent Substances 0.000 claims abstract description 9
- 239000002518 antifoaming agent Substances 0.000 claims abstract description 7
- 238000005245 sintering Methods 0.000 claims abstract description 7
- 238000007493 shaping process Methods 0.000 claims abstract description 6
- VYFYYTLLBUKUHU-UHFFFAOYSA-N dopamine Chemical compound NCCC1=CC=C(O)C(O)=C1 VYFYYTLLBUKUHU-UHFFFAOYSA-N 0.000 claims description 99
- 229910052582 BN Inorganic materials 0.000 claims description 59
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 claims description 59
- 229960003638 dopamine Drugs 0.000 claims description 49
- 239000008103 glucose Substances 0.000 claims description 29
- FPYJFEHAWHCUMM-UHFFFAOYSA-N maleic anhydride Chemical compound O=C1OC(=O)C=C1 FPYJFEHAWHCUMM-UHFFFAOYSA-N 0.000 claims description 28
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 23
- 239000003822 epoxy resin Substances 0.000 claims description 23
- 229920000647 polyepoxide Polymers 0.000 claims description 23
- 239000000047 product Substances 0.000 claims description 22
- WQZGKKKJIJFFOK-VFUOTHLCSA-N beta-D-glucose Chemical compound OC[C@H]1O[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-VFUOTHLCSA-N 0.000 claims description 21
- 239000000243 solution Substances 0.000 claims description 21
- 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 19
- 238000005406 washing Methods 0.000 claims description 18
- 239000004816 latex Substances 0.000 claims description 16
- 229920000126 latex Polymers 0.000 claims description 16
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 15
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 15
- 229910052580 B4C Inorganic materials 0.000 claims description 14
- INAHAJYZKVIDIZ-UHFFFAOYSA-N boron carbide Chemical compound B12B3B4C32B41 INAHAJYZKVIDIZ-UHFFFAOYSA-N 0.000 claims description 14
- 238000000498 ball milling Methods 0.000 claims description 11
- 239000000203 mixture Substances 0.000 claims description 11
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 claims description 10
- 229910052796 boron Inorganic materials 0.000 claims description 10
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims description 10
- 239000003795 chemical substances by application Substances 0.000 claims description 9
- 238000000227 grinding Methods 0.000 claims description 8
- 238000000465 moulding Methods 0.000 claims description 7
- 238000009210 therapy by ultrasound Methods 0.000 claims description 7
- 229920002873 Polyethylenimine Polymers 0.000 claims description 6
- 239000007983 Tris buffer Substances 0.000 claims description 5
- 239000003921 oil Substances 0.000 claims description 5
- OTYBMLCTZGSZBG-UHFFFAOYSA-L potassium sulfate Chemical compound [K+].[K+].[O-]S([O-])(=O)=O OTYBMLCTZGSZBG-UHFFFAOYSA-L 0.000 claims description 5
- 229910052939 potassium sulfate Inorganic materials 0.000 claims description 5
- 235000011151 potassium sulphates Nutrition 0.000 claims description 5
- 238000010992 reflux Methods 0.000 claims description 5
- 229910001961 silver nitrate Inorganic materials 0.000 claims description 5
- 239000006228 supernatant Substances 0.000 claims description 5
- LENZDBCJOHFCAS-UHFFFAOYSA-N tris Chemical compound OCC(N)(CO)CO LENZDBCJOHFCAS-UHFFFAOYSA-N 0.000 claims description 5
- KWYHDKDOAIKMQN-UHFFFAOYSA-N N,N,N',N'-tetramethylethylenediamine Chemical compound CN(C)CCN(C)C KWYHDKDOAIKMQN-UHFFFAOYSA-N 0.000 claims description 4
- 230000018044 dehydration Effects 0.000 claims description 4
- 238000006297 dehydration reaction Methods 0.000 claims description 4
- 239000002994 raw material Substances 0.000 claims description 3
- 239000002253 acid Substances 0.000 claims description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-O ammonium group Chemical group [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims description 2
- 230000000694 effects Effects 0.000 abstract description 13
- 230000000052 comparative effect Effects 0.000 description 31
- 229960001031 glucose Drugs 0.000 description 27
- 238000005452 bending Methods 0.000 description 23
- 238000005336 cracking Methods 0.000 description 19
- 238000002360 preparation method Methods 0.000 description 18
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 12
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 6
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 6
- 239000000843 powder Substances 0.000 description 6
- 238000001291 vacuum drying Methods 0.000 description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 5
- 239000000919 ceramic Substances 0.000 description 5
- 235000015895 biscuits Nutrition 0.000 description 4
- 238000011056 performance test Methods 0.000 description 4
- QOSSAOTZNIDXMA-UHFFFAOYSA-N Dicylcohexylcarbodiimide Chemical group C1CCCCC1N=C=NC1CCCCC1 QOSSAOTZNIDXMA-UHFFFAOYSA-N 0.000 description 3
- 238000005054 agglomeration Methods 0.000 description 3
- 230000002776 aggregation Effects 0.000 description 3
- KBPLFHHGFOOTCA-UHFFFAOYSA-N caprylic alcohol Natural products CCCCCCCCO KBPLFHHGFOOTCA-UHFFFAOYSA-N 0.000 description 3
- 230000007547 defect Effects 0.000 description 3
- 238000001514 detection method Methods 0.000 description 3
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- 238000004108 freeze drying Methods 0.000 description 3
- 230000001105 regulatory effect Effects 0.000 description 3
- 238000002791 soaking Methods 0.000 description 3
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical group NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 description 2
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical group [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
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- 238000004132 cross linking Methods 0.000 description 2
- 238000004090 dissolution Methods 0.000 description 2
- 239000000835 fiber Substances 0.000 description 2
- ZIUHHBKFKCYYJD-UHFFFAOYSA-N n,n'-methylenebisacrylamide Chemical group C=CC(=O)NCNC(=O)C=C ZIUHHBKFKCYYJD-UHFFFAOYSA-N 0.000 description 2
- 238000003825 pressing Methods 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
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- 239000004593 Epoxy Substances 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
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- GZCGUPFRVQAUEE-SLPGGIOYSA-N aldehydo-D-glucose Chemical compound OC[C@@H](O)[C@@H](O)[C@H](O)[C@@H](O)C=O GZCGUPFRVQAUEE-SLPGGIOYSA-N 0.000 description 1
- 229910001870 ammonium persulfate Inorganic materials 0.000 description 1
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- 238000005253 cladding Methods 0.000 description 1
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- Ceramic Products (AREA)
Abstract
The application relates to a method for preparing a large-size recrystallized silicon carbide board by using a gypsum board mould for gel casting, which comprises the following steps: preparing slurry: mixing a monomer, a crosslinking agent and deionized water, stirring, adding a dispersing agent, a defoaming agent, modified silicon carbide powder, a carbon fiber composite material and a sintering aid, and stirring, and adding tetramethyl ammonium hydroxide to obtain slurry; preparing a blank: mixing the slurry balls, vacuum defoaming, and adding a catalyst and an initiator to obtain a blank; and (3) curing a blank: pouring the blank body in a mould, and solidifying; and (3) drying: and demolding the solidified green body, shaping the demolded green body, then continuously vacuumizing and drying in a constant temperature and humidity drying box, and finally drying the green body in the constant temperature and humidity drying box to obtain the silicon carbide board product. The application has the effect of improving the quality of the silicon carbide board product.
Description
Technical Field
The application relates to the field of silicon carbide preparation, in particular to a method for preparing a large-size recrystallized silicon carbide plate by using a gypsum board die for gel casting.
Background
The recrystallized silicon carbide plate has the advantages of excellent high temperature resistance, corrosion resistance, hardness, strength, thermal conductivity and the like, and has wide application in various fields such as metal processing, furnaces, semiconductors and the like.
The preparation method of the recrystallized silicon carbide board in mass production in the market at present mainly comprises dry pressing molding and slip casting, but both have larger defects, and the dry pressing molding has the defects of high cost, incapability of preparing large-size recrystallized silicon carbide board and the like; slip casting has the problems that the product is easy to crack in a layering way, warp and deform, and a large-size recrystallized silicon carbide plate cannot be prepared.
The gel casting process is one near net shape forming process, and utilizes netted gel produced through in-situ polymerization of organic monomer to fix ceramic grains in colloidal system, so as to obtain ceramic biscuit in complicated shape. The strength of the biscuit obtained by gel casting is generally higher, fine processing of the biscuit can be performed, and the common additive is an organic substance, and no impurity remains, so that the biscuit can be used for producing ceramic products with larger sizes, accords with the preparation method of the recrystallized silicon carbide plate and has lower cost. However, the recrystallized silicon carbide board prepared by the method still has the defect of warp deformation.
Disclosure of Invention
In order to improve the product quality of the silicon carbide board, the application provides a method for preparing a large-size recrystallized silicon carbide board by using a gypsum board die for gel casting.
The application provides a method for preparing a large-size recrystallized silicon carbide board by using a gypsum board mould for gel casting, which adopts the following technical scheme:
A method for preparing a large-size recrystallized silicon carbide board by using a gypsum board mould for gel casting molding comprises the following steps:
preparing slurry: mixing a monomer, a crosslinking agent and deionized water, stirring, adding a dispersing agent, a defoaming agent, modified silicon carbide powder, a carbon fiber composite material and a sintering aid, and stirring, and adding tetramethyl ammonium hydroxide to obtain slurry;
preparing a blank: mixing the slurry balls, vacuum defoaming, and adding a catalyst and an initiator to obtain a blank;
And (3) curing a blank: pouring the blank body in a mould, and solidifying;
And (3) drying: and demolding the solidified green body, shaping the demolded green body, then continuously vacuumizing and drying in a constant temperature and humidity drying box, and finally drying the green body in the constant temperature and humidity drying box to obtain the silicon carbide board product.
By adopting the technical scheme, the slurry system is prepared after the silicon carbide powder is modified, the overall dispersion performance of the slurry can be effectively improved, the agglomeration phenomenon of the silicon carbide powder is reduced, the powder can be more stable in the slurry, and the product quality of the prepared silicon carbide board is effectively improved; the carbon fiber composite material is added in the system, so that the connection tightness between all components in the system can be promoted, the system is more stable, the bending stress resistance of the prepared silicon carbide board is effectively improved, the cracking phenomenon of the system is further reduced, and the product quality is further improved.
Preferably, the mass ratio between the monomer and the crosslinking agent is (7-15): 1; the dispersing agent comprises a high molecular dispersing agent, wherein the dispersing agent is 1-2.5% of the mass of the modified silicon carbide powder; the catalyst comprises tetramethyl ethylenediamine, and the catalyst accounts for 0.005-0.01% of the mass of the modified silicon carbide powder; the initiator is ammonium overcurrent acid with the mass fraction of 5%, and the mass ratio of the catalyst to the initiator is 1:1.
By adopting the technical scheme, the quality of each component in the control system is in the range, so that a more stable silicon carbide board product can be obtained.
Preferably, the modified silicon carbide powder is prepared by the following method:
mixing maleic anhydride and sodium hydroxide to obtain maleic anhydride solution, mixing silicon carbide powder and the maleic anhydride solution, stirring to obtain maleic anhydride treated silicon carbide, adding a silane coupling agent, stirring, centrifuging, washing, and drying to obtain modified silicon carbide powder;
the silane coupling agent comprises any one of KH550, KH560, KH570, KH580 and KH 590.
Through adopting above-mentioned technical scheme, carry out preliminary treatment through maleic anhydride to carborundum ceramic powder, cladding carborundum powder, introduce negatively the back, can promote the silane coupling agent of follow-up adding positively charged for silane coupling agent enriches at carborundum powder surface, has promoted the collision of silane coupling agent and carborundum surface, and then has promoted the grafting efficiency of coupling agent, makes carborundum powder in the system can distribute more evenly, thereby has promoted product quality.
Preferably, the carbon fiber composite material comprises dopamine composite carbon fiber, epoxy resin and boron nitride component.
By adopting the technical scheme, the carbon fiber composite material is prepared by compounding the dopamine composite carbon fiber, the epoxy resin and the boron carbide component, so that the carbon fiber composite material has good interface bonding strength, the carbon fiber composite material can be tightly combined in a system, the system is more stable, and the occurrence of cracking is reduced.
Preferably, the dopamine composite carbon fiber is prepared by the following method:
mixing silver nitrate solution, potassium sulfate and carbon fiber, washing after ultrasonic treatment, drying, adding the mixture into Tris buffer solution, adjusting the pH value to be alkaline, adding dopamine, stirring and drying to obtain dopamine-treated carbon fiber, mixing polyethyleneimine and N, N-dimethylformamide, adding a dehydration condensing agent, washing after reflux, and drying to obtain the dopamine composite carbon fiber.
Through adopting above-mentioned technical scheme, through the method of chemical grafting with flexible polyethylenimine and rigid dopamine once graft to the carbon fiber surface, introduce active group, can make dopamine composite carbon fiber have good interfacial effect, with can better combination between epoxy and the thick liquids system, simultaneously, the roughness promotion on carbon fiber surface, make the system can better with the carbon fiber between combine, promoted the even propagation of stress, reduced the bending of the panel of preparation obtain, and promoted the holistic mechanical properties of panel.
Preferably, the boron nitride component raw materials include boron nitride, glucose and latex.
Preferably, the boron nitride component is prepared by the following method:
Mixing boron nitride and glucose, ball milling, mixing the mixture with deionized water, centrifuging, removing supernatant, drying to obtain boron nitride-glucose compound, mixing latex, boron nitride-glucose compound and deionized water, stirring, drying, and crushing to obtain boron carbide component.
Through adopting above-mentioned technical scheme, modify boron nitride surface through glucose, the C-O bond fracture between hydroxyl and the carbon of glucose molecule forms B-O bond with the polar atom B between the boron nitride to make glucose molecule graft on the boron nitride, promoted the dispersibility of boron nitride, after adding the latex, the three forms stable crosslinked structure, thereby make the mechanical properties of boron nitride component obtain improving, further promoted holistic mechanical properties and the homogeneity of product.
Preferably, the mass ratio of the boron nitride, the glucose and the latex is (0.4-0.5) 1:1.5.
By adopting the technical scheme, the mass ratio of boron nitride, glucose and latex is preferably within the range, so that the stability of the prepared boron nitride component can be further improved.
Preferably, the carbon fiber composite material is prepared by the following method:
Mixing the boron nitride component, the dopamine composite carbon fiber and the epoxy resin, stirring under the oil bath condition after ultrasonic treatment, adding a curing agent, stirring, exhausting, drying and grinding to obtain the carbon fiber composite material.
Preferably, the mass ratio of the epoxy resin to the dopamine composite carbon fiber to the boron carbide component is 5:1 (0.62-0.68).
By adopting the technical scheme, the mass ratio of the epoxy resin, the dopamine composite carbon fiber and the boron carbide component is preferably within the range, so that the overall stability of the carbon fiber composite material can be further improved.
In summary, the present application includes at least one of the following beneficial technical effects:
The modified silicon carbide powder is used, so that the modified silicon carbide powder can be dispersed more uniformly in the system, the product quality is improved, and meanwhile, the carbon fiber composite material is added in the system, so that the combination of all components in the system is more stable, and the overall combination stability of the system is improved;
After the silicon carbide powder is treated by using maleic anhydride, the maleic anhydride is coated on the surface of the silicon carbide powder, and then the silane coupling agent is used for modifying the powder, so that the grafting efficiency of the silane coupling agent is improved, the interface effect of the silicon carbide powder in a system is improved, and meanwhile, the dispersion performance of the silicon carbide in the system is improved, and the product quality is further improved;
The carbon fiber composite material is prepared from the dopamine composite carbon fiber, the epoxy resin and the boron carbide component, the interface performance of the carbon fiber is improved after the carbon fiber is modified by the dopamine, the connection performance of each component in a system can be improved, the stress propagation is promoted, the bending phenomenon of the plate in the preparation process is reduced, the boron nitride component is formed by compounding glucose and latex, the integral mechanical performance of the plate is improved, and the stable three-dimensional network structure is formed among the boron nitride component, the dopamine composite fiber and the epoxy resin and is uniformly distributed in the system, so that the product quality of the plate is effectively improved.
Detailed Description
The application is further illustrated by the following examples:
The raw material description: all the starting materials in the examples are commercially available; wherein, the silicon carbide powder adopts grain composition, the grain diameter is 0.5-1 mu m, 40-60 mu m, and the mass ratio of 100-125 mu m is 3.5:3:3.5; the mold for preparing the silicon carbide plate adopts a gypsum board mold, graphite powder is coated on the inner wall of the mold as a mold release agent before grouting a blank, four sides of the gypsum board mold are in a zigzag shape, and cracking, deformation and layering in the blank are reduced;
The dehydration condensing agent is N, N' -dicyclohexyl carbodiimide (CAS number: 538-75-0); the monomer is acrylamide (CAS number: 79-06-1), the cross-linking agent is N, N' -methylene bisacrylamide (CAS number: 110-26-9), the dispersing agent is DolaPIX CE dispersing agent and SOPA (model: DYSP-270) dispersing agent, and the mass ratio is 1:1; the defoaming agent is n-octanol (CAS number: 111-87-5), and the sintering aid is prepared by mixing carbon and boron carbide in a mass ratio of 1:1; the catalyst is tetramethyl ethylenediamine (CAS number: 110-18-9); the initiator is ammonium persulfate with the mass fraction of 5%.
Examples
Preparing modified silicon carbide powder:
mixing maleic anhydride (CAS number: 108-31-6) with a sodium hydroxide solution, regulating the pH value to 8 to obtain a maleic anhydride solution, mixing silicon carbide powder with the maleic anhydride solution, stirring to obtain maleic anhydride treated silicon carbide, continuously adding a silane coupling agent, stirring at a rotating speed of 300r/min for 2 hours, centrifuging, washing with deionized water, transferring to a drying oven at 75 ℃ and drying for 24 hours to obtain modified silicon carbide powder; wherein the mass ratio of maleic anhydride to the silane coupling agent is 5:1; the silane coupling agent is KH-550.
Preparing dopamine composite carbon fiber:
washing carbon fiber with acetone under 80 ℃, drying for 8 hours in a vacuum drying oven at 40 ℃, mixing 500ml of silver nitrate solution with 0.01mol/L and 0.05mol of potassium sulfate with the dried carbon fiber, ultrasonically dissolving, washing with deionized water and ethanol, drying in an oven at 40 ℃, adding into 10mM/L Tris buffer solution, adjusting the pH value to 8.5 with hydrochloric acid, adding dopamine, enabling the concentration of the dopamine (CAS number: 51-61-6) in the system to be 2g/L, stirring and drying in the environment at 25 ℃ to obtain the dopamine-treated carbon fiber, mixing polyethylenimine and N, N-dimethylformamide in a volume ratio of 1:10, adding a dehydration condensing agent, refluxing for 24 hours in the environment at 100 ℃, alternately washing with deionized water and ethanol for 3 times, and drying in the environment at 40 ℃ for 12 hours to obtain the dopamine-treated carbon fiber.
Preparing a boron nitride component:
Mixing 5.51g of boron nitride with 13.79g of anhydrous glucose (CAS number: 58367-01-4), putting into a ball milling tank, adding grinding balls, setting the rotating speed of the ball mill to 400r/min, ball milling for 16h, mixing the ball-milled mixture with deionized water, centrifuging, removing supernatant, repeatedly centrifuging for 3 times, freeze-drying to obtain a boron nitride-glucose compound, mixing 20.7g of latex, the prepared boron nitride-glucose compound with 300g of deionized water, stirring at the rotating speed of 800r/min for 1.5h in an environment of 25 ℃, and crushing to obtain a boron carbide component.
Preparing a carbon fiber composite material:
Mixing 28.09g of boron nitride component, 45.32g of dopamine composite carbon fiber and 226.59g of epoxy resin, carrying out ultrasonic treatment, stirring at a constant temperature of 900r/min under an oil bath condition at 90 ℃ for 3 hours, adding 75g of curing agent D230, stirring at a rotating speed of 600r/min for 10 minutes, exhausting in a vacuum freeze dryer, drying in a vacuum drying oven at 25 ℃, and grinding to obtain the carbon fiber composite material.
Preparing large-size recrystallized silicon carbide plates by using a gypsum board die for gel casting molding:
preparing slurry: 63g of monomer, 9g of cross-linking agent and 485g of deionized water are mixed and stirred for 10min at a rotating speed of 300r/min, then 12g of dispersing agent, 12g of defoaming agent, 1200g of modified silicon carbide powder, 200g of carbon fiber composite material and 12g of sintering aid are added, and are stirred for 2h at a rotating speed of 800r/min, 10g of tetramethyl ammonium hydroxide is added, and stirring is carried out for 2h at a rotating speed to obtain slurry;
preparing a blank: maintaining the temperature of the slurry at 16 ℃, ball-milling and mixing the slurry for 4 hours, adding 0.1g of catalyst and 0.1g of initiator after vacuum defoaming, and obtaining a blank after 10 minutes;
and (3) curing a blank: pouring the blank in a mould, and solidifying the blank after 30 min;
And (3) drying: and demolding the cured blank, clamping the demolded blank between two gypsum boards with the thickness of 10mm, shaping the blank, transferring the shaped blank into a constant temperature and humidity drying oven (35 ℃ and 50 RH) for drying, continuously vacuumizing and drying the blank for 3 hours after the water soaking rate of the blank is 3%, and finally, placing the blank in the constant temperature and humidity drying oven (25 RH and 60 ℃) again for drying for 2 hours to finish drying to obtain the silicon carbide board product.
Examples
Preparing modified silicon carbide powder:
mixing maleic anhydride and sodium hydroxide, regulating the pH value to 8 to obtain maleic anhydride solution, mixing silicon carbide powder and the maleic anhydride solution, stirring to obtain maleic anhydride treated silicon carbide, continuously adding a silane coupling agent, stirring at a rotating speed of 300r/min for 2 hours, centrifuging, washing with deionized water, transferring to a drying oven at 75 ℃ and drying for 24 hours to obtain modified silicon carbide powder; wherein the mass ratio of maleic anhydride to the silane coupling agent is 5:1; the silane coupling agent is KH-560.
Preparing dopamine composite carbon fiber:
Washing carbon fiber with acetone under the condition of 80 ℃, drying for 8 hours in a vacuum drying oven at 40 ℃, mixing 500ml of silver nitrate solution with 0.01mol/L and 0.05mol of potassium sulfate with the dried carbon fiber, washing with deionized water and ethanol after ultrasonic dissolution, drying in an oven at 40 ℃, adding into 10mM/L Tris buffer solution, adjusting the pH value to 8.5 with hydrochloric acid, adding dopamine, stirring in the environment at 25 ℃ to obtain dopamine-treated carbon fiber, mixing polyethylenimine and N, N-dimethylformamide in a volume ratio of 1:10, refluxing for 24 hours in the environment at 100 ℃, alternately washing with deionized water and ethanol for 3 times, and drying in the environment at 40 ℃ for 12 hours to obtain the dopamine composite carbon fiber.
Preparing a boron nitride component:
Mixing 6.67g of boron nitride with 13.33g of anhydrous glucose, putting the mixture into a ball milling tank, adding grinding balls, setting the rotating speed of the ball mill to 400r/min, ball milling for 16h, mixing the ball-milled mixture with deionized water, centrifuging, removing supernatant, repeatedly centrifuging for 3 times, freeze-drying to obtain a boron nitride-glucose compound, mixing 20g of latex, the prepared boron nitride-glucose compound with 300g of deionized water, stirring for 1.5h at the rotating speed of 800r/min under the environment of 25 ℃, drying, and crushing to obtain a boron carbide component.
Preparing a carbon fiber composite material:
Mixing 28.09g of boron nitride component, 44.91g of dopamine composite carbon fiber and 224.55g of epoxy resin, carrying out ultrasonic treatment, stirring at a constant temperature of 900r/min under an oil bath condition at 90 ℃ for 3 hours, adding 75g of curing agent D230, stirring at a rotating speed of 600r/min for 10 minutes, exhausting in a vacuum freeze dryer, drying in a vacuum drying oven at 25 ℃, and grinding to obtain the carbon fiber composite material.
Preparing large-size recrystallized silicon carbide plates by using a gypsum board die for gel casting molding:
Preparing slurry: mixing 175.5g of monomer, 11.7g of cross-linking agent and 520g of deionized water, stirring at a speed of 300r/min for 10min, then adding 31.2g of dispersing agent, 39g of defoaming agent, 1560g of modified silicon carbide powder, 260g of carbon fiber composite material and 18.72g of sintering aid, stirring at a speed of 800r/min for 2h, adding 26g of tetramethylammonium hydroxide, and stirring at a speed of 2h to obtain slurry;
Preparing a blank: maintaining the temperature of the slurry at 16 ℃, ball-milling and mixing the slurry for 4 hours, adding 0.26g of catalyst and 0.26g of initiator after vacuum defoaming, and obtaining a blank after 10 minutes;
and (3) curing a blank: pouring the blank in a mould, and solidifying the blank after 30 min;
And (3) drying: and demolding the cured blank, clamping the demolded blank between two gypsum boards with the thickness of 10mm, shaping the blank, transferring the shaped blank into a constant temperature and humidity drying oven (35 ℃ and 50 RH) for drying, continuously vacuumizing and drying the blank for 3 hours after the water soaking rate of the blank is 3%, and finally, placing the blank in the constant temperature and humidity drying oven (25 RH and 60 ℃) again for drying for 2 hours to finish drying to obtain the silicon carbide board product.
Examples
Preparing modified silicon carbide powder:
Mixing maleic anhydride and sodium hydroxide, regulating the pH value to 8 to obtain maleic anhydride solution, mixing silicon carbide powder and the maleic anhydride solution, stirring to obtain maleic anhydride treated silicon carbide, continuously adding a silane coupling agent, stirring at a rotating speed of 300r/min for 2 hours, centrifuging, washing with deionized water, transferring to a drying oven at 75 ℃ and drying for 24 hours to obtain modified silicon carbide powder; wherein the mass ratio of maleic anhydride to the silane coupling agent is 5:1; the silane coupling agent is KH-570.
Preparing dopamine composite carbon fiber:
Washing carbon fiber with acetone under the condition of 80 ℃, drying for 8 hours in a vacuum drying oven at 40 ℃, mixing 500ml of silver nitrate solution with 0.01mol/L and 0.05mol of potassium sulfate with the dried carbon fiber, washing with deionized water and ethanol after ultrasonic dissolution, drying in an oven at 40 ℃, adding into 10mM/L Tris buffer solution, adjusting the pH value to 8.5 with hydrochloric acid, adding dopamine, stirring in the environment at 25 ℃ to obtain dopamine-treated carbon fiber, mixing polyethylenimine and N, N-dimethylformamide in a volume ratio of 1:10, refluxing for 24 hours in the environment at 100 ℃, alternately washing with deionized water and ethanol for 3 times, and drying in the environment at 40 ℃ for 12 hours to obtain the dopamine composite carbon fiber.
Preparing a boron nitride component:
Mixing 6.1g of boron nitride with 13.56g of anhydrous glucose, putting into a ball milling tank, adding grinding balls, setting the rotating speed of a ball mill to 400r/min, ball milling for 16h, mixing the ball-milled mixture with deionized water, centrifuging, removing supernatant, repeatedly centrifuging for 3 times, freeze-drying to obtain a boron nitride-glucose compound, mixing 20.34g of latex, the prepared boron nitride-glucose compound with 300g of deionized water, stirring for 1.5h at the rotating speed of 800r/min under the environment of 25 ℃, drying, and crushing to obtain a boron carbide component.
Preparing a carbon fiber composite material:
29.32g of boron nitride component, 45.11g of dopamine composite carbon fiber and 225.57g of epoxy resin are mixed, after ultrasonic treatment, stirring is carried out for 3 hours at the constant temperature of 900r/min under the oil bath condition of 90 ℃, 75g of curing agent D230 is added, stirring is carried out for 10 minutes at the rotating speed of 600r/min, the mixture is exhausted in a vacuum freeze dryer, then drying is carried out in a vacuum drying box at the temperature of 25 ℃, and the carbon fiber composite material is obtained after grinding.
Preparing large-size recrystallized silicon carbide plates by using a gypsum board die for gel casting molding:
Preparing slurry: mixing 113.85g of monomer, 10.35g of cross-linking agent and 500g of deionized water, stirring at a speed of 300r/min for 10min, then adding 20.7g of dispersing agent, 24.15g of defoaming agent, 1380g of modified silicon carbide powder, 230g of carbon fiber composite material and 15.18g of sintering aid, stirring at a speed of 800r/min for 2h, adding 17.25g of tetramethyl ammonium hydroxide, and stirring at a speed of 2h to obtain slurry;
preparing a blank: maintaining the temperature of the slurry at 16 ℃, ball-milling and mixing the slurry for 4 hours, adding 0.1725g of catalyst and 0.1725g of initiator after vacuum defoaming, and obtaining a blank after 10 minutes;
and (3) curing a blank: pouring the blank in a mould, and solidifying the blank after 30 min;
And (3) drying: and demolding the cured blank, clamping the demolded blank between two gypsum boards with the thickness of 10mm, shaping the blank, transferring the shaped blank into a constant temperature and humidity drying oven (35 ℃ and 50 RH) for drying, continuously vacuumizing and drying the blank for 3 hours after the water soaking rate of the blank is 3%, and finally, placing the blank in the constant temperature and humidity drying oven (25 RH and 60 ℃) again for drying for 2 hours to finish drying to obtain the silicon carbide board product.
Examples
Example 4 the difference between example 4 and example 3, based on example 3, is that in example 4 the silane coupling agent used in the preparation of the modified silicon carbide powder was KH-580.
Examples
Example 5 the difference between example 5 and example 3, based on example 3, is that in example 5 the silane coupling agent used in the preparation of the modified silicon carbide powder was KH5-90.
Examples
Example 6 the difference between example 6 and example 3, based on example 3, is that in example 6, 4.29g of boron nitride, 14.29g of glucose and 21.42g of latex were used in the preparation of the boron nitride component.
Examples
Example 7 the difference between example 7 and example 3, based on example 3, is that in example 7, 7.74g of boron nitride, 12.9g of glucose and 19.36g of latex were used in the preparation of the boron nitride component.
Examples
Example 8 the difference between example 8 and example 3, based on example 3, is that in example 8, 26.03g of boron nitride component was used, 45.66g of dopamine composite carbon fiber was used, and 228.31g of epoxy resin was used in the preparation of carbon fiber composite material.
Examples
Example 9 the difference between example 9 and example 3, based on example 3, is that in example 9, a boron nitride composition of 32.54g, a dopamine composite fiber of 44.58g, and an epoxy resin of 222.88g were used in the preparation of the carbon fiber composite material.
Examples
Example 10 the difference between example 10 and example 3, based on example 3, is that in example 10 no glucose was added in the preparation of the boron nitride component.
Examples
Example 11 based on example 3, the difference between example 11 and example 3 is that in example 11, carbon fibers were not treated with dopamine at the time of preparing the carbon fiber composite material.
Examples
Example 12 the difference between example 12 and example 3, based on example 3, is that in example 12 the boron nitride composite component was replaced with ordinary boron nitride when preparing the carbon fiber composite.
Examples
Example 13 the difference between example 13 and example 3, based on example 3, is that in example 13 no epoxy resin was added in the preparation of the carbon fiber composite.
Examples
Example 14 the difference between example 14 and example 3, based on example 3, is that in example 14 no boron nitride composite component was added in the preparation of the carbon fiber composite material.
Examples
Example 15 based on example 3, the difference between example 15 and example 3 is that silicon carbide powder was modified using only a silane coupling agent in example 15.
Comparative example 1
Comparative example 1 based on example 3, the carbon fiber composite material in comparative example 1 was free of dopamine composite carbon fiber and was only epoxy resin and boron nitride components.
Comparative example 2
Comparative example 2 based on example 3, the carbon fiber composite material of comparative example 2 was only ordinary carbon fiber.
Comparative example 3
Comparative example 3 the carbon fiber composite material was replaced with an equivalent amount of boron nitride component based on example 3.
Comparative example 4
Comparative example 4 the four sides of the gypsum board mold in comparative example 4 were flat based on example 3.
Comparative example 5
Comparative example 5 in comparative example 5, on the basis of example 3, the inner wall of the gypsum board mold was not coated with graphite powder.
Comparative example 6
Comparative example 6 the silicon carbide powder was not modified in comparative example 6 based on example 3.
Performance test
Samples of examples 1-14, comparative examples 1-5 were sampled and subjected to the following performance tests:
(1) Bending resistance test
The bending strength test is carried out on the samples by taking the GB/T6569-2006 fine ceramic bending strength test method as a detection standard, each sample is tested for three times at room temperature, an average value is taken, and the detection result is filled in the table 1.
(2) Surface Performance test
The surface condition of the dried product was observed, and the detection result was filled in table 1.
TABLE 1 results of Performance test of silicon carbide plate samples of examples 1-14, comparative examples 1-5
Detecting items | Flexural Strength/MPa | Surface phenomenon |
Example 1 | 436 | The surface is smooth, and no bending and cracking occur |
Example 2 | 438 | The surface is smooth, and no bending and cracking occur |
Example 3 | 448 | The surface is smooth, and no bending and cracking occur |
Example 4 | 442 | The surface is smooth, and no bending and cracking occur |
Example 5 | 445 | The surface is smooth, and no bending and cracking occur |
Example 6 | 430 | The surface evenness is reduced, and no bending and cracking occur |
Example 7 | 431 | The surface evenness is reduced, and no bending and cracking occur |
Example 8 | 427 | The surface evenness is reduced, and no bending and cracking occur |
Example 9 | 426 | The surface evenness is reduced, and no bending and cracking occur |
Example 10 | 432 | The surface evenness is reduced, and no bending and cracking occur |
Example 11 | 421 | The surface evenness is reduced, and no bending and cracking occur |
Example 12 | 423 | The surface is smooth, and no bending and cracking occur |
Example 13 | 419 | The surface evenness is reduced, the surface is slightly bent and is not cracked |
Example 14 | 417 | The surface evenness is reduced, the surface is slightly bent and is not cracked |
Example 15 | 428 | The surface is smooth, and no bending and cracking occur |
Comparative example 1 | 412 | The surface evenness is reduced, the surface is slightly bent and slightly cracked |
Comparative example 2 | 405 | The surface evenness is reduced, the surface is slightly bent and slightly cracked |
Comparative example 3 | 403 | The surface evenness is reduced, the surface is slightly bent and slightly cracked |
Comparative example 4 | 419 | The surface evenness is reduced, the surface is slightly bent and is not cracked |
Comparative example 5 | 422 | The surface is smooth, and no bending and cracking occur |
Comparative example 6 | 418 | The surface evenness is reduced, and no bending and cracking occur |
As shown in Table 1, the bending strength of examples 1-5 is 426MPa and above, which indicates that the silicon carbide board prepared by the application has good bending resistance; the surfaces of the examples 1-5 are all smooth, and no cracking phenomenon occurs, which indicates that the silicon carbide board prepared by the preparation method has good product quality.
In the preparation of the boron nitride component in the embodiment 6 and the embodiment 7, the mass ratio of the boron nitride, the glucose and the latex is not in the range defined by the application, when the content of the latex is too high, the lamellar isolation effect after the boron nitride and the glucose are compounded is greater than the restraint and crosslinking effect, the crosslinking degree of the composite material is difficult to be further improved, and the boron nitride and the glucose are difficult to form a sufficient three-dimensional stable structure in the system, so that the performance of the system is influenced; when the content of the emulsion is too small, the agglomeration phenomenon of the boron carbide occurs in the system, and the stability of the boron carbide component is affected.
In the preparation of the carbon fiber composite material in examples 8 and 9, the mass ratio of the boron nitride component, the dopamine composite carbon fiber and the epoxy resin is not within the scope of the application, and when the content of the boron nitride component is too small or too large, the bonding effect between the boron nitride component and the dopamine carbon fiber is affected, and the stable rigid-flexible structure between the dopamine composite component and the epoxy resin is affected.
In example 10, when the boron nitride component is prepared, glucose is not added, the compatibility of the boron nitride interface which is not compounded by glucose is reduced, the boron nitride sheets are difficult to separate further, an agglomeration phenomenon is generated, the overall stability of the boron nitride component is affected, and the performance of the prepared carbon fiber composite material is affected.
In example 11, the carbon fiber was not treated with dopamine, the surface roughness of the carbon fiber was hardly improved, the interfacial bonding property was lowered, the dispersibility in the system was also affected, and the bonding effect between the respective components in the system was hardly further promoted.
In example 12, only ordinary boron nitride was used, and unmodified and composite boron nitride was agglomerated in the system, which affected the bonding effect with dopamine composite carbon fiber and epoxy resin, and was difficult to form a stable network structure.
In the preparation of the carbon fiber composite material in example 13, epoxy resin is not added, and the system without epoxy resin is difficult to combine with the dopamine composite carbon fiber and boron nitride to form a stable structure, and meanwhile, the dopamine composite carbon fiber is influenced to form a stable rigid-flexible structure, so that the comprehensive performance of the system is reduced.
The absence of added boron nitride composite component in example 14 has an effect on the toughness of the multi-carbon fiber composite while affecting the formation of a stable structure of the carbon fiber composite.
In example 15, silicon carbide powder was modified only with a silane coupling agent, and the electrostatic binding force of silicon carbide powder not modified with maleic anhydride was reduced, so that it was difficult to graft more silane coupling agent, and the dispersion effect of silicon carbide powder in the system was affected.
In comparative example 1, no dopamine composite carbon fiber is added, so that the epoxy resin is difficult to form a stable rigid-flexible structure, and meanwhile, the bonding performance of each component between systems is reduced, so that the quality of the prepared product is influenced.
In comparative example 2, the carbon fiber composite material was replaced with a common carbon fiber, and the roughness of the surface of the common carbon fiber was difficult to be further improved, and a stable crosslinked structure and a rigid-flexible structure were difficult to be formed, and the compatibility between systems was also lowered.
The carbon fiber composite component in comparative example 3 is replaced with a boron carbide component, and the promotion effect on the mechanical properties in the system is difficult to further improve.
In comparative example 4, the four sides of the gypsum board mold do not adopt a saw tooth structure, but a flat structure, the stress is difficult to concentrate at the edge after the blank is solidified, and the inside of the blank is cracked, deformed and layered, so that the quality of the product is affected, and the mechanical property is reduced to some extent.
In comparative example 5, graphite powder is not coated on the inner wall of the gypsum template, so that the blank is difficult to demold, and the quick demolding is difficult, the drying effect of the subsequent blank is affected, and the product quality is affected.
In comparative example 6, the silicon carbide powder is not modified, so that the silicon carbide powder is agglomerated in a system, the uniformity of the system is reduced, and the quality of the product is affected.
The present embodiment is merely illustrative of the present application, and the present application is not limited thereto, and a worker can make various changes and modifications without departing from the scope of the technical idea of the present application. The technical scope of the present application is not limited to the contents of the specification, and must be determined according to the scope of claims.
Claims (10)
1. A method for preparing a large-size recrystallized silicon carbide board by using a gypsum board mould for gel casting molding is characterized by comprising the following steps of: the method comprises the following steps:
preparing slurry: mixing a monomer, a crosslinking agent and deionized water, stirring, adding a dispersing agent, a defoaming agent, modified silicon carbide powder, a carbon fiber composite material and a sintering aid, and stirring, and adding tetramethyl ammonium hydroxide to obtain slurry;
preparing a blank: mixing the slurry balls, vacuum defoaming, and adding a catalyst and an initiator to obtain a blank;
And (3) curing a blank: pouring the blank body in a mould, and solidifying;
And (3) drying: and demolding the solidified green body, shaping the demolded green body, then continuously vacuumizing and drying in a constant temperature and humidity drying box, and finally drying the green body in the constant temperature and humidity drying box to obtain the silicon carbide board product.
2. A method of preparing large-size recrystallized silicon carbide board by using a gypsum board mold for gel casting according to claim 1, wherein: the mass ratio between the monomer and the cross-linking agent is (7-15) 1; the dispersing agent comprises a high molecular dispersing agent, wherein the dispersing agent is 1-2.5% of the mass of the modified silicon carbide powder; the catalyst comprises tetramethyl ethylenediamine, and the catalyst accounts for 0.005-0.01% of the mass of the modified silicon carbide powder; the initiator is ammonium overcurrent acid with the mass fraction of 5%, and the mass ratio of the catalyst to the initiator is 1:1.
3. A method of preparing large-size recrystallized silicon carbide board by using a gypsum board mold for gel casting according to claim 1, wherein: the modified silicon carbide powder is prepared by the following method:
mixing maleic anhydride and sodium hydroxide to obtain maleic anhydride solution, mixing silicon carbide powder and the maleic anhydride solution, stirring to obtain maleic anhydride treated silicon carbide, adding a silane coupling agent, stirring, centrifuging, washing, and drying to obtain modified silicon carbide powder;
the silane coupling agent comprises any one of KH550, KH560, KH570, KH580 and KH 590.
4. A method of preparing large-size recrystallized silicon carbide board by using a gypsum board mold for gel casting according to claim 1, wherein: the carbon fiber composite material comprises dopamine composite carbon fiber, epoxy resin and boron nitride components.
5. The method for preparing a large-size recrystallized silicon carbide board by using a gypsum board mold for gel casting according to claim 4, wherein the method comprises the following steps: the dopamine composite carbon fiber is prepared by the following method:
mixing silver nitrate solution, potassium sulfate and carbon fiber, washing after ultrasonic treatment, drying, adding the mixture into Tris buffer solution, adjusting the pH value to be alkaline, adding dopamine, stirring and drying to obtain dopamine-treated carbon fiber, mixing polyethyleneimine and N, N-dimethylformamide, adding a dehydration condensing agent, washing after reflux, and drying to obtain the dopamine composite carbon fiber.
6. The method for preparing a large-size recrystallized silicon carbide board by using a gypsum board mold for gel casting according to claim 4, wherein the method comprises the following steps: the raw materials of the boron nitride component comprise boron nitride, glucose and latex.
7. The method for preparing a large-size recrystallized silicon carbide board by using a gypsum board mold for gel casting according to claim 6, wherein the method comprises the following steps: the boron nitride component is prepared by the following method:
Mixing boron nitride and glucose, ball milling, mixing the mixture with deionized water, centrifuging, removing supernatant, drying to obtain boron nitride-glucose compound, mixing latex, boron nitride-glucose compound and deionized water, stirring, drying, and crushing to obtain boron carbide component.
8. The method for preparing a large-size recrystallized silicon carbide board by using a gypsum board mold for gel casting according to claim 7, wherein the method comprises the following steps: the mass ratio of the boron nitride to the glucose to the latex is (0.4-0.5) 1:1.5.
9. The method for preparing a large-size recrystallized silicon carbide board by using a gypsum board mold for gel casting according to claim 4, wherein the method comprises the following steps: the carbon fiber composite material is prepared by the following method:
Mixing the boron nitride component, the dopamine composite carbon fiber and the epoxy resin, stirring under the oil bath condition after ultrasonic treatment, adding a curing agent, stirring, exhausting, drying and grinding to obtain the carbon fiber composite material.
10. The method for preparing a large-size recrystallized silicon carbide board by using a gypsum board mold for gel casting according to claim 6, wherein the method comprises the following steps: the mass ratio of the epoxy resin to the dopamine composite carbon fiber to the boron carbide component is 5:1 (0.62-0.68).
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