CN115259859B - Boron carbide bulletproof ceramic material and preparation method thereof - Google Patents
Boron carbide bulletproof ceramic material and preparation method thereof Download PDFInfo
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Abstract
The invention relates to the technical field of bulletproof materials, in particular to a boron carbide bulletproof ceramic material and a preparation method thereof, wherein the bulletproof ceramic material is prepared by vacuum siliconizing a ceramic blank; the raw materials of the ceramic body comprise a ceramic main material, a reinforcing agent and a binder; the ceramic main material comprises three boron carbide particles with different particle sizes, wherein the particle size of the first-level boron carbide particle is 20-25 mu m, the particle size of the second-level boron carbide particle is 1-5 mu m, and the particle size of the third-level boron carbide particle is 50nm-500nm; and the reinforcing agent is carbon nano tube, titanium dioxide, aluminum oxide and the like modified by a coupling agent. According to the invention, the boron carbide bulletproof ceramic material is prepared by selecting boron carbide particles with different particle grades and adopting a vacuum siliconizing reaction sintering method, the sintering temperature is low, the preparation process is simple, the cost is low, and meanwhile, the mechanical property of the boron carbide bulletproof ceramic material is improved.
Description
Technical Field
The invention relates to the technical field of bulletproof materials, in particular to a boron carbide bulletproof ceramic material and a preparation method thereof.
Background
With the rapid development of modern science and technology and national economy, the fields of aerospace, military industry, nuclear industry, mechanical manufacturing and the like are continuously developed, and the performance requirements of various materials are continuously improved. Compared with the traditional metal material, the ceramic material has the advantages of low density, high hardness, high strength, heat resistance, shock resistance and the like, is stand out in the field of bulletproof armors, and is widely applied to military industry or civil special vehicles. Among them, boron carbide (B) 4 C) As an important structural ceramic, the ceramic has the most wide application as a bulletproof material due to low density, ultrahigh hardness, high-temperature wear resistance, high melting point, chemical corrosion resistance and excellent neutron absorption performance, and is an important structural ceramic material.
At present, boron carbide ceramic materials are mainly prepared by powder metallurgy methods, and commonly used sintering methods include hot-pressing sintering, pressureless sintering, hot isostatic pressing, spark plasma sintering, reactive sintering, and the like. Various sintering methods have advantages and disadvantages, the hot-pressing sintering temperature is high, sintering aids must be added, and therefore, the energy consumption is high and the cost is high; the temperature required by pressureless sintering is extremely high; hot isostatic pressing sintering equipment is expensive and has limited sintering size; the spark plasma sintering equipment is expensive, the process is complex, the cost is high, and the method is not suitable for industrialization. In recent years, the reaction sintering method has been receiving much attention and research in the field. The reactive sintering method generally refers to a vacuum infiltration method, and infiltrates molten silicon or metal and the like into a blank body at a certain temperature by virtue of a capillary action, and fills gaps in the blank body after reaction to form a compact blank body. The reaction sintering method has remarkable advantages, such as low sintering temperature, short time consumption, low cost, simple process and the like.
However, the reaction sintering method has some disadvantages, and the mechanical property of the simple substance silicon is poor, so that the existence of the simple substance silicon reduces the mechanical property of the ceramic material to a certain extent, and therefore, how to improve the reaction sintering method to improve the mechanical property of the ceramic material is still a research hotspot in the field.
Disclosure of Invention
Technical problem to be solved
In view of the above disadvantages and defects of the prior art, the invention provides a boron carbide bulletproof ceramic material and a preparation method thereof, wherein a ceramic blank is prepared by selecting boron carbide particles with different particle sizes, and the boron carbide bulletproof ceramic material is prepared by adopting a vacuum siliconizing reaction sintering method, so that the sintering temperature is low, the preparation process is simple, the cost is low, and the mechanical properties of the boron carbide bulletproof ceramic material are improved.
(II) technical scheme
In order to achieve the purpose, the invention adopts the main technical scheme that:
in a first aspect, the invention provides a boron carbide bulletproof ceramic material, which is prepared by vacuum siliconizing a ceramic blank;
the raw materials of the ceramic body comprise a ceramic main material, a reinforcing agent and a binder;
the ceramic main material comprises primary boron carbide particles, secondary boron carbide particles and tertiary boron carbide particles, wherein the particle size of the primary boron carbide particles is 20-25 mu m, the particle size of the secondary boron carbide particles is 1-5 mu m, and the particle size of the tertiary boron carbide particles is 50nm-500nm;
in addition, the reinforcing agent is modified by a coupling agent; the reinforcing agent is one or a combination of more of carbon nano tube, titanium dioxide, titanium diboride, titanium carbide and aluminum oxide.
More preferably, the primary boron carbide particles have a particle size of 25 μm, the secondary boron carbide particles have a particle size of 3 μm, and the tertiary boron carbide particles have a particle size of 300nm.
More preferably, the binder is a phenolic resin.
More preferably, the mass ratio of the primary boron carbide particles to the secondary boron carbide particles to the tertiary boron carbide particles is 7 to 10:3~6:3~6.
More preferably, the mass ratio of the primary boron carbide particles, the secondary boron carbide particles and the tertiary boron carbide particles is 8:4:5.
preferably, the reinforcing agent accounts for 0.5-2% of the mass of the ceramic body.
More preferably, the reinforcing agent is 0.5 percent of carbon nano tubes and 1.5 percent of titanium dioxide based on the total mass of the ceramic body.
More preferably, the coupling agent is one of silane coupling agents KH550, KH560 and KH 570.
In a second aspect, the invention provides a preparation method of a boron carbide bulletproof ceramic material, which mainly comprises the following steps:
s1, taking primary boron carbide particles, secondary boron carbide particles and tertiary boron carbide particles according to a ratio, respectively dissolving the primary boron carbide particles, the secondary boron carbide particles and the tertiary boron carbide particles in a certain amount of deionized water, then performing ultrasonic dispersion, sequentially adding a secondary boron carbide particle dispersion liquid and a primary boron carbide particle dispersion liquid into the dispersed tertiary boron carbide particle dispersion liquid, continuously stirring, and uniformly stirring to obtain a ceramic main material;
s2, dissolving a certain amount of reinforcing agent and coupling agent in an ethanol aqueous solution for modification, then adding the modified reinforcing agent into the ceramic main material, adding a binder, continuously stirring to form a mixed material, and then drying, grinding and sieving to form a material to be molded;
s3, pressing and forming the material to be molded, and drying to obtain a ceramic blank;
and S4, placing the silicon block on the ceramic blank, and performing vacuum siliconizing reaction sintering in a vacuum furnace to obtain the boron carbide bulletproof ceramic material.
Preferably, in step S1, the particle size of the first-level boron carbide particles is 20 to 25 μm, the particle size of the second-level boron carbide particles is 1 to 5 μm, and the particle size of the third-level boron carbide particles is 50nm to 500nm.
Preferably, the reinforcing agent is one or a combination of more of carbon nano tube, titanium dioxide, titanium diboride, titanium carbide and aluminum oxide.
More preferably, the mass ratio of the primary boron carbide particles to the secondary boron carbide particles to the tertiary boron carbide particles is 7 to 10:3~6:3~6.
Preferably, the ultrasonic dispersion of the third-level boron carbide particles is 30 to 40min, the ultrasonic dispersion of the second-level boron carbide particles is 20 to 30min, and the ultrasonic dispersion of the first-level boron carbide particles is 5 to 15min.
Preferably, in step S2, the drying temperature is 50-55 ℃ and the drying time is 10-12 hours.
Preferably, the one-way compression molding is adopted in the step S3, the pressure is 150MPa to 200MPa, and the dwell time is 10s to 15s.
Preferably, in the step S4, in the vacuum siliconizing reaction sintering process, the temperature is raised to 1450-1600 ℃ at a temperature rise speed of 5-10 ℃/min, and the temperature is kept for 20-50min.
(III) advantageous effects
According to the boron carbide bulletproof ceramic material and the preparation method thereof, the ceramic main material is prepared by selecting the boron carbide particles with three particle sizes and reasonably matching the boron carbide particles. When in compression molding, the primary boron carbide particles and the secondary boron carbide particles are micron-sized boron carbide particles with different sizes and mainly serve as frameworks of the green bodies; the three-level boron carbide particles are nano boron carbide particles, on one hand, small particles can fill pores among large-particle frameworks, so that a ceramic blank is tightly stacked, and a more compact blank is favorably formed.
In addition, the boron carbide bulletproof ceramic material and the preparation method thereof of the invention also add a reinforcing agent besides the ceramic main material, wherein the reinforcing agent is selected from one or more of carbon nano tube, titanium dioxide, titanium diboride, titanium carbide and aluminum oxide. The addition of reinforcing agents such as carbon nano tubes, titanium dioxide and the like can effectively improve the fracture toughness of the ceramic material. Meanwhile, the reinforcing agent is modified by the coupling agent, and the modified reinforcing agent can be more uniformly dispersed and is easier to combine with the ceramic main material. Furthermore, in the vacuum siliconizing process, the carbon nano tube is added to promote the infiltration of silicon, so that the ceramic material is more compact, and the hardness of the ceramic material is improved.
Furthermore, the phenolic resin is used as the binder, on one hand, the phenolic resin can well combine the ceramic main material and the reinforcing agent together, on the other hand, the phenolic resin can also provide a carbon source for the vacuum siliconizing process, and the carbon source can be more fully infiltrated into the green body and more uniformly distributed due to better fluidity, so that the carbon source can be more fully reacted with silicon, the residual carbon in the final ceramic material is reduced, and the formed product silicon carbide is more uniformly distributed in the ceramic material, thereby improving the mechanical property of the ceramic material.
In conclusion, according to the boron carbide bulletproof ceramic material and the preparation method thereof, the boron carbide particles with different particle grades are selected as the main ceramic material to prepare the ceramic body, so that the ceramic body is more compact; in addition, the ceramic body is also added with a reinforcing agent, so that the mechanical property of the ceramic body is further improved; meanwhile, the boron carbide bulletproof ceramic material is prepared by adopting a vacuum siliconizing reaction sintering method, the sintering temperature is low, the preparation process is simple, the cost is low, and various mechanical properties of the boron carbide bulletproof ceramic material can be improved.
Detailed Description
In order to better understand the technical solution, the present invention will be described in detail by the following embodiments. It should be understood, however, that the present invention may be embodied in various forms and should not be construed as limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete, and will fully convey the scope of the invention to those skilled in the art.
One embodiment of the invention provides a boron carbide bulletproof ceramic material, which is prepared by vacuum siliconizing a ceramic blank; the raw materials of the ceramic body comprise a ceramic main material, a reinforcing agent and a binder; the ceramic main material comprises primary boron carbide particles, secondary boron carbide particles and tertiary boron carbide particles, the particle size of the primary boron carbide particles is 20-25 mu m, the particle size of the secondary boron carbide particles is 1-5 mu m, and the particle size of the tertiary boron carbide particles is 50nm-500nm; in addition, the reinforcing agent is modified by adopting a coupling agent; the reinforcing agent is one or a combination of more of carbon nano tube, titanium dioxide, titanium diboride, titanium carbide and aluminum oxide, and the binder is phenolic resin. In the embodiment, the reinforcing agent accounts for 0.5-2% of the mass of the ceramic body. More preferably, the primary boron carbide particles have a particle size of 25 μm, the secondary boron carbide particles have a particle size of 3 μm, and the tertiary boron carbide particles have a particle size of 300nm. In the embodiment, the mass ratio of the primary boron carbide particles to the secondary boron carbide particles to the tertiary boron carbide particles is 7 to 10:3~6:3~6. More preferably, the mass ratio of the primary boron carbide particles, the secondary boron carbide particles and the tertiary boron carbide particles is 8:4:5.
in the boron carbide bulletproof ceramic material, three boron carbide particles with different particle sizes are selected, and the particle sizes are respectively 20-25 μm, 1-5 μm and 50nm-500nm from coarse to fine, wherein the boron carbide particles with larger particle sizes are used as a framework of a ceramic blank, and the boron carbide particles with small particle sizes can be filled into the framework of the ceramic blank, so that the ceramic blank is more compact, and the boron carbide particles with nanometer levels can be dispersed among grains with large particle sizes and inside the grains, so that abnormal growth of the grains is inhibited, more uniform grains are formed, and the mechanical property of the ceramic material is improved. In addition, the boron carbide ceramic particles with larger particle size can also enable the reaction with silicon to be more moderate in the siliconizing process, thereby reducing the generation of high-density SiC and controlling the density of the ceramic material.
However, with the addition of boron carbide particles with larger particle size, the hardness of the ceramic material is continuously increased, but the strength and toughness of the ceramic material are reduced by adding too much boron carbide particles, so that secondary boron carbide particles need to be further added for regulation, and meanwhile, the boron carbide particles of three particle grades need to be kept in a reasonable proportion range to enable the ceramic material to have certain hardness and improve the density. In addition, in order to compensate for the problem of reduced toughness of the ceramic material in the preparation process, the embodiment adds carbon nanotubes, titanium dioxide, titanium carbide, aluminum oxide and the like as reinforcing agents, and the reinforcing agents are modified by silane coupling agents, so that the modified reinforcing agents improve the binding capacity with the ceramic main material, improve the dispersibility, and enable the ceramic main material to be dispersed more uniformly, wherein the addition of a proper amount of carbon nanotubes can effectively improve the fracture toughness of the ceramic material, promote the infiltration of silicon, further improve the compactness of the ceramic material, and improve the mechanical properties of the ceramic material.
Another embodiment of the invention provides a preparation method of a boron carbide bulletproof ceramic material, which mainly comprises the following steps:
s1, taking the primary boron carbide particles, the secondary boron carbide particles and the tertiary boron carbide particles according to the proportion, respectively dissolving the primary boron carbide particles, the secondary boron carbide particles and the tertiary boron carbide particles in a certain amount of deionized water, and then performing ultrasonic dispersion. Wherein the mass ratio of the first-level boron carbide particles to the second-level boron carbide particles to the third-level boron carbide particles is 7 to 10:3~6:3~6, the particle size of the first-level boron carbide particles is 20-25 μm, the particle size of the second-level boron carbide particles is 1-5 μm, and the particle size of the third-level boron carbide particles is 50nm-500nm. And then, sequentially adding the secondary boron carbide particle dispersion liquid and the primary boron carbide particle dispersion liquid into the dispersed tertiary boron carbide particle dispersion liquid, continuously stirring, and uniformly stirring to obtain the ceramic main material. In the embodiment, according to different particle sizes of three boron carbide particles, three particle grades of boron carbide are subjected to ultrasonic dispersion respectively, different ultrasonic dispersion times are set, three-grade boron carbide particles are subjected to ultrasonic dispersion for 30 to 40min, two-grade boron carbide particles are subjected to ultrasonic dispersion for 20 to 30min, and one-grade boron carbide particles are subjected to ultrasonic dispersion for 5 to 15min, and then three dispersed particle grade boron carbide dispersions are sequentially mixed from fine to coarse and are continuously stirred, so that the three particle grades of boron carbide can be uniformly dispersed, and the preparation efficiency is also improved.
S2, dissolving a reinforcing agent accounting for 0.5-2% of the total mass of the ceramic body and a silane coupling agent accounting for 0.1-0.3% of the total mass of the ceramic body into an ethanol water solution for modification, wherein the reinforcing agent can be one or a combination of more of carbon nano tubes, titanium dioxide, titanium diboride, titanium carbide and aluminum oxide. And then adding the modified reinforcing agent into the ceramic main material which is continuously stirred, and simultaneously adding a binder, wherein the binder in the embodiment is phenolic resin, the mass of carbon in the phenolic resin is 8-10% of the total mass of the boron carbide particles of the three particle grades, continuously stirring for 8-10 hours to form a mixed material, and then drying, grinding and sieving to form a material to be molded, wherein in the embodiment, an oven is adopted for drying, the drying temperature is 50-55 ℃, and the drying time is 10-12 hours.
And S3, pressing and forming the material to be molded, and drying to obtain a ceramic blank. The embodiment adopts one-way compression molding, the pressure is 150MPa to 200MPa, and the dwell time is 10s to 15s.
And S4, placing the silicon block on the ceramic blank, and performing vacuum siliconizing reaction sintering in a vacuum furnace to obtain the boron carbide bulletproof ceramic material. In the process of vacuum siliconizing, the temperature is increased to 1450 ℃ to 1600 ℃ at the temperature increase speed of 5 to 10 ℃/min, then the temperature is maintained for 20 to 50min, then the temperature is cooled to the room temperature, and finally the infiltration is finished, so that the boron carbide bulletproof ceramic material is prepared.
Example 1
The embodiment provides a preparation method of a boron carbide bulletproof ceramic material, which comprises the following steps:
s1, taking first-stage boron carbide particles (25 micrometers), adding a proper amount of deionized water, performing ultrasonic dispersion for 5min, taking second-stage boron carbide particles (3 micrometers), adding a proper amount of deionized water, performing ultrasonic dispersion for 25min, taking third-stage boron carbide particles (300 nm), adding a proper amount of deionized water, performing ultrasonic dispersion for 30min, wherein the mass ratio of the first-stage boron carbide particles to the second-stage boron carbide particles to the third-stage boron carbide particles is 8:4:5. and after dispersion, adding the secondary boron carbide particle dispersion liquid into the tertiary boron carbide particle dispersion liquid and then adding the primary boron carbide particle dispersion liquid in the process of continuously stirring to obtain the ceramic main material.
S2, dissolving a carbon nano tube accounting for 0.5 percent of the total mass of the ceramic body, titanium dioxide powder accounting for 1.5 percent of the total mass of the ceramic body and a silane coupling agent accounting for 0.3 percent of the total mass of the ceramic body in an ethanol water solution for modification, then adding the modified carbon nano tube and titanium dioxide powder into the ceramic main material which is continuously stirred, then adding a certain amount of phenolic resin to ensure that the carbon content in the phenolic resin is 10 percent of the total mass of three particle-level boron carbides, continuously stirring for 9 hours, then placing the obtained mixed material into an oven for drying at the drying temperature of 50 ℃, grinding after drying for 12 hours, and then sieving by a 50-mesh sieve to form a material to be molded.
And S3, performing one-way compression molding on the material to be molded under the pressure of 150MPa for 15S. Then placing the ceramic blank into a drying oven for drying at the temperature of 50 ℃ for 12 hours to obtain a ceramic blank.
And S4, placing the silicon block on the ceramic blank, performing vacuum siliconizing reaction sintering in a vacuum furnace, heating to 1500 ℃ at a heating rate of 5 ℃/min, then preserving heat for 30min, cooling to room temperature, and finishing infiltration to obtain the boron carbide bulletproof ceramic material.
Example 2
The embodiment provides a preparation method of a boron carbide bulletproof ceramic material, which comprises the following steps:
s1, taking primary boron carbide particles (25 micrometers), adding a proper amount of deionized water, performing ultrasonic dispersion for 5min, taking secondary boron carbide particles (3 micrometers), adding a proper amount of deionized water, performing ultrasonic dispersion for 25min, taking tertiary boron carbide particles (300 nm), adding a proper amount of deionized water, performing ultrasonic dispersion for 30min, wherein the mass ratio of the primary boron carbide particles to the secondary boron carbide particles to the tertiary boron carbide particles is 9:5:5. and after dispersion, adding the secondary boron carbide particle dispersion liquid into the tertiary boron carbide particle dispersion liquid and then adding the primary boron carbide particle dispersion liquid in the process of continuously stirring to obtain the ceramic main material.
S2, dissolving a carbon nano tube accounting for 0.5 percent of the total mass of the ceramic body, titanium dioxide powder accounting for 1.5 percent of the total mass of the ceramic body and a silane coupling agent accounting for 0.3 percent of the total mass of the ceramic body in an ethanol water solution for modification, then adding the modified carbon nano tube and titanium dioxide powder into the ceramic main material which is continuously stirred, then adding a certain amount of phenolic resin to ensure that the carbon content in the phenolic resin is 10 percent of the total mass of three particle-level boron carbides, continuously stirring for 9 hours, then placing the obtained mixed material into an oven for drying at the drying temperature of 50 ℃, grinding after drying for 12 hours, and then sieving by a 50-mesh sieve to form a material to be molded.
S3, performing one-way compression molding on the material to be molded, keeping the pressure at 150MPa for 15S. Then placing the ceramic blank into a drying oven for drying at the temperature of 50 ℃ for 12 hours to obtain a ceramic blank.
And S4, placing the silicon block on the ceramic blank, performing vacuum siliconizing reaction sintering in a vacuum furnace, heating to 1500 ℃ at a heating rate of 5 ℃/min, then preserving heat for 30min, cooling to room temperature, and finishing infiltration to obtain the boron carbide bulletproof ceramic material.
Example 3
The embodiment provides a preparation method of a boron carbide bulletproof ceramic material, which comprises the following steps:
s1, taking primary boron carbide particles (25 micrometers), adding a proper amount of deionized water, performing ultrasonic dispersion for 5min, taking secondary boron carbide particles (3 micrometers), adding a proper amount of deionized water, performing ultrasonic dispersion for 25min, taking tertiary boron carbide particles (300 nm), adding a proper amount of deionized water, performing ultrasonic dispersion for 30min, wherein the mass ratio of the primary boron carbide particles to the secondary boron carbide particles to the tertiary boron carbide particles is 7:4:6. and after dispersion, adding the secondary boron carbide particle dispersion liquid into the tertiary boron carbide particle dispersion liquid and then adding the primary boron carbide particle dispersion liquid in the process of continuously stirring to obtain the ceramic main material.
S2, dissolving a carbon nano tube accounting for 0.8 percent of the total mass of the ceramic body, titanium dioxide powder accounting for 1 percent of the total mass of the ceramic body and a silane coupling agent accounting for 0.2 percent of the total mass of the ceramic body in an ethanol water solution for modification, then adding the modified carbon nano tube and titanium dioxide powder into the ceramic main material which is continuously stirred, then adding a certain amount of phenolic resin to ensure that the carbon content in the phenolic resin is 10 percent of the total mass of three particle-level boron carbides, continuously stirring for 9 hours, then placing the obtained mixed material into an oven for drying at the drying temperature of 50 ℃, grinding after drying for 12 hours, and then sieving by a 50-mesh sieve to form the material to be molded.
And S3, performing one-way compression molding on the material to be molded under the pressure of 150MPa for 15S. Then placing the ceramic blank into a drying oven for drying at the temperature of 50 ℃ for 12 hours to obtain a ceramic blank.
And S4, placing the silicon block on the ceramic blank, performing vacuum siliconizing reaction sintering in a vacuum furnace, heating to 1500 ℃ at a heating rate of 5 ℃/min, then preserving heat for 30min, cooling to room temperature, and finishing infiltration to obtain the boron carbide bulletproof ceramic material.
Example 4
The embodiment provides a preparation method of a boron carbide bulletproof ceramic material, which comprises the following steps:
s1, adding a proper amount of deionized water into primary boron carbide particles (20 microns), performing ultrasonic dispersion for 10min, adding a proper amount of deionized water into secondary boron carbide particles (5 microns), performing ultrasonic dispersion for 25min, adding a proper amount of deionized water into tertiary boron carbide particles (500 nm), performing ultrasonic dispersion for 30min, wherein the mass ratio of the primary boron carbide particles to the secondary boron carbide particles to the tertiary boron carbide particles is 8:4:5. and after dispersion, adding the secondary boron carbide particle dispersion liquid into the tertiary boron carbide particle dispersion liquid and then adding the primary boron carbide particle dispersion liquid in the process of continuously stirring to obtain the ceramic main material.
S2, dissolving a carbon nano tube accounting for 0.5 percent of the total mass of the ceramic body, titanium dioxide powder accounting for 1.5 percent of the total mass of the ceramic body and a silane coupling agent accounting for 0.3 percent of the total mass of the ceramic body in an ethanol water solution for modification, then adding the modified carbon nano tube and titanium dioxide powder into the ceramic main material which is continuously stirred, then adding a certain amount of phenolic resin to ensure that the carbon content in the phenolic resin is 10 percent of the total mass of three particle-level boron carbides, continuously stirring for 9 hours, then placing the obtained mixed material into an oven for drying at the drying temperature of 50 ℃, grinding after drying for 12 hours, and then sieving by a 50-mesh sieve to form a material to be molded.
S3, performing one-way compression molding on the material to be molded, keeping the pressure at 150MPa for 15S. Then placing the ceramic blank into a drying oven for drying at the temperature of 50 ℃ for 12 hours to obtain a ceramic blank.
And S4, placing the silicon block on the ceramic blank, performing vacuum siliconizing reaction sintering in a vacuum furnace, heating to 1500 ℃ at a heating rate of 5 ℃/min, then preserving heat for 30min, cooling to room temperature, and finishing infiltration to obtain the boron carbide bulletproof ceramic material.
Example 5
The embodiment provides a preparation method of a boron carbide bulletproof ceramic material, which comprises the following steps:
s1, taking first-stage boron carbide particles (25 micrometers), adding a proper amount of deionized water, performing ultrasonic dispersion for 5min, taking second-stage boron carbide particles (3 micrometers), adding a proper amount of deionized water, performing ultrasonic dispersion for 25min, taking third-stage boron carbide particles (300 nm), adding a proper amount of deionized water, performing ultrasonic dispersion for 30min, wherein the mass ratio of the first-stage boron carbide particles to the second-stage boron carbide particles to the third-stage boron carbide particles is 8:4:5. and after dispersion, adding the secondary boron carbide particle dispersion liquid into the tertiary boron carbide particle dispersion liquid and then adding the primary boron carbide particle dispersion liquid in the process of continuously stirring to obtain the ceramic main material.
S2, dissolving 1% of carbon nano tubes and 0.2% of silane coupling agent by the total mass of the ceramic body in an ethanol water solution for modification, then adding the modified carbon nano tubes into the ceramic main material which is continuously stirred, adding a certain amount of phenolic resin to enable the carbon content in the phenolic resin to be 8% of the total mass of the three particle-level boron carbides, continuously stirring for 9 hours, then placing the obtained mixed material in an oven for drying at the drying temperature of 55 ℃, grinding after drying for 10 hours, and then sieving by a 50-mesh sieve to form the material to be molded.
And S3, performing one-way compression molding on the material to be molded under the pressure of 150MPa for 15S. Then placing the ceramic blank into an oven for drying at the temperature of 55 ℃ for 10 hours to obtain a ceramic blank.
And S4, placing the silicon block on the ceramic blank, performing vacuum siliconizing reaction sintering in a vacuum furnace, heating to 1550 ℃ at the heating rate of 6 ℃/min, then preserving heat for 20min, cooling to room temperature, and finishing infiltration to obtain the boron carbide bulletproof ceramic material.
Example 6
The embodiment provides a preparation method of a boron carbide bulletproof ceramic material, which comprises the following steps:
s1, taking primary boron carbide particles (25 micrometers), adding a proper amount of deionized water, performing ultrasonic dispersion for 5min, taking secondary boron carbide particles (3 micrometers), adding a proper amount of deionized water, performing ultrasonic dispersion for 25min, taking tertiary boron carbide particles (300 nm), adding a proper amount of deionized water, performing ultrasonic dispersion for 30min, wherein the mass ratio of the primary boron carbide particles to the secondary boron carbide particles to the tertiary boron carbide particles is 8:4:5. and after dispersion, adding the secondary boron carbide particle dispersion liquid into the tertiary boron carbide particle dispersion liquid and then adding the primary boron carbide particle dispersion liquid in the process of continuously stirring to obtain the ceramic main material.
S2, taking alumina powder accounting for 2% of the total mass of the ceramic body and a silane coupling agent accounting for 0.2% of the total mass of the ceramic body, dissolving the alumina powder and the silane coupling agent in an ethanol water solution for modification, adding the modified alumina powder into the ceramic main material which is continuously stirred, adding a certain amount of phenolic resin to enable the carbon content in the phenolic resin to be 8% of the total mass of the three particle-grade boron carbides, continuously stirring for 9 hours, then placing the obtained mixed material in a drying oven for drying at the drying temperature of 55 ℃, grinding after drying for 10 hours, and then sieving by a 50-mesh sieve to form the material to be molded.
S3, performing one-way compression molding on the material to be molded, keeping the pressure at 150MPa for 15S. Then placing the ceramic blank into a drying oven for drying at the temperature of 55 ℃ for 10 hours to obtain a ceramic blank.
And S4, placing the silicon block on the ceramic blank, performing vacuum siliconizing reaction sintering in a vacuum furnace, heating to 1550 ℃ at a heating rate of 6 ℃/min, then preserving heat for 20min, then cooling to room temperature, and finishing infiltration to obtain the boron carbide bulletproof ceramic material.
Comparative example 1
In this example, conditions were changed based on example 1, and in this example, unlike example 1, the mass ratio of primary boron carbide particles (25 μm), secondary boron carbide particles (3 μm), and tertiary boron carbide particles (300 nm) was 12.
Comparative example 2
In this example, conditions were changed based on example 1, and unlike example 1, this example contained only micrometer-sized boron carbide particles, i.e., only primary boron carbide particles (25 μm) and secondary boron carbide particles (3 μm), and the boron carbide bulletproof ceramic material was obtained without changing the process and conditions.
Comparative example 3
In this example, conditions were changed based on example 1, and unlike example 1, the three particle-size boron carbide particles in this example were not subjected to respective ultrasonic dispersion processes, specifically:
s1, mixing the components in a mass ratio of 8:4: and 5, adding primary boron carbide particles (25 mu m), secondary boron carbide particles (3 mu m) and tertiary boron carbide particles (300 nm) into a certain amount of deionized water, ultrasonically dispersing for 20min, and mechanically stirring to obtain the ceramic main material.
The rest processes and conditions are unchanged, and the boron carbide bulletproof ceramic material is prepared.
Comparative example 4
In the present example, conditions are changed on the basis of example 1, and different from example 1, the mass fraction of the reinforcing agent in the ceramic green body is 3.5%, wherein the mass fraction of the carbon nanotubes is 1%, the mass fraction of the titanium dioxide powder is 2.5%, and the rest processes and conditions are not changed, so that the boron carbide bulletproof ceramic material is prepared.
The examples 1 to 6 and comparative examples 1 to 4 were subjected to the performance test, and the results are shown in table 1.
Table 1 boron carbide ballistic ceramic material performance test results
From the above results, it can be seen that the boron carbide bulletproof ceramic materials prepared in examples 1 to 6 all have high vickers hardness, fracture toughness and bending strength, high overall mechanical properties, and excellent performance. The boron carbide bulletproof ceramic materials prepared in comparative examples 1 to 4 have slightly poor performances, and the results prove that the mass ratio of the boron carbide of three particle grades is changed, excessive boron carbide particles with larger particle sizes are added, the using amount of the nano-scale boron carbide particles is reduced, and although the ceramic materials still have higher hardness, the fracture toughness is obviously reduced; and all mechanical properties of the ceramic material without the added nano-scale boron carbide particles are obviously reduced, so that the addition of a certain amount of nano-scale boron carbide particles can increase the compactness of the ceramic material and improve the mechanical properties of the ceramic material.
In addition, as can be seen from comparative example 3, the ultrasonic dispersion of the boron carbide of the three particle grades respectively helps to mix uniformly, so that a more uniform and dense ceramic material can be formed in the subsequent preparation process. In contrast, as shown in comparative example 4, although the addition of the reinforcing agent in an excessive amount increases the fracture toughness and the bending strength of the ceramic material, the hardness of the ceramic material is significantly reduced because the hardness of the reinforcing agent itself is lower than that of boron carbide, and thus the amount of the reinforcing agent needs to be controlled within a certain range to ensure that the ceramic material has appropriate hardness, fracture toughness and bending strength.
Finally, it should be noted that: the above embodiments are only used to illustrate the technical solution of the present invention, and not to limit the same; while the invention has been described in detail and with reference to the foregoing embodiments, it will be understood by those skilled in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; and the modifications or the substitutions do not make the essence of the corresponding technical solutions depart from the scope of the technical solutions of the embodiments of the present invention.
Claims (3)
1. A preparation method of a boron carbide bulletproof ceramic material is characterized by comprising the following steps:
s1, taking primary boron carbide particles, secondary boron carbide particles and tertiary boron carbide particles according to a ratio, respectively dissolving the primary boron carbide particles, the secondary boron carbide particles and the tertiary boron carbide particles in a certain amount of deionized water, then carrying out ultrasonic dispersion, sequentially adding a secondary boron carbide particle dispersion liquid and a primary boron carbide particle dispersion liquid into the dispersed tertiary boron carbide particle dispersion liquid, continuously stirring, and uniformly stirring to obtain a ceramic main material;
the three-level boron carbide particles are subjected to ultrasonic dispersion for 30 to 40min, the two-level boron carbide particles are subjected to ultrasonic dispersion for 20 to 30min, and the first-level boron carbide particles are subjected to ultrasonic dispersion for 5 to 15min;
the particle size of the primary boron carbide particles is 20-25 mu m, the particle size of the secondary boron carbide particles is 1~5 mu m, and the particle size of the tertiary boron carbide particles is 50-500nm;
the mass ratio of the primary boron carbide particles to the secondary boron carbide particles to the tertiary boron carbide particles is 7 to 10:3~6:3~6;
s2, dissolving a certain amount of reinforcing agent and coupling agent in an ethanol aqueous solution for modification, then adding the modified reinforcing agent into the ceramic main material, adding a binder, continuously stirring to form a mixed material, and then drying, grinding and sieving to form a material to be molded;
the reinforcing agent is one or a combination of more of carbon nano tube, titanium dioxide, titanium diboride, titanium carbide and aluminum oxide;
s3, pressing and forming the material to be molded, and drying to obtain a ceramic blank; the reinforcing agent accounts for 0.5-2% of the mass of the ceramic body;
and S4, placing the silicon block on the ceramic blank, and performing vacuum siliconizing reaction sintering in a vacuum furnace to obtain the boron carbide bulletproof ceramic material.
2. The preparation method of the boron carbide bulletproof ceramic material according to claim 1, wherein in the step S3, unidirectional compression molding is adopted, the pressure is 150MPa to 200MPa, and the pressure maintaining time is 10s to 15s.
3. The preparation method of the boron carbide bulletproof ceramic material according to claim 1, wherein in the vacuum siliconizing reaction sintering process in the step S4, the temperature is raised to 1450-1600 ℃ at a temperature raising speed of 5-10 ℃/min, and the temperature is kept for 20-50min.
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