CN116675546B - Composite ceramic and protective plugboard based on titanium boride - Google Patents
Composite ceramic and protective plugboard based on titanium boride Download PDFInfo
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- CN116675546B CN116675546B CN202310949285.2A CN202310949285A CN116675546B CN 116675546 B CN116675546 B CN 116675546B CN 202310949285 A CN202310949285 A CN 202310949285A CN 116675546 B CN116675546 B CN 116675546B
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- titanium boride
- composite ceramic
- graphene
- aluminum oxide
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- 239000000919 ceramic Substances 0.000 title claims abstract description 60
- 239000002131 composite material Substances 0.000 title claims abstract description 41
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 title claims abstract description 34
- 239000010936 titanium Substances 0.000 title claims abstract description 32
- 229910052719 titanium Inorganic materials 0.000 title claims abstract description 32
- 230000001681 protective effect Effects 0.000 title claims abstract description 14
- 239000000463 material Substances 0.000 claims abstract description 36
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 31
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 31
- 239000000835 fiber Substances 0.000 claims abstract description 25
- 229910052580 B4C Inorganic materials 0.000 claims abstract description 21
- INAHAJYZKVIDIZ-UHFFFAOYSA-N boron carbide Chemical compound B12B3B4C32B41 INAHAJYZKVIDIZ-UHFFFAOYSA-N 0.000 claims abstract description 21
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims abstract description 21
- 229910052751 metal Inorganic materials 0.000 claims abstract description 12
- 239000002184 metal Substances 0.000 claims abstract description 12
- 239000011159 matrix material Substances 0.000 claims abstract description 9
- QYEXBYZXHDUPRC-UHFFFAOYSA-N B#[Ti]#B Chemical compound B#[Ti]#B QYEXBYZXHDUPRC-UHFFFAOYSA-N 0.000 claims abstract description 6
- 238000010438 heat treatment Methods 0.000 claims description 20
- 238000013016 damping Methods 0.000 claims description 19
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 16
- 239000000203 mixture Substances 0.000 claims description 16
- JOXIMZWYDAKGHI-UHFFFAOYSA-N toluene-4-sulfonic acid Chemical compound CC1=CC=C(S(O)(=O)=O)C=C1 JOXIMZWYDAKGHI-UHFFFAOYSA-N 0.000 claims description 16
- 239000002002 slurry Substances 0.000 claims description 13
- 238000003756 stirring Methods 0.000 claims description 13
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 12
- 229920006150 hyperbranched polyester Polymers 0.000 claims description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 12
- 238000006243 chemical reaction Methods 0.000 claims description 11
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- 229910052757 nitrogen Inorganic materials 0.000 claims description 8
- PTBDIHRZYDMNKB-UHFFFAOYSA-N 2,2-Bis(hydroxymethyl)propionic acid Chemical compound OCC(C)(CO)C(O)=O PTBDIHRZYDMNKB-UHFFFAOYSA-N 0.000 claims description 7
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 7
- 238000002156 mixing Methods 0.000 claims description 7
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- 229910052710 silicon Inorganic materials 0.000 claims description 7
- 238000005245 sintering Methods 0.000 claims description 7
- KOMNUTZXSVSERR-UHFFFAOYSA-N 1,3,5-tris(prop-2-enyl)-1,3,5-triazinane-2,4,6-trione Chemical compound C=CCN1C(=O)N(CC=C)C(=O)N(CC=C)C1=O KOMNUTZXSVSERR-UHFFFAOYSA-N 0.000 claims description 6
- XMNIXWIUMCBBBL-UHFFFAOYSA-N 2-(2-phenylpropan-2-ylperoxy)propan-2-ylbenzene Chemical compound C=1C=CC=CC=1C(C)(C)OOC(C)(C)C1=CC=CC=C1 XMNIXWIUMCBBBL-UHFFFAOYSA-N 0.000 claims description 6
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- KRADHMIOFJQKEZ-UHFFFAOYSA-N Tri-2-ethylhexyl trimellitate Chemical compound CCCCC(CC)COC(=O)C1=CC=C(C(=O)OCC(CC)CCCC)C(C(=O)OCC(CC)CCCC)=C1 KRADHMIOFJQKEZ-UHFFFAOYSA-N 0.000 claims description 6
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- DEQZTKGFXNUBJL-UHFFFAOYSA-N n-(1,3-benzothiazol-2-ylsulfanyl)cyclohexanamine Chemical compound C1CCCCC1NSC1=NC2=CC=CC=C2S1 DEQZTKGFXNUBJL-UHFFFAOYSA-N 0.000 claims description 6
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- 239000004014 plasticizer Substances 0.000 claims description 6
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims description 6
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- 239000011115 styrene butadiene Substances 0.000 claims description 6
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- KUAZQDVKQLNFPE-UHFFFAOYSA-N thiram Chemical compound CN(C)C(=S)SSC(=S)N(C)C KUAZQDVKQLNFPE-UHFFFAOYSA-N 0.000 claims description 6
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- HXIQYSLFEXIOAV-UHFFFAOYSA-N 2-tert-butyl-4-(5-tert-butyl-4-hydroxy-2-methylphenyl)sulfanyl-5-methylphenol Chemical compound CC1=CC(O)=C(C(C)(C)C)C=C1SC1=CC(C(C)(C)C)=C(O)C=C1C HXIQYSLFEXIOAV-UHFFFAOYSA-N 0.000 claims description 2
- 238000011049 filling Methods 0.000 claims description 2
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- 229910000831 Steel Inorganic materials 0.000 description 15
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- 239000008187 granular material Substances 0.000 description 11
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 8
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- CGRTZESQZZGAAU-UHFFFAOYSA-N [2-[3-[1-[3-(3-tert-butyl-4-hydroxy-5-methylphenyl)propanoyloxy]-2-methylpropan-2-yl]-2,4,8,10-tetraoxaspiro[5.5]undecan-9-yl]-2-methylpropyl] 3-(3-tert-butyl-4-hydroxy-5-methylphenyl)propanoate Chemical compound CC(C)(C)C1=C(O)C(C)=CC(CCC(=O)OCC(C)(C)C2OCC3(CO2)COC(OC3)C(C)(C)COC(=O)CCC=2C=C(C(O)=C(C)C=2)C(C)(C)C)=C1 CGRTZESQZZGAAU-UHFFFAOYSA-N 0.000 description 4
- 229910052786 argon Inorganic materials 0.000 description 4
- 150000001875 compounds Chemical class 0.000 description 4
- 230000006378 damage Effects 0.000 description 4
- 239000007789 gas Substances 0.000 description 4
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- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 description 3
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 description 3
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- 239000010453 quartz Substances 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- 238000007599 discharging Methods 0.000 description 2
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- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 2
- 229920002379 silicone rubber Polymers 0.000 description 2
- 239000004945 silicone rubber Substances 0.000 description 2
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- 208000027418 Wounds and injury Diseases 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- XALVHDZWUBSWES-UHFFFAOYSA-N bis(trifluoromethylsulfonyl)azanide;tributyl(methyl)azanium Chemical compound CCCC[N+](C)(CCCC)CCCC.FC(F)(F)S(=O)(=O)[N-]S(=O)(=O)C(F)(F)F XALVHDZWUBSWES-UHFFFAOYSA-N 0.000 description 1
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- C04B35/58—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 borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides
- C04B35/5805—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 borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides based on borides
- C04B35/58064—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 borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides based on borides based on refractory borides
- C04B35/58071—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 borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides based on borides based on refractory borides based on titanium borides
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F41—WEAPONS
- F41H—ARMOUR; ARMOURED TURRETS; ARMOURED OR ARMED VEHICLES; MEANS OF ATTACK OR DEFENCE, e.g. CAMOUFLAGE, IN GENERAL
- F41H5/00—Armour; Armour plates
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- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
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- C04B2235/50—Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
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Abstract
The invention relates to the field of bulletproof materials, in particular to a titanium boride-based composite ceramic and a protective plugboard, which comprise a metal fiber preform, a ceramic matrix and toughening whiskers; the ceramic matrix comprises boron carbide, graphene, aluminum oxide and titanium boride; the graphene comprises graphene microplates and a graphene film coated on the surfaces of the boron carbide, the aluminum oxide and the titanium boride, and the bulletproof composite ceramic prepared by the invention has excellent mechanical strength and bulletproof performance.
Description
Technical Field
The invention relates to the field of protective materials, in particular to a titanium boride-based composite ceramic and a protective plugboard.
Background
Ballistic protection equipment requires materials that can absorb and dissipate the kinetic energy of bullets and fragments, prevent penetration, and effectively protect the protected parts of the human body. The traditional bulletproof materials mostly adopt bulletproof steel plates, and ceramic materials gradually become the main stream of bulletproof materials due to the high specific stiffness, high specific strength and chemical inertness under complex environments of the ceramic materials and the low density, high strength, high hardness and high compressive strength of the ceramic materials relative to the metal materials.
The energy absorption mode of the ceramic bulletproof material mainly comprises crushing and breaking, when the bullets impact the ceramic bulletproof material at a high speed, the hardness of the ceramic bulletproof material is far higher than that of the bullets, passivation deformation can be generated on the bullets, the ceramic surface can be crushed into fine particles, a part of impact energy is taken away, and when the passivated bullets continue to penetrate the ceramic, shearing damage mainly occurs in the ceramic. When the reinforcing fiber is added into the ceramic bulletproof material, the bullet warhead passes through the ceramic, and the reinforcing fiber is damaged by stretching at the moment when penetrating the reinforcing fiber, so that the kinetic energy of the bullet warhead is absorbed, and the damage caused by the bullet warhead can be reduced, but the reinforcing fiber in the ceramic bulletproof material is directly added at present, and the hysteresis and injury reducing effects on the bullet are limited.
Disclosure of Invention
The invention aims to: aiming at the technical problems, the invention provides a titanium boride-based composite ceramic and a protective plugboard.
The technical scheme adopted is as follows:
a composite ceramic based on titanium boride comprises a metal fiber preform, a ceramic matrix and toughening whiskers;
the ceramic matrix comprises boron carbide, graphene, aluminum oxide and titanium boride;
the graphene comprises graphene microplates and a graphene film coated on the surfaces of the boron carbide, the aluminum oxide and the titanium boride.
Further, the metal fiber preform is formed by alternately laminating and needling a plurality of metal fiber mesh tires.
Further, the weight ratio of the boron carbide to the graphene microchip to the aluminum oxide to the titanium boride is 2-4:1-2:2-5:10-20.
Further, the toughening whisker is silicon carbide grown in situ.
The invention also provides a preparation method of the titanium boride-based composite ceramic, which comprises the following steps:
depositing simple substance silicon on the surface of the metal fiber preform, depositing a graphene film on the surface of the boron carbide, aluminum oxide and titanium boride, ball-milling and mixing the boron carbide, aluminum oxide, titanium boride and graphene microchip, adding water to disperse and prepare slurry, adding a coupling agent and a binder into the slurry, continuously stirring to obtain a mixture, performing spray drying granulation on the mixture to obtain granules, molding the granules into a blank, uniformly filling the granules on the upper surface and the lower surface of the metal fiber preform during molding, heating the blank to 550-600 ℃, performing heat preservation degreasing for 30-90min, heating the blank to 1600-1800 ℃ for heat preservation and sintering for 2-4h, and cooling to obtain the composite ceramic.
Further, the coupling agent is a titanate coupling agent and/or a silane coupling agent.
Further, the first stage heating speed is 8-15 ℃/min, and the second stage heating speed is 1-5 ℃/min.
The invention also provides a protective plugboard which comprises the composite ceramic and a damping material, wherein the damping material is arranged between two layers of composite ceramics.
Further, the damping material comprises the following components in parts by weight:
40-60 parts of natural rubber, 20-30 parts of hydrogenated carboxylated nitrile rubber, 10-20 parts of hyperbranched polyester, 5-10 parts of styrene-butadiene thermoplastic elastomer, 20-30 parts of carbon black, 10-20 parts of zinc oxide, 1-2 parts of plasticizer TOTM, 1-80-2 parts of antioxidant AO, 1-3 parts of sulfur, 0.1-0.5 part of dicumyl peroxide, 0.5-1 part of accelerator CZ, 0.5-1 part of accelerator TMTD and 1-2 parts of cross-linking agent TAIC.
Further, the preparation method of the hyperbranched polyester comprises the following steps:
mixing pentaerythritol, a first part of 2, 2-dimethylolpropionic acid and a first part of p-toluenesulfonic acid, heating to 130-140 ℃ under the protection of nitrogen for reaction for 2-4 hours, continuously reacting for 2-4 hours under the vacuum condition, then adding a second part of 2, 2-dimethylolpropionic acid and a second part of p-toluenesulfonic acid, introducing nitrogen, keeping the temperature for reaction for 2-4 hours, continuously reacting for 2-4 hours under the vacuum condition, adding a third part of 2, 2-dimethylolpropionic acid and a third part of p-toluenesulfonic acid, introducing nitrogen, keeping the temperature for reaction for 2-4 hours, continuously reacting for 2-4 hours under the vacuum condition, cooling the reaction liquid to 40-50 ℃ after the reaction is finished, pouring into ice water for stirring, filtering out precipitated solids, washing with deionized water, and drying in vacuum.
The invention has the beneficial effects that:
the invention provides a composite ceramic based on titanium boride, silicon carbide whisker is generated in situ in the sintering process of elemental silicon deposited on the surface of a steel fiber preform, and graphene microchip and graphene film, because the silicon carbide whisker is formed in a ceramic matrix, ceramic particles are connected with the steel fiber preform, load can be effectively transmitted, the expansion of microcracks can be prevented through crack deflection and bridging action, the kinetic energy of a bullet warhead can be absorbed through tensile failure and winding action, the advancing of the bullet is delayed, the damage caused by the bullet warhead is reduced, compared with the method of directly adding the composite ceramic, the method has better dispersing and toughening effects, the addition of the graphene microchip can refine grains, the promotion of the mechanical property of the bulletproof composite ceramic is promoted through the combined action of strong interface bonding with boron carbide, aluminum oxide and titanium boride, the hyperbranched polyester with polar groups is added into a damping material, the damping material can be obviously improved through the hydrogen bond interaction between hydrogenated carboxylated nitrile rubber and hyperbranched polyester and the hydrogen bond interaction of the hyperbranched polyester, the damping material can be used as an intermediate layer, the impact resistance of the composite ceramic can be remarkably improved, and the composite ceramic has high impact resistance and the shock resistance performance can be remarkably improved through the preparation of the composite ceramic.
Drawings
FIG. 1 is a photograph of a composite ceramic prepared in example 1 of the present invention;
fig. 2 is a schematic structural diagram of a protective board according to embodiment 4 of the present invention;
the reference numerals in the figures represent:
1-composite ceramic; 2-damping material.
Detailed Description
The specific conditions are not noted in the examples and are carried out according to conventional conditions or conditions recommended by the manufacturer. The reagents or apparatus used were conventional products commercially available without the manufacturer's attention. The technology not mentioned in the present invention refers to the prior art, and unless otherwise indicated, the following examples and comparative examples are parallel tests, employing the same processing steps and parameters.
Example 1
A composite ceramic based on titanium boride comprises 6 layers of steel fiber mesh (steel grade: SUS316L, thickness 1mm, 900g/m per square weight) 2 ) Alternately laminating a steel fiber preform, a ceramic matrix and silicon carbide toughening whiskers, wherein the steel fiber preform is formed by needling and compounding;
the ceramic matrix comprises boron carbide, graphene microplates, aluminum oxide and titanium boride;
a graphene film is deposited on the surface of the boron carbide, the aluminum oxide and the titanium boride;
the preparation method of the composite ceramic based on titanium boride comprises the following steps:
SiCl is added to 4 Dissolving in N4441 (tributyl methyl ammonium bis (trifluoromethanesulfonyl) imide) ionic liquid with concentration of 0.1M, using steel fiber preform as working electrode, auxiliary electrode as glassy carbon electrode, and reference electrode as Ag/(AgNO) 3 Acetonitrile), performing constant voltage electrodeposition, wherein the working voltage is 2.4V, the temperature is 50 ℃, the steel fiber preform is subjected to electrodeposition for 4 hours to obtain elemental silicon, the steel fiber preform is taken out, washed with dichloromethane for multiple times and then placed in a vacuum oven at 60 ℃ for vacuum drying for 12 hours to obtain a metal fiber preform with elemental silicon deposited on the surface;
placing boron carbide, aluminum oxide and titanium boride on a clean quartz boat, placing the quartz boat on a slide rail furnace heating area of a chemical vapor deposition system, vacuumizing and cleaning with argon three times to ensure an anaerobic environment, introducing argon to ensure that the interior of the quartz tube is in a normal pressure state, and then adjusting the atmosphere to be a mixed gas (volume ratio of hydrogen to argon is 1:1) with the flow rate of the mixed gas being 20cm 3 Heating to 1000deg.C at 10deg.C/min, and introducing mixed gas (volume ratio of 2:1) of hydrogen and methane at flow rate of 30cm 3 /min, holding for 30min, and introducing 150cm 3 Cooling the argon gas for/min to room temperature to obtain boron carbide, aluminum oxide and titanium boride with the surface deposited with the graphene film;
adding 300g of boron carbide, 400g of aluminum oxide, 1800g of titanium boride and 150g of graphene microplates into a ball mill, ball milling for 10 hours, adding 10L of water into the obtained mixture, stirring and dispersing to prepare slurry, adding 100mL of silane coupling agent KH-800 and 400g of polyvinyl alcohol as binders into the slurry, continuously stirring for 30 minutes to obtain a mixture, performing spray drying granulation on the mixture to obtain granules, dividing the granules into two parts, uniformly paving one part at the bottom of a mould, putting a steel fiber preform, uniformly covering with another part of granulating material, pressing and forming under the pressure of 80MPa to prepare a blank, heating the blank to 580 ℃ at the first stage at the speed of 12 ℃/min, performing heat preservation degreasing for 60 minutes, heating to 1750 ℃ at the second stage at the speed of 3 ℃/min, performing heat preservation sintering for 3 hours, and cooling to obtain the composite ceramic.
Example 2
Substantially the same as in example 1, except that the composite ceramic was prepared:
adding 380g of boron carbide, 400g of aluminum oxide, 1500g of titanium boride and 160g of graphene microplates into a ball mill, ball milling for 10 hours, adding 10L of water into the obtained mixture, stirring and dispersing to prepare slurry, adding 100mL of silane coupling agent KH-800 and 400g of polyvinyl alcohol as binders into the slurry, continuously stirring for 30 minutes to obtain a mixture, performing spray drying granulation on the mixture to obtain granules, dividing the granules into two parts, uniformly paving one part at the bottom of a mould, putting a steel fiber preform, uniformly covering with another part of granulating material, pressing and forming under the pressure of 80MPa to prepare a blank, heating the blank to 600 ℃ for 90 minutes at the speed of 15 ℃/min, heating to 1800 ℃ for sintering at the temperature for 4 hours at the speed of 5 ℃/min, and cooling to obtain the composite ceramic.
Example 3
Substantially the same as in example 1, except that substantially the same as in example 1 was used in the preparation of the composite ceramic:
adding 250g of boron carbide, 250g of aluminum oxide, 1200g of titanium boride and 130g of graphene microplates into a ball mill, ball milling for 10 hours, adding 10L of water into the obtained mixture, stirring and dispersing to prepare slurry, adding 100mL of silane coupling agent KH-800 and 400g of polyvinyl alcohol as binders into the slurry, continuously stirring for 30 minutes to obtain a mixture, performing spray drying granulation on the mixture to obtain granules, dividing the granules into two parts, uniformly paving one part at the bottom of a mould, putting a steel fiber preform, uniformly covering with another part of granulating material, pressing and forming under the pressure of 80MPa to prepare a blank, heating the blank to 550 ℃ at the speed of 8 ℃/min for one section, performing heat preservation degreasing for 30 minutes, heating to 1600 ℃ for two sections at the speed of 1 ℃/min, performing heat preservation and sintering for 2 hours, and cooling to obtain the composite ceramic.
Comparative example 1: substantially the same as in example 1, except that no silicon carbide toughening whisker was contained (i.e., no graphene film was deposited on the surface of boron carbide, aluminum oxide, titanium boride, no elemental silicon was deposited on the surface of the steel fiber preform);
the preparation method comprises the following steps:
adding 300g of boron carbide, 400g of aluminum oxide, 1800g of titanium boride and 150g of graphene microplates into a ball mill, ball milling for 10 hours, adding 10L of water into the obtained mixture, stirring and dispersing to prepare slurry, adding 100mL of silane coupling agent KH-800 and 400g of polyvinyl alcohol as binders into the slurry, continuously stirring for 30 minutes to obtain a mixture, performing spray drying granulation on the mixture to obtain granules, dividing the granules into two parts, uniformly paving one part at the bottom of a die, putting a steel fiber preform, uniformly covering with another part of granulating material, pressing and forming under the pressure of 80MPa to prepare a blank, heating the blank to 580 ℃ at the speed of 12 ℃/min for one part, performing heat preservation degreasing for 60 minutes, heating to 1750 ℃ at the speed of 3 ℃/min for two parts, performing heat preservation and sintering for 3 hours, and cooling to obtain the composite ceramic.
(1) The composite ceramics prepared in examples 1 to 3 and comparative example 1 were subjected to performance test, and the results are shown in table 1 below:
table 1:
；
as can be seen from Table 1 above, the composite ceramic prepared by the present invention has excellent mechanical strength.
Example 4
A protective plugboard comprises two layers of composite ceramics (10 mm on a single sheet) and damping materials (5 mm on a single sheet) prepared in the embodiment 1, wherein the damping materials are arranged between the two layers of composite ceramics and are bonded with each other through strong all-purpose adhesive.
The damping material comprises the following components in parts by weight:
50 parts of natural rubber, 25 parts of hydrogenated carboxylated nitrile rubber, 18 parts of hyperbranched polyester, 6 parts of styrene-butadiene thermoplastic elastomer, 22 parts of carbon black, 15 parts of zinc oxide, 1.5 parts of plasticizer TOTM, 2 parts of antioxidant AO-80, 2 parts of sulfur, 0.25 part of dicumyl peroxide, 1 part of accelerator CZ, 0.5 part of accelerator TMTD and 1.5 parts of cross-linking agent TAIC.
The preparation method of the hyperbranched polyester comprises the following steps:
in a reactor with a condenser pipe and a water separator, 20.42g of pentaerythritol, 81.69g of 2, 2-dimethylolpropionic acid and 0.51g of p-toluenesulfonic acid are mixed, the temperature is raised to 140 ℃ under the protection of nitrogen, the reaction is continued for 2 hours under the vacuum condition, then 160.96g of 2, 2-dimethylolpropionic acid and 0.8g of p-toluenesulfonic acid are added, nitrogen is introduced, the reaction is kept for 2 hours under the vacuum condition, 321.91g of 2, 2-dimethylolpropionic acid and 1.61g of p-toluenesulfonic acid are added, nitrogen is introduced, the reaction is kept for 2 hours under the vacuum condition, the water generated by the reaction is discharged through the water separator all the time during the reaction, the reaction liquid is cooled to 45 ℃ and poured into ice water for stirring under the vacuum condition, the reaction liquid is filtered, the precipitated solid is washed with deionized water after the filtering, and the solid is dried under the vacuum at 60 ℃ for 24 hours.
The preparation method of the damping material comprises the following steps:
adding natural rubber into an internal mixer to plasticate for 1min at an initial temperature of 60 ℃ and a rotor rotating speed of 80r/min, then heating to 80 ℃, adding hydrogenated carboxylated nitrile rubber, hyperbranched polyester and styrene-butadiene thermoplastic elastomer, mixing for 2min, heating to 90 ℃, adding carbon black, zinc oxide, a plasticizer TOTM and an antioxidant AO-80, mixing for 3min, discharging rubber, setting the initial temperature of the internal mixer to 40 ℃ and the rotating speed of 60r/min, adding the obtained rubber, sulfur, dicumyl peroxide, an accelerator CZ, an accelerator TMTD and a cross-linking agent TAIC into the internal mixer, mixing again for 4.5min, discharging rubber, obtaining a rubber compound, passing the obtained rubber compound once on an open mill with a roll spacing of 0.5mm and a roll temperature of 50+/-5 ℃, regulating the roll spacing to 5mm, standing the obtained rubber compound twice, vulcanizing the obtained rubber compound on a flat vulcanizing machine for 24h under a vulcanizing condition of 143 ℃ of 10MPa x 10min.
Example 5
Substantially the same as in example 4, except that the damping material comprises, in parts by weight:
60 parts of natural rubber, 30 parts of hydrogenated carboxylated nitrile rubber, 20 parts of hyperbranched polyester, 10 parts of styrene-butadiene thermoplastic elastomer, 30 parts of carbon black, 20 parts of zinc oxide, 2 parts of plasticizer TOTM, 2 parts of antioxidant AO-80, 3 parts of sulfur, 0.5 part of dicumyl peroxide, 1 part of accelerator CZ, 1 part of accelerator TMTD and 2 parts of cross-linking agent TAIC.
Example 6
Substantially the same as in example 4, except that the damping material comprises, in parts by weight:
40 parts of natural rubber, 20 parts of hydrogenated carboxylated nitrile rubber, 10 parts of hyperbranched polyester, 5 parts of styrene-butadiene thermoplastic elastomer, 20 parts of carbon black, 10 parts of zinc oxide, 1 part of plasticizer TOTM, 1 part of antioxidant AO-80, 1 part of sulfur, 0.1 part of dicumyl peroxide, 0.5 part of accelerator CZ, 0.5 part of accelerator TMTD and 1 part of cross-linking agent TAIC.
Comparative example 2: substantially the same as in example 4, except that the damping material was hydrogenated nitrile rubber (rayleigh ZP 4310) of the same thickness.
Comparative example 3: substantially the same as in example 4, except that the damping material was high phenyl silicone rubber (phenyl silicone rubber produced in the united states of america by MOMENTIVE michaeli) having the same thickness.
Comparative example 4: substantially the same as in example 4, except that polyurethane (basf B90A) of the same thickness was used as the damping material.
(2) The protective inserts prepared in examples 4-6 and comparative examples 2-4 were shot tested under the same conditions using M80 conventional bullets, and the results are shown in Table 2 below:
table 2:
；
as can be seen from Table 2, the protective insert plate prepared by the invention has good anti-elastic performance.
The above embodiments are only for illustrating the technical solution of the present invention, and are not limiting; although the invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical scheme described in the foregoing embodiments can be modified or some technical features thereof can be replaced by equivalents; such modifications and substitutions do not depart from the spirit and scope of the technical solutions of the embodiments of the present invention.
Claims (9)
1. The composite ceramic based on titanium boride is characterized by comprising a metal fiber preform, a ceramic matrix and toughening whiskers;
the ceramic matrix comprises boron carbide, graphene, aluminum oxide and titanium boride;
the graphene comprises graphene microplates and a graphene film coated on the surfaces of the boron carbide, the aluminum oxide and the titanium boride;
the preparation method of the titanium boride-based composite ceramic comprises the following steps:
depositing elemental silicon on the surface of the metal fiber preform, depositing a graphene film on the surface of the boron carbide, the aluminum oxide and the titanium boride, ball-milling and mixing the graphene film with graphene microplates, adding water to disperse the graphene microplates to prepare slurry, adding a coupling agent and a binder into the slurry, continuously stirring the slurry to obtain a mixture, performing spray drying granulation on the mixture to obtain granulated materials, molding the granulated materials into green bodies, uniformly filling the granulated materials on the upper and lower surfaces of the metal fiber preform with the elemental silicon deposited on the surface during molding, heating the green bodies to 550-600 ℃, preserving heat and degreasing the green bodies for 30-90min, heating the green bodies to 1600-1800 ℃, preserving heat and sintering the green bodies for 2-4h, and cooling the green bodies to obtain the composite ceramic.
2. The titanium boride-based composite ceramic according to claim 1, wherein the metal fiber preform is composited by alternately laminating and needling a plurality of metal fiber mesh tubes.
3. The titanium boride-based composite ceramic according to claim 1, wherein the weight ratio of boron carbide, graphene microplates, aluminum oxide, titanium boride is 2-4:1-2:2-5:10-20.
4. The titanium boride-based composite ceramic of claim 1, wherein the toughening whiskers are in-situ grown silicon carbide.
5. The titanium boride-based composite ceramic of claim 1, wherein the coupling agent is a titanate coupling agent and/or a silane coupling agent.
6. The titanium boride-based composite ceramic according to claim 1, wherein the first stage is heated at a rate of 8-15 ℃/min and the second stage is heated at a rate of 1-5 ℃/min.
7. A protective insert plate comprising a composite ceramic according to any one of claims 1 to 6 and a damping material, said damping material being arranged between two layers of composite ceramic.
8. The protective insert of claim 7, wherein the damping material comprises, in parts by weight:
40-60 parts of natural rubber, 20-30 parts of hydrogenated carboxylated nitrile rubber, 10-20 parts of hyperbranched polyester, 5-10 parts of styrene-butadiene thermoplastic elastomer, 20-30 parts of carbon black, 10-20 parts of zinc oxide, 1-2 parts of plasticizer TOTM, 1-80-2 parts of antioxidant AO, 1-3 parts of sulfur, 0.1-0.5 part of dicumyl peroxide, 0.5-1 part of accelerator CZ, 0.5-1 part of accelerator TMTD and 1-2 parts of cross-linking agent TAIC.
9. The protective package of claim 8, wherein the hyperbranched polyester is prepared by a process comprising:
mixing pentaerythritol, 2-dimethylolpropionic acid and p-toluenesulfonic acid, heating to 130-140 ℃ under the protection of nitrogen, reacting for 2-4 hours, continuously reacting for 2-4 hours under the vacuum condition, adding 2, 2-dimethylolpropionic acid and p-toluenesulfonic acid, introducing nitrogen, keeping the temperature for 2-4 hours, continuously reacting for 2-4 hours under the vacuum condition, cooling the reaction solution to 40-50 ℃ after the reaction is finished, pouring into ice water, stirring, filtering out precipitated solids, washing with deionized water, and vacuum drying.
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