CN108863321B - Aluminum oxide-silicon carbonitride complex-phase bulletproof ceramic and preparation method thereof - Google Patents

Aluminum oxide-silicon carbonitride complex-phase bulletproof ceramic and preparation method thereof Download PDF

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CN108863321B
CN108863321B CN201810748871.XA CN201810748871A CN108863321B CN 108863321 B CN108863321 B CN 108863321B CN 201810748871 A CN201810748871 A CN 201810748871A CN 108863321 B CN108863321 B CN 108863321B
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alumina
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silicon
complex phase
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CN108863321A (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
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Abstract

The invention relates to an alumina-silicon carbonitride complex phase bulletproof ceramic and a preparation method thereof. The technical scheme is as follows: dissolving 0.1-8 parts by mass of soluble salt in 4-10 parts by mass of water to obtain a salt solution; taking 85-90 parts by mass of alumina micro powder, 3-10 parts by mass of a silicon-containing material and 1-8 parts by mass of a carbon-containing material as raw materials; uniformly mixing the raw materials and the salt solution in a planetary ball mill to obtain a mixture; then, mechanically pressing the mixture under the condition of 100-150 MPa to obtain a green body; and finally, drying the green body at the temperature of 110-200 ℃ for 12-36 hours, and preserving heat at the temperature of 1600-1800 ℃ for 1-8 hours in a nitrogen atmosphere to obtain the alumina-silicon carbonitride complex phase bulletproof ceramic. The invention has low cost and simple process, and the prepared alumina-silicon carbonitride complex phase bulletproof ceramic has the characteristics of high strength, high hardness, high toughness, large amount of nano-scale intragranular pores and lower volume density.

Description

Aluminum oxide-silicon carbonitride complex-phase bulletproof ceramic and preparation method thereof
Technical Field
The present invention belongs to the field of alumina-base composite bulletproof ceramic technology. In particular to an alumina-silicon carbonitride complex phase bulletproof ceramic and a preparation method thereof.
Background
The bulletproof armor material is one of indispensable key materials in modern military equipment, the performance quality of the bulletproof armor material directly restricts the operational capability of the military equipment, and the development of the high-performance bulletproof armor material has extremely important significance for national defense construction. In order to achieve excellent penetration resistance, impact resistance, and collapse resistance without greatly affecting the maneuverability of military equipment, ballistic armor materials are generally required to have high hardness, high toughness, high strength, and low density. The alumina bulletproof ceramic armor material is the mainstream bulletproof material used at present, however, the energy absorption rate and the multiple-strike resistance of the alumina ceramic material are reduced due to the defects of poor toughness and high density of the alumina ceramic material, and further expanded application of the alumina ceramic armor material is hindered. Therefore, the development of the alumina-based bulletproof ceramic armor material with high toughness and low density meets the national important development requirements, and has irreplaceable significance for improving the national defense capability.
A great deal of research is carried out at home and abroad aiming at the toughening of the alumina ceramics, and the toughening method can be generally divided into the following two types: (1) the microstructure of the material is regulated and controlled to carry out self toughening, such as the shape and the size of crystal grains, and defects are eliminated or reduced; (2) and introducing a second phase for toughening, such as metal particles, intermetallic compounds, non-metal particles, whiskers, fibers and the like. The existing research results show that the toughness of the alumina ceramic can be improved by controlling the microstructure of the material and introducing a second reinforcement and other measures, however, the improvement degree of the fracture toughness of the alumina ceramic by the existing toughening method is limited, and part of the methods can also cause the increase of the material density and the reduction of the strength and the hardness, and the adverse effect is generated on the anti-elasticity performance of the alumina ceramic.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and aims to provide a preparation method of the alumina-silicon carbonitride complex phase bulletproof ceramic with low cost and simple process; the alumina-silicon carbonitride complex phase bulletproof ceramic prepared by the method has high strength, high hardness, high toughness, large amount of nano-scale intragranular pores and lower volume density.
In order to realize the task, the technical scheme adopted by the invention is as follows: dissolving 0.1-8 parts by mass of soluble salt in 4-10 parts by mass of water to obtain a salt solution; taking 85-90 parts by mass of alumina micro powder, 3-10 parts by mass of a silicon-containing material and 1-8 parts by mass of a carbon-containing material as raw materials; uniformly mixing the raw materials and the salt solution in a planetary ball mill to obtain a mixture; then, mechanically pressing the mixture under the condition of 100-150 MPa to obtain a green body; and finally, drying the green body at the temperature of 110-200 ℃ for 12-36 hours, and preserving heat at the temperature of 1600-1800 ℃ for 1-8 hours in a nitrogen atmosphere to obtain the alumina-silicon carbonitride complex phase bulletproof ceramic.
The soluble salt is 1-4 of aluminum chloride, aluminum nitrate, magnesium chloride, magnesium nitrate, magnesium sulfate, zirconium tetrachloride, zirconium oxychloride, zirconyl nitrate, zirconium sulfate, ammonium zirconium carbonate, zirconium nitrate and titanium chloride.
Al of the alumina micropowder2O3Content (wt.)>97wt% particle diameter D501 to 8 μm.
The silicon-containing material is elemental silicon powder, silicon micropowder and Si3N4More than one of them.
The carbon-containing material is 1-4 of carbon black, expanded graphite, starch, phenolic resin, cane sugar and asphalt.
Due to the adoption of the technical scheme, compared with the prior art, the invention has the following positive effects:
(1) the present invention incorporates a soluble salt which, when dissolved in water, undergoes hydrolysis, allowing the formation of hydrated cations. The hydrated cations exist in the form of tetramer or dimer, and the bridging hydroxyl groups can be connected with each other, so that a network structure with nanopores is formed in situ. In the heat treatment process, the nanometer pores are quickly sealed in the crystal grains due to the difference of sintering performance of the nanometer particles generated by the decomposition of the tetramer or the dimer and the alumina micro powder, so as to form nanometer-sized intracrystalline pores. The existence of the nanocrystalline internal pores can effectively absorb energy for reducing crack propagation, leads cracks to be bridged and deflected, and improves the mechanical property of the alumina-silicon carbonitride complex phase bulletproof ceramic; in addition, the introduction of air holes can reduce the density of the alumina-silicon carbonitride complex phase bulletproof ceramic.
(2) The silicon-containing material and the carbon-containing material introduced by the invention can form a SiCN phase in situ in the heat treatment process in the nitrogen atmosphere, and the SiCN phase has excellent mechanical property, so that on one hand, a secondary interface can be formed on the material, and the pinning dislocation effect can hinder crack propagation; on the other hand, due to the difference in thermal expansion coefficient between the SiCN phase and the matrix, residual thermal stress is formed inside the material, causing the cracks to bridge and deflect, and the propagation path to be extended. Therefore, the toughness and strength of the material can be further improved.
The detection shows that the prepared alumina-silicon carbonitride complex phase bulletproof ceramic has the following characteristics: the fracture toughness is 7-12 MPam1 /2(ii) a The compressive strength is 2700-3200 MPa; the Vickers hardness is 14-20 GPa; the bulk density is 3.1 to 3.5g/cm3(ii) a The average pore diameter is 100 to 250 nm.
Therefore, the invention has low cost and simple process, and the prepared alumina-silicon carbonitride complex phase bulletproof ceramic has the characteristics of high strength, high hardness, high toughness, large amount of nano-scale intragranular pores and lower volume density.
Detailed Description
The invention is further described with reference to specific embodiments, without limiting the scope of protection.
In this embodiment: al of the alumina micropowder2O3Content (wt.)>97wt%, particle diameter D501 to 8 μm. The detailed description is omitted in the embodiments.
Example 1
An alumina-silicon carbonitride complex phase bulletproof ceramic and a preparation method thereof. Dissolving 0.1-4 parts by mass of soluble salt in 4-7 parts by mass of water to obtain a salt solution; 87-90 parts by mass of alumina micro powder, 5-10 parts by mass of a silicon-containing material and 1-5 parts by mass of a carbon-containing material are used as raw materials; uniformly mixing the raw materials and the salt solution in a planetary ball mill to obtain a mixture; then, mechanically pressing the mixture under the condition of 100-130 MPa to obtain a green body; and finally, drying the green body at the temperature of 150-200 ℃ for 12-24 hours, and preserving heat at the temperature of 1600-1700 ℃ for 4-8 hours in a nitrogen atmosphere to obtain the alumina-silicon carbonitride complex phase bulletproof ceramic.
The soluble salt is one of aluminum chloride, aluminum nitrate, magnesium chloride, magnesium nitrate, magnesium sulfate, zirconium tetrachloride, zirconium oxychloride, zirconyl nitrate, zirconium sulfate, ammonium zirconium carbonate, zirconium nitrate, and titanium chloride.
The carbonaceous material is one of carbon black, expanded graphite, starch, phenolic resin, sucrose and asphalt.
The silicon-containing material is elemental silicon powder.
The alumina-silicon carbonitride complex phase bulletproof ceramic prepared by the embodiment is detected as follows: the fracture toughness is 8-10 MPa m1/2(ii) a The compressive strength is 2900-3100 MPa; the Vickers hardness is 18-19 GPa; the bulk density is 3.3-3.45 g/cm3(ii) a The average pore diameter is 100 to 200 nm.
Example 2
An alumina-silicon carbonitride complex phase bulletproof ceramic and a preparation method thereof. Dissolving 0.1-4 parts by mass of soluble salt in 4-7 parts by mass of water to obtain a salt solution; 87-90 parts by mass of alumina micro powder, 5-10 parts by mass of a silicon-containing material and 1-5 parts by mass of a carbon-containing material are used as raw materials; uniformly mixing the raw materials and the salt solution in a planetary ball mill to obtain a mixture; then, mechanically pressing the mixture under the condition of 120-150 MPa to obtain a green body; and finally, drying the green body at the temperature of 110-160 ℃ for 24-36 hours, and preserving heat at the temperature of 1700-1800 ℃ for 1-5 hours in a nitrogen atmosphere to obtain the alumina-silicon carbonitride complex phase bulletproof ceramic.
The soluble salt is a mixture of two of aluminum chloride, aluminum nitrate, magnesium chloride, magnesium nitrate, magnesium sulfate, zirconium tetrachloride, zirconium oxychloride, zirconyl nitrate, zirconium sulfate, ammonium zirconium carbonate, zirconium nitrate and titanium chloride.
The carbonaceous material is a mixture of two substances of carbon black, expanded graphite, starch, phenolic resin, sucrose and asphalt.
The silicon-containing material is silicon micropowder.
The alumina-silicon carbonitride complex phase bulletproof ceramic prepared by the embodiment is detected as follows: the fracture toughness is 7.5-10 MPa m1/2(ii) a The compressive strength is 2800-3000 MPa; the Vickers hardness is 18-20 GPa; the bulk density is 3.3-3.45 g/cm3(ii) a The average pore diameter is 100 to 200 nm.
Example 3
An alumina-silicon carbonitride complex phase bulletproof ceramic and a preparation method thereof. Dissolving 0.1-4 parts by mass of soluble salt in 4-7 parts by mass of water to obtain a salt solution; 87-90 parts by mass of alumina micro powder, 3-7 parts by mass of a silicon-containing material and 4-8 parts by mass of a carbon-containing material are used as raw materials; uniformly mixing the raw materials and the salt solution in a planetary ball mill to obtain a mixture; then, mechanically pressing the mixture under the condition of 100-130 MPa to obtain a green body; and finally, drying the green body at the temperature of 150-200 ℃ for 12-24 hours, and preserving heat at the temperature of 1600-1700 ℃ for 4-8 hours in a nitrogen atmosphere to obtain the alumina-silicon carbonitride complex phase bulletproof ceramic.
The soluble salt is a mixture of three substances of aluminum chloride, aluminum nitrate, magnesium chloride, magnesium nitrate, magnesium sulfate, zirconium tetrachloride, zirconium oxychloride, zirconyl nitrate, zirconium sulfate, ammonium zirconium carbonate, zirconium nitrate and titanium chloride.
The carbon-containing material is a mixture of three substances of carbon black, expanded graphite, starch, phenolic resin, cane sugar and asphalt.
The silicon-containing material is Si3N4。
The alumina-silicon carbonitride complex phase bulletproof ceramic prepared by the embodiment is detected as follows: the fracture toughness is 8-10 MPa m1/2(ii) a The compressive strength is 3000-3200 MPa; the Vickers hardness is 19-20 GPa; the bulk density is 3.4-3.5 g/cm3(ii) a The average pore diameter is 100 to 250 nm.
Example 4
An alumina-silicon carbonitride complex phase bulletproof ceramic and a preparation method thereof. Dissolving 0.1-4 parts by mass of soluble salt in 4-7 parts by mass of water to obtain a salt solution; 87-90 parts by mass of alumina micro powder, 3-7 parts by mass of a silicon-containing material and 4-8 parts by mass of a carbon-containing material are used as raw materials; uniformly mixing the raw materials and the salt solution in a planetary ball mill to obtain a mixture; then, mechanically pressing the mixture under the condition of 120-150 MPa to obtain a green body; and finally, drying the green body at the temperature of 110-160 ℃ for 24-36 hours, and preserving heat at the temperature of 1700-1800 ℃ for 1-5 hours in a nitrogen atmosphere to obtain the alumina-silicon carbonitride complex phase bulletproof ceramic.
The soluble salt is a mixture of four substances of aluminum chloride, aluminum nitrate, magnesium chloride, magnesium nitrate, magnesium sulfate, zirconium tetrachloride, zirconium oxychloride, zirconyl nitrate, zirconium sulfate, ammonium zirconium carbonate, zirconium nitrate and titanium chloride.
The silicon-containing material is a mixture of elemental silicon powder and silicon micropowder.
The carbon-containing material is a mixture of four substances of carbon black, expanded graphite, starch, phenolic resin, cane sugar and asphalt.
Prepared by the present exampleThe detection shows that the alumina-silicon carbonitride complex phase bulletproof ceramic comprises the following components in percentage by weight: the fracture toughness is 7-9 MPa m1/2(ii) a The compressive strength is 2900-3100 MPa; the Vickers hardness is 19-20 GPa; the bulk density is 3.4-3.5 g/cm3(ii) a The average pore diameter is 100 to 200 nm.
Example 5
An alumina-silicon carbonitride complex phase bulletproof ceramic and a preparation method thereof. Dissolving 0.1-4 parts by mass of soluble salt in 4-7 parts by mass of water to obtain a salt solution; taking 85-87 parts by mass of alumina micro powder, 5-10 parts by mass of a silicon-containing material and 1-5 parts by mass of a carbon-containing material as raw materials; uniformly mixing the raw materials and the salt solution in a planetary ball mill to obtain a mixture; then, mechanically pressing the mixture under the condition of 100-130 MPa to obtain a green body; and finally, drying the green body at the temperature of 150-200 ℃ for 12-24 hours, and preserving heat at the temperature of 1600-1700 ℃ for 4-8 hours in a nitrogen atmosphere to obtain the alumina-silicon carbonitride complex phase bulletproof ceramic.
The soluble salt is one of aluminum chloride, aluminum nitrate, magnesium chloride, magnesium nitrate, magnesium sulfate, zirconium tetrachloride, zirconium oxychloride, zirconyl nitrate, zirconium sulfate, ammonium zirconium carbonate, zirconium nitrate, and titanium chloride.
The carbonaceous material is one of carbon black, expanded graphite, starch, phenolic resin, sucrose and asphalt.
The silicon-containing material is elemental silicon powder and Si3N4A mixture of (a).
The alumina-silicon carbonitride complex phase bulletproof ceramic prepared by the embodiment is detected as follows: the fracture toughness is 9-11 MPa m1/2(ii) a The compressive strength is 2900-3100 MPa; the Vickers hardness is 17-19 GPa; the bulk density is 3.25 to 3.35g/cm3(ii) a The average pore diameter is 150 to 200 nm.
Example 6
An alumina-silicon carbonitride complex phase bulletproof ceramic and a preparation method thereof. Dissolving 0.1-4 parts by mass of soluble salt in 4-7 parts by mass of water to obtain a salt solution; taking 85-87 parts by mass of alumina micro powder, 5-10 parts by mass of a silicon-containing material and 1-5 parts by mass of a carbon-containing material as raw materials; uniformly mixing the raw materials and the salt solution in a planetary ball mill to obtain a mixture; then, mechanically pressing the mixture under the condition of 120-150 MPa to obtain a green body; and finally, drying the green body at the temperature of 110-160 ℃ for 24-36 hours, and preserving heat at the temperature of 1700-1800 ℃ for 1-5 hours in a nitrogen atmosphere to obtain the alumina-silicon carbonitride complex phase bulletproof ceramic.
The soluble salt is a mixture of two of aluminum chloride, aluminum nitrate, magnesium chloride, magnesium nitrate, magnesium sulfate, zirconium tetrachloride, zirconium oxychloride, zirconyl nitrate, zirconium sulfate, ammonium zirconium carbonate, zirconium nitrate and titanium chloride.
The carbonaceous material is a mixture of two substances of carbon black, expanded graphite, starch, phenolic resin, sucrose and asphalt.
The silicon-containing material is silicon micropowder and Si3N4A mixture of (a).
The alumina-silicon carbonitride complex phase bulletproof ceramic prepared by the embodiment is detected as follows: the fracture toughness is 10-11 MPa m1/2(ii) a The compressive strength is 2850-3100 MPa; the Vickers hardness is 18-19 GPa; the bulk density is 3.25 to 3.35g/cm3(ii) a The average pore diameter is 150 to 250 nm.
Example 7
An alumina-silicon carbonitride complex phase bulletproof ceramic and a preparation method thereof. Dissolving 0.1-4 parts by mass of soluble salt in 4-7 parts by mass of water to obtain a salt solution; taking 85-87 parts by mass of alumina micro powder, 3-7 parts by mass of a silicon-containing material and 4-8 parts by mass of a carbon-containing material as raw materials; uniformly mixing the raw materials and the salt solution in a planetary ball mill to obtain a mixture; then, mechanically pressing the mixture under the condition of 100-130 MPa to obtain a green body; and finally, drying the green body at the temperature of 150-200 ℃ for 12-24 hours, and preserving heat at the temperature of 1600-1700 ℃ for 4-8 hours in a nitrogen atmosphere to obtain the alumina-silicon carbonitride complex phase bulletproof ceramic.
The soluble salt is a mixture of three substances of aluminum chloride, aluminum nitrate, magnesium chloride, magnesium nitrate, magnesium sulfate, zirconium tetrachloride, zirconium oxychloride, zirconyl nitrate, zirconium sulfate, ammonium zirconium carbonate, zirconium nitrate and titanium chloride.
The carbon-containing material is a mixture of three substances of carbon black, expanded graphite, starch, phenolic resin, cane sugar and asphalt.
The silicon-containing material is elemental silicon powder, silicon micropowder and Si3N4The mixture of (1).
The alumina-silicon carbonitride complex phase bulletproof ceramic prepared by the embodiment is detected as follows: the fracture toughness is 9-11 MPa m1/2(ii) a The compressive strength is 2800-3000 MPa; the Vickers hardness is 18-19 GPa; the bulk density is 3.3 to 3.4g/cm3(ii) a The average pore diameter is 150 to 200 nm.
Example 8
An alumina-silicon carbonitride complex phase bulletproof ceramic and a preparation method thereof. Dissolving 0.1-4 parts by mass of soluble salt in 4-7 parts by mass of water to obtain a salt solution; taking 85-87 parts by mass of alumina micro powder, 3-7 parts by mass of a silicon-containing material and 4-8 parts by mass of a carbon-containing material as raw materials; uniformly mixing the raw materials and the salt solution in a planetary ball mill to obtain a mixture; then, mechanically pressing the mixture under the condition of 120-150 MPa to obtain a green body; and finally, drying the green body at the temperature of 110-160 ℃ for 24-36 hours, and preserving heat at the temperature of 1700-1800 ℃ for 1-5 hours in a nitrogen atmosphere to obtain the alumina-silicon carbonitride complex phase bulletproof ceramic.
The soluble salt is a mixture of four substances of aluminum chloride, aluminum nitrate, magnesium chloride, magnesium nitrate, magnesium sulfate, zirconium tetrachloride, zirconium oxychloride, zirconyl nitrate, zirconium sulfate, ammonium zirconium carbonate, zirconium nitrate and titanium chloride.
The carbon-containing material is a mixture of four substances of carbon black, expanded graphite, starch, phenolic resin, cane sugar and asphalt.
The silicon-containing material is elemental silicon powder.
The alumina-silicon carbonitride complex phase bulletproof ceramic prepared by the embodiment is detected as follows: the fracture toughness is 9.5-11 MPa m1/2(ii) a The compressive strength is 2800-3000 MPa; the Vickers hardness is 17-18 GPa; the bulk density is 3.3 to 3.4g/cm3(ii) a The average pore diameter is 150 to 200 nm.
Example 9
An alumina-silicon carbonitride complex phase bulletproof ceramic and a preparation method thereof. Dissolving 4-8 parts by mass of soluble salt in 7-10 parts by mass of water to obtain a salt solution; 87-90 parts by mass of alumina micro powder, 5-10 parts by mass of a silicon-containing material and 1-5 parts by mass of a carbon-containing material are used as raw materials; uniformly mixing the raw materials and the salt solution in a planetary ball mill to obtain a mixture; then, mechanically pressing the mixture under the condition of 100-130 MPa to obtain a green body; and finally, drying the green body at the temperature of 150-200 ℃ for 12-24 hours, and preserving heat at the temperature of 1600-1700 ℃ for 4-8 hours in a nitrogen atmosphere to obtain the alumina-silicon carbonitride complex phase bulletproof ceramic.
The soluble salt is one of aluminum chloride, aluminum nitrate, magnesium chloride, magnesium nitrate, magnesium sulfate, zirconium tetrachloride, zirconium oxychloride, zirconyl nitrate, zirconium sulfate, ammonium zirconium carbonate, zirconium nitrate, and titanium chloride.
The carbonaceous material is one of carbon black, expanded graphite, starch, phenolic resin, sucrose and asphalt.
The silicon-containing material is silicon micropowder.
The alumina-silicon carbonitride complex phase bulletproof ceramic prepared by the embodiment is detected as follows: the fracture toughness is 10.5-11.5 MPa m1/2(ii) a The compressive strength is 2800-3000 MPa; the Vickers hardness is 15-16 GPa; the bulk density is 3.15 to 3.25g/cm3(ii) a The average pore diameter is 200 to 250 nm.
Example 10
An alumina-silicon carbonitride complex phase bulletproof ceramic and a preparation method thereof. Dissolving 4-8 parts by mass of soluble salt in 7-10 parts by mass of water to obtain a salt solution; 87-90 parts by mass of alumina micro powder, 5-10 parts by mass of a silicon-containing material and 1-5 parts by mass of a carbon-containing material are used as raw materials; uniformly mixing the raw materials and the salt solution in a planetary ball mill to obtain a mixture; then, mechanically pressing the mixture under the condition of 120-150 MPa to obtain a green body; and finally, drying the green body at the temperature of 110-160 ℃ for 24-36 hours, and preserving heat at the temperature of 1700-1800 ℃ for 1-5 hours in a nitrogen atmosphere to obtain the alumina-silicon carbonitride complex phase bulletproof ceramic.
The soluble salt is a mixture of two of aluminum chloride, aluminum nitrate, magnesium chloride, magnesium nitrate, magnesium sulfate, zirconium tetrachloride, zirconium oxychloride, zirconyl nitrate, zirconium sulfate, ammonium zirconium carbonate, zirconium nitrate and titanium chloride.
The carbonaceous material is a mixture of two substances of carbon black, expanded graphite, starch, phenolic resin, sucrose and asphalt.
The silicon-containing material is Si3N4。
The alumina-silicon carbonitride complex phase bulletproof ceramic prepared by the embodiment is detected as follows: the fracture toughness is 10-11 MPa m1/2(ii) a The compressive strength is 2750-2900 MPa; the Vickers hardness is 16-17 GPa; the bulk density is 3.15 to 3.25g/cm3(ii) a The average pore diameter is 150 to 200 nm.
Example 11
An alumina-silicon carbonitride complex phase bulletproof ceramic and a preparation method thereof. Dissolving 4-8 parts by mass of soluble salt in 7-10 parts by mass of water to obtain a salt solution; 87-90 parts by mass of alumina micro powder, 3-7 parts by mass of a silicon-containing material and 4-8 parts by mass of a carbon-containing material are used as raw materials; uniformly mixing the raw materials and the salt solution in a planetary ball mill to obtain a mixture; then, mechanically pressing the mixture under the condition of 100-130 MPa to obtain a green body; and finally, drying the green body at the temperature of 150-200 ℃ for 12-24 hours, and preserving heat at the temperature of 1600-1700 ℃ for 4-8 hours in a nitrogen atmosphere to obtain the alumina-silicon carbonitride complex phase bulletproof ceramic.
The soluble salt is a mixture of three substances of aluminum chloride, aluminum nitrate, magnesium chloride, magnesium nitrate, magnesium sulfate, zirconium tetrachloride, zirconium oxychloride, zirconyl nitrate, zirconium sulfate, ammonium zirconium carbonate, zirconium nitrate and titanium chloride.
The carbon-containing material is a mixture of three substances of carbon black, expanded graphite, starch, phenolic resin, cane sugar and asphalt.
The silicon-containing material is a mixture of elemental silicon powder and silicon micropowder.
Oxygen prepared in this exampleThe detection shows that the aluminum oxide-silicon carbonitride complex phase bulletproof ceramic comprises the following components in percentage by weight: the fracture toughness is 10.5-12 MPa m1/2(ii) a The compressive strength is 2850-2950 MPa; the Vickers hardness is 15-17 GPa; the bulk density is 3.2 to 3.3g/cm3(ii) a The average pore diameter is 150 to 200 nm.
Example 12
An alumina-silicon carbonitride complex phase bulletproof ceramic and a preparation method thereof. Dissolving 4-8 parts by mass of soluble salt in 7-10 parts by mass of water to obtain a salt solution; 87-90 parts by mass of alumina micro powder, 3-7 parts by mass of a silicon-containing material and 4-8 parts by mass of a carbon-containing material are used as raw materials; uniformly mixing the raw materials and the salt solution in a planetary ball mill to obtain a mixture; then, mechanically pressing the mixture under the condition of 120-150 MPa to obtain a green body; and finally, drying the green body at the temperature of 110-160 ℃ for 24-36 hours, and preserving heat at the temperature of 1700-1800 ℃ for 1-5 hours in a nitrogen atmosphere to obtain the alumina-silicon carbonitride complex phase bulletproof ceramic.
The soluble salt is a mixture of four substances of aluminum chloride, aluminum nitrate, magnesium chloride, magnesium nitrate, magnesium sulfate, zirconium tetrachloride, zirconium oxychloride, zirconyl nitrate, zirconium sulfate, ammonium zirconium carbonate, zirconium nitrate and titanium chloride.
The carbon-containing material is a mixture of four substances of carbon black, expanded graphite, starch, phenolic resin, cane sugar and asphalt.
The silicon-containing material is elemental silicon powder and Si3N4A mixture of (a).
The alumina-silicon carbonitride complex phase bulletproof ceramic prepared by the embodiment is detected as follows: the fracture toughness is 10-11 MPa m1/2(ii) a The compressive strength is 2800-2950 MPa; the Vickers hardness is 16-18 GPa; the bulk density is 3.2 to 3.3g/cm3(ii) a The average pore diameter is 200 to 250 nm.
Example 13
An alumina-silicon carbonitride complex phase bulletproof ceramic and a preparation method thereof. Dissolving 4-8 parts by mass of soluble salt in 7-10 parts by mass of water to obtain a salt solution; taking 85-87 parts by mass of alumina micro powder, 5-10 parts by mass of a silicon-containing material and 1-5 parts by mass of a carbon-containing material as raw materials; uniformly mixing the raw materials and the salt solution in a planetary ball mill to obtain a mixture; then, mechanically pressing the mixture under the condition of 100-130 MPa to obtain a green body; and finally, drying the green body at the temperature of 150-200 ℃ for 12-24 hours, and preserving heat at the temperature of 1600-1700 ℃ for 4-8 hours in a nitrogen atmosphere to obtain the alumina-silicon carbonitride complex phase bulletproof ceramic.
The soluble salt is one of aluminum chloride, aluminum nitrate, magnesium chloride, magnesium nitrate, magnesium sulfate, zirconium tetrachloride, zirconium oxychloride, zirconyl nitrate, zirconium sulfate, ammonium zirconium carbonate, zirconium nitrate, and titanium chloride.
The carbonaceous material is one of carbon black, expanded graphite, starch, phenolic resin, sucrose and asphalt.
The silicon-containing material is silicon micropowder and Si3N4A mixture of (a).
The alumina-silicon carbonitride complex phase bulletproof ceramic prepared by the embodiment is detected as follows: the fracture toughness is 11-12 MPa m1/2(ii) a The compressive strength is 2700-2800 MPa; the Vickers hardness is 14-16 GPa; the bulk density is 3.1-3.2 g/cm3(ii) a The average pore diameter is 150 to 200 nm.
Example 14
An alumina-silicon carbonitride complex phase bulletproof ceramic and a preparation method thereof. Dissolving 4-8 parts by mass of soluble salt in 7-10 parts by mass of water to obtain a salt solution; taking 85-87 parts by mass of alumina micro powder, 5-10 parts by mass of a silicon-containing material and 1-5 parts by mass of a carbon-containing material as raw materials; uniformly mixing the raw materials and the salt solution in a planetary ball mill to obtain a mixture; then, mechanically pressing the mixture under the condition of 120-150 MPa to obtain a green body; and finally, drying the green body at the temperature of 110-160 ℃ for 24-36 hours, and preserving heat at the temperature of 1700-1800 ℃ for 1-5 hours in a nitrogen atmosphere to obtain the alumina-silicon carbonitride complex phase bulletproof ceramic.
The soluble salt is a mixture of two of aluminum chloride, aluminum nitrate, magnesium chloride, magnesium nitrate, magnesium sulfate, zirconium tetrachloride, zirconium oxychloride, zirconyl nitrate, zirconium sulfate, ammonium zirconium carbonate, zirconium nitrate and titanium chloride.
The carbonaceous material is a mixture of two substances of carbon black, expanded graphite, starch, phenolic resin, sucrose and asphalt.
The silicon-containing material is elemental silicon powder, silicon micropowder and Si3N4The mixture of (1).
The alumina-silicon carbonitride complex phase bulletproof ceramic prepared by the embodiment is detected as follows: the fracture toughness is 10.5-11 MPa m1/2(ii) a The compressive strength is 2700-2800 MPa; the Vickers hardness is 15-17 GPa; the bulk density is 3.1-3.2 g/cm3(ii) a The average pore diameter is 150 to 200 nm.
Example 15
An alumina-silicon carbonitride complex phase bulletproof ceramic and a preparation method thereof. Dissolving 4-8 parts by mass of soluble salt in 7-10 parts by mass of water to obtain a salt solution; taking 85-87 parts by mass of alumina micro powder, 3-7 parts by mass of a silicon-containing material and 4-8 parts by mass of a carbon-containing material as raw materials; uniformly mixing the raw materials and the salt solution in a planetary ball mill to obtain a mixture; then, mechanically pressing the mixture under the condition of 100-130 MPa to obtain a green body; and finally, drying the green body at the temperature of 150-200 ℃ for 12-24 hours, and preserving heat at the temperature of 1600-1700 ℃ for 4-8 hours in a nitrogen atmosphere to obtain the alumina-silicon carbonitride complex phase bulletproof ceramic.
The soluble salt is a mixture of three substances of aluminum chloride, aluminum nitrate, magnesium chloride, magnesium nitrate, magnesium sulfate, zirconium tetrachloride, zirconium oxychloride, zirconyl nitrate, zirconium sulfate, ammonium zirconium carbonate, zirconium nitrate and titanium chloride.
The carbon-containing material is a mixture of three substances of carbon black, expanded graphite, starch, phenolic resin, cane sugar and asphalt.
The silicon-containing material is elemental silicon powder.
The alumina-silicon carbonitride complex phase bulletproof ceramic prepared by the embodiment is detected as follows: the fracture toughness is 10-12 MPa m1/2(ii) a The compressive strength is 2750-2900 MPa; the Vickers hardness is 14-16 GPa; the bulk density is 3.15 to 3.25g/cm3(ii) a The average pore diameter is 200 to 250 nm.
Example 16
An alumina-silicon carbonitride complex phase bulletproof ceramic and a preparation method thereof. Dissolving 4-8 parts by mass of soluble salt in 7-10 parts by mass of water to obtain a salt solution; taking 85-87 parts by mass of alumina micro powder, 3-7 parts by mass of a silicon-containing material and 4-8 parts by mass of a carbon-containing material as raw materials; uniformly mixing the raw materials and the salt solution in a planetary ball mill to obtain a mixture; then, mechanically pressing the mixture under the condition of 120-150 MPa to obtain a green body; and finally, drying the green body at the temperature of 110-160 ℃ for 24-36 hours, and preserving heat at the temperature of 1700-1800 ℃ for 1-5 hours in a nitrogen atmosphere to obtain the alumina-silicon carbonitride complex phase bulletproof ceramic.
The soluble salt is a mixture of four substances of aluminum chloride, aluminum nitrate, magnesium chloride, magnesium nitrate, magnesium sulfate, zirconium tetrachloride, zirconium oxychloride, zirconyl nitrate, zirconium sulfate, ammonium zirconium carbonate, zirconium nitrate and titanium chloride.
The carbon-containing material is a mixture of four substances of carbon black, expanded graphite, starch, phenolic resin, cane sugar and asphalt.
The silicon-containing material is silicon micropowder.
The alumina-silicon carbonitride complex phase bulletproof ceramic prepared by the embodiment is detected as follows: the fracture toughness is 11-12 MPa m1/2(ii) a The compressive strength is 2750-2900 MPa; the Vickers hardness is 15-17 GPa; the bulk density is 3.15 to 3.25g/cm3(ii) a The average pore diameter is 200 to 250 nm.
Compared with the prior art, the specific implementation mode has the following positive effects:
(1) this embodiment incorporates a soluble salt that, when dissolved in water, undergoes hydrolysis, which can form hydrated cations. The hydrated cations exist in the form of tetramer or dimer, and the bridging hydroxyl groups can be connected with each other, so that a network structure with nanopores is formed in situ. In the heat treatment process, the nanometer pores are quickly sealed in the crystal grains due to the difference of sintering performance of the nanometer particles generated by the decomposition of the tetramer or the dimer and the alumina micro powder, so as to form nanometer-sized intracrystalline pores. The existence of the nanocrystalline internal pores can effectively absorb energy for reducing crack propagation, leads cracks to be bridged and deflected, and improves the mechanical property of the alumina-silicon carbonitride complex phase bulletproof ceramic; in addition, the introduction of air holes can reduce the density of the alumina-silicon carbonitride complex phase bulletproof ceramic.
(2) The silicon-containing material and the carbon-containing material introduced by the specific embodiment can form a SiCN phase in situ in the heat treatment process in the nitrogen atmosphere, and the SiCN phase has excellent mechanical properties, so that on one hand, a secondary interface can be formed on the material, and the pinning dislocation effect can hinder crack propagation; on the other hand, due to the difference in thermal expansion coefficient between the SiCN phase and the matrix, residual thermal stress is formed inside the material, causing the cracks to bridge and deflect, and the propagation path to be extended. Therefore, the toughness and strength of the material can be further improved.
The detection shows that the alumina-silicon carbonitride complex phase bulletproof ceramic prepared by the embodiment has the following characteristics: the fracture toughness is 7-12 MPam1/2(ii) a The compressive strength is 2700-3200 MPa; the Vickers hardness is 14-20 GPa; the bulk density is 3.1 to 3.5g/cm3(ii) a The average pore diameter is 100 to 250 nm.
Therefore, the specific implementation mode has low cost and simple process, and the prepared alumina-silicon carbonitride complex phase bulletproof ceramic has the characteristics of high strength, high hardness, high toughness, large amount of nano-scale intragranular pores and lower volume density.

Claims (4)

1. A preparation method of an alumina-silicon carbonitride complex phase bulletproof ceramic is characterized in that 0.1-8 parts by mass of soluble salt is dissolved in 4-10 parts by mass of water to obtain a salt solution; taking 85-90 parts by mass of alumina micro powder, 3-10 parts by mass of a silicon-containing material and 1-8 parts by mass of a carbon-containing material as raw materials; uniformly mixing the raw materials and the salt solution in a planetary ball mill to obtain a mixture; then, mechanically pressing the mixture under the condition of 100-150 MPa to obtain a green body; finally, drying the green body at the temperature of 110-200 ℃ for 12-36 hours, and preserving heat at the temperature of 1600-1800 ℃ for 1-8 hours in a nitrogen atmosphere to obtain the alumina-silicon carbonitride complex phase bulletproof ceramic;
the soluble salt is 1-4 of aluminum chloride, aluminum nitrate, magnesium chloride, magnesium nitrate, magnesium sulfate, zirconium tetrachloride, zirconium oxychloride, zirconyl nitrate, zirconium sulfate, ammonium zirconium carbonate, zirconium nitrate and titanium chloride;
the silicon-containing material is elemental silicon powder, silicon micropowder and Si3N4More than one of them.
2. The method for preparing the alumina-silicon carbonitride complex phase bulletproof ceramic as claimed in claim 1, characterized in that Al of the alumina micropowder2O3Content (wt.)>97wt%, particle diameter D501 to 8 μm.
3. The preparation method of the alumina-silicon carbonitride complex phase bulletproof ceramic of claim 1, wherein the carbonaceous material is 1-4 of carbon black, expanded graphite, starch, phenolic resin, sucrose and asphalt.
4. An alumina-silicon carbonitride complex phase bulletproof ceramic, which is characterized in that the alumina-silicon carbonitride complex phase bulletproof ceramic is prepared by the preparation method of the alumina-silicon carbonitride complex phase bulletproof ceramic according to any claim 1 to 3.
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