CN108863321A - A kind of aluminium oxide-carbonitride of silicium complex phase bulletproof ceramic and preparation method thereof - Google Patents

A kind of aluminium oxide-carbonitride of silicium complex phase bulletproof ceramic and preparation method thereof Download PDF

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CN108863321A
CN108863321A CN201810748871.XA CN201810748871A CN108863321A CN 108863321 A CN108863321 A CN 108863321A CN 201810748871 A CN201810748871 A CN 201810748871A CN 108863321 A CN108863321 A CN 108863321A
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silicium
carbonitride
aluminium oxide
mass parts
complex phase
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CN108863321B (en
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付绿平
顾华志
黄奥
张美杰
倪红卫
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Wuhan University of Science and Engineering WUSE
Wuhan University of Science and Technology WHUST
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Abstract

The present invention relates to a kind of aluminium oxide-carbonitride of silicium complex phase bulletproof ceramics and preparation method thereof.Its technical solution is：The soluble salt of 0.1~8 mass parts is dissolved in the water of 4~10 mass parts, obtains salting liquid；Using the carbonaceous material of the alumina powder of 85~90 mass parts, the material of 3~10 mass parts and 1~8 mass parts as raw material；The raw material is uniformly mixed in planetary ball mill with the salting liquid again, obtains mixture；Then by the mixture under the conditions of 100~150MPa mechanical pressing, obtain green compact；Finally, the green compact are 12~36 hours dry under the conditions of 110~200 DEG C, 1~8 hour is kept the temperature under the conditions of nitrogen atmosphere and 1600~1800 DEG C to get aluminium oxide-carbonitride of silicium complex phase bulletproof ceramic.At low cost and simple process of the invention, prepared aluminium oxide-carbonitride of silicium complex phase bulletproof ceramic have the characteristics that intensity is high, hardness is high, toughness is high, lower containing the transgranular stomata of a large amount of nanoscales and bulk density.

Description

A kind of aluminium oxide-carbonitride of silicium complex phase bulletproof ceramic and preparation method thereof
Technical field
The invention belongs to alumina base complex phase bulletproof ceramic technical fields.It is multiple more particularly to a kind of aluminium oxide-carbonitride of silicium Phase bulletproof ceramic and preparation method thereof.
Background technique
Ballistic armor materials are one of critical materials indispensable in modern military equipment, and the superiority and inferiority of performance is directly made About the fight capability of military equipment, develop high performance ballistic armour material, have extremely important meaning for national defense construction. In order to have both excellent capability of resistance to penetration, impact resistance and anti-avalanche ability, while again not to the motor-driven of military equipment Ability causes tremendous influence, usually requires that ballistic armor materials have high rigidity, high tenacity, high intensity and low-density.Aluminium oxide Bulletproof ceramic armour material is mainstream bullet resistant material used at present, however, alumina ceramic material poor toughness, density are higher Defect reduces its S. E. A. and resists multiple impact ability, hinders its further expanded application.Therefore, exploitation has The alumina base bulletproof ceramic armour material of high tenacity and low-density meets national significant development demand, for promoting national defence ability With the meaning that do not replace.
Numerous studies are carried out for the toughening of aluminium oxide ceramics both at home and abroad, method for toughening can be generally divided into following two Class：(1) microstructure of controlled material carries out self toughening, such as grain shape, crystallite dimension, elimination or reduction defect；(2) draw Enter the second phase and carries out toughening, such as metallic particles, intermetallic compound, non-metallic particle, whisker, fiber.Existing research knot Fruit shows can be by the toughness of the measures improvement aluminium oxide ceramics such as second reinforced phase of control material microstructure and introducing, so And method for toughening is limited to the promotion degree of aluminium oxide ceramics fracture toughness at present, and also to will cause material close for Part Methods Degree increases, intensity and hardness reduce, and has an adverse effect for its bulletproof performance.
Summary of the invention
The present invention is directed to overcome prior art defect, task is to provide a kind of aluminium oxide-carbon at low cost and simple process The preparation method of silicon nitride complex phase bulletproof ceramic；The aluminium oxide prepared with this method-carbonitride of silicium complex phase bulletproof ceramic intensity height, Hardness is high, toughness is high, lower containing the transgranular stomata of a large amount of nanoscales and bulk density.
To realize above-mentioned task, the technical scheme adopted by the invention is that：The soluble salt of 0.1~8 mass parts is dissolved in 4 In the water of~10 mass parts, salting liquid is obtained；With the alumina powder of 85~90 mass parts, the material of 3~10 mass parts Carbonaceous material with 1~8 mass parts is raw material；The raw material is uniformly mixed in planetary ball mill with the salting liquid again, Obtain mixture；Then by the mixture under the conditions of 100~150MPa mechanical pressing, obtain green compact；Finally, by the life Base is 12~36 hours dry under the conditions of 110~200 DEG C, and it is small that 1~8 is kept the temperature under the conditions of nitrogen atmosphere and 1600~1800 DEG C When to get aluminium oxide-carbonitride of silicium complex phase bulletproof ceramic.
The soluble salt is aluminium chloride, aluminum nitrate, magnesium chloride, magnesium nitrate, magnesium sulfate, zirconium chloride, basic zirconium chloride, nitric acid 1~4 kind in oxygen zirconium, zirconium sulfate, zirconium carbonate ammonium, zirconium nitrate and titanium chloride.
The Al of the alumina powder2O3Content>97wt%, partial size D50It is 1~8 μm.
The material is simple substance silica flour, silicon powder and Si3N4One or more of.
The carbonaceous material is 1~4 kind in carbon black, expanded graphite, starch, phenolic resin, sucrose and pitch.
Due to the adoption of the above technical scheme, the present invention has following good effect compared with prior art：
(1) present invention introduces soluble salt, it is described can salt hydrolyze when being dissolved in the water, hydrated cation can be formed. Hydrated cation exists in the form of the tetramer or dimer, and the bridge formation hydroxyl having can be connected with each other, to be formed in situ Network structure with nanoaperture.During heat treatment, since the tetramer or dimer decompose the nanoparticle generated With the difference of alumina powder sintering character so that above-mentioned nanoaperture by quick closure in intra-die, to form nanometer The transgranular stomata of size.The presence of the nanocrystalline inner air vent can effectively absorb the energy for reducing crack propagation, and make crackle Bridging and deflection occurs, promotes aluminium oxide-carbonitride of silicium complex phase bulletproof ceramic mechanical property；In addition, the introducing of stomata can Reduce aluminium oxide-carbonitride of silicium complex phase bulletproof ceramic density.
(2) present invention introduces material and carbonaceous material, can be formed in situ in nitrogen atmosphere heat treatment process SiCN phase, since SiCN phase has excellent mechanical property, on the one hand, time interface, the effect of pinning dislocation can be formed in material It can hinder crack propagation；On the other hand, due to the difference of SiCN phase and matrix thermal expansion coefficient, remnants will be formed in material internal Thermal stress, so that bridging and deflection occur for crackle, extensions path extends.Therefore, toughness of material and intensity can further be promoted.
Aluminium oxide prepared by the present invention-carbonitride of silicium complex phase bulletproof ceramic is through detecting：Fracture toughness is 7~12MPam1 /2；Compressive resistance is 2700~3200MPa；Vickers hardness is 14~20GPa；Bulk density is 3.1~3.5g/cm3；Average hole Diameter is 100~250nm.
Therefore, at low cost and simple process of the invention, prepared aluminium oxide-carbonitride of silicium complex phase bulletproof ceramic have strong Degree is high, hardness is high, toughness is high, containing the lower feature of the transgranular stomata of a large amount of nanoscales and bulk density.
Specific embodiment
The invention will be further described With reference to embodiment, not limiting of its scope.
In present embodiment：The Al of the alumina powder2O3Content>97wt%, partial size D50It is 1~8 μm.Implement It is repeated no more in example.
Embodiment 1
A kind of aluminium oxide-carbonitride of silicium complex phase bulletproof ceramic and preparation method thereof.The soluble salt of 0.1~4 mass parts is molten Solution obtains salting liquid in the water of 4~7 mass parts；With the alumina powder of 87~90 mass parts, 5~10 mass parts it is siliceous Material and the carbonaceous material of 1~5 mass parts are raw material；The raw material is mixed with the salting liquid in planetary ball mill again It is even, obtain mixture；Then by the mixture under the conditions of 100~130MPa mechanical pressing, obtain green compact；Finally, by institute It is 12~24 hours dry under the conditions of 150~200 DEG C to state green compact, 4~8 are kept the temperature under the conditions of nitrogen atmosphere and 1600~1700 DEG C Hour is to get aluminium oxide-carbonitride of silicium complex phase bulletproof ceramic.
The soluble salt is aluminium chloride, aluminum nitrate, magnesium chloride, magnesium nitrate, magnesium sulfate, zirconium chloride, basic zirconium chloride, nitric acid One of oxygen zirconium, zirconium sulfate, zirconium carbonate ammonium, zirconium nitrate and titanium chloride.
The carbonaceous material is one of carbon black, expanded graphite, starch, phenolic resin, sucrose and pitch.
The material is simple substance silica flour.
Aluminium oxide prepared by the present embodiment-carbonitride of silicium complex phase bulletproof ceramic is through detecting：Fracture toughness is 8~10MPa m1/2；Compressive resistance is 2900~3100MPa；Vickers hardness is 18~19GPa；Bulk density is 3.3~3.45g/cm3；It is average Aperture is 100~200nm.
Embodiment 2
A kind of aluminium oxide-carbonitride of silicium complex phase bulletproof ceramic and preparation method thereof.The soluble salt of 0.1~4 mass parts is molten Solution obtains salting liquid in the water of 4~7 mass parts；With the alumina powder of 87~90 mass parts, 5~10 mass parts it is siliceous Material and the carbonaceous material of 1~5 mass parts are raw material；The raw material is mixed with the salting liquid in planetary ball mill again It is even, obtain mixture；Then by the mixture under the conditions of 120~150MPa mechanical pressing, obtain green compact；Finally, by institute It is 24~36 hours dry under the conditions of 110~160 DEG C to state green compact, 1~5 is kept the temperature under the conditions of nitrogen atmosphere and 1700~1800 DEG C Hour is to get aluminium oxide-carbonitride of silicium complex phase bulletproof ceramic.
The soluble salt is aluminium chloride, aluminum nitrate, magnesium chloride, magnesium nitrate, magnesium sulfate, zirconium chloride, basic zirconium chloride, nitric acid The mixture of two kinds of substances in oxygen zirconium, zirconium sulfate, zirconium carbonate ammonium, zirconium nitrate and titanium chloride.
The carbonaceous material is the mixed of two kinds of substances in carbon black, expanded graphite, starch, phenolic resin, sucrose and pitch Close object.
The material is silicon powder.
Aluminium oxide prepared by the present embodiment-carbonitride of silicium complex phase bulletproof ceramic is through detecting：Fracture toughness be 7.5~ 10MPa m1/2；Compressive resistance is 2800~3000MPa；Vickers hardness is 18~20GPa；Bulk density is 3.3~3.45g/ cm3；Average pore size is 100~200nm.
Embodiment 3
A kind of aluminium oxide-carbonitride of silicium complex phase bulletproof ceramic and preparation method thereof.The soluble salt of 0.1~4 mass parts is molten Solution obtains salting liquid in the water of 4~7 mass parts；With the alumina powder of 87~90 mass parts, the siliceous material of 3~7 mass parts Material and the carbonaceous material of 4~8 mass parts are raw material；The raw material is mixed with the salting liquid in planetary ball mill again It is even, obtain mixture；Then by the mixture under the conditions of 100~130MPa mechanical pressing, obtain green compact；Finally, by institute It is 12~24 hours dry under the conditions of 150~200 DEG C to state green compact, 4~8 are kept the temperature under the conditions of nitrogen atmosphere and 1600~1700 DEG C Hour is to get aluminium oxide-carbonitride of silicium complex phase bulletproof ceramic.
The soluble salt is aluminium chloride, aluminum nitrate, magnesium chloride, magnesium nitrate, magnesium sulfate, zirconium chloride, basic zirconium chloride, nitric acid The mixture of three kinds of substances in oxygen zirconium, zirconium sulfate, zirconium carbonate ammonium, zirconium nitrate and titanium chloride.
The carbonaceous material is the mixed of three kinds of substances in carbon black, expanded graphite, starch, phenolic resin, sucrose and pitch Close object.
The material is Si3N4。
Aluminium oxide prepared by the present embodiment-carbonitride of silicium complex phase bulletproof ceramic is through detecting：Fracture toughness is 8~10MPa m1/2；Compressive resistance is 3000~3200MPa；Vickers hardness is 19~20GPa；Bulk density is 3.4~3.5g/cm3；It is average Aperture is 100~250nm.
Embodiment 4
A kind of aluminium oxide-carbonitride of silicium complex phase bulletproof ceramic and preparation method thereof.The soluble salt of 0.1~4 mass parts is molten Solution obtains salting liquid in the water of 4~7 mass parts；With the alumina powder of 87~90 mass parts, the siliceous material of 3~7 mass parts Material and the carbonaceous material of 4~8 mass parts are raw material；The raw material is mixed with the salting liquid in planetary ball mill again It is even, obtain mixture；Then by the mixture under the conditions of 120~150MPa mechanical pressing, obtain green compact；Finally, by institute It is 24~36 hours dry under the conditions of 110~160 DEG C to state green compact, 1~5 is kept the temperature under the conditions of nitrogen atmosphere and 1700~1800 DEG C Hour is to get aluminium oxide-carbonitride of silicium complex phase bulletproof ceramic.
The soluble salt is aluminium chloride, aluminum nitrate, magnesium chloride, magnesium nitrate, magnesium sulfate, zirconium chloride, basic zirconium chloride, nitric acid The mixture of four kinds of substances in oxygen zirconium, zirconium sulfate, zirconium carbonate ammonium, zirconium nitrate and titanium chloride.
The material is the mixture of simple substance silica flour and silicon powder.
The carbonaceous material is the mixed of four kinds of substances in carbon black, expanded graphite, starch, phenolic resin, sucrose and pitch Close object.
Aluminium oxide prepared by the present embodiment-carbonitride of silicium complex phase bulletproof ceramic is through detecting：Fracture toughness is 7~9MPa m1/2；Compressive resistance is 2900~3100MPa；Vickers hardness is 19~20GPa；Bulk density is 3.4~3.5g/cm3；It is average Aperture is 100~200nm.
Embodiment 5
A kind of aluminium oxide-carbonitride of silicium complex phase bulletproof ceramic and preparation method thereof.The soluble salt of 0.1~4 mass parts is molten Solution obtains salting liquid in the water of 4~7 mass parts；With the alumina powder of 85~87 mass parts, 5~10 mass parts it is siliceous Material and the carbonaceous material of 1~5 mass parts are raw material；The raw material is mixed with the salting liquid in planetary ball mill again It is even, obtain mixture；Then by the mixture under the conditions of 100~130MPa mechanical pressing, obtain green compact；Finally, by institute It is 12~24 hours dry under the conditions of 150~200 DEG C to state green compact, 4~8 are kept the temperature under the conditions of nitrogen atmosphere and 1600~1700 DEG C Hour is to get aluminium oxide-carbonitride of silicium complex phase bulletproof ceramic.
The soluble salt is aluminium chloride, aluminum nitrate, magnesium chloride, magnesium nitrate, magnesium sulfate, zirconium chloride, basic zirconium chloride, nitric acid One of oxygen zirconium, zirconium sulfate, zirconium carbonate ammonium, zirconium nitrate and titanium chloride.
The carbonaceous material is one of carbon black, expanded graphite, starch, phenolic resin, sucrose and pitch.
The material is simple substance silica flour and Si3N4Mixture.
Aluminium oxide prepared by the present embodiment-carbonitride of silicium complex phase bulletproof ceramic is through detecting：Fracture toughness is 9~11MPa m1/2；Compressive resistance is 2900~3100MPa；Vickers hardness is 17~19GPa；Bulk density is 3.25~3.35g/cm3；It is flat Equal aperture is 150~200nm.
Embodiment 6
A kind of aluminium oxide-carbonitride of silicium complex phase bulletproof ceramic and preparation method thereof.The soluble salt of 0.1~4 mass parts is molten Solution obtains salting liquid in the water of 4~7 mass parts；With the alumina powder of 85~87 mass parts, 5~10 mass parts it is siliceous Material and the carbonaceous material of 1~5 mass parts are raw material；The raw material is mixed with the salting liquid in planetary ball mill again It is even, obtain mixture；Then by the mixture under the conditions of 120~150MPa mechanical pressing, obtain green compact；Finally, by institute It is 24~36 hours dry under the conditions of 110~160 DEG C to state green compact, 1~5 is kept the temperature under the conditions of nitrogen atmosphere and 1700~1800 DEG C Hour is to get aluminium oxide-carbonitride of silicium complex phase bulletproof ceramic.
The soluble salt is aluminium chloride, aluminum nitrate, magnesium chloride, magnesium nitrate, magnesium sulfate, zirconium chloride, basic zirconium chloride, nitric acid The mixture of two kinds of substances in oxygen zirconium, zirconium sulfate, zirconium carbonate ammonium, zirconium nitrate and titanium chloride.
The carbonaceous material is the mixed of two kinds of substances in carbon black, expanded graphite, starch, phenolic resin, sucrose and pitch Close object.
The material is silicon powder and Si3N4Mixture.
Aluminium oxide prepared by the present embodiment-carbonitride of silicium complex phase bulletproof ceramic is through detecting：Fracture toughness is 10~11MPa m1/2；Compressive resistance is 2850~3100MPa；Vickers hardness is 18~19GPa；Bulk density is 3.25~3.35g/cm3；It is flat Equal aperture is 150~250nm.
Embodiment 7
A kind of aluminium oxide-carbonitride of silicium complex phase bulletproof ceramic and preparation method thereof.The soluble salt of 0.1~4 mass parts is molten Solution obtains salting liquid in the water of 4~7 mass parts；With the alumina powder of 85~87 mass parts, the siliceous material of 3~7 mass parts Material and the carbonaceous material of 4~8 mass parts are raw material；The raw material is mixed with the salting liquid in planetary ball mill again It is even, obtain mixture；Then by the mixture under the conditions of 100~130MPa mechanical pressing, obtain green compact；Finally, by institute It is 12~24 hours dry under the conditions of 150~200 DEG C to state green compact, 4~8 are kept the temperature under the conditions of nitrogen atmosphere and 1600~1700 DEG C Hour is to get aluminium oxide-carbonitride of silicium complex phase bulletproof ceramic.
The soluble salt is aluminium chloride, aluminum nitrate, magnesium chloride, magnesium nitrate, magnesium sulfate, zirconium chloride, basic zirconium chloride, nitric acid The mixture of three kinds of substances in oxygen zirconium, zirconium sulfate, zirconium carbonate ammonium, zirconium nitrate and titanium chloride.
The carbonaceous material is the mixed of three kinds of substances in carbon black, expanded graphite, starch, phenolic resin, sucrose and pitch Close object.
The material is simple substance silica flour, silicon powder and Si3N4In mixture.
Aluminium oxide prepared by the present embodiment-carbonitride of silicium complex phase bulletproof ceramic is through detecting：Fracture toughness is 9~11MPa m1/2；Compressive resistance is 2800~3000MPa；Vickers hardness is 18~19GPa；Bulk density is 3.3~3.4g/cm3；It is average Aperture is 150~200nm.
Embodiment 8
A kind of aluminium oxide-carbonitride of silicium complex phase bulletproof ceramic and preparation method thereof.The soluble salt of 0.1~4 mass parts is molten Solution obtains salting liquid in the water of 4~7 mass parts；With the alumina powder of 85~87 mass parts, the siliceous material of 3~7 mass parts Material and the carbonaceous material of 4~8 mass parts are raw material；The raw material is mixed with the salting liquid in planetary ball mill again It is even, obtain mixture；Then by the mixture under the conditions of 120~150MPa mechanical pressing, obtain green compact；Finally, by institute It is 24~36 hours dry under the conditions of 110~160 DEG C to state green compact, 1~5 is kept the temperature under the conditions of nitrogen atmosphere and 1700~1800 DEG C Hour is to get aluminium oxide-carbonitride of silicium complex phase bulletproof ceramic.
The soluble salt is aluminium chloride, aluminum nitrate, magnesium chloride, magnesium nitrate, magnesium sulfate, zirconium chloride, basic zirconium chloride, nitric acid The mixture of four kinds of substances in oxygen zirconium, zirconium sulfate, zirconium carbonate ammonium, zirconium nitrate and titanium chloride.
The carbonaceous material is the mixed of four kinds of substances in carbon black, expanded graphite, starch, phenolic resin, sucrose and pitch Close object.
The material is simple substance silica flour.
Aluminium oxide prepared by the present embodiment-carbonitride of silicium complex phase bulletproof ceramic is through detecting：Fracture toughness be 9.5~ 11MPa m1/2；Compressive resistance is 2800~3000MPa；Vickers hardness is 17~18GPa；Bulk density is 3.3~3.4g/ cm3；Average pore size is 150~200nm.
Embodiment 9
A kind of aluminium oxide-carbonitride of silicium complex phase bulletproof ceramic and preparation method thereof.The soluble salt of 4~8 mass parts is dissolved In the water of 7~10 mass parts, salting liquid is obtained；With the alumina powder of 87~90 mass parts, the siliceous material of 5~10 mass parts Material and the carbonaceous material of 1~5 mass parts are raw material；The raw material is mixed with the salting liquid in planetary ball mill again It is even, obtain mixture；Then by the mixture under the conditions of 100~130MPa mechanical pressing, obtain green compact；Finally, by institute It is 12~24 hours dry under the conditions of 150~200 DEG C to state green compact, 4~8 are kept the temperature under the conditions of nitrogen atmosphere and 1600~1700 DEG C Hour is to get aluminium oxide-carbonitride of silicium complex phase bulletproof ceramic.
The soluble salt is aluminium chloride, aluminum nitrate, magnesium chloride, magnesium nitrate, magnesium sulfate, zirconium chloride, basic zirconium chloride, nitric acid One of oxygen zirconium, zirconium sulfate, zirconium carbonate ammonium, zirconium nitrate and titanium chloride.
The carbonaceous material is one of carbon black, expanded graphite, starch, phenolic resin, sucrose and pitch.
The material is silicon powder.
Aluminium oxide prepared by the present embodiment-carbonitride of silicium complex phase bulletproof ceramic is through detecting：Fracture toughness be 10.5~ 11.5MPa m1/2；Compressive resistance is 2800~3000MPa；Vickers hardness is 15~16GPa；Bulk density be 3.15~ 3.25g/cm3；Average pore size is 200~250nm.
Embodiment 10
A kind of aluminium oxide-carbonitride of silicium complex phase bulletproof ceramic and preparation method thereof.The soluble salt of 4~8 mass parts is dissolved In the water of 7~10 mass parts, salting liquid is obtained；With the alumina powder of 87~90 mass parts, the siliceous material of 5~10 mass parts Material and the carbonaceous material of 1~5 mass parts are raw material；The raw material is mixed with the salting liquid in planetary ball mill again It is even, obtain mixture；Then by the mixture under the conditions of 120~150MPa mechanical pressing, obtain green compact；Finally, by institute It is 24~36 hours dry under the conditions of 110~160 DEG C to state green compact, 1~5 is kept the temperature under the conditions of nitrogen atmosphere and 1700~1800 DEG C Hour is to get aluminium oxide-carbonitride of silicium complex phase bulletproof ceramic.
The soluble salt is aluminium chloride, aluminum nitrate, magnesium chloride, magnesium nitrate, magnesium sulfate, zirconium chloride, basic zirconium chloride, nitric acid The mixture of two kinds of substances in oxygen zirconium, zirconium sulfate, zirconium carbonate ammonium, zirconium nitrate and titanium chloride.
The carbonaceous material is the mixed of two kinds of substances in carbon black, expanded graphite, starch, phenolic resin, sucrose and pitch Close object.
The material is Si3N4。
Aluminium oxide prepared by the present embodiment-carbonitride of silicium complex phase bulletproof ceramic is through detecting：Fracture toughness is 10~11MPa m1/2；Compressive resistance is 2750~2900MPa；Vickers hardness is 16~17GPa；Bulk density is 3.15~3.25g/cm3；It is flat Equal aperture is 150~200nm.
Embodiment 11
A kind of aluminium oxide-carbonitride of silicium complex phase bulletproof ceramic and preparation method thereof.The soluble salt of 4~8 mass parts is dissolved In the water of 7~10 mass parts, salting liquid is obtained；With the alumina powder of 87~90 mass parts, the siliceous material of 3~7 mass parts Material and the carbonaceous material of 4~8 mass parts are raw material；The raw material is mixed with the salting liquid in planetary ball mill again It is even, obtain mixture；Then by the mixture under the conditions of 100~130MPa mechanical pressing, obtain green compact；Finally, by institute It is 12~24 hours dry under the conditions of 150~200 DEG C to state green compact, 4~8 are kept the temperature under the conditions of nitrogen atmosphere and 1600~1700 DEG C Hour is to get aluminium oxide-carbonitride of silicium complex phase bulletproof ceramic.
The soluble salt is aluminium chloride, aluminum nitrate, magnesium chloride, magnesium nitrate, magnesium sulfate, zirconium chloride, basic zirconium chloride, nitric acid The mixture of three kinds of substances in oxygen zirconium, zirconium sulfate, zirconium carbonate ammonium, zirconium nitrate and titanium chloride.
The carbonaceous material is the mixed of three kinds of substances in carbon black, expanded graphite, starch, phenolic resin, sucrose and pitch Close object.
The material is the mixture of simple substance silica flour and silicon powder.
Aluminium oxide prepared by the present embodiment-carbonitride of silicium complex phase bulletproof ceramic is through detecting：Fracture toughness be 10.5~ 12MPa m1/2；Compressive resistance is 2850~2950MPa；Vickers hardness is 15~17GPa；Bulk density is 3.2~3.3g/ cm3；Average pore size is 150~200nm.
Embodiment 12
A kind of aluminium oxide-carbonitride of silicium complex phase bulletproof ceramic and preparation method thereof.The soluble salt of 4~8 mass parts is dissolved In the water of 7~10 mass parts, salting liquid is obtained；With the alumina powder of 87~90 mass parts, the siliceous material of 3~7 mass parts Material and the carbonaceous material of 4~8 mass parts are raw material；The raw material is mixed with the salting liquid in planetary ball mill again It is even, obtain mixture；Then by the mixture under the conditions of 120~150MPa mechanical pressing, obtain green compact；Finally, by institute It is 24~36 hours dry under the conditions of 110~160 DEG C to state green compact, 1~5 is kept the temperature under the conditions of nitrogen atmosphere and 1700~1800 DEG C Hour is to get aluminium oxide-carbonitride of silicium complex phase bulletproof ceramic.
The soluble salt is aluminium chloride, aluminum nitrate, magnesium chloride, magnesium nitrate, magnesium sulfate, zirconium chloride, basic zirconium chloride, nitric acid The mixture of four kinds of substances in oxygen zirconium, zirconium sulfate, zirconium carbonate ammonium, zirconium nitrate and titanium chloride.
The carbonaceous material is the mixed of four kinds of substances in carbon black, expanded graphite, starch, phenolic resin, sucrose and pitch Close object.
The material is simple substance silica flour and Si3N4Mixture.
Aluminium oxide prepared by the present embodiment-carbonitride of silicium complex phase bulletproof ceramic is through detecting：Fracture toughness is 10~11MPa m1/2；Compressive resistance is 2800~2950MPa；Vickers hardness is 16~18GPa；Bulk density is 3.2~3.3g/cm3；It is average Aperture is 200~250nm.
Embodiment 13
A kind of aluminium oxide-carbonitride of silicium complex phase bulletproof ceramic and preparation method thereof.The soluble salt of 4~8 mass parts is dissolved In the water of 7~10 mass parts, salting liquid is obtained；With the alumina powder of 85~87 mass parts, the siliceous material of 5~10 mass parts Material and the carbonaceous material of 1~5 mass parts are raw material；The raw material is mixed with the salting liquid in planetary ball mill again It is even, obtain mixture；Then by the mixture under the conditions of 100~130MPa mechanical pressing, obtain green compact；Finally, by institute It is 12~24 hours dry under the conditions of 150~200 DEG C to state green compact, 4~8 are kept the temperature under the conditions of nitrogen atmosphere and 1600~1700 DEG C Hour is to get aluminium oxide-carbonitride of silicium complex phase bulletproof ceramic.
The soluble salt is aluminium chloride, aluminum nitrate, magnesium chloride, magnesium nitrate, magnesium sulfate, zirconium chloride, basic zirconium chloride, nitric acid One of oxygen zirconium, zirconium sulfate, zirconium carbonate ammonium, zirconium nitrate and titanium chloride.
The carbonaceous material is one of carbon black, expanded graphite, starch, phenolic resin, sucrose and pitch.
The material is silicon powder and Si3N4Mixture.
Aluminium oxide prepared by the present embodiment-carbonitride of silicium complex phase bulletproof ceramic is through detecting：Fracture toughness is 11~12MPa m1/2；Compressive resistance is 2700~2800MPa；Vickers hardness is 14~16GPa；Bulk density is 3.1~3.2g/cm3；It is average Aperture is 150~200nm.
Embodiment 14
A kind of aluminium oxide-carbonitride of silicium complex phase bulletproof ceramic and preparation method thereof.The soluble salt of 4~8 mass parts is dissolved In the water of 7~10 mass parts, salting liquid is obtained；With the alumina powder of 85~87 mass parts, the siliceous material of 5~10 mass parts Material and the carbonaceous material of 1~5 mass parts are raw material；The raw material is mixed with the salting liquid in planetary ball mill again It is even, obtain mixture；Then by the mixture under the conditions of 120~150MPa mechanical pressing, obtain green compact；Finally, by institute It is 24~36 hours dry under the conditions of 110~160 DEG C to state green compact, 1~5 is kept the temperature under the conditions of nitrogen atmosphere and 1700~1800 DEG C Hour is to get aluminium oxide-carbonitride of silicium complex phase bulletproof ceramic.
The soluble salt is aluminium chloride, aluminum nitrate, magnesium chloride, magnesium nitrate, magnesium sulfate, zirconium chloride, basic zirconium chloride, nitric acid The mixture of two kinds of substances in oxygen zirconium, zirconium sulfate, zirconium carbonate ammonium, zirconium nitrate and titanium chloride.
The carbonaceous material is the mixed of two kinds of substances in carbon black, expanded graphite, starch, phenolic resin, sucrose and pitch Close object.
The material is simple substance silica flour, silicon powder and Si3N4In mixture.
Aluminium oxide prepared by the present embodiment-carbonitride of silicium complex phase bulletproof ceramic is through detecting：Fracture toughness be 10.5~ 11MPa m1/2；Compressive resistance is 2700~2800MPa；Vickers hardness is 15~17GPa；Bulk density is 3.1~3.2g/ cm3；Average pore size is 150~200nm.
Embodiment 15
A kind of aluminium oxide-carbonitride of silicium complex phase bulletproof ceramic and preparation method thereof.The soluble salt of 4~8 mass parts is dissolved In the water of 7~10 mass parts, salting liquid is obtained；With the alumina powder of 85~87 mass parts, the siliceous material of 3~7 mass parts Material and the carbonaceous material of 4~8 mass parts are raw material；The raw material is mixed with the salting liquid in planetary ball mill again It is even, obtain mixture；Then by the mixture under the conditions of 100~130MPa mechanical pressing, obtain green compact；Finally, by institute It is 12~24 hours dry under the conditions of 150~200 DEG C to state green compact, 4~8 are kept the temperature under the conditions of nitrogen atmosphere and 1600~1700 DEG C Hour is to get aluminium oxide-carbonitride of silicium complex phase bulletproof ceramic.
The soluble salt is aluminium chloride, aluminum nitrate, magnesium chloride, magnesium nitrate, magnesium sulfate, zirconium chloride, basic zirconium chloride, nitric acid The mixture of three kinds of substances in oxygen zirconium, zirconium sulfate, zirconium carbonate ammonium, zirconium nitrate and titanium chloride.
The carbonaceous material is the mixed of three kinds of substances in carbon black, expanded graphite, starch, phenolic resin, sucrose and pitch Close object.
The material is simple substance silica flour.
Aluminium oxide prepared by the present embodiment-carbonitride of silicium complex phase bulletproof ceramic is through detecting：Fracture toughness is 10~12MPa m1/2；Compressive resistance is 2750~2900MPa；Vickers hardness is 14~16GPa；Bulk density is 3.15~3.25g/cm3；It is flat Equal aperture is 200~250nm.
Embodiment 16
A kind of aluminium oxide-carbonitride of silicium complex phase bulletproof ceramic and preparation method thereof.The soluble salt of 4~8 mass parts is dissolved In the water of 7~10 mass parts, salting liquid is obtained；With the alumina powder of 85~87 mass parts, the siliceous material of 3~7 mass parts Material and the carbonaceous material of 4~8 mass parts are raw material；The raw material is mixed with the salting liquid in planetary ball mill again It is even, obtain mixture；Then by the mixture under the conditions of 120~150MPa mechanical pressing, obtain green compact；Finally, by institute It is 24~36 hours dry under the conditions of 110~160 DEG C to state green compact, 1~5 is kept the temperature under the conditions of nitrogen atmosphere and 1700~1800 DEG C Hour is to get aluminium oxide-carbonitride of silicium complex phase bulletproof ceramic.
The soluble salt is aluminium chloride, aluminum nitrate, magnesium chloride, magnesium nitrate, magnesium sulfate, zirconium chloride, basic zirconium chloride, nitric acid The mixture of four kinds of substances in oxygen zirconium, zirconium sulfate, zirconium carbonate ammonium, zirconium nitrate and titanium chloride.
The carbonaceous material is the mixed of four kinds of substances in carbon black, expanded graphite, starch, phenolic resin, sucrose and pitch Close object.
The material is silicon powder.
Aluminium oxide prepared by the present embodiment-carbonitride of silicium complex phase bulletproof ceramic is through detecting：Fracture toughness is 11~12MPa m1/2；Compressive resistance is 2750~2900MPa；Vickers hardness is 15~17GPa；Bulk density is 3.15~3.25g/cm3；It is flat Equal aperture is 200~250nm.
Present embodiment has following good effect compared with prior art：
(1) present embodiment introduces soluble salt, it is described can salt hydrolyze when being dissolved in the water, hydration can be formed Cation.Hydrated cation exists in the form of the tetramer or dimer, and the bridge formation hydroxyl having can be connected with each other, thus former Position forms the network structure with nanoaperture.During heat treatment, since the tetramer or dimer decompose receiving for generation The difference of rice corpuscles and alumina powder sintering character so that above-mentioned nanoaperture by quick closure in intra-die, thus shape At the transgranular stomata of nano-scale.The presence of the nanocrystalline inner air vent can effectively absorb the energy for reducing crack propagation, and make It obtains crackle and bridging and deflection occurs, promote aluminium oxide-carbonitride of silicium complex phase bulletproof ceramic mechanical property；In addition, stomata draws Enter can reduce aluminium oxide-carbonitride of silicium complex phase bulletproof ceramic density.
(2) material and carbonaceous material that present embodiment introduces, can in nitrogen atmosphere heat treatment process SiCN phase is formed in situ, since SiCN phase has excellent mechanical property, on the one hand, time interface, pinning can be formed in material Dislocation effect can hinder crack propagation；It on the other hand, will be in material internal due to the difference of SiCN phase and matrix thermal expansion coefficient Residual thermal stress is formed, so that bridging and deflection occur for crackle, extensions path extends.Therefore, can further to promote material tough Property and intensity.
Aluminium oxide prepared by present embodiment-carbonitride of silicium complex phase bulletproof ceramic is through detecting：Fracture toughness be 7~ 12MPam1/2；Compressive resistance is 2700~3200MPa；Vickers hardness is 14~20GPa；Bulk density is 3.1~3.5g/cm3； Average pore size is 100~250nm.
Therefore, present embodiment is at low cost and simple process, the prepared aluminium oxide-shellproof pottery of carbonitride of silicium complex phase Porcelain has the characteristics that intensity is high, hardness is high, toughness is high, lower containing the transgranular stomata of a large amount of nanoscales and bulk density.

Claims (6)

1. a kind of aluminium oxide-carbonitride of silicium complex phase bulletproof ceramic preparation method, it is characterised in that by 0.1~8 mass parts can Dissolved salt is dissolved in the water of 4~10 mass parts, obtains salting liquid；With the alumina powder of 85~90 mass parts, 3~10 mass parts Material and 1~8 mass parts carbonaceous material be raw material；Again by the raw material and the salting liquid in planetary ball mill It is uniformly mixed, obtains mixture；Then by the mixture under the conditions of 100~150MPa mechanical pressing, obtain green compact；Most Afterwards, the green compact are 12~36 hours dry under the conditions of 110~200 DEG C, under the conditions of nitrogen atmosphere and 1600~1800 DEG C Heat preservation 1~8 hour to get aluminium oxide-carbonitride of silicium complex phase bulletproof ceramic.
2. aluminium oxide according to claim 1-carbonitride of silicium complex phase bulletproof ceramic preparation method, it is characterised in that described Soluble salt be aluminium chloride, aluminum nitrate, magnesium chloride, magnesium nitrate, magnesium sulfate, zirconium chloride, basic zirconium chloride, zirconyl nitrate, zirconium sulfate, 1~4 kind in zirconium carbonate ammonium, zirconium nitrate and titanium chloride.
3. aluminium oxide according to claim 1-carbonitride of silicium complex phase bulletproof ceramic preparation method, it is characterised in that described The Al of alumina powder2O3Content>97wt%, partial size D50It is 1~8 μm.
4. aluminium oxide according to claim 1-carbonitride of silicium complex phase bulletproof ceramic preparation method, it is characterised in that described Material is simple substance silica flour, silicon powder and Si3N4One or more of.
5. aluminium oxide according to claim 1-carbonitride of silicium complex phase bulletproof ceramic preparation method, it is characterised in that described Carbonaceous material is 1~4 kind in carbon black, expanded graphite, starch, phenolic resin, sucrose and pitch.
6. a kind of aluminium oxide-carbonitride of silicium complex phase bulletproof ceramic, it is characterised in that the aluminium oxide-carbonitride of silicium complex phase is shellproof Ceramics are the aluminium oxide according to any one of claims 1~5-carbonitride of silicium complex phase bulletproof ceramic preparation methods Prepared aluminium oxide-carbonitride of silicium complex phase bulletproof ceramic.
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CN102259378A (en) * 2011-08-01 2011-11-30 北京雷特新技术实业公司 Method for preparing ceramic bulletproof plate
TWM555938U (en) * 2017-08-18 2018-02-21 國家中山科學研究院 Bullet-proof structure with dent resistance
CN108249898A (en) * 2018-01-22 2018-07-06 吴亚良 A kind of preparation method of high-performance bullet proof composite plating
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* Cited by examiner, † Cited by third party
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WO1993006060A1 (en) * 1991-09-26 1993-04-01 Mamoru Omori Composite mixed oxide ceramic and production thereof
JPH06293559A (en) * 1993-04-05 1994-10-21 Hitachi Zosen Corp Production of refractory and refractory
CN101508574A (en) * 2009-03-25 2009-08-19 王铀 Ceramic material with amorphous/nanocrystalline structure and method of producing the same
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