CN111018531A - Preparation method of carbon nano tube toughened boron carbide ceramic - Google Patents
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Abstract
A preparation method of carbon nano tube toughened boron carbide ceramic belongs to the technical field of composite materials. The preparation method of the carbon nano tube toughened boron carbide ceramic comprises the following steps: s1, uniformly mixing the carbon nano tube and the carbon black in proportion, putting the mixture into a synthesis cavity, and putting the boric acid powder into a preheating cavity; s2, continuously introducing inert gas into the synthesis cavity from the preheating cavity, heating the synthesis cavity to a set temperature, and then heating the preheating cavity to the set temperature for reaction; s3, naturally cooling to room temperature, opening the synthesis cavity and taking out the high-purity boron carbide/carbon nanotube composite material; s4, adding water and glucose into the high-purity boron carbide/carbon nano tube composite material, ball-milling and mixing uniformly, spraying and granulating, cold-press molding, and vacuum hot-press sintering to obtain the high-toughness and high-hardness carbon nano tube toughened boron carbide ceramic. The invention can efficiently prepare the carbon nano tube toughened boron carbide ceramic.
Description
Technical Field
The invention relates to a technology in the field of composite materials, in particular to a preparation method of carbon nanotube toughened boron carbide ceramic.
Background
Boron carbide has the advantages of high melting point, low density, high strength, large neutron absorption cross section, excellent thermoelectric property, good mechanical stability and the like, has hardness second to diamond and cubic boron nitride, and has wide application in the fields of aerospace, national defense, nuclear energy, wear-resisting technology and the like. However, the current boron carbide-based composite ceramic still faces a plurality of problems in production, and is high in cost and difficult to industrialize.
The present invention has been made to solve the above-mentioned problems occurring in the prior art.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides a preparation method of carbon nanotube toughened boron carbide ceramic, which can efficiently prepare the carbon nanotube toughened boron carbide ceramic.
The invention relates to a preparation method of carbon nano tube toughened boron carbide ceramic, which comprises the following steps:
s1, uniformly mixing carbon nanotubes and carbon black in proportion, putting the mixture into a synthesis cavity, putting boric acid powder into a preheating cavity, sequentially connecting the preheating cavity, the synthesis cavity and a condensation cavity through flanges, vacuumizing and sealing, and filling a porous graphite heat insulation felt with a boron carbide coated surface at the joint of the flanges for heat insulation;
s2, continuously introducing inert gas into the synthesis cavity from the preheating cavity, then heating the preheating cavity and the synthesis cavity to the temperature of 300-400 ℃, heating the condensation cavity to the temperature of not less than 100 ℃, decomposing the boric acid powder to generate steam and boron oxide, and discharging the steam along with the inert gas; after the water vapor is completely discharged, heating the synthesis cavity to 1500-1800 ℃, then heating the preheating cavity to 500-1000 ℃, melting and continuously evaporating boron oxide, reacting the boron oxide and carbon black to generate boron carbide, allowing the residual unreacted boron oxide vapor to enter a condensation cavity for condensation and recrystallization, and eliminating the tail gas CO by long-time open fire;
s3, after the boron oxide in the preheating cavity is exhausted, continuously introducing inert gas to purge for a period of time, then stopping heating, naturally cooling to room temperature, then stopping introducing gas, opening the synthesis cavity and taking out the high-purity boron carbide/carbon nanotube composite material;
s4, adding water and glucose into the high-purity boron carbide/carbon nano tube composite material, ball-milling and mixing uniformly, spraying and granulating, cold-press molding, and vacuum hot-press sintering to obtain the high-toughness and high-hardness carbon nano tube toughened boron carbide ceramic.
In step S2, the flow rate of the inert gas is 0.2-3.0L/min.
In step S2, the weight ratio of boric acid powder to carbon black is (3-5): 1, and the weight ratio of carbon black to carbon nanotubes is (8-10): 1.
In step S3, the weight ratio of the boron carbide to the carbon nanotubes in the high purity boron carbide/carbon nanotube composite material is taken out as follows: (8.5-11): 1.
In step S4, the weight ratio of the high-purity boron carbide/carbon nanotube composite material to water and glucose is (93-100): 100 (5-7).
In step S4, the vacuum hot-pressing sintering temperature is 2000-2200 ℃, and the pressure is 50-70 MPa.
Technical effects
Compared with the prior art, the invention has the following technical effects:
1) the carbon nano tube and the carbon black are uniformly mixed and then synthesized into the boron carbide/carbon nano tube composite material to prepare the composite ceramic, and compared with the composite ceramic prepared by directly mixing the boron carbide and the carbon nano tube, the composite ceramic has more excellent performance;
2) the characteristics of high-temperature dehydration and gasification and carbon thermal reduction reaction of cheap boric acid powder are utilized to synthesize the high-purity boron carbide/carbon nano tube composite material, and then the boron carbide ceramic is fired, so that the production cost is low.
Drawings
FIG. 1 is a schematic view showing the structure of a preheating chamber, a synthesizing chamber and a condensing chamber in example 1;
FIG. 2 is an SEM photograph of carbon nanotubes in example 1;
FIG. 3 is an SEM photograph of the carbon nanotubes uniformly mixed with carbon black in example 1;
FIG. 4 is an SEM photograph of the boron carbide/carbon nanotube composite of example 1;
FIG. 5 is a SEM photograph of a cross-section of a carbon nanotube-toughened boron carbide ceramic (not polished and etched) in example 1;
in the figure: preheating cavity 1, purification cavity 2, condensation cavity 3, air vent 4.
Detailed Description
The invention is described in detail below with reference to the drawings and the detailed description.
Example 1
The embodiment relates to a preparation method of carbon nanotube toughened boron carbide ceramic, which comprises the following specific steps:
s1, uniformly mixing 100g of carbon nanotubes (SEM picture is shown in figure 2) and 850g of carbon black to obtain a mixture, putting the mixture into a synthesis cavity as shown in figure 3, putting 2.5kg of chemically pure boric acid powder into a preheating cavity, sequentially connecting the preheating cavity, the synthesis cavity and a condensation cavity through flanges, vacuumizing and sealing, and filling a porous graphite heat insulation felt with a surface coated with boron carbide at the joint of the flanges for heat insulation, as shown in figure 1;
s2, continuously introducing argon gas from the preheating cavity to the synthesis cavity at a flow rate of 0.5L/min, heating the preheating cavity and the synthesis cavity to a temperature of 400 ℃, heating the condensation cavity to a temperature of 100 ℃, decomposing the boric acid powder to generate steam and boron oxide, and discharging the steam along with inert gas; after the water vapor is completely discharged, heating the synthesis cavity to 1600 ℃, and then preheating the cavity to 600 ℃; boron oxide steam enters the synthesis cavity and reacts with carbon black to generate boron carbide, the residual unreacted boron oxide steam enters the condensation cavity for condensation and recrystallization, and tail gas CO is eliminated by long-term open fire;
s3, after boron oxide in the preheating cavity is exhausted, continuously introducing inert gas to purge for a period of time, such as 30min, stopping heating, naturally cooling to room temperature, stopping introducing gas, opening the synthesis cavity, and taking out the high-purity boron carbide/carbon nanotube composite material, wherein the boron carbide crystal grain is less than 500nm, and an SEM photograph is shown in figure 4, wherein the boron carbide content is 90.5 wt% and the carbon nanotube content is 9.5 wt%;
s4, mixing the high-purity boron carbide/carbon nanotube composite material with 600g of water and 20g of glucose by ball milling, uniformly mixing, performing spray granulation and cold press molding, and performing vacuum hot-pressing sintering at the sintering temperature of 2050 ℃ under the pressure of 50MPa to obtain the high-toughness and high-hardness carbon nanotube toughened boron carbide ceramic, wherein an SEM photograph is shown in FIG. 5.
The performance of the carbon nano tube toughened boron carbide ceramic is tested, the relative density is 99.5 percent TD, the bending strength is 710GPa, the Vickers hardness is 43GPa, and the fracture toughness is 7.9 MPa.m1/2。
Steps S1-S3 are carried out in an apparatus as shown in fig. 1, which comprises a preheating chamber 1, a synthesizing chamber 2 and a condensing chamber 3 connected in sequence by flanges; the preheating cavity 1 and the condensing cavity 3 are provided with vent holes 4 for introducing inert gas argon; the preheating cavity 1, the synthesis cavity 2 and the condensation cavity 3 are respectively made of one of quartz, alumina, zirconia and boron carbide, and different temperatures of the cavities can be guaranteed by setting a heating sleeve for heating.
It is to be emphasized that: the above embodiments are only preferred embodiments of the present invention, and are not intended to limit the present invention in any way, and all simple modifications, equivalent changes and modifications made to the above embodiments according to the technical spirit of the present invention are within the scope of the technical solution of the present invention.
Claims (6)
1. A preparation method of carbon nanotube toughened boron carbide ceramic is characterized by comprising the following steps:
s1, uniformly mixing carbon nanotubes and carbon black in proportion, putting the mixture into a synthesis cavity, putting boric acid powder into a preheating cavity, sequentially connecting the preheating cavity, the synthesis cavity and a condensation cavity through flanges, vacuumizing and sealing, and filling a porous graphite heat insulation felt with a boron carbide coated surface at the joint of the flanges for heat insulation;
s2, continuously introducing inert gas into the synthesis cavity from the preheating cavity, then heating the preheating cavity and the synthesis cavity to the temperature of 300-400 ℃, heating the condensation cavity to the temperature of not less than 100 ℃, decomposing the boric acid powder to generate steam and boron oxide, and discharging the steam along with the inert gas; after the water vapor is completely discharged, heating the synthesis cavity to 1500-1800 ℃, then heating the preheating cavity to 500-1000 ℃, melting and continuously evaporating boron oxide, reacting the boron oxide and carbon black to generate boron carbide, allowing the residual unreacted boron oxide vapor to enter a condensation cavity for condensation and recrystallization, and eliminating the tail gas CO by long-time open fire;
s3, after the boron oxide in the preheating cavity is exhausted, continuously introducing inert gas to purge for a period of time, then stopping heating, naturally cooling to room temperature, then stopping introducing gas, opening the synthesis cavity and taking out the high-purity boron carbide/carbon nanotube composite material;
s4, adding water and glucose into the high-purity boron carbide/carbon nano tube composite material, ball-milling and mixing uniformly, spraying and granulating, cold-press molding, and vacuum hot-press sintering to obtain the high-toughness and high-hardness carbon nano tube toughened boron carbide ceramic.
2. The method for preparing a carbon nanotube-toughened boron carbide ceramic according to claim 1, wherein in step S2, the flow rate of the inert gas is 0.2 to 3.0L/min.
3. The method for preparing a carbon nanotube-toughened boron carbide ceramic according to claim 1, wherein in step S2, the weight ratio of the boric acid powder to the carbon black is (3-5): 1, and the weight ratio of the carbon black to the carbon nanotubes is (8-10): 1.
4. The method for preparing the carbon nanotube toughened boron carbide ceramic according to claim 1, wherein the weight ratio of the boron carbide to the carbon nanotubes in the taken high-purity boron carbide/carbon nanotube composite material is (8.5-11): 1.
5. The method for preparing the carbon nanotube-toughened boron carbide ceramic according to claim 1, wherein in step S4, the weight ratio of the high-purity boron carbide/carbon nanotube composite material to water and glucose is (93-100): 100, (5-7).
6. The method for preparing a carbon nanotube-toughened boron carbide ceramic according to claim 1, wherein in step S4, the vacuum hot-pressing sintering temperature is 2000 to 2200 ℃, and the pressure is 50 to 70 MPa.
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Cited By (4)
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| CN113004052A (en) * | 2021-02-07 | 2021-06-22 | 沈阳中钛装备制造有限公司 | Multi-walled carbon nanotube toughened boron carbide-based ceramic material and preparation method and application thereof |
| CN113666750A (en) * | 2021-08-16 | 2021-11-19 | 中硼科技(威海)有限公司 | Light high-performance boron carbide-based bulletproof ceramic and preparation method thereof |
| CN115108835A (en) * | 2021-03-19 | 2022-09-27 | 广东金鑫得新材料有限公司 | Method for manufacturing rapid high-densification boron carbide plate |
| CN115448723A (en) * | 2022-07-11 | 2022-12-09 | 中晶城康资源再生利用技术有限公司 | Preparation method and application of boron carbide-based ceramic modified by magnesium-aluminum hydrotalcite |
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| CN115108835A (en) * | 2021-03-19 | 2022-09-27 | 广东金鑫得新材料有限公司 | Method for manufacturing rapid high-densification boron carbide plate |
| CN113666750A (en) * | 2021-08-16 | 2021-11-19 | 中硼科技(威海)有限公司 | Light high-performance boron carbide-based bulletproof ceramic and preparation method thereof |
| CN115448723A (en) * | 2022-07-11 | 2022-12-09 | 中晶城康资源再生利用技术有限公司 | Preparation method and application of boron carbide-based ceramic modified by magnesium-aluminum hydrotalcite |
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Application publication date: 20200417 |