CN108794045B - High-toughness aluminum oxide-based bulletproof ceramic and preparation method thereof - Google Patents

High-toughness aluminum oxide-based bulletproof ceramic and preparation method thereof Download PDF

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CN108794045B
CN108794045B CN201810749927.3A CN201810749927A CN108794045B CN 108794045 B CN108794045 B CN 108794045B CN 201810749927 A CN201810749927 A CN 201810749927A CN 108794045 B CN108794045 B CN 108794045B
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alumina
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bulletproof ceramic
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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 a high-toughness alumina-based bulletproof ceramic and a preparation method thereof. The technical scheme is as follows: taking 85-95 parts by mass of alumina micro powder and 5-15 parts by mass of silica micro powder as raw materials; dissolving 0.1-8 parts by mass of soluble salt in 4-10 parts by mass of water to obtain a salt solution; placing the raw materials, the salt solution and 1-5 parts by mass of a binding agent into a planetary ball mill, and uniformly mixing to obtain a mixture; performing mechanical pressing on the mixture under the condition of 100-150 MPa to obtain a green body; and then 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 to obtain the high-toughness alumina-based bulletproof ceramic. The high-toughness aluminum oxide-based bulletproof ceramic prepared by the invention has the characteristics of high strength, high hardness, high toughness and lower volume density.

Description

High-toughness aluminum oxide-based bulletproof ceramic and preparation method thereof
Technical Field
The invention belongs to the technical field of alumina-based bulletproof ceramics. In particular to high-toughness alumina-based bulletproof ceramic and a preparation method thereof.
Background
The bulletproof armor material is one of indispensable key materials in modern military wars, the performance quality of the bulletproof armor material directly restricts the operational capability of 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. Early used bulletproof armor materials were traditional high strength steel, aluminum alloy, titanium alloy, and other metal materials with good toughness and strength, but hardness was not ideal, and in addition, generally had higher density for militaryThe mobility of equipment and personnel is not good. In contrast, ceramic materials and composite materials have become common ballistic armor materials at present due to their high hardness, high strength, corrosion resistance, low density, and high cost performance. A commonly used bulletproof ceramic armor material has B4C、SiC、Si3N4、Al2O3And the like. B is4C. SiC and Si3N4Non-oxide materials, such as these, while having high hardness, low density, and excellent ballistic performance, are expensive, difficult to sinter, and difficult to prepare, and therefore, are used only in certain critical locations. In contrast, due to Al2O3The material has excellent sintering performance, mature preparation process, low production cost, rich raw materials and Al2O3Bulletproof ceramic armor materials are the mainstream bulletproof materials used in China at present. However, Al is compared to non-oxide ceramic materials2O3The defects of poor toughness and high density of the ceramic material reduce the energy absorption rate and the multiple-strike resistance of the ceramic material, and further expansion of application of the ceramic material is hindered. Therefore, Al having high toughness and low density has been developed2O3The base bulletproof ceramic armor material meets the national important development requirements and has irreplaceable significance for improving the integral national defense capability of China.
At home and abroad against Al2O3The research on bulletproof ceramics mainly focuses on toughening. Al (Al)2O3Ceramic toughening methods can be generally classified into the following two categories: (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. However, current toughening methods work on Al2O3The improvement degree of the ceramic fracture toughness is limited, and the requirements of low density, high strength and high hardness of the bulletproof ceramic armor material are difficult to meet. Therefore, for Al2O3The service condition of the bulletproof ceramic armor material needs to be provided with a novel strengthening and toughening measure which can greatly improve the fracture toughness of the ceramic, and simultaneously improve the strength and hardness of the material and reduce the densityAnd (4) applying.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and aims to provide a preparation method of high-toughness alumina-based bulletproof ceramic; the high-toughness alumina-based bulletproof ceramic prepared by the method has high strength, high hardness, high toughness and lower volume density.
In order to realize the task, the technical scheme adopted by the invention is as follows: taking 85-95 parts by mass of alumina micro powder and 5-15 parts by mass of silica micro powder as raw materials; dissolving 0.1-8 parts by mass of soluble salt in 4-10 parts by mass of water to obtain a salt solution; placing the raw materials, the salt solution and 1-5 parts by mass of a binding agent into a planetary ball mill, and uniformly mixing to obtain a mixture; performing mechanical pressing on the mixture under the condition of 100-150 MPa to obtain a green body; and then 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 to obtain the high-toughness alumina-based 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 content of Al2O3 in the alumina micro powder is more than 97 wt%, and the particle size D50 of the alumina micro powder is 1-8 μm.
The content of SiO2 in the silicon dioxide micro powder is more than 90 wt%, and the particle size D50 of the silicon dioxide micro powder is 0.1-3 mu m.
The binding agent is more than one of polyethylene glycol, phenolic resin, hydroxymethyl cellulose and paraffin.
Due to the adoption of the technical scheme, compared with the prior art, the invention has the following positive effects:
(1) according to the invention, soluble salt is introduced, and the salt is hydrolyzed when being dissolved in water, so that hydrated cations can be formed, the hydrated cations exist in a tetramer or dimer form, and bridging hydroxyl groups of the hydrated cations can be connected with each other, so that a network structure with nanopores is formed in situ. SiO introduced during the heat treatment2The micro powder can react with the alumina micro powder, the volume expansion in the reaction process can form in-situ stress in the material, the nano particles formed by decomposing the tetramer or the dimer can be promoted to exert high-temperature superplasticity, the crystal boundary moves rapidly, and the nano pores are rapidly sealed in the crystal grains, so that micro-nano intra-crystal pores are formed. The nano-crystal inner pores can effectively relieve stress concentration in the use process of the material, prevent the material from being damaged, absorb energy for reducing crack propagation, enable cracks to be bridged and deflected and improve the mechanical property of the ceramic material; in addition, the introduction of pores can reduce the density of the ceramic material.
(2) SiO introduced by the invention2The micro powder can react with the alumina micro powder to form mullite in situ. Firstly, the volume expansion accompanied in the reaction process can generate compressive stress on cracks and prevent the cracks from further expanding; in addition, columnar mullite grains are distributed among alumina grains in a cross way to form a secondary interface, and the pinning dislocation effect of the secondary interface can block crack propagation; finally, residual thermal stresses will form inside the material due to the difference in thermal expansion coefficient of the second phase and the matrix, which will relax when the crack propagates into the residual stress region, with a tendency to close the crack, thus preventing further propagation of the crack. Therefore, the mechanical property of the bulletproof ceramic can be further improved.
The high-toughness aluminum oxide-based bulletproof ceramic prepared by the invention is detected as follows: the fracture toughness is 7-11 MPa m1/2(ii) a The compressive strength is 2600-3100 MPa; the Vickers hardness is 12-18 GPa; the bulk density is 3.0 to 3.3g/cm3(ii) a The average pore diameter is 100 to 250 nm.
Therefore, the high-toughness alumina-based bulletproof ceramic prepared by the invention has the characteristics of high strength, high hardness, high toughness and lower volume density.
Detailed Description
The invention is further described with reference to specific embodiments, without limiting the scope of protection:
in order to avoid repetition, the raw materials related to this specific embodiment are uniformly described as follows, and are not described in detail in the embodiments:
al of the alumina micropowder2O3Content (wt.)>97 wt%, particle diameter D of alumina micropowder501 to 8 μm.
SiO of the fine silica powder2Content (wt.)>90 wt%, particle diameter D of fine silica powder500.1 to 3 μm.
Example 1
A high-toughness alumina-based bulletproof ceramic and a preparation method thereof. Taking 90-95 parts by mass of alumina micro powder and 5-10 parts by mass of silica micro powder as raw materials; dissolving 0.1-4 parts by mass of soluble salt in 4-7 parts by mass of water to obtain a salt solution; placing the raw materials, the salt solution and 1-3 parts by mass of a binding agent into a planetary ball mill, and uniformly mixing to obtain a mixture; performing mechanical pressing on the mixture under the condition of 100-130 MPa to obtain a green body; and then 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 to obtain the high-toughness alumina-based 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 binding agent is one of polyethylene glycol, phenolic resin, hydroxymethyl cellulose and paraffin.
The high-toughness alumina-based bulletproof ceramic prepared by the embodiment is detected as follows: the fracture toughness is 8-9 MPa m1/2(ii) a The compressive strength is 2800-3000 MPa; the Vickers hardness is 16-18 GPa; the bulk density is 3.2 to 3.25g/cm3(ii) a The average pore diameter is 100 to 200 nm.
Example 2
A high-toughness alumina-based bulletproof ceramic and a preparation method thereof. Taking 90-95 parts by mass of alumina micro powder and 5-10 parts by mass of silica micro powder as raw materials; dissolving 0.1-4 parts by mass of soluble salt in 4-7 parts by mass of water to obtain a salt solution; placing the raw materials, the salt solution and 1-3 parts by mass of a binding agent into a planetary ball mill, and uniformly mixing to obtain a mixture; performing mechanical pressing on the mixture under the condition of 120-150 MPa to obtain a green body; and then drying the green body at 110-160 ℃ for 24-36 hours, and preserving heat at 1700-1800 ℃ for 1-5 hours to obtain the high-toughness alumina-based 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 binding agent is one of polyethylene glycol, phenolic resin, hydroxymethyl cellulose and paraffin.
The high-toughness alumina-based bulletproof ceramic prepared by the embodiment is detected as follows: the fracture toughness is 7.5-9 MPa m1/2(ii) a The compressive strength is 2700-2900 MPa; the Vickers hardness is 16-17 GPa; the bulk density is 3.2 to 3.25g/cm3(ii) a The average pore diameter is 100 to 200 nm.
Example 3
A high-toughness alumina-based bulletproof ceramic and a preparation method thereof. Taking 90-95 parts by mass of alumina micro powder and 5-10 parts by mass of silica micro powder as raw materials; dissolving 0.1-4 parts by mass of soluble salt in 4-7 parts by mass of water to obtain a salt solution; placing the raw materials, the salt solution and 3-5 parts by mass of a binding agent into a planetary ball mill, and uniformly mixing to obtain a mixture; performing mechanical pressing on the mixture under the condition of 100-130 MPa to obtain a green body; and then 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 to obtain the high-toughness alumina-based 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 binding agent is one of polyethylene glycol, phenolic resin, hydroxymethyl cellulose and paraffin.
The high-toughness alumina-based bulletproof ceramic prepared by the embodiment is detected as follows: a fracture toughness of7.5～9MPa m1/2(ii) a The compressive strength is 2900-3100 MPa; the Vickers hardness is 17-18 GPa; the bulk density is 3.2 to 3.3g/cm3(ii) a The average pore diameter is 100 to 250 nm.
Example 4
A high-toughness alumina-based bulletproof ceramic and a preparation method thereof. Taking 90-95 parts by mass of alumina micro powder and 5-10 parts by mass of silica micro powder as raw materials; dissolving 0.1-4 parts by mass of soluble salt in 4-7 parts by mass of water to obtain a salt solution; placing the raw materials, the salt solution and 3-5 parts by mass of a binding agent into a planetary ball mill, and uniformly mixing to obtain a mixture; performing mechanical pressing on the mixture under the condition of 120-150 MPa to obtain a green body; and then drying the green body at 110-160 ℃ for 24-36 hours, and preserving heat at 1700-1800 ℃ for 1-5 hours to obtain the high-toughness alumina-based 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 binding agent is one of polyethylene glycol, phenolic resin, hydroxymethyl cellulose and paraffin.
The high-toughness alumina-based bulletproof ceramic prepared by the embodiment is detected as follows: the fracture toughness is 7-8.5 MPa m1/2(ii) a The compressive strength is 2800-3000 MPa; the Vickers hardness is 17-18 GPa; the bulk density is 3.2 to 3.3g/cm3(ii) a The average pore diameter is 100 to 200 nm.
Example 5
A high-toughness alumina-based bulletproof ceramic and a preparation method thereof. Taking 85-90 parts by mass of alumina micro powder and 10-15 parts by mass of silica micro powder as raw materials; dissolving 0.1-4 parts by mass of soluble salt in 4-7 parts by mass of water to obtain a salt solution; placing the raw materials, the salt solution and 1-3 parts by mass of a binding agent into a planetary ball mill, and uniformly mixing to obtain a mixture; performing mechanical pressing on the mixture under the condition of 100-130 MPa to obtain a green body; and then 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 to obtain the high-toughness alumina-based 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 binding agent is a mixture of two substances of polyethylene glycol, phenolic resin, hydroxymethyl cellulose and paraffin.
The high-toughness alumina-based bulletproof ceramic prepared by the embodiment is detected as follows: the fracture toughness is 8.5-10 MPa m1 /2(ii) a The compressive strength is 2800-3000 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 6
A high-toughness alumina-based bulletproof ceramic and a preparation method thereof. Taking 85-90 parts by mass of alumina micro powder and 10-15 parts by mass of silica micro powder as raw materials; dissolving 0.1-4 parts by mass of soluble salt in 4-7 parts by mass of water to obtain a salt solution; placing the raw materials, the salt solution and 1-3 parts by mass of a binding agent into a planetary ball mill, and uniformly mixing to obtain a mixture; performing mechanical pressing on the mixture under the condition of 120-150 MPa to obtain a green body; and then drying the green body at 110-160 ℃ for 24-36 hours, and preserving heat at 1700-1800 ℃ for 1-5 hours to obtain the high-toughness alumina-based 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 binding agent is a mixture of two substances of polyethylene glycol, phenolic resin, hydroxymethyl cellulose and paraffin.
The high-toughness alumina-based bulletproof ceramic prepared by the embodiment is detected as follows: the fracture toughness is 9-10 MPa m1/2(ii) a The compressive strength is 2750-3000 MPa; the Vickers hardness is 16-18 GPa; the bulk density is 3.0 to 3.15g/cm3(ii) a The average pore diameter is 150 to 250 nm.
Example 7
A high-toughness alumina-based bulletproof ceramic and a preparation method thereof. Taking 85-90 parts by mass of alumina micro powder and 10-15 parts by mass of silica micro powder as raw materials; dissolving 0.1-4 parts by mass of soluble salt in 4-7 parts by mass of water to obtain a salt solution; placing the raw materials, the salt solution and 3-5 parts by mass of a binding agent into a planetary ball mill, and uniformly mixing to obtain a mixture; performing mechanical pressing on the mixture under the condition of 100-130 MPa to obtain a green body; and then 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 to obtain the high-toughness alumina-based 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 binding agent is a mixture of two substances of polyethylene glycol, phenolic resin, hydroxymethyl cellulose and paraffin.
The high-toughness alumina-based 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 2700-2900 MPa; the Vickers hardness is 16-17 GPa; the bulk density is 3.1 to 3.25g/cm3(ii) a The average pore diameter is 150 to 200 nm.
Example 8
A high-toughness alumina-based bulletproof ceramic and a preparation method thereof. Taking 85-90 parts by mass of alumina micro powder and 10-15 parts by mass of silica micro powder as raw materials; dissolving 0.1-4 parts by mass of soluble salt in 4-7 parts by mass of water to obtain a salt solution; placing the raw materials, the salt solution and 3-5 parts by mass of a binding agent into a planetary ball mill, and uniformly mixing to obtain a mixture; performing mechanical pressing on the mixture under the condition of 120-150 MPa to obtain a green body; and then drying the green body at 110-160 ℃ for 24-36 hours, and preserving heat at 1700-1800 ℃ for 1-5 hours to obtain the high-toughness alumina-based 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 binding agent is a mixture of two substances of polyethylene glycol, phenolic resin, hydroxymethyl cellulose and paraffin.
The high-toughness alumina-based bulletproof ceramic prepared by the embodiment is detected as follows: the fracture toughness is 8.5-10 MPa m1 /2(ii) a The compressive strength is 2700-2900 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 150 to 200 nm.
Example 9
A high-toughness alumina-based bulletproof ceramic and a preparation method thereof. Taking 90-95 parts by mass of alumina micro powder and 5-10 parts by mass of silica micro powder as raw materials; dissolving 4-8 parts by mass of soluble salt in 7-10 parts by mass of water to obtain a salt solution; placing the raw materials, the salt solution and 1-3 parts by mass of a binding agent into a planetary ball mill, and uniformly mixing to obtain a mixture; performing mechanical pressing on the mixture under the condition of 100-130 MPa to obtain a green body; and then 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 to obtain the high-toughness alumina-based 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 binding agent is a mixture of three substances of polyethylene glycol, phenolic resin, hydroxymethyl cellulose and paraffin.
The high-toughness alumina-based bulletproof ceramic prepared by the embodiment is detected as follows: the fracture toughness is 9.5-10.5 MPa m1/2(ii) a The compressive strength is 2700-2900 MPa; the Vickers hardness is 13-14 GPa; the bulk density is 3.05-3.15 g/cm3(ii) a The average pore diameter is 200 to 250 nm.
Example 10
A high-toughness alumina-based bulletproof ceramic and a preparation method thereof. Taking 90-95 parts by mass of alumina micro powder and 5-10 parts by mass of silica micro powder as raw materials; dissolving 4-8 parts by mass of soluble salt in 7-10 parts by mass of water to obtain a salt solution; placing the raw materials, the salt solution and 1-3 parts by mass of a binding agent into a planetary ball mill, and uniformly mixing to obtain a mixture; performing mechanical pressing on the mixture under the condition of 120-150 MPa to obtain a green body; and then drying the green body at 110-160 ℃ for 24-36 hours, and preserving heat at 1700-1800 ℃ for 1-5 hours to obtain the high-toughness alumina-based 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 binding agent is a mixture of three substances of polyethylene glycol, phenolic resin, hydroxymethyl cellulose and paraffin.
The high-toughness alumina-based bulletproof ceramic prepared by the embodiment is detected as follows: the fracture toughness is 9-10 MPa m1/2(ii) a The compressive strength is 2650-2800 MPa; the Vickers hardness is 14-15 GPa; the bulk density is 3.05-3.1 g/cm3(ii) a The average pore diameter is 150 to 200 nm.
Example 11
A high-toughness alumina-based bulletproof ceramic and a preparation method thereof. Taking 90-95 parts by mass of alumina micro powder and 5-10 parts by mass of silica micro powder as raw materials; dissolving 4-8 parts by mass of soluble salt in 7-10 parts by mass of water to obtain a salt solution; placing the raw materials, the salt solution and 3-5 parts by mass of a binding agent into a planetary ball mill, and uniformly mixing to obtain a mixture; performing mechanical pressing on the mixture under the condition of 100-130 MPa to obtain a green body; and then 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 to obtain the high-toughness alumina-based 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 binding agent is a mixture of three substances of polyethylene glycol, phenolic resin, hydroxymethyl cellulose and paraffin.
The high-toughness alumina-based 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 2750-2850 MPa; the Vickers hardness is 13-15 GPa; the bulk density is 3.1-3.2 g/cm3(ii) a The average pore diameter is 150 to 200 nm.
Example 12
A high-toughness alumina-based bulletproof ceramic and a preparation method thereof. Taking 90-95 parts by mass of alumina micro powder and 5-10 parts by mass of silica micro powder as raw materials; dissolving 4-8 parts by mass of soluble salt in 7-10 parts by mass of water to obtain a salt solution; placing the raw materials, the salt solution and 3-5 parts by mass of a binding agent into a planetary ball mill, and uniformly mixing to obtain a mixture; performing mechanical pressing on the mixture under the condition of 120-150 MPa to obtain a green body; and then drying the green body at 110-160 ℃ for 24-36 hours, and preserving heat at 1700-1800 ℃ for 1-5 hours to obtain the high-toughness alumina-based 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 binding agent is a mixture of three substances of polyethylene glycol, phenolic resin, hydroxymethyl cellulose and paraffin.
The high-toughness alumina-based bulletproof ceramic prepared by the embodiment is detected as follows: the fracture toughness is 9-10 MPa m1/2(ii) a The compressive strength is 2700-2850 MPa; the Vickers hardness is 14-15 GPa; the bulk density is 3.1 to 3.15g/cm3(ii) a The average pore diameter is 200 to 250 nm.
Example 13
A high-toughness alumina-based bulletproof ceramic and a preparation method thereof. Taking 85-90 parts by mass of alumina micro powder and 10-15 parts by mass of silica micro powder as raw materials; dissolving 4-8 parts by mass of soluble salt in 7-10 parts by mass of water to obtain a salt solution; placing the raw materials, the salt solution and 1-3 parts by mass of a binding agent into a planetary ball mill, and uniformly mixing to obtain a mixture; performing mechanical pressing on the mixture under the condition of 100-130 MPa to obtain a green body; and then 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 to obtain the high-toughness alumina-based 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 binding agent is a mixture of four substances of polyethylene glycol, phenolic resin, hydroxymethyl cellulose and paraffin.
The high-toughness alumina-based 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 2600-2700 MPa; the Vickers hardness is 12-13 GPa; the bulk density is 3.0 to 3.1g/cm3(ii) a The average pore diameter is 150 to 200 nm.
Example 14
A high-toughness alumina-based bulletproof ceramic and a preparation method thereof. Taking 85-90 parts by mass of alumina micro powder and 10-15 parts by mass of silica micro powder as raw materials; dissolving 4-8 parts by mass of soluble salt in 7-10 parts by mass of water to obtain a salt solution; placing the raw materials, the salt solution and 1-3 parts by mass of a binding agent into a planetary ball mill, and uniformly mixing to obtain a mixture; performing mechanical pressing on the mixture under the condition of 120-150 MPa to obtain a green body; and then drying the green body at 110-160 ℃ for 24-36 hours, and preserving heat at 1700-1800 ℃ for 1-5 hours to obtain the high-toughness alumina-based 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 binding agent is a mixture of four substances of polyethylene glycol, phenolic resin, hydroxymethyl cellulose and paraffin.
The high-toughness alumina-based bulletproof ceramic prepared by the embodiment is detected as follows: the fracture toughness is 9.5-10 MPa m1 /2(ii) a The compressive strength is 2600-2700 MPa; the Vickers hardness is 13-14 GPa; the bulk density is 3.0 to 3.05g/cm3(ii) a The average pore diameter is 150 to 200 nm.
Example 15
A high-toughness alumina-based bulletproof ceramic and a preparation method thereof. Taking 85-90 parts by mass of alumina micro powder and 10-15 parts by mass of silica micro powder as raw materials; dissolving 4-8 parts by mass of soluble salt in 7-10 parts by mass of water to obtain a salt solution; placing the raw materials, the salt solution and 3-5 parts by mass of a binding agent into a planetary ball mill, and uniformly mixing to obtain a mixture; placing the raw materials, the salt solution and 3-5 parts by mass of a binding agent into a planetary ball mill, and uniformly mixing to obtain a mixture; performing mechanical pressing on the mixture under the condition of 100-130 MPa to obtain a green body; and then 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 to obtain the high-toughness alumina-based 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 binding agent is a mixture of four substances of polyethylene glycol, phenolic resin, hydroxymethyl cellulose and paraffin.
The high-toughness alumina-based 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 2650-2800 MPa; the Vickers hardness is 12-14 GPa; the bulk density is 3.05-3.1 g/cm3(ii) a The average pore diameter is 200 to 250 nm.
Example 16
A high-toughness alumina-based bulletproof ceramic and a preparation method thereof. Taking 85-90 parts by mass of alumina micro powder and 10-15 parts by mass of silica micro powder as raw materials; dissolving 4-8 parts by mass of soluble salt in 7-10 parts by mass of water to obtain a salt solution; placing the raw materials, the salt solution and 3-5 parts by mass of a binding agent into a planetary ball mill, and uniformly mixing to obtain a mixture; placing the raw materials, the salt solution and 3-5 parts by mass of a binding agent into a planetary ball mill, and uniformly mixing to obtain a mixture; performing mechanical pressing on the mixture under the condition of 120-150 MPa to obtain a green body; and then drying the green body at 110-160 ℃ for 24-36 hours, and preserving heat at 1700-1800 ℃ for 1-5 hours to obtain the high-toughness alumina-based 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 binding agent is a mixture of four substances of polyethylene glycol, phenolic resin, hydroxymethyl cellulose and paraffin.
The high-toughness alumina-based 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 2650-2800 MPa; the Vickers hardness is 13-15 GPa; the bulk density is 3.05-3.15 g/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 introduces a soluble salt that hydrolyzes when dissolved in water, forming hydrated cations that exist as tetramers or dimers, with bridging hydroxyl groups that the hydrated cations have capable of interconnecting, thereby forming in situ a network structure with nanopores. SiO introduced during the heat treatment2The micro powder can react with the alumina micro powder, the volume expansion in the reaction process can form in-situ stress in the material, the nano particles formed by decomposing the tetramer or the dimer can be promoted to exert high-temperature superplasticity, and the grain boundaryAnd the nano pores are quickly sealed in the crystal grains by the quick movement, so that micro-nano intra-crystal pores are formed. The nano-crystal inner pores can effectively relieve stress concentration in the use process of the material, prevent the material from being damaged, absorb energy for reducing crack propagation, enable cracks to be bridged and deflected and improve the mechanical property of the ceramic material; in addition, the introduction of pores can reduce the density of the ceramic material.
(2) SiO introduced in this embodiment2The micro powder can react with the alumina micro powder to form mullite in situ. Firstly, the volume expansion accompanied in the reaction process can generate compressive stress on cracks and prevent the cracks from further expanding; in addition, columnar mullite grains are distributed among alumina grains in a cross way to form a secondary interface, and the pinning dislocation effect of the secondary interface can block crack propagation; finally, residual thermal stresses will form inside the material due to the difference in thermal expansion coefficient of the second phase and the matrix, which will relax when the crack propagates into the residual stress region, with a tendency to close the crack, thus preventing further propagation of the crack. Therefore, the mechanical property of the bulletproof ceramic can be further improved.
The high-toughness alumina-based bulletproof ceramic prepared by the embodiment is detected as follows: the fracture toughness is 7-11 MPa m1/2(ii) a The compressive strength is 2600-3100 MPa; the Vickers hardness is 12-18 GPa; the bulk density is 3.0 to 3.3g/cm3(ii) a The average pore diameter is 100 to 250 nm.
Therefore, the high-toughness alumina-based bulletproof ceramic prepared by the embodiment has the characteristics of high strength, high hardness, high toughness and lower volume density.

Claims (6)

1. A preparation method of a high-toughness alumina-based bulletproof ceramic is characterized in that 85-95 parts by mass of alumina micro powder and 5-15 parts by mass of silicon dioxide micro powder are used as raw materials; dissolving 0.1-8 parts by mass of soluble salt in 4-10 parts by mass of water to obtain a salt solution; placing the raw materials, the salt solution and 1-5 parts by mass of a binding agent into a planetary ball mill, and uniformly mixing to obtain a mixture; performing mechanical pressing on the mixture under the condition of 100-150 MPa to obtain a green body; and then 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 to obtain the high-toughness alumina-based bulletproof ceramic.
2. The method for preparing the high-toughness alumina-based bulletproof ceramic of claim 1, wherein the soluble salt is 1 to 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.
3. The process for the preparation of high toughness alumina-based ballistic ceramics according to claim 1, characterized in that the Al of the alumina micropowder2O3Content (wt.)>97 wt%, particle diameter D of alumina micropowder501 to 8 μm.
4. The process for preparing a high toughness alumina-based ballistic resistant ceramic according to claim 1, characterized in that the fine silica powder has a SiO2 content>90 wt%, particle diameter D of fine silica powder500.1 to 3 μm.
5. The method for preparing the high toughness alumina-based bulletproof ceramic of claim 1, wherein the binder is one or more of polyethylene glycol, phenolic resin, hydroxymethyl cellulose and paraffin.
6. A high-toughness alumina-based bulletproof ceramic is characterized in that the high-toughness alumina-based bulletproof ceramic is prepared by the preparation method of the high-toughness alumina-based bulletproof ceramic according to any claim 1 to 5.
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