CN117466647A - High-heat-conductivity high-strength silicon carbide ceramic and preparation method thereof - Google Patents
High-heat-conductivity high-strength silicon carbide ceramic and preparation method thereof Download PDFInfo
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- CN117466647A CN117466647A CN202311430077.8A CN202311430077A CN117466647A CN 117466647 A CN117466647 A CN 117466647A CN 202311430077 A CN202311430077 A CN 202311430077A CN 117466647 A CN117466647 A CN 117466647A
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- silicon carbide
- carbide ceramic
- heat
- conductivity
- nitrate solution
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- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 title claims abstract description 63
- 229910010271 silicon carbide Inorganic materials 0.000 title claims abstract description 63
- 239000000919 ceramic Substances 0.000 title claims abstract description 50
- 238000002360 preparation method Methods 0.000 title abstract description 15
- 238000005245 sintering Methods 0.000 claims abstract description 34
- 239000007791 liquid phase Substances 0.000 claims abstract description 22
- 238000001354 calcination Methods 0.000 claims abstract description 18
- 238000001816 cooling Methods 0.000 claims abstract description 18
- 239000011812 mixed powder Substances 0.000 claims abstract description 18
- 239000002994 raw material Substances 0.000 claims abstract description 18
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000000498 ball milling Methods 0.000 claims abstract description 14
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 13
- 238000001035 drying Methods 0.000 claims abstract description 11
- 238000000137 annealing Methods 0.000 claims abstract description 10
- 230000003647 oxidation Effects 0.000 claims abstract description 10
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 10
- 239000002135 nanosheet Substances 0.000 claims abstract description 9
- 238000009694 cold isostatic pressing Methods 0.000 claims abstract description 8
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 claims abstract description 8
- 229910052582 BN Inorganic materials 0.000 claims abstract description 7
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 claims abstract description 7
- 229910052581 Si3N4 Inorganic materials 0.000 claims abstract description 7
- 229910052786 argon Inorganic materials 0.000 claims abstract description 7
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 claims abstract description 7
- 238000011049 filling Methods 0.000 claims abstract description 6
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 6
- 239000010439 graphite Substances 0.000 claims abstract description 6
- 238000007731 hot pressing Methods 0.000 claims abstract description 6
- 238000000462 isostatic pressing Methods 0.000 claims abstract description 6
- 238000005498 polishing Methods 0.000 claims abstract description 6
- 238000007873 sieving Methods 0.000 claims abstract description 6
- 238000000227 grinding Methods 0.000 claims abstract description 3
- -1 rare earth nitrate Chemical class 0.000 claims description 39
- 239000000243 solution Substances 0.000 claims description 22
- 229910052761 rare earth metal Inorganic materials 0.000 claims description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 16
- 229910002651 NO3 Inorganic materials 0.000 claims description 13
- 239000008367 deionised water Substances 0.000 claims description 11
- 229910021641 deionized water Inorganic materials 0.000 claims description 11
- 239000002243 precursor Substances 0.000 claims description 10
- 238000003756 stirring Methods 0.000 claims description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 9
- 238000000034 method Methods 0.000 claims description 9
- FYDKNKUEBJQCCN-UHFFFAOYSA-N lanthanum(3+);trinitrate Chemical compound [La+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O FYDKNKUEBJQCCN-UHFFFAOYSA-N 0.000 claims description 7
- CFYGEIAZMVFFDE-UHFFFAOYSA-N neodymium(3+);trinitrate Chemical compound [Nd+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O CFYGEIAZMVFFDE-UHFFFAOYSA-N 0.000 claims description 7
- 238000002156 mixing Methods 0.000 claims description 6
- 239000002904 solvent Substances 0.000 claims description 6
- 238000001914 filtration Methods 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 5
- 239000002244 precipitate Substances 0.000 claims description 5
- 239000002002 slurry Substances 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 5
- 239000012752 auxiliary agent Substances 0.000 claims description 3
- 239000000047 product Substances 0.000 claims description 2
- 238000005452 bending Methods 0.000 abstract description 11
- 229910010293 ceramic material Inorganic materials 0.000 abstract description 3
- 230000000052 comparative effect Effects 0.000 description 9
- 230000007547 defect Effects 0.000 description 5
- MRELNEQAGSRDBK-UHFFFAOYSA-N lanthanum(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[La+3].[La+3] MRELNEQAGSRDBK-UHFFFAOYSA-N 0.000 description 4
- 230000009471 action Effects 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- 239000002105 nanoparticle Substances 0.000 description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 238000000280 densification Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- PLDDOISOJJCEMH-UHFFFAOYSA-N neodymium(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Nd+3].[Nd+3] PLDDOISOJJCEMH-UHFFFAOYSA-N 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 229910001404 rare earth metal oxide Inorganic materials 0.000 description 2
- 239000012783 reinforcing fiber Substances 0.000 description 2
- 238000005728 strengthening Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- BYMUNNMMXKDFEZ-UHFFFAOYSA-K trifluorolanthanum Chemical compound F[La](F)F BYMUNNMMXKDFEZ-UHFFFAOYSA-K 0.000 description 2
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical group [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- CAVCGVPGBKGDTG-UHFFFAOYSA-N alumanylidynemethyl(alumanylidynemethylalumanylidenemethylidene)alumane Chemical compound [Al]#C[Al]=C=[Al]C#[Al] CAVCGVPGBKGDTG-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 125000004432 carbon atom Chemical group C* 0.000 description 1
- 238000000975 co-precipitation Methods 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 229910052731 fluorine Inorganic materials 0.000 description 1
- 239000011737 fluorine Substances 0.000 description 1
- 238000005087 graphitization Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000002608 ionic liquid Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000000877 morphologic effect Effects 0.000 description 1
- 230000006911 nucleation Effects 0.000 description 1
- 238000010899 nucleation Methods 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 238000013001 point bending Methods 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 230000003014 reinforcing effect Effects 0.000 description 1
- 230000008439 repair process Effects 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 239000006104 solid solution Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 230000001360 synchronised effect Effects 0.000 description 1
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Abstract
The invention discloses a high-heat-conductivity high-strength silicon carbide ceramic and a preparation method thereof, belonging to the technical field of ceramic materials, and comprising the following raw materials: silicon carbide, aluminum nitride, a liquid phase sintering aid, silicon nitride whiskers, boron nitride nanosheets and carbon powder; the silicon carbide ceramic comprises the following steps: step S1, adding raw materials of a formula into a ball mill for ball milling, then drying to obtain mixed powder, sieving the mixed powder, and then adding the sieved mixed powder into an isostatic pressing machine for cold isostatic pressing treatment to obtain a pressed block; s2, filling the pressed block into a graphite mold of a hot-pressing sintering furnace, calcining for 1h at 2000 ℃ under the protection of argon and external pressure, then cooling to 1800 ℃ and continuously calcining for 2h, cooling and demolding, then carrying out surface grinding and polishing, then carrying out oxidation annealing treatment, and naturally cooling to room temperature to obtain the product; the invention combines the raw material formula with the preparation method, so that the prepared silicon carbide ceramic has excellent bending strength and heat conduction performance.
Description
Technical Field
The invention belongs to the technical field of ceramic materials, and particularly relates to a high-heat-conductivity high-strength silicon carbide ceramic and a preparation method thereof.
Background
The silicon carbide ceramic has the characteristics of high heat conductivity, small expansion coefficient, small volume density, high hardness, good wear resistance, high temperature resistance, good chemical stability, high strength and the like, is an important structural ceramic material, and is widely applied to the fields of chemical industry, aviation, military industry, electronic devices and the like.
The carbon atoms and silicon atoms in the silicon carbide are combined by strong covalent bonds, and the higher bond energy of the silicon carbide can lead to the problems of brittleness, sensitivity to defects and poor reliability of the silicon carbide ceramic, so that the thermal conductivity and the bending strength of the traditional silicon carbide ceramic are not high enough, and the application range of the traditional silicon carbide ceramic cannot be further expanded. At present, the bending strength of the silicon carbide ceramic is improved by adding reinforcing fibers into the silicon carbide ceramic, but the graphitization degree of the reinforcing fibers is low, so that an effective heat transport network is difficult to form, and the heat conducting property of the silicon carbide ceramic is negatively influenced; in the prior art, the performance of the silicon carbide ceramic is comprehensively improved by binary compounding of rare earth fluoride and rare earth oxide as a sintering aid, but the problems of uniformity in dispersion of the rare earth fluoride and the rare earth oxide exist, and the respective advantages of the two sintering aids cannot be fully exerted.
Therefore, how to prepare silicon carbide ceramics with higher bending strength and excellent heat conduction performance is a technical problem to be solved at present.
Disclosure of Invention
The invention aims to provide a high-heat-conductivity high-strength silicon carbide ceramic and a preparation method thereof, so as to solve the problems in the background technology.
The aim of the invention can be achieved by the following technical scheme:
the high-heat-conductivity high-strength silicon carbide ceramic comprises the following raw materials in parts by weight:
90-92 parts of silicon carbide, 4-4.5 parts of aluminum nitride, 3-4 parts of liquid phase sintering auxiliary agent, 0.3-0.5 part of silicon nitride whisker, 0.8-1 part of boron nitride nanosheet and 0.2-0.25 part of carbon powder;
the liquid phase sintering aid is prepared by the following steps:
adding the mixed rare earth nitrate solution into a beaker, then dropwise adding deionized water and imidazole tetrafluoroborate, uniformly stirring, stirring and reacting for 10min under the water bath heating condition of 90-95 ℃, naturally cooling to room temperature, filtering, centrifugally washing filter residues with deionized water and absolute ethyl alcohol for 2-3 times, collecting precipitate, and drying in a baking oven of 60 ℃ for 12h to obtain a precursor; calcining the precursor for 2 hours in the air atmosphere at 700-720 ℃ to obtain the liquid phase sintering aid.
The imidazole tetrafluoroborate is used as a fluorine source and a solvent, and is mixed with a mixed rare earth nitrate solution, rare earth cations are surrounded by tetrafluoroborate ions to form a crosslinked nano-sheet, after the crosslinked nano-sheet is heated, the tetrafluoroborate ions start to hydrolyze to generate fluoride ions, nano-particle aggregates are gradually formed by nucleation with the rare earth cations, and the nano-particle liquid phase sintering aid is obtained after calcination.
Further, the dosage ratio of the mixed rare earth nitrate solution, deionized water and imidazole tetrafluoroborate is 2mL:20mL:1-1.2mmol.
Further, the mixed rare earth nitrate solution is lanthanum nitrate solution and neodymium nitrate solution according to the volume ratio of 3-5:1, mixing to obtain the product; the concentration of the lanthanum nitrate solution and the neodymium nitrate solution is 1mol/L.
Further, the imidazole tetrafluoroborate is any one of 1-butyl-3-methylimidazole tetrafluoroborate, 1-octyl-3-methylimidazole tetrafluoroborate and 1-hexadecyl-3-methylimidazole tetrafluoroborate.
A preparation method of high-heat-conductivity high-strength silicon carbide ceramic comprises the following steps:
step S1, adding the formula raw materials into a ball mill for ball milling, drying the ball-milled slurry at 70-80 ℃ to obtain mixed powder, sieving the mixed powder with a 200-300-mesh sieve, and adding the mixed powder into an isostatic pressing machine for cold isostatic pressing treatment to obtain a pressing block;
and S2, filling the pressed block into a graphite mold of a hot-pressing sintering furnace, calcining the pressed block at 2000 ℃ for 1h under the protection of argon and under the pressure of 40-60MPa, then continuously calcining the pressed block at 30 ℃/min to 1800 ℃ for 2h, cooling and demolding, then carrying out surface grinding and polishing, carrying out oxidation annealing treatment, and naturally cooling to room temperature to obtain the high-heat-conductivity high-strength silicon carbide ceramic.
Further, the solvent used in the ball milling is absolute ethyl alcohol, the ball milling rotating speed is 350-400r/min, and the ball milling time is 6-8h.
Further, the pressure of the cold isostatic pressing treatment is 300MPa, and the pressure maintaining time is 10-20min.
Further, the temperature of the oxidation annealing treatment is 1280-1300 ℃, and the treatment time is 1h.
The invention has the beneficial effects that:
the invention rapidly prepares the neodymium-doped lanthanum oxyfluoride compound (La) by utilizing imidazole tetrafluoroborate ionic liquid to assist rare earth ion coprecipitation 7 O 6 F 9 ) Compared with the liquid phase sintering aid which is independently added with lanthanum oxide, lanthanum fluoride or neodymium oxide, the nano-particle liquid phase sintering aid can be uniformly dispersed in silicon carbide without long-time ball milling and mixing, and the components of the sintered silicon carbide ceramic are more uniform;
according to the invention, aluminum carbide and a liquid phase sintering aid are used in a matched manner, the aluminum nitride can form a reinforced solid solution in the silicon carbide, the liquid phase sintering aid can promote densification of the silicon carbide ceramic and remove oxygen impurity defects in the silicon carbide, so that the sintering performance of the silicon carbide is effectively improved, the impurity defect removal and a crystal boundary reinforcing mechanism are combined in the matched manner, the defects of the silicon carbide ceramic can be made up, and meanwhile, the bending strength and the heat conducting performance of the silicon carbide ceramic are improved; the boron nitride nanosheets and the silicon nitride whiskers can be well compatible with silicon carbide, so that a strengthening phase with strengthening effect on grain boundaries is generated, and the bending strength of the silicon carbide ceramic is further improved; the carbon powder further eliminates oxygen-containing impurities in the silicon carbide, repairs microscopic morphological defects, and cooperatively improves heat conductivity and bending strength;
according to the invention, the raw material formula is matched with the preparation method, and through hot press sintering at 2000 ℃ and 1800 ℃ under the protection of argon and the external pressure, the deoxidization effect of the sintering aid can be improved, the grain size can be effectively reduced, the densification of the ceramic is promoted, and the synchronous improvement of the heat conducting performance and the bending strength of the silicon carbide ceramic is realized; finally, through oxidation annealing treatment, the residual stress of the silicon carbide ceramic is regulated and controlled, the thermal resistance of the grain boundary is reduced, and the bending strength and the heat conducting property of the silicon carbide ceramic are further improved.
Detailed Description
The technical solutions of the embodiments of the present invention will be clearly and completely described below in conjunction with the embodiments of the present invention, and it is apparent that the described embodiments are only some embodiments of the present invention, not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1
The liquid phase sintering aid is prepared by the following steps:
1mol/L lanthanum nitrate solution and 1mol/L neodymium nitrate solution are mixed according to a volume ratio of 3:1, mixing to prepare mixed rare earth nitrate solution; adding 2mL of mixed rare earth nitrate solution into a beaker, then dropwise adding 20mL of deionized water and 1mmol of 1-butyl-3-methylimidazole tetrafluoroborate, stirring uniformly, stirring and reacting for 10min under the heating condition of a water bath at 90 ℃, naturally cooling to room temperature, filtering, centrifugally washing filter residues with deionized water and absolute ethyl alcohol for 2 times, collecting precipitate, and drying in a baking oven at 60 ℃ for 12h to obtain a precursor; calcining the precursor for 2 hours in an air atmosphere at 700 ℃ to obtain the liquid phase sintering aid.
Example 2
The liquid phase sintering aid is prepared by the following steps:
1mol/L lanthanum nitrate solution and 1mol/L neodymium nitrate solution are mixed according to the volume ratio of 4:1, mixing to prepare mixed rare earth nitrate solution; adding 2mL of mixed rare earth nitrate solution into a beaker, then dropwise adding 20mL of deionized water and 1.1mmol of 1-octyl-3-methylimidazole tetrafluoroborate, stirring uniformly, stirring and reacting for 10min under the heating condition of 92 ℃ water bath, naturally cooling to room temperature, filtering, centrifugally washing filter residues with deionized water and absolute ethyl alcohol for 3 times, collecting precipitate, and drying in a 60 ℃ oven for 12h to obtain a precursor; calcining the precursor for 2 hours in an air atmosphere at 710 ℃ to obtain the liquid phase sintering aid.
Example 3
The liquid phase sintering aid is prepared by the following steps:
1mol/L lanthanum nitrate solution and 1mol/L neodymium nitrate solution are mixed according to the volume ratio of 5:1, mixing to prepare mixed rare earth nitrate solution; adding 2mL of mixed rare earth nitrate solution into a beaker, then dropwise adding 20mL of deionized water and 1.2mmol of 1-hexadecyl-3-methylimidazole tetrafluoroborate, stirring uniformly, stirring and reacting for 10min under the heating condition of a 95 ℃ water bath, naturally cooling to room temperature, filtering, centrifugally washing filter residues with deionized water and absolute ethyl alcohol for 3 times, collecting precipitate, and drying in a 60 ℃ oven for 12h to obtain a precursor; calcining the precursor for 2 hours in an air atmosphere at 720 ℃ to obtain the liquid phase sintering aid.
Example 4
The high-heat-conductivity high-strength silicon carbide ceramic comprises the following raw materials in parts by weight:
90 parts of silicon carbide, 4 parts of aluminum nitride, 3 parts of the liquid phase sintering aid prepared in example 1, 0.3 part of silicon nitride whisker, 0.8 part of boron nitride nanosheets and 0.2 part of carbon powder;
the preparation method of the high-heat-conductivity high-strength silicon carbide ceramic comprises the following steps:
step S1, adding raw materials in parts by weight of a formula into a ball mill, ball milling for 6 hours at a rotating speed of 350r/min by taking absolute ethyl alcohol as a solvent, drying the ball-milled slurry at 70 ℃ to obtain mixed powder, sieving the mixed powder with a 200-mesh sieve, adding the mixed powder into an isostatic pressing machine, and performing cold isostatic pressing treatment for 10 minutes at a pressure of 300MPa to obtain a pressed block;
and S2, filling the pressed block into a graphite mold of a hot-pressing sintering furnace, calcining the pressed block at 2000 ℃ for 1h under the protection of argon and under the pressure of 40MPa, then continuously calcining the pressed block at 30 ℃/min to 1800 ℃ for 2h, cooling and demolding, polishing the surface, performing oxidation annealing treatment at 1280 ℃ for 1h, and naturally cooling to room temperature to obtain the high-heat-conductivity high-strength silicon carbide ceramic.
Example 5
The high-heat-conductivity high-strength silicon carbide ceramic comprises the following raw materials in parts by weight:
91 parts of silicon carbide, 4.3 parts of aluminum nitride, 3.5 parts of the liquid phase sintering additive prepared in example 2, 0.4 part of silicon nitride whisker, 0.9 part of boron nitride nanosheets and 0.25 part of carbon powder;
the preparation method of the high-heat-conductivity high-strength silicon carbide ceramic comprises the following steps:
step S1, adding raw materials in parts by weight of a formula into a ball mill, ball-milling for 7 hours at a rotating speed of 380r/min by taking absolute ethyl alcohol as a solvent, drying the ball-milled slurry at 75 ℃ to obtain mixed powder, sieving the mixed powder with a 250-mesh sieve, adding the sieved mixed powder into an isostatic pressing machine, and performing cold isostatic pressing treatment for 15 minutes at a pressure of 300MPa to obtain a pressed block;
and S2, filling the pressed block into a graphite mold of a hot-pressing sintering furnace, calcining the pressed block at 2000 ℃ for 1h under the protection of argon and the pressure of 50MPa, then continuously calcining the pressed block at 30 ℃/min to 1800 ℃ for 2h, cooling and demolding, polishing the surface, performing oxidation annealing treatment at 1290 ℃ for 1h, and naturally cooling to room temperature to obtain the high-heat-conductivity high-strength silicon carbide ceramic.
Example 6
The high-heat-conductivity high-strength silicon carbide ceramic comprises the following raw materials in parts by weight:
92 parts of silicon carbide, 4.5 parts of aluminum nitride, 4 parts of the liquid phase sintering auxiliary agent prepared in example 3, 0.5 part of silicon nitride whisker, 1 part of boron nitride nanosheets and 0.25 part of carbon powder;
the preparation method of the high-heat-conductivity high-strength silicon carbide ceramic comprises the following steps:
step S1, adding raw materials in parts by weight of a formula into a ball mill, ball milling for 8 hours at a rotating speed of 400r/min by taking absolute ethyl alcohol as a solvent, drying the ball-milled slurry at 80 ℃ to obtain mixed powder, sieving the mixed powder with a 300-mesh sieve, adding the mixed powder into an isostatic pressing machine, and performing cold isostatic pressing treatment for 20 minutes at a pressure of 300MPa to obtain a pressed block;
and S2, filling the pressed block into a graphite mold of a hot-pressing sintering furnace, calcining the pressed block at 2000 ℃ for 1h under the protection of argon and under the pressure of 60MPa, then continuously calcining the pressed block at 30 ℃/min to 1800 ℃ for 2h, cooling and demolding, polishing the surface, performing oxidation annealing treatment at 1300 ℃ for 1h, and naturally cooling to room temperature to obtain the high-heat-conductivity high-strength silicon carbide ceramic.
Comparative example 1
In this comparative example, compared with example 5, the liquid phase sintering aid was replaced with lanthanum oxide and lanthanum fluoride in a mass ratio of 1:2, the rest raw materials and the preparation method are the same.
Comparative example 2
In this comparative example, aluminum nitride was not added to the raw materials, and the other raw materials and the production method were the same as those in example 5.
Comparative example 3
In this comparative example, the compacts were calcined in a hot press sintering furnace at 1900℃for 3 hours under the same atmosphere and applied pressure as in example 5, and the other preparation methods were the same.
Comparative example 4
In this comparative example, the oxidation annealing treatment was not performed, and the other preparation methods were the same as in example 5.
Performance tests were performed on examples 4-6 and comparative examples 1-4, and the thermal conductivity of the silicon carbide ceramics was measured and calculated using a laser thermal conductivity analyzer; the flexural strength of the silicon carbide ceramics was measured by a three-point bending method using a universal tester by making 40mm×8mm×4mm standard bars, and the results are shown in table 1:
TABLE 1
As can be seen from the data in table 1, the silicon carbide ceramics prepared in examples 4-6 have more excellent thermal conductivity and higher bending strength, and the reasonable arrangement of the raw material formula and the cooperation of the preparation method significantly improve the bending strength and the thermal conductivity of the silicon carbide ceramics.
It is noted that relational terms such as first and second, and the like are used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Moreover, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus.
Although embodiments of the present invention have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and alterations can be made therein without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (8)
1. The high-heat-conductivity high-strength silicon carbide ceramic is characterized by comprising the following raw materials in parts by weight:
90-92 parts of silicon carbide, 4-4.5 parts of aluminum nitride, 3-4 parts of liquid phase sintering auxiliary agent, 0.3-0.5 part of silicon nitride whisker, 0.8-1 part of boron nitride nanosheet and 0.2-0.25 part of carbon powder;
the liquid phase sintering aid is prepared by the following steps:
adding the mixed rare earth nitrate solution into a beaker, then dropwise adding deionized water and imidazole tetrafluoroborate, uniformly stirring, stirring and reacting for 10min under the water bath heating condition of 90-95 ℃, naturally cooling to room temperature, filtering, centrifugally washing filter residues, collecting precipitate, and drying to obtain a precursor; calcining the precursor for 2 hours in the air atmosphere at 700-720 ℃ to obtain the liquid phase sintering aid.
2. The high thermal conductivity and high strength silicon carbide ceramic according to claim 1, wherein the mixed rare earth nitrate solution, deionized water and imidazole tetrafluoroborate are used in an amount ratio of 2mL:20mL:1-1.2mmol.
3. The high-heat-conductivity high-strength silicon carbide ceramic according to claim 1, wherein the mixed rare earth nitrate solution is a lanthanum nitrate solution and a neodymium nitrate solution according to a volume ratio of 3-5:1, mixing to obtain the product; the concentration of the lanthanum nitrate solution and the neodymium nitrate solution is 1mol/L.
4. The high thermal conductivity and high strength silicon carbide ceramic as claimed in claim 1, wherein the imidazole tetrafluoroborate is any one of 1-butyl-3-methylimidazolium tetrafluoroborate, 1-octyl-3-methylimidazolium tetrafluoroborate and 1-hexadecyl-3-methylimidazolium tetrafluoroborate.
5. The method for preparing the high-heat-conductivity high-strength silicon carbide ceramic according to claim 1, which is characterized by comprising the following steps:
step S1, adding the formula raw materials into a ball mill for ball milling, drying the slurry after ball milling to obtain mixed powder, sieving the mixed powder with a 200-300-mesh sieve, and adding the mixed powder into an isostatic pressing machine for cold isostatic pressing treatment to obtain a pressed block;
and S2, filling the pressed block into a graphite mold of a hot-pressing sintering furnace, calcining at 2000 ℃ for 1h under the protection of argon and under the pressure of 40-60MPa, then continuously calcining at 30 ℃/min to 1800 ℃ for 2h, cooling and demolding, then carrying out surface grinding and polishing, carrying out oxidation annealing treatment, and naturally cooling to room temperature to obtain the high-heat-conductivity high-strength silicon carbide ceramic.
6. The method for preparing the high-heat-conductivity high-strength silicon carbide ceramic according to claim 5, wherein the solvent used in the ball milling is absolute ethyl alcohol, the ball milling rotating speed is 350-400r/min, and the ball milling time is 6-8h.
7. The method for preparing high-heat-conductivity and high-strength silicon carbide ceramic according to claim 5, wherein the pressure of the cold isostatic pressing treatment is 300MPa and the pressure maintaining time is 10-20min.
8. The method for preparing high-heat-conductivity high-strength silicon carbide ceramic according to claim 5, wherein the temperature of the oxidation annealing treatment is 1280-1300 ℃ and the treatment time is 1h.
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