CN112851355A - Pressureless sintering silicon carbide bulletproof ceramic and preparation method thereof - Google Patents
Pressureless sintering silicon carbide bulletproof ceramic and preparation method thereof Download PDFInfo
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- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 title claims abstract description 135
- 229910010271 silicon carbide Inorganic materials 0.000 title claims abstract description 128
- 239000000919 ceramic Substances 0.000 title claims abstract description 69
- 238000001272 pressureless sintering Methods 0.000 title abstract description 23
- 238000002360 preparation method Methods 0.000 title abstract description 19
- 238000005469 granulation Methods 0.000 claims abstract description 50
- 230000003179 granulation Effects 0.000 claims abstract description 50
- 239000000843 powder Substances 0.000 claims abstract description 41
- 238000000034 method Methods 0.000 claims abstract description 13
- 229920005989 resin Polymers 0.000 claims abstract description 13
- 239000011347 resin Substances 0.000 claims abstract description 13
- 239000002270 dispersing agent Substances 0.000 claims abstract description 12
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 80
- 238000005245 sintering Methods 0.000 claims description 60
- 229910002804 graphite Inorganic materials 0.000 claims description 53
- 239000010439 graphite Substances 0.000 claims description 53
- 229920001568 phenolic resin Polymers 0.000 claims description 45
- 239000005011 phenolic resin Substances 0.000 claims description 45
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 claims description 44
- 239000002245 particle Substances 0.000 claims description 39
- 229910052580 B4C Inorganic materials 0.000 claims description 34
- INAHAJYZKVIDIZ-UHFFFAOYSA-N boron carbide Chemical compound B12B3B4C32B41 INAHAJYZKVIDIZ-UHFFFAOYSA-N 0.000 claims description 34
- 239000002202 Polyethylene glycol Substances 0.000 claims description 33
- 229920001223 polyethylene glycol Polymers 0.000 claims description 33
- QYEXBYZXHDUPRC-UHFFFAOYSA-N B#[Ti]#B Chemical compound B#[Ti]#B QYEXBYZXHDUPRC-UHFFFAOYSA-N 0.000 claims description 31
- 238000001035 drying Methods 0.000 claims description 26
- 238000003756 stirring Methods 0.000 claims description 26
- 239000000758 substrate Substances 0.000 claims description 26
- 238000000498 ball milling Methods 0.000 claims description 24
- 238000002156 mixing Methods 0.000 claims description 24
- 239000000463 material Substances 0.000 claims description 23
- 239000000956 alloy Substances 0.000 claims description 22
- 229910045601 alloy Inorganic materials 0.000 claims description 22
- 238000003825 pressing Methods 0.000 claims description 18
- 239000002002 slurry Substances 0.000 claims description 15
- 238000006243 chemical reaction Methods 0.000 claims description 14
- 230000002457 bidirectional effect Effects 0.000 claims description 13
- 238000005507 spraying Methods 0.000 claims description 13
- 239000012258 stirred mixture Substances 0.000 claims description 13
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 9
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 6
- QIJNJJZPYXGIQM-UHFFFAOYSA-N 1lambda4,2lambda4-dimolybdacyclopropa-1,2,3-triene Chemical compound [Mo]=C=[Mo] QIJNJJZPYXGIQM-UHFFFAOYSA-N 0.000 claims description 3
- 239000004925 Acrylic resin Substances 0.000 claims description 3
- 229920000178 Acrylic resin Polymers 0.000 claims description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims description 3
- 229910039444 MoC Inorganic materials 0.000 claims description 3
- 229920002873 Polyethylenimine Polymers 0.000 claims description 3
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 3
- JXOOCQBAIRXOGG-UHFFFAOYSA-N [B].[B].[B].[B].[B].[B].[B].[B].[B].[B].[B].[B].[Al] Chemical compound [B].[B].[B].[B].[B].[B].[B].[B].[B].[B].[B].[B].[Al] JXOOCQBAIRXOGG-UHFFFAOYSA-N 0.000 claims description 3
- LGLOITKZTDVGOE-UHFFFAOYSA-N boranylidynemolybdenum Chemical compound [Mo]#B LGLOITKZTDVGOE-UHFFFAOYSA-N 0.000 claims description 3
- 239000003822 epoxy resin Substances 0.000 claims description 3
- 239000000395 magnesium oxide Substances 0.000 claims description 3
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 3
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims description 3
- 229920006122 polyamide resin Polymers 0.000 claims description 3
- 229920000647 polyepoxide Polymers 0.000 claims description 3
- 229920000193 polymethacrylate Polymers 0.000 claims description 3
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims description 3
- 229910003470 tongbaite Inorganic materials 0.000 claims description 3
- UONOETXJSWQNOL-UHFFFAOYSA-N tungsten carbide Chemical compound [W+]#[C-] UONOETXJSWQNOL-UHFFFAOYSA-N 0.000 claims description 3
- 239000011787 zinc oxide Substances 0.000 claims description 3
- UFGZSIPAQKLCGR-UHFFFAOYSA-N chromium carbide Chemical compound [Cr]#C[Cr]C#[Cr] UFGZSIPAQKLCGR-UHFFFAOYSA-N 0.000 claims 1
- LNEPOXFFQSENCJ-UHFFFAOYSA-N haloperidol Chemical compound C1CC(O)(C=2C=CC(Cl)=CC=2)CCN1CCCC(=O)C1=CC=C(F)C=C1 LNEPOXFFQSENCJ-UHFFFAOYSA-N 0.000 claims 1
- 238000000227 grinding Methods 0.000 abstract description 9
- 239000002994 raw material Substances 0.000 abstract description 3
- 239000002131 composite material Substances 0.000 abstract description 2
- 238000000746 purification Methods 0.000 abstract description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 37
- 229910033181 TiB2 Inorganic materials 0.000 description 26
- 229910052799 carbon Inorganic materials 0.000 description 18
- 239000000126 substance Substances 0.000 description 14
- 238000005516 engineering process Methods 0.000 description 10
- 229920002565 Polyethylene Glycol 400 Polymers 0.000 description 9
- 229910021389 graphene Inorganic materials 0.000 description 9
- 239000007769 metal material Substances 0.000 description 9
- 238000003466 welding Methods 0.000 description 9
- 238000012360 testing method Methods 0.000 description 6
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 3
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical group [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 3
- 239000010936 titanium Substances 0.000 description 3
- 229910052719 titanium Inorganic materials 0.000 description 3
- 238000005452 bending Methods 0.000 description 2
- GVEHJMMRQRRJPM-UHFFFAOYSA-N chromium(2+);methanidylidynechromium Chemical compound [Cr+2].[Cr]#[C-].[Cr]#[C-] GVEHJMMRQRRJPM-UHFFFAOYSA-N 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 1
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 1
- 239000006004 Quartz sand Substances 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 238000003723 Smelting Methods 0.000 description 1
- 238000007545 Vickers hardness test Methods 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 238000000889 atomisation Methods 0.000 description 1
- 235000019658 bitter taste Nutrition 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 229910052796 boron Inorganic materials 0.000 description 1
- 239000006229 carbon black Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 239000011335 coal coke Substances 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 229910052593 corundum Inorganic materials 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 230000007794 irritation Effects 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 239000004005 microsphere Substances 0.000 description 1
- 239000011858 nanopowder Substances 0.000 description 1
- 229910052755 nonmetal Inorganic materials 0.000 description 1
- 150000002843 nonmetals Chemical class 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 239000004482 other powder Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000002006 petroleum coke Substances 0.000 description 1
- 238000013001 point bending Methods 0.000 description 1
- 238000006068 polycondensation reaction Methods 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000011819 refractory material Substances 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 238000004154 testing of material Methods 0.000 description 1
- 239000002023 wood Substances 0.000 description 1
- 229910001845 yogo sapphire Inorganic materials 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/56—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides
- C04B35/565—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on silicon carbide
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- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/62605—Treating the starting powders individually or as mixtures
- C04B35/6261—Milling
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/62605—Treating the starting powders individually or as mixtures
- C04B35/62695—Granulation or pelletising
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/64—Burning or sintering processes
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3217—Aluminum oxide or oxide forming salts thereof, e.g. bauxite, alpha-alumina
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/38—Non-oxide ceramic constituents or additives
- C04B2235/3804—Borides
- C04B2235/3813—Refractory metal borides
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Abstract
The invention relates to the technical field of composite material ceramic preparation, in particular to pressureless sintering silicon carbide bulletproof ceramic and a preparation method thereof. The pressureless sintering silicon carbide bulletproof ceramic is prepared from the following components in parts by weight: 96.5 to 98.5 parts of carbide A, 1.1 to 1.8 parts of carbide B, 0.1 to 1 part of boride, 12 to 18 parts of resin, 1 to 3 parts of oxide and 0.15 to 0.45 part of dispersing agent. A closed wet continuous grinding mode is adopted in a preparation process, so that raw material pollution in a grinding process is reduced; self-made silicon carbide balls are taken as a grinding medium, so that pollution-free grinding is realized, and the difficulty in powder purification is lowered; an atomizing granulation formula and a process are adopted, so that the technical indexes of granulated powder meet the technical requirements of imported similar products; the silicon carbide bulletproof ceramic prepared by adopting the process has high toughness and high strength.
Description
Technical Field
The invention relates to the technical field of composite ceramic preparation, in particular to pressureless sintering silicon carbide bulletproof ceramic and a preparation method thereof.
Background
The bulletproof ceramic is widely applied to safety protection of military equipment and special operation workers such as coal, mines and the like. In modern large-scale war and anti-violence and anti-terrorism, it is also very important to resist the damage of guns, cannons and missiles to military equipment and personnel. The application of the bulletproof ceramic plays a key role in reducing casualties, improving fighting capacity and increasing victory factors.
Silicon carbide ceramic is a novel ceramic material with excellent mechanical property, good oxidation resistance, corrosion resistance and high temperature performance, and has attracted extensive attention and application in industrial production due to its excellent mechanical, chemical and even electrical conductivity. Common silicon carbide ceramic products can be classified into reaction-sintered silicon carbide ceramics and pressureless solid-phase sintered silicon carbide ceramics according to different sintering modes.
At present, carbon microspheres (graphite or carbon black) are usually used as a carbon source in the preparation process of silicon carbide ceramic, but the carbon source has the problems of easy agglomeration, uneven carbon source dispersion, overlarge carbon particle size, limited ceramic density and the like before or in the sintering process due to the inherent form of the carbon source; in addition, in the preparation of silicon carbide ceramics at present, slurry is usually simply mixed before sintering, and since ceramic slurry formed by silicon carbide, a carbon source and other materials cannot be kept in a uniform and stable state in the sintering process (even before sintering), silicon carbide is not uniformly distributed, and the sintering temperature is improperly controlled, the temperature of each part in the sintering process is not uniform, the hardness and toughness of each part of the final ceramic product are not uniform, and the product quality is affected.
Disclosure of Invention
In order to solve the above problems, the first aspect of the present invention provides a pressureless sintered silicon carbide bulletproof ceramic, which comprises the following components in parts by weight: 96.5-98.5 parts of carbide A, 1.1-1.8 parts of carbide B, 0.1-1 part of boride, 12-18 parts of resin, 1-3 parts of oxide and 0.15-0.45 part of dispersant; the particle size of the carbide A is 50-500nm, the carbide A is silicon carbide, and the silicon carbide comprises 0.1-1 part of silicon carbide whiskers.
Preferably, the carbide B has a grain size of 50-500nm and is selected from one or more of boron carbide, tungsten carbide, chromium carbide and molybdenum carbide.
Further, the carbide B is boron carbide.
Preferably, the particle size of the boride is 30-80nm, and the boride is selected from one or more of titanium boride, aluminum boride and molybdenum boride.
Further, the boride is titanium boride.
Preferably, the resin is selected from one or more of acrylic resin, phenolic resin, polyamide resin and epoxy resin.
Preferably, the resin is a phenolic resin.
Further, the phenolic resin is water-soluble phenolic resin.
Further, the weight ratio of the water-soluble phenolic resin to the silicon carbide is 1: (1-10).
Furthermore, the weight ratio of the water-soluble phenolic resin to the silicon carbide is 1: 7.
Preferably, the dispersant is selected from one or more of ammonium polymethacrylate, polyethylene glycol and polyethyleneimine.
Further, the dispersant is polyethylene glycol.
Preferably, the boride to oxide weight ratio is 1: (1-10).
Further, the boride to oxide weight ratio is 1: (3-10).
Still further, the boride to oxide weight ratio is 1: 5.
preferably, the particle size of the oxide is 0.5-1 um.
Preferably, the oxide is selected from one or more of magnesium oxide, aluminum oxide, zinc oxide and titanium oxide.
Further, the oxide is alumina.
In the experimental process, it is unexpectedly found that when the water-soluble phenolic resin is added into the system, the electric charge of the nano powder is inconsistent, the dispersion of the powder can be influenced, the aluminum oxide is coated on the surface of the silicon carbide powder by grinding, so that the silicon carbide can be uniformly mixed with other powder, part of silicon carbide whiskers are added into the system, the prepared ceramic has uniform performance, and the electric charge performance of the system can be adjusted more uniformly and stably after the silicon carbide whiskers and the aluminum oxide are mixed, so that the bulletproof ceramic with better strength and toughness performance is obtained; dissolving in waterThe phenolic resin can better bond silicon carbide powder and improve the strength of ceramics, and the phenolic resin is carbonized at high temperature, can act with boron carbide and aluminum oxide in a synergistic manner to serve as a carbon source and reduce the generation of Si from silicon carbide at high temperature2The amount of O improves the free energy of the surface of the silicon carbide, improves the density of the ceramic and improves the strength of the ceramic.
The invention provides a preparation method of pressureless sintering silicon carbide bulletproof ceramic, which comprises the following steps:
(1) adding 96.5-98.5 parts of carbide A, 1.1-1.8 parts of carbide B, 0.1-1 part of boride, 12-18 parts of resin, 1-3 parts of oxide and 0.15-0.45 part of dispersing agent into a ball mill, carrying out ball milling and mixing for 18-30h, and putting the materials after ball milling and mixing into a stirring device to stir for 1-4 h;
(2) spraying the stirred mixture into a granulation tower, wherein the centrifugal frequency conversion of the granulation tower is 26-32HZ, the air inlet temperature is 250-280 ℃, the air outlet temperature is 100-120 ℃, and the slurry inlet pressure is 40-60MPa, so as to obtain granulation powder;
(3) placing the granulated powder in a hard alloy die for pressing to obtain a green body a, wherein the pressing mode is bidirectional pressurization, and the pressure tonnage of a machine tool is 150-1500 tons;
(4) putting the green body a pressed in the step 3 into a drying oven with the temperature of 80 ℃ for drying and curing for 0.5-2h to obtain a green body b;
(5) and placing the green bodies b on a graphite crucible or a graphite substrate with a radian, keeping 0.5-5cm of gap arrangement among the green bodies, placing the graphite crucible or the graphite substrate with the radian filled with the green bodies into a vacuum sintering furnace for sintering, setting the temperature of the sintering furnace to 2200-2250 ℃, keeping the temperature for 1-2h, closing a switch of the vacuum sintering furnace, and taking out the prepared silicon carbide bulletproof ceramic after the temperature is reduced to room temperature.
Further, the method comprises the following steps:
(1) adding 96.5-98.5 parts of silicon carbide, 1.1-1.8 parts of boron carbide, 0.1-1 part of titanium boride, 12-18 parts of water-soluble phenolic resin, 1-3 parts of alumina and 0.15-0.45 part of polyethylene glycol into a ball mill for ball-milling and mixing for 18-30h, and putting the ball-milled and mixed materials into a stirring device for stirring for 1-4 h;
(2) spraying the stirred mixture into a granulation tower, wherein the centrifugal frequency conversion of the granulation tower is 26-32HZ, the air inlet temperature is 250-280 ℃, the air outlet temperature is 100-120 ℃, and the slurry inlet pressure is 40-60MPa, so as to obtain granulation powder;
(3) placing the granulated powder in a hard alloy die for pressing to obtain a green body a, wherein the pressing mode is bidirectional pressurization, and the pressure tonnage of a machine tool is 150-1500 tons;
(4) putting the green body a pressed in the step 3 into a drying oven with the temperature of 80 ℃ for drying and curing for 0.5-2h to obtain a green body b;
(5) and placing the green bodies b on a graphite crucible or a graphite substrate with a radian, keeping 0.5-5cm of gap arrangement among the green bodies, placing the graphite crucible or the graphite substrate with the radian filled with the green bodies into a vacuum sintering furnace for sintering, setting the temperature of the sintering furnace to 2200-2250 ℃, keeping the temperature for 1-2h, closing a switch of the vacuum sintering furnace, and taking out the prepared silicon carbide bulletproof ceramic after the temperature is reduced to room temperature.
Advantageous effects
1. And a closed wet continuous grinding mode is adopted, so that raw material pollution in the grinding process is reduced.
2. Self-made silicon carbide balls are used as grinding media, pollution-free grinding is achieved, and the difficulty of powder purification is reduced.
3. The technical index of the granulated powder reaches the technical requirements of imported like products by adopting an atomization granulation formula and process.
4. The silicon carbide bulletproof ceramic prepared by the process has good toughness and high strength.
Detailed Description
The technical features of the technical solutions provided by the present invention are further clearly and completely described below with reference to the specific embodiments, and the scope of protection is not limited thereto.
The words "preferred", "more preferred", and the like, in the present invention refer to embodiments of the invention that may provide certain benefits, under certain circumstances. However, other embodiments may be preferred, under the same or other circumstances. Furthermore, the recitation of one or more preferred embodiments does not imply that other embodiments are not useful, nor is it intended to exclude other embodiments from the scope of the invention.
When a range of values is disclosed herein, the range is considered to be continuous and includes both the minimum and maximum values of the range, as well as each value between such minimum and maximum values. Further, when a range refers to an integer, each integer between the minimum and maximum values of the range is included. Further, when multiple range-describing features or characteristics are provided, the ranges may be combined. In other words, unless otherwise indicated, all ranges disclosed herein are to be understood to encompass any and all subranges subsumed therein. For example, a stated range from "1 to 10" should be considered to include any and all subranges between the minimum value of 1 and the maximum value of 10. Exemplary subranges of the range 1 to 10 include, but are not limited to, 1 to 6.1, 3.5 to 7.8, 5.5 to 10, and the like.
In order to solve the above problems, the first aspect of the present invention provides a pressureless sintered silicon carbide bulletproof ceramic, which comprises the following components in parts by weight: 96.5-98.5 parts of carbide A, 1.1-1.8 parts of carbide B, 0.1-1 part of boride, 12-18 parts of resin, 1-3 parts of oxide and 0.15-0.45 part of dispersant; the particle size of the carbide A is 50-500nm, the carbide A is silicon carbide, and the silicon carbide comprises 0.1-1 part of silicon carbide whiskers.
Silicon carbide: the silicon carbide is an inorganic substance, has a chemical formula of SiC, and is prepared by smelting quartz sand, petroleum coke (or coal coke), wood chips (salt is required when green silicon carbide is produced) and other raw materials in a resistance furnace at high temperature.
In a preferred embodiment, the silicon carbide supplier is aerospace Metal materials, Inc. under the designation 0311, and has an average particle size of 50 nm.
The silicon carbide whisker purchasing manufacturer is Suzhou carbon Feng graphene science and technology limited company, the model is TF-001, and the particle size is 0.1-2.5 um.
In a preferred embodiment, the carbide B has a particle size of 50 to 500nm and is selected from one or more of boron carbide, tungsten carbide, chromium carbide, and molybdenum carbide.
In a more preferred embodiment, the carbide B is boron carbide.
The boron carbide purchasing manufacturer is boron carbide powder of Wuhan Meiqilin new material Co., Ltd, and the particle size is 0.55 um.
In a preferred embodiment, the boride has a particle size of 30 to 80nm and is selected from one or more of titanium boride, aluminum boride and molybdenum boride.
Boride: binary compounds formed by boron, metals and certain nonmetals (such as carbon) can be represented by the general formula MmBn, are generally mesenchymal compounds and do not follow the valence rule.
In a more preferred embodiment, the boride is titanium boride.
In a most preferred embodiment, the titanium boride is titanium diboride.
In a more preferred embodiment, the titanium diboride manufacturer is Hebei Huazui alloy welding materials, Inc. model HZ-TiB2-02, with a 1um grain size.
In a preferred embodiment, the resin is selected from one or more of acrylic resin, phenolic resin, polyamide resin, epoxy resin.
In a more preferred embodiment, the resin is a phenolic resin.
In a most preferred embodiment, the phenolic resin is a water soluble phenolic resin.
Water-soluble phenolic resin: is prepared through the polycondensation of phenol and formaldehyde in the presence of alkali catalyst and proper control of the reaction end point.
In a preferred embodiment, the water-soluble phenolic resin is purchased from Hubei Hengheng technology, Inc. under CAS number 9000-71-9.
In a more preferred embodiment, the weight ratio of the water-soluble phenolic resin to the silicon carbide is 1: (1-10).
In a more preferred embodiment, the weight ratio of the water-soluble phenolic resin to the silicon carbide is 1: 7.
In a preferred embodiment, the dispersant is selected from one or more of ammonium polymethacrylate, polyethylene glycol and polyethyleneimine.
In a more preferred embodiment, the dispersant is polyethylene glycol.
Polyethylene glycol: is a high molecular polymer with the chemical formula of HO (CH)2CH2O)nH, no irritation, slightly bitter taste, good water solubility and good compatibility with a plurality of organic matter components.
In a more preferred embodiment, the polyethylene glycol purchaser is John's Henry chemical Co., Ltd, model number PEG-400.
In a preferred embodiment, the boride to oxide weight ratio is 1: (1-10).
In a more preferred embodiment, the boride to oxide weight ratio is 1: (3-10).
In a most preferred embodiment, the boride to oxide weight ratio is 1: 5.
in a preferred embodiment, the particle size of the oxide is 0.5 to 1 um.
In a preferred embodiment, the oxide is selected from one or more of magnesium oxide, aluminum oxide, zinc oxide, titanium oxide.
In a more preferred embodiment, the oxide is alumina.
Alumina, an inorganic substance, of the chemical formula Al2O3, is a high-hardness compound, has a melting point of 2054 ℃ and a boiling point of 2980 ℃, is an ionic crystal which can be ionized at high temperature, and is commonly used for manufacturing refractory materials.
The alumina is selected from Shanghai Suming industry Co., Ltd, and the specification is VITAL alumina granulation powder.
The invention provides a preparation method of pressureless sintering silicon carbide bulletproof ceramic, which comprises the following steps:
(1) adding 96.5-98.5 parts of carbide A, 1.1-1.8 parts of carbide B, 0.1-1 part of boride, 12-18 parts of resin, 1-3 parts of oxide and 0.15-0.45 part of dispersing agent into a ball mill, carrying out ball milling and mixing for 18-30h, and putting the materials after ball milling and mixing into a stirring device to stir for 1-4 h;
(2) spraying the stirred mixture into a granulation tower, wherein the centrifugal frequency conversion of the granulation tower is 26-32HZ, the air inlet temperature is 250-280 ℃, the air outlet temperature is 100-120 ℃, and the slurry inlet pressure is 40-60MPa, so as to obtain granulation powder;
(3) placing the granulated powder in a hard alloy die for pressing to obtain a green body a, wherein the pressing mode is bidirectional pressurization, and the pressure tonnage of a machine tool is 150-1500 tons;
(4) putting the green body a pressed in the step 3 into a drying oven with the temperature of 80 ℃ for drying and curing for 0.5-2h to obtain a green body b;
(5) and placing the green bodies b on a graphite crucible or a graphite substrate with a radian, keeping 0.5-5cm of gap arrangement among the green bodies, placing the graphite crucible or the graphite substrate with the radian filled with the green bodies into a vacuum sintering furnace for sintering, setting the temperature of the sintering furnace to 2200-2250 ℃, keeping the temperature for 1-2h, closing a switch of the vacuum sintering furnace, and taking out the prepared silicon carbide bulletproof ceramic after the temperature is reduced to room temperature.
In a preferred embodiment, the method comprises the following steps:
(1) adding 96.5-98.5 parts of silicon carbide, 1.1-1.8 parts of boron carbide, 0.1-1 part of titanium boride, 12-18 parts of water-soluble phenolic resin, 1-3 parts of alumina and 0.15-0.45 part of polyethylene glycol into a ball mill for ball-milling and mixing for 18-30h, and putting the ball-milled and mixed materials into a stirring device for stirring for 1-4 h;
(2) spraying the stirred mixture into a granulation tower, wherein the centrifugal frequency conversion of the granulation tower is 26-32HZ, the air inlet temperature is 250-280 ℃, the air outlet temperature is 100-120 ℃, and the slurry inlet pressure is 40-60MPa, so as to obtain granulation powder;
(3) placing the granulated powder in a hard alloy die for pressing to obtain a green body a, wherein the pressing mode is bidirectional pressurization, and the pressure tonnage of a machine tool is 150-1500 tons;
(4) putting the green body a pressed in the step 3 into a drying oven with the temperature of 80 ℃ for drying and curing for 0.5-2h to obtain a green body b;
(5) and placing the green bodies b on a graphite crucible or a graphite substrate with a radian, keeping 0.5-5cm of gap arrangement among the green bodies, placing the graphite crucible or the graphite substrate with the radian filled with the green bodies into a vacuum sintering furnace for sintering, setting the temperature of the sintering furnace to 2200-2250 ℃, keeping the temperature for 1-2h, closing a switch of the vacuum sintering furnace, and taking out the prepared silicon carbide bulletproof ceramic after the temperature is reduced to room temperature.
Example 1
A pressureless sintering silicon carbide bulletproof ceramic comprises the following components in parts by weight: 97.4 parts of silicon carbide, 0.6 part of silicon carbide whisker, 1.5 parts of boron carbide, 0.4 part of titanium diboride, 14 parts of water-soluble phenolic resin, 2 parts of alumina and 0.3 part of polyethylene glycol.
The silicon carbide purchasing manufacturer is aerospace metal materials, and has a mark of 0311 and an average particle size of 50 nm.
The silicon carbide whisker purchasing manufacturer is Suzhou carbon Feng graphene science and technology limited company, the model is TF-001, and the particle size is 0.1-2.5 um.
The boron carbide purchasing manufacturer is Wuhan Meiqilin new material Co., Ltd, and the particle size is 0.55 um.
The titanium diboride purchasing manufacturer is Hebei Huazui alloy welding material limited company, the model is HZ-TiB2-02, and the grain diameter is 1 um.
The water-soluble phenolic resin is purchased from Hubei Hengheng science and technology Co., Ltd, and the CAS number is 9000-71-9.
The polyethylene glycol purchasing manufacturer is Jiangsu Henheng chemical industry Co., Ltd, and the model is PEG-400.
The alumina is selected from Shanghai Suming industry Co., Ltd, and the specification is VITAL alumina granulation powder.
A preparation method of pressureless sintering silicon carbide bulletproof ceramic comprises the following steps:
(1) adding 97.4 parts of silicon carbide, 0.6 part of silicon carbide whisker, 1.5 parts of boron carbide, 0.4 part of titanium diboride, 14 parts of water-soluble phenolic resin, 2 parts of alumina and 0.3 part of polyethylene glycol into a ball mill, carrying out ball milling and mixing for 24 hours, and putting the materials after ball milling and mixing into a stirring device for stirring for 2 hours;
(2) spraying the stirred mixture into a granulation tower, wherein the centrifugal frequency conversion of the granulation tower is 28HZ, the air inlet temperature is 265 ℃, the air outlet temperature is 110 ℃, and the slurry inlet pressure is 50MPa, so as to obtain granulation powder;
(3) placing the granulated powder in a hard alloy die to be pressed to obtain a green body a, wherein the pressing mode is bidirectional pressurization, and the pressure tonnage of a machine tool is 350 tons;
(4) putting the green body a pressed in the step 3 into a drying oven at 80 ℃ for drying and curing for 1h to obtain a green body b;
(5) and (3) placing the green bodies b on a graphite crucible or a graphite substrate with radian, keeping 2cm of gap arrangement among the green bodies, placing the graphite crucible or the graphite substrate with the radian filled with the green bodies into a vacuum sintering furnace for sintering, setting the temperature of the sintering furnace at 2250 ℃, keeping the temperature for 2h, closing a switch of the vacuum sintering furnace, and taking out the prepared silicon carbide bulletproof ceramic after the temperature is reduced to room temperature.
Example 2
A pressureless sintering silicon carbide bulletproof ceramic comprises the following components in parts by weight: 97.5 parts of silicon carbide, 1 part of silicon carbide whisker, 1.8 parts of boron carbide, 1 part of titanium diboride, 18 parts of water-soluble phenolic resin, 3 parts of aluminum oxide and 0.45 part of polyethylene glycol.
The silicon carbide purchasing manufacturer is aerospace metal materials, and has a mark of 0311 and an average particle size of 50 nm.
The silicon carbide whisker purchasing manufacturer is Suzhou carbon Feng graphene science and technology limited company, the model is TF-001, and the particle size is 0.1-2.5 um.
The boron carbide purchasing manufacturer is Wuhan Meiqilin new material Co., Ltd, and the particle size is 0.55 um.
The titanium diboride purchasing manufacturer is Hebei Huazui alloy welding material limited company, the model is HZ-TiB2-02, and the grain diameter is 1 um.
The water-soluble phenolic resin is purchased from Hubei Hengheng science and technology Co., Ltd, and the CAS number is 9000-71-9.
The polyethylene glycol purchasing manufacturer is Jiangsu Henheng chemical industry Co., Ltd, and the model is PEG-400.
The alumina is selected from Shanghai Suming industry Co., Ltd, and the specification is VITAL alumina granulation powder.
A preparation method of pressureless sintering silicon carbide bulletproof ceramic comprises the following steps:
(1) adding 97.5 parts of silicon carbide, 1 part of silicon carbide whisker, 1.8 parts of boron carbide, 1 part of titanium diboride, 18 parts of water-soluble phenolic resin, 3 parts of aluminum oxide and 0.45 part of polyethylene glycol into a ball mill, carrying out ball milling and mixing for 24 hours, and putting the materials subjected to ball milling and mixing into a stirring device, and stirring for 2 hours;
(2) spraying the stirred mixture into a granulation tower, wherein the centrifugal frequency conversion of the granulation tower is 28HZ, the air inlet temperature is 265 ℃, the air outlet temperature is 110 ℃, and the slurry inlet pressure is 50MPa, so as to obtain granulation powder;
(3) placing the granulated powder in a hard alloy die to be pressed to obtain a green body a, wherein the pressing mode is bidirectional pressurization, and the pressure tonnage of a machine tool is 350 tons;
(4) putting the green body a pressed in the step 3 into a drying oven at 80 ℃ for drying and curing for 1h to obtain a green body b;
(5) and (3) placing the green bodies b on a graphite crucible or a graphite substrate with radian, keeping 2cm of gap arrangement among the green bodies, placing the graphite crucible or the graphite substrate with the radian filled with the green bodies into a vacuum sintering furnace for sintering, setting the temperature of the sintering furnace at 2250 ℃, keeping the temperature for 2h, closing a switch of the vacuum sintering furnace, and taking out the prepared silicon carbide bulletproof ceramic after the temperature is reduced to room temperature.
Example 3
A pressureless sintering silicon carbide bulletproof ceramic comprises the following components in parts by weight: 96.4 parts of silicon carbide, 0.1 part of silicon carbide whisker, 1.1 parts of boron carbide, 0.1 part of titanium diboride, 12 parts of water-soluble phenolic resin, 1 part of alumina and 0.15 part of polyethylene glycol.
The silicon carbide purchasing manufacturer is aerospace metal materials, and has a mark of 0311 and an average particle size of 50 nm.
The silicon carbide whisker purchasing manufacturer is Suzhou carbon Feng graphene science and technology limited company, the model is TF-001, and the particle size is 0.1-2.5 um.
The boron carbide purchasing manufacturer is Wuhan Meiqilin new material Co., Ltd, and the particle size is 0.55 um.
The titanium diboride purchasing manufacturer is Hebei Huazui alloy welding material limited company, the model is HZ-TiB2-02, and the grain diameter is 1 um.
The water-soluble phenolic resin is purchased from Hubei Hengheng science and technology Co., Ltd, and the CAS number is 9000-71-9.
The polyethylene glycol purchasing manufacturer is Jiangsu Henheng chemical industry Co., Ltd, and the model is PEG-400.
The alumina is selected from Shanghai Suming industry Co., Ltd, and the specification is VITAL alumina granulation powder.
A preparation method of pressureless sintering silicon carbide bulletproof ceramic comprises the following steps:
(1) adding 96.4 parts of silicon carbide, 0.1 part of silicon carbide whisker, 1.1 parts of boron carbide, 0.1 part of titanium diboride, 12 parts of water-soluble phenolic resin, 1 part of alumina and 0.15 part of polyethylene glycol into a ball mill, carrying out ball milling and mixing for 24 hours, and putting the materials after ball milling and mixing into a stirring device for stirring for 2 hours;
(2) spraying the stirred mixture into a granulation tower, wherein the centrifugal frequency conversion of the granulation tower is 28HZ, the air inlet temperature is 265 ℃, the air outlet temperature is 110 ℃, and the slurry inlet pressure is 50MPa, so as to obtain granulation powder;
(3) placing the granulated powder in a hard alloy die to be pressed to obtain a green body a, wherein the pressing mode is bidirectional pressurization, and the pressure tonnage of a machine tool is 350 tons;
(4) putting the green body a pressed in the step 3 into a drying oven at 80 ℃ for drying and curing for 1h to obtain a green body b;
(5) and (3) placing the green bodies b on a graphite crucible or a graphite substrate with radian, keeping 2cm of gap arrangement among the green bodies, placing the graphite crucible or the graphite substrate with the radian filled with the green bodies into a vacuum sintering furnace for sintering, setting the temperature of the sintering furnace at 2250 ℃, keeping the temperature for 2h, closing a switch of the vacuum sintering furnace, and taking out the prepared silicon carbide bulletproof ceramic after the temperature is reduced to room temperature.
Example 4
A pressureless sintering silicon carbide bulletproof ceramic comprises the following components in parts by weight: 98 parts of silicon carbide, 1.5 parts of boron carbide, 0.4 part of titanium diboride, 14 parts of water-soluble phenolic resin, 2 parts of alumina and 0.3 part of polyethylene glycol.
The silicon carbide purchasing manufacturer is aerospace metal materials, and has a mark of 0311 and an average particle size of 50 nm.
The silicon carbide whisker purchasing manufacturer is Suzhou carbon Feng graphene science and technology limited company, the model is TF-001, and the particle size is 0.1-2.5 um.
The boron carbide purchasing manufacturer is Wuhan Meiqilin new material Co., Ltd, and the particle size is 0.55 um.
The titanium diboride purchasing manufacturer is Hebei Huazui alloy welding material limited company, the model is HZ-TiB2-02, and the grain diameter is 1 um.
The water-soluble phenolic resin is purchased from Hubei Hengheng science and technology Co., Ltd, and the CAS number is 9000-71-9.
The polyethylene glycol purchasing manufacturer is Jiangsu Henheng chemical industry Co., Ltd, and the model is PEG-400.
The alumina is selected from Shanghai Suming industry Co., Ltd, and the specification is VITAL alumina granulation powder.
A preparation method of pressureless sintering silicon carbide bulletproof ceramic comprises the following steps:
(1) adding 98 parts of silicon carbide, 1.5 parts of boron carbide, 0.4 part of titanium diboride, 14 parts of water-soluble phenolic resin, 2 parts of alumina and 0.3 part of polyethylene glycol into a ball mill for ball milling and mixing for 24 hours, and putting the materials after ball milling and mixing into a stirring device for stirring for 2 hours;
(2) spraying the stirred mixture into a granulation tower, wherein the centrifugal frequency conversion of the granulation tower is 28HZ, the air inlet temperature is 265 ℃, the air outlet temperature is 110 ℃, and the slurry inlet pressure is 50MPa, so as to obtain granulation powder;
(3) placing the granulated powder in a hard alloy die to be pressed to obtain a green body a, wherein the pressing mode is bidirectional pressurization, and the pressure tonnage of a machine tool is 350 tons;
(4) putting the green body a pressed in the step 3 into a drying oven at 80 ℃ for drying and curing for 1h to obtain a green body b;
(5) and (3) placing the green bodies b on a graphite crucible or a graphite substrate with radian, keeping 2cm of gap arrangement among the green bodies, placing the graphite crucible or the graphite substrate with the radian filled with the green bodies into a vacuum sintering furnace for sintering, setting the temperature of the sintering furnace at 2250 ℃, keeping the temperature for 2h, closing a switch of the vacuum sintering furnace, and taking out the prepared silicon carbide bulletproof ceramic after the temperature is reduced to room temperature.
Example 5
A pressureless sintering silicon carbide bulletproof ceramic comprises the following components in parts by weight: 97.4 parts of silicon carbide, 0.6 part of silicon carbide whisker, 1.5 parts of boron carbide, 0.4 part of titanium diboride, 8 parts of water-soluble phenolic resin, 2 parts of alumina and 0.3 part of polyethylene glycol.
The silicon carbide purchasing manufacturer is aerospace metal materials, and has a mark of 0311 and an average particle size of 50 nm.
The silicon carbide whisker purchasing manufacturer is Suzhou carbon Feng graphene science and technology limited company, the model is TF-001, and the particle size is 0.1-2.5 um.
The boron carbide purchasing manufacturer is Wuhan Meiqilin new material Co., Ltd, and the particle size is 0.55 um.
The titanium diboride purchasing manufacturer is Hebei Huazui alloy welding material limited company, the model is HZ-TiB2-02, and the grain diameter is 1 um.
The water-soluble phenolic resin is purchased from Hubei Hengheng science and technology Co., Ltd, and the CAS number is 9000-71-9.
The polyethylene glycol purchasing manufacturer is Jiangsu Henheng chemical industry Co., Ltd, and the model is PEG-400.
The alumina is selected from Shanghai Suming industry Co., Ltd, and the specification is VITAL alumina granulation powder.
A preparation method of pressureless sintering silicon carbide bulletproof ceramic comprises the following steps:
(1) adding 97.4 parts of silicon carbide, 0.6 part of silicon carbide whisker, 1.5 parts of boron carbide, 0.4 part of titanium diboride, 8 parts of water-soluble phenolic resin, 2 parts of alumina and 0.3 part of polyethylene glycol into a ball mill, carrying out ball milling and mixing for 24 hours, and putting the materials subjected to ball milling and mixing into a stirring device for stirring for 2 hours;
(2) spraying the stirred mixture into a granulation tower, wherein the centrifugal frequency conversion of the granulation tower is 28HZ, the air inlet temperature is 265 ℃, the air outlet temperature is 110 ℃, and the slurry inlet pressure is 50MPa, so as to obtain granulation powder;
(3) placing the granulated powder in a hard alloy die to be pressed to obtain a green body a, wherein the pressing mode is bidirectional pressurization, and the pressure tonnage of a machine tool is 350 tons;
(4) putting the green body a pressed in the step 3 into a drying oven at 80 ℃ for drying and curing for 1h to obtain a green body b;
(5) and (3) placing the green bodies b on a graphite crucible or a graphite substrate with radian, keeping 2cm of gap arrangement among the green bodies, placing the graphite crucible or the graphite substrate with the radian filled with the green bodies into a vacuum sintering furnace for sintering, setting the temperature of the sintering furnace at 2250 ℃, keeping the temperature for 2h, closing a switch of the vacuum sintering furnace, and taking out the prepared silicon carbide bulletproof ceramic after the temperature is reduced to room temperature.
Example 6
A pressureless sintering silicon carbide bulletproof ceramic comprises the following components in parts by weight: 97.4 parts of silicon carbide, 0.6 part of silicon carbide whisker, 1.5 parts of boron carbide, 0.05 part of titanium diboride, 14 parts of water-soluble phenolic resin, 2 parts of alumina and 0.3 part of polyethylene glycol.
The silicon carbide purchasing manufacturer is aerospace metal materials, and has a mark of 0311 and an average particle size of 50 nm.
The silicon carbide whisker purchasing manufacturer is Suzhou carbon Feng graphene science and technology limited company, the model is TF-001, and the particle size is 0.1-2.5 um.
The boron carbide purchasing manufacturer is Wuhan Meiqilin new material Co., Ltd, and the particle size is 0.55 um.
The titanium diboride purchasing manufacturer is Hebei Huazui alloy welding material limited company, the model is HZ-TiB2-02, and the grain diameter is 1 um.
The water-soluble phenolic resin is purchased from Hubei Hengheng science and technology Co., Ltd, and the CAS number is 9000-71-9.
The polyethylene glycol purchasing manufacturer is Jiangsu Henheng chemical industry Co., Ltd, and the model is PEG-400.
The alumina is selected from Shanghai Suming industry Co., Ltd, and the specification is VITAL alumina granulation powder.
A preparation method of pressureless sintering silicon carbide bulletproof ceramic comprises the following steps:
(1) adding 97.4 parts of silicon carbide, 0.6 part of silicon carbide whisker, 1.5 parts of boron carbide, 0.05 part of titanium diboride, 14 parts of water-soluble phenolic resin, 2 parts of aluminum oxide and 0.3 part of polyethylene glycol into a ball mill, carrying out ball milling and mixing for 24 hours, and putting the materials subjected to ball milling and mixing into a stirring device, and stirring for 2 hours;
(2) spraying the stirred mixture into a granulation tower, wherein the centrifugal frequency conversion of the granulation tower is 28HZ, the air inlet temperature is 265 ℃, the air outlet temperature is 110 ℃, and the slurry inlet pressure is 50MPa, so as to obtain granulation powder;
(3) placing the granulated powder in a hard alloy die to be pressed to obtain a green body a, wherein the pressing mode is bidirectional pressurization, and the pressure tonnage of a machine tool is 350 tons;
(4) putting the green body a pressed in the step 3 into a drying oven at 80 ℃ for drying and curing for 1h to obtain a green body b;
(5) and (3) placing the green bodies b on a graphite crucible or a graphite substrate with radian, keeping 2cm of gap arrangement among the green bodies, placing the graphite crucible or the graphite substrate with the radian filled with the green bodies into a vacuum sintering furnace for sintering, setting the temperature of the sintering furnace at 2250 ℃, keeping the temperature for 2h, closing a switch of the vacuum sintering furnace, and taking out the prepared silicon carbide bulletproof ceramic after the temperature is reduced to room temperature.
Example 7
A pressureless sintering silicon carbide bulletproof ceramic comprises the following components in parts by weight: 97.4 parts of silicon carbide, 0.6 part of silicon carbide whisker, 1.5 parts of boron carbide, 0.4 part of titanium diboride, 14 parts of water-soluble phenolic resin, 0.3 part of alumina and 0.3 part of polyethylene glycol.
The silicon carbide purchasing manufacturer is aerospace metal materials, and has a mark of 0311 and an average particle size of 50 nm.
The silicon carbide whisker purchasing manufacturer is Suzhou carbon Feng graphene science and technology limited company, the model is TF-001, and the particle size is 0.1-2.5 um.
The boron carbide purchasing manufacturer is Wuhan Meiqilin new material Co., Ltd, and the particle size is 0.55 um.
The titanium diboride purchasing manufacturer is Hebei Huazui alloy welding material limited company, the model is HZ-TiB2-02, and the grain diameter is 1 um.
The water-soluble phenolic resin is purchased from Hubei Hengheng science and technology Co., Ltd, and the CAS number is 9000-71-9.
The polyethylene glycol purchasing manufacturer is Jiangsu Henheng chemical industry Co., Ltd, and the model is PEG-400.
The alumina is selected from Shanghai Suming industry Co., Ltd, and the specification is VITAL alumina granulation powder.
A preparation method of pressureless sintering silicon carbide bulletproof ceramic comprises the following steps:
(1) adding 97.4 parts of silicon carbide, 0.6 part of silicon carbide whisker, 1.5 parts of boron carbide, 0.4 part of titanium diboride, 14 parts of water-soluble phenolic resin, 0.3 part of alumina and 0.3 part of polyethylene glycol into a ball mill, carrying out ball milling and mixing for 24 hours, and putting the materials subjected to ball milling and mixing into a stirring device, and stirring for 2 hours;
(2) spraying the stirred mixture into a granulation tower, wherein the centrifugal frequency conversion of the granulation tower is 28HZ, the air inlet temperature is 265 ℃, the air outlet temperature is 110 ℃, and the slurry inlet pressure is 50MPa, so as to obtain granulation powder;
(3) placing the granulated powder in a hard alloy die to be pressed to obtain a green body a, wherein the pressing mode is bidirectional pressurization, and the pressure tonnage of a machine tool is 350 tons;
(4) putting the green body a pressed in the step 3 into a drying oven at 80 ℃ for drying and curing for 1h to obtain a green body b;
(5) and (3) placing the green bodies b on a graphite crucible or a graphite substrate with radian, keeping 2cm of gap arrangement among the green bodies, placing the graphite crucible or the graphite substrate with the radian filled with the green bodies into a vacuum sintering furnace for sintering, setting the temperature of the sintering furnace at 2250 ℃, keeping the temperature for 2h, closing a switch of the vacuum sintering furnace, and taking out the prepared silicon carbide bulletproof ceramic after the temperature is reduced to room temperature.
Example 8
A pressureless sintering silicon carbide bulletproof ceramic comprises the following components in parts by weight: 97.4 parts of silicon carbide, 0.6 part of silicon carbide whisker, 1.5 parts of boron carbide, 0.4 part of titanium diboride, 14 parts of water-soluble phenolic resin, 2 parts of alumina and 0.3 part of polyethylene glycol.
The silicon carbide purchasing manufacturer is aerospace metal materials, and has a mark of 0311 and an average particle size of 50 nm.
The silicon carbide whisker purchasing manufacturer is Suzhou carbon Feng graphene science and technology limited company, the model is TF-001, and the particle size is 0.1-2.5 um.
The boron carbide purchasing manufacturer is Wuhan Meiqilin new material Co., Ltd, and the particle size is 0.55 um.
The titanium diboride purchasing manufacturer is Hebei Huazui alloy welding material limited company, the model is HZ-TiB2-02, and the grain diameter is 1 um.
The water-soluble phenolic resin is purchased from Hubei Hengheng science and technology Co., Ltd, and the CAS number is 9000-71-9.
The polyethylene glycol purchasing manufacturer is Jiangsu Henheng chemical industry Co., Ltd, and the model is PEG-400.
The alumina is selected from Shanghai Suming industry Co., Ltd, and the specification is VITAL alumina granulation powder.
A preparation method of pressureless sintering silicon carbide bulletproof ceramic comprises the following steps:
(1) adding 97.4 parts of silicon carbide, 0.6 part of silicon carbide whisker, 1.5 parts of boron carbide, 0.4 part of titanium diboride, 14 parts of water-soluble phenolic resin, 2 parts of alumina and 0.3 part of polyethylene glycol into a ball mill, carrying out ball milling and mixing for 24 hours, and putting the materials after ball milling and mixing into a stirring device for stirring for 2 hours;
(2) spraying the stirred mixture into a granulation tower, wherein the centrifugal frequency conversion of the granulation tower is 28HZ, the air inlet temperature is 265 ℃, the air outlet temperature is 110 ℃, and the slurry inlet pressure is 50MPa, so as to obtain granulation powder;
(3) placing the granulated powder in a hard alloy die to be pressed to obtain a green body a, wherein the pressing mode is bidirectional pressurization, and the pressure tonnage of a machine tool is 350 tons;
(4) putting the green body a pressed in the step 3 into a drying oven at 80 ℃ for drying and curing for 1h to obtain a green body b;
(5) and placing the green bodies b on a graphite crucible or a graphite substrate with radian, keeping 2cm of gap arrangement among the green bodies, placing the graphite crucible or the graphite substrate with radian filled with the green bodies into a vacuum sintering furnace for sintering, setting the temperature of the sintering furnace at 2300 ℃, keeping the temperature for 2h, closing a switch of the vacuum sintering furnace, and taking out the prepared silicon carbide bulletproof ceramic after the temperature is reduced to room temperature.
Performance testing
1. Testing of sintering density: the sintered density of the sample was measured using a densitometer using archimedes' principle.
2. And (3) testing the bending strength: the three-point bending strength was measured in an INSTRON-5566 universal material testing machine using digital display bending strength, with a test specimen specification of 3mm x 4mm x 36mm, span of 20mm, and loading speed of 0.5 mm/min.
3. Vickers hardness test: the vickers hardness of the test specimen was measured using a digital vickers hardness tester.
The silicon carbide ballistic resistant ceramics prepared in examples 1-8 were tested for performance using the test methods described above and the test data is shown in table 1.
TABLE 1
The description and applications of the present invention are illustrative, and not intended to limit the scope of the invention to the embodiments described above, therefore, the present invention is not limited by the embodiments, and any technical solutions obtained by equivalent substitution are within the scope of the present invention.
Claims (10)
1. The pressureless sintered silicon carbide bulletproof ceramic is characterized by comprising the following components in parts by weight: 96.5-98.5 parts of carbide A, 1.1-1.8 parts of carbide B, 0.1-1 part of boride, 12-18 parts of resin, 1-3 parts of oxide and 0.15-0.45 part of dispersant; the particle size of the carbide A is 50-500nm, the carbide A is silicon carbide, and the silicon carbide comprises 0.1-1 part of silicon carbide whiskers.
2. The pressureless sintered silicon carbide ballistic resistant ceramic of claim 1, wherein the carbide B has a particle size of 50-500nm and is selected from one or more of boron carbide, tungsten carbide, chromium carbide, molybdenum carbide.
3. The pressureless sintered silicon carbide ballistic resistant ceramic of claim 1, wherein the boride has a particle size of 30-80nm and is selected from one or more of titanium boride, aluminum boride, molybdenum boride.
4. The pressureless sintered silicon carbide ballistic ceramic of claim 1, wherein the resin is selected from one or more of acrylic resins, phenolic resins, polyamide resins, epoxy resins.
5. The pressureless sintered silicon carbide ballistic ceramic of claim 4, wherein the resin is a phenolic resin.
6. The pressureless sintered silicon carbide ballistic resistant ceramic of claim 1, wherein the dispersant is selected from one or more of ammonium polymethacrylate, polyethylene glycol, polyethylene imine.
7. The pressureless sintered silicon carbide ballistic ceramic of claim 1, wherein the boride to oxide weight ratio is from 1: (1-10).
8. The pressureless sintered silicon carbide ballistic ceramic of claim 7, wherein the boride to oxide weight ratio is from 1: (3-10).
9. The pressureless sintered silicon carbide ballistic resistant ceramic of claim 1 wherein the oxide has a particle size of 0.5-1um and is selected from one or more of magnesium oxide, aluminum oxide, zinc oxide, titanium oxide.
10. A method for preparing pressureless sintered silicon carbide ballistic ceramics according to claim 1, comprising the steps of:
(1) adding 96.5-98.5 parts of carbide A, 1.1-1.8 parts of carbide B, 0.1-1 part of boride, 12-18 parts of resin, 1-3 parts of oxide and 0.15-0.45 part of dispersing agent into a ball mill, carrying out ball milling and mixing for 18-30h, and putting the materials after ball milling and mixing into a stirring device to stir for 1-4 h;
(2) spraying the stirred mixture into a granulation tower, wherein the centrifugal frequency conversion of the granulation tower is 26-32HZ, the air inlet temperature is 250-280 ℃, the air outlet temperature is 100-120 ℃, and the slurry inlet pressure is 40-60MPa, so as to obtain granulation powder;
(3) placing the granulated powder in a hard alloy die for pressing to obtain a green body a, wherein the pressing mode is bidirectional pressurization, and the pressure tonnage of a machine tool is 150-1500 tons;
(4) putting the green body a pressed in the step 3 into a drying oven with the temperature of 80 ℃ for drying and curing for 0.5-2h to obtain a green body b;
(5) and placing the green bodies b on a graphite crucible or a graphite substrate with a radian, keeping 0.5-5cm of gap arrangement among the green bodies, placing the graphite crucible or the graphite substrate with the radian filled with the green bodies into a vacuum sintering furnace for sintering, setting the temperature of the sintering furnace to 2200-2250 ℃, keeping the temperature for 1-2h, closing a switch of the vacuum sintering furnace, and taking out the prepared silicon carbide bulletproof ceramic after the temperature is reduced to room temperature.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113480314A (en) * | 2021-07-30 | 2021-10-08 | 浙江吉成新材股份有限公司 | Boron carbide ceramic pressureless sintering preparation process |
| CN113912399A (en) * | 2021-12-15 | 2022-01-11 | 山东金鸿新材料股份有限公司 | Preparation method of high-density pressureless sintered silicon carbide ceramic |
| CN114621012A (en) * | 2022-03-17 | 2022-06-14 | 景德镇华迅特种陶瓷有限公司 | Preparation method of bulletproof boron carbide composite ceramic |
| CN116675546A (en) * | 2023-07-31 | 2023-09-01 | 湖南华威景程材料科技有限公司 | Composite ceramic and protective plugboard based on titanium boride |
| CN116924771A (en) * | 2023-08-15 | 2023-10-24 | 应县通盛陶瓷有限公司 | Domestic ceramic with smooth surface and preparation process thereof |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1803714A (en) * | 2006-01-18 | 2006-07-19 | 山东大学 | Boron carbide based bulletproof composite ceramic and preparation method thereof |
| CN105198434A (en) * | 2014-05-28 | 2015-12-30 | 扬州三山工业陶瓷有限公司 | High-performance pressureless sintered silicon carbide bulletproof ceramic and preparation method thereof |
| CN110484795A (en) * | 2019-08-30 | 2019-11-22 | 潍坊华美精细技术陶瓷股份有限公司 | A kind of silicon carbide-based bulletproof composite ceramic and its preparation process |
| KR20200112008A (en) * | 2019-03-20 | 2020-10-05 | 국방과학연구소 | Silicon carbide ceramic armor containing zirconium diboride as an additive and manufacturing method thereof |
-
2021
- 2021-03-09 CN CN202110255600.2A patent/CN112851355A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1803714A (en) * | 2006-01-18 | 2006-07-19 | 山东大学 | Boron carbide based bulletproof composite ceramic and preparation method thereof |
| CN105198434A (en) * | 2014-05-28 | 2015-12-30 | 扬州三山工业陶瓷有限公司 | High-performance pressureless sintered silicon carbide bulletproof ceramic and preparation method thereof |
| KR20200112008A (en) * | 2019-03-20 | 2020-10-05 | 국방과학연구소 | Silicon carbide ceramic armor containing zirconium diboride as an additive and manufacturing method thereof |
| CN110484795A (en) * | 2019-08-30 | 2019-11-22 | 潍坊华美精细技术陶瓷股份有限公司 | A kind of silicon carbide-based bulletproof composite ceramic and its preparation process |
Non-Patent Citations (1)
| Title |
|---|
| 强亮生等: "《新型功能材料制备技术与分析表征方法》", 30 June 2017, 哈尔滨工业大学出版社 * |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113480314A (en) * | 2021-07-30 | 2021-10-08 | 浙江吉成新材股份有限公司 | Boron carbide ceramic pressureless sintering preparation process |
| CN113912399A (en) * | 2021-12-15 | 2022-01-11 | 山东金鸿新材料股份有限公司 | Preparation method of high-density pressureless sintered silicon carbide ceramic |
| CN113912399B (en) * | 2021-12-15 | 2022-02-25 | 山东金鸿新材料股份有限公司 | Preparation method of high-density pressureless sintered silicon carbide ceramic |
| CN114621012A (en) * | 2022-03-17 | 2022-06-14 | 景德镇华迅特种陶瓷有限公司 | Preparation method of bulletproof boron carbide composite ceramic |
| CN114621012B (en) * | 2022-03-17 | 2022-11-25 | 景德镇华迅特种陶瓷有限公司 | Preparation method of bulletproof boron carbide composite ceramic |
| CN116675546A (en) * | 2023-07-31 | 2023-09-01 | 湖南华威景程材料科技有限公司 | Composite ceramic and protective plugboard based on titanium boride |
| CN116675546B (en) * | 2023-07-31 | 2023-09-29 | 湖南华威景程材料科技有限公司 | Composite ceramic and protective plugboard based on titanium boride |
| CN116924771A (en) * | 2023-08-15 | 2023-10-24 | 应县通盛陶瓷有限公司 | Domestic ceramic with smooth surface and preparation process thereof |
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