CN110371951B - Boron carbide coated carbon nanotube, and preparation method and application thereof - Google Patents
Boron carbide coated carbon nanotube, and preparation method and application thereof Download PDFInfo
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Abstract
A boron carbide coated carbon nanotube, a preparation method and an application thereof belong to the technical field of functional materials. The preparation method of the boron carbide coated carbon nano tube comprises the following steps: s1, preparing a solution A of boric acid and trihydroxypropane; s2, preparing carbon nano tube slurry B; s3, adding the carbon nanotube slurry B into the solution A, carrying out ultrasonic treatment, stirring and heating in water bath to obtain a paste C in which the carbon nanotube, boric acid and trihydroxypropane are uniformly mixed; s4, placing the paste C in an inert gas atmosphere, heating to dehydrate boric acid and carbonize trihydroxypropane to obtain boron oxide/amorphous carbon-coated carbon nanotube powder; s5, loosely packing the boron oxide/amorphous carbon coated carbon nano tube powder in a high-pressure reaction kettle, vacuumizing, introducing inert gas, heating to 1400-1500 ℃, preserving heat for 1-5 h, and naturally cooling to obtain the boron carbide coated carbon nano tube powder. According to the invention, the boron carbide coating layer is synthesized on the surface of the carbon nano tube, so that the interface bonding capability of the carbon nano tube and the aluminum alloy material is improved.
Description
Technical Field
The invention relates to a technology in the field of functional materials, in particular to a boron carbide coated carbon nanotube, a preparation method and an application thereof.
Background
The aluminum matrix composite has the advantages of low density, corrosion resistance, good processing performance and the like, and is very suitable for being applied to the aerospace and automobile manufacturing industries. However, with the development of the above industries, higher requirements are put on the specific strength, specific stiffness, wear resistance, heat resistance, fatigue resistance and other properties of the materials, and the common aluminum matrix composite materials are difficult to meet the requirements.
The aluminum alloy doped carbon nanotube can improve the performance of the aluminum matrix composite material, and has certain application in aerospace and automobile manufacturing industries. However, carbon nanotubes are difficult to disperse, have poor interfacial bonding ability with aluminum alloys, and are difficult to fully exert the advantages of composite materials.
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 the boron carbide coated carbon nano tube, the preparation method and the application thereof.
The invention relates to a preparation method of a boron carbide coated carbon nanotube, which comprises the following steps:
s1, mixing and stirring boric acid and trihydroxy propane uniformly, heating in a water bath, and carrying out ultrasonic treatment to completely dissolve boric acid in trihydroxy propane to obtain a transparent solution A;
s2, soaking the carbon nano tube in an ethanol solution, and then carrying out ultrasonic treatment to obtain carbon nano tube slurry B;
s3, adding the carbon nanotube slurry B prepared in the step S2 into the transparent solution A prepared in the step S1, uniformly mixing, performing ultrasonic treatment, and heating in a water bath while stirring to evaporate ethanol to obtain a paste C in which the carbon nanotube, the boric acid and the trihydroxypropane are uniformly mixed;
s4, placing the paste C prepared in the step S3 in an inert gas atmosphere, heating to 400-600 ℃ at a heating rate of 5-10 ℃/min, dehydrating boric acid, carbonizing trihydroxypropane, preserving heat for 2-3 hours, and cooling to obtain boron oxide/amorphous carbon coated carbon nanotube powder;
s5, loosely packing the boron oxide/amorphous carbon-coated carbon nanotube powder prepared in the step S4 in a high-pressure reaction kettle to fill the whole kettle cavity; vacuumizing the high-pressure reaction kettle to 0.1-100 Pa, and introducing inert gas to increase the pressure in the kettle to 1-2 atm; and then sealing the high-pressure reaction kettle, heating to 1400-1500 ℃ at the heating rate of 10-20 ℃/min, preserving the heat for 1-5 h, and naturally cooling to obtain the boron carbide coated carbon nanotube powder.
Preferably, in the step S1, the molar ratio of the boric acid to the trihydroxypropane is (1.7-2.4): 1;
preferably, in the step S1, the water bath temperature is 75-95 ℃; the ultrasonic treatment conditions were: the working frequency is 20kHz, the ultrasonic power is 1000-1800W, and the ultrasonic time is 5-10 min.
Preferably, in step S2, the carbon nanotubes are at least one of single-walled carbon nanotubes and multi-walled carbon nanotubes, and have a diameter of 10 to 200nm and a length of 5 to 20 μm.
Preferably, in step S2, the ultrasonic processing conditions are: the working frequency is 20kHz, the ultrasonic power is 800-1000W, the single ultrasonic time is 1-5 min, and the ultrasonic is performed again at an interval of 2min, wherein the total time is 5-10 times.
Preferably, in step S3, the ultrasonic processing conditions are: the working frequency is 20kHz, the ultrasonic power is 1000-1800W, and the ultrasonic time is 1-2 min.
Preferably, in the step S3, the stirring speed is 300-500 r/min, and the water bath temperature is 75-95 ℃.
Preferably, in step S5, the bulk density is 0.1 to 0.3g/cm based on the carbon nanotubes3。
The invention relates to a boron carbide coated carbon nanotube which is prepared by adopting the method, wherein the thickness of the boron carbide coating layer is 5-20 nm.
The invention relates to an application of a boron carbide coated carbon nano tube, which is used for preparing an aluminum-based composite material by using the boron carbide coated carbon nano tube as a dual-phase reinforcing toughening agent.
Technical effects
Compared with the prior art, the invention has the following technical effects:
1) the boron carbide coated carbon nano tube is prepared by adopting a chemical process, and on one hand, a large amount of carbon elements (7C + 2B) are needed for converting boron oxide into boron carbide2O3→6CO↑+B4C) The content of amorphous carbon provided by trihydroxy propane carbonization in the preparation process is limited, the surface of the carbon nano tube needs to participate in reaction simultaneously to make up for the defect, the firmness of combination of boron carbide and the carbon nano tube is ensured, and on the other hand, the wettability of the interface of boron carbide and aluminum alloy is good, so that the affinity of the carbon nano tube and an aluminum alloy matrix can be greatly improved, the rejection of an aluminum crystal boundary to the carbon nano tube is effectively avoided, and the mechanical property and the toughness of the aluminum-based composite material are improved to the maximum extent;
2) the introduction of boron carbide ensures that the reinforced aluminum-based composite material not only can keep the characteristics of light weight, good toughness and low cost of the aluminum alloy material, but also has the advantages of high specific strength, high specific rigidity, high elastic modulus, excellent wear resistance, low density, controllable expansion coefficient and the like.
Drawings
FIG. 1 is an SEM photograph of a boron carbide coated carbon nanotube composite prepared in example 1;
fig. 2 is a large-magnification SEM photograph of the boron carbide-coated carbon nanotube composite material prepared in example 1.
Detailed Description
The invention is described in detail below with reference to the drawings and the detailed description.
The embodiment of the invention relates to a preparation method of a boron carbide coated carbon nano tube, which comprises the following steps:
s1, placing boric acid in a beaker, adding trihydroxypropane into the boric acid and trihydroxypropane according to the molar ratio of the boric acid to the trihydroxypropane (1.7-2.4): 1, mixing and stirring uniformly, heating in a water bath, and carrying out ultrasonic treatment to completely dissolve the boric acid in the trihydroxypropane to obtain a transparent solution A;
s2, placing the carbon nano tube into another beaker, dropwise adding an ethanol solution into the beaker, and carrying out ultrasonic treatment after complete infiltration to obtain carbon nano tube slurry B;
s3, adding the carbon nanotube slurry B prepared in the step S2 into the transparent solution A prepared in the step S1, uniformly mixing, performing ultrasonic treatment, and heating in a water bath while stirring to evaporate ethanol to obtain a paste C in which the carbon nanotube, the boric acid and the trihydroxypropane are uniformly mixed;
s4, transferring the paste C prepared in the step S3 into a crucible, placing the crucible in a tube furnace in an inert gas atmosphere, heating to 400-600 ℃ at a heating rate of 5-10 ℃/min to dehydrate boric acid and carbonize trihydroxypropane, preserving heat for 2-3 hours, and cooling along with the furnace to obtain boron oxide/amorphous carbon coated carbon nanotube powder;
s5, loosely packing the boron oxide/amorphous carbon-coated carbon nanotube powder prepared in the step S4 in a high-pressure reaction kettle, wherein the loose packing density is 0.1-0.3 g/cm3Filling the whole kettle cavity; vacuumizing the high-pressure reaction kettle to 0.1-100 Pa, and introducing inert gas to increase the pressure in the kettle to 1-2 atm; and then sealing the high-pressure reaction kettle, heating to 1400-1500 ℃ at a heating rate of 10-20 ℃/min, preserving heat for 1-5 h, and naturally cooling to obtain the boron carbide coated carbon nanotube powder, wherein the thickness of the boron carbide coating layer is 5-20 nm.
In step S1, the water bath temperature is 75-95 ℃; the ultrasonic treatment conditions were: the working frequency is 20kHz, the ultrasonic power is 1000-1800W, and the ultrasonic time is 5-10 min.
In step S2, the carbon nanotube is at least one of a single-walled carbon nanotube and a multi-walled carbon nanotube, the diameter is 10-200 nm, and the length is 5-20 μm; the ultrasonic treatment conditions were: the working frequency is 20kHz, the ultrasonic power is 800-1000W, the single ultrasonic time is 1-5 min, and the ultrasonic is performed again at an interval of 2min, wherein the total time is 5-10 times.
In step S3, the sonication conditions are: the working frequency is 20kHz, the ultrasonic power is 1000-1800W, and the ultrasonic time is 1-2 min; the stirring speed is 300-500 r/min, and the water bath temperature is 75-95 ℃.
Example 1
The embodiment relates to a preparation method of a boron carbide coated carbon nanotube, which comprises the following steps:
s1, placing 30g of boric acid in a beaker, adding 20mL of trihydroxypropane into the beaker, uniformly stirring the boric acid by using a glass rod, heating the boric acid in a water bath to 75 ℃, and carrying out ultrasonic treatment on the boric acid with the working frequency of 20kHz, the ultrasonic power of 1000W and the ultrasonic time of 10min to obtain a solution A;
s2, placing 22g of carbon nanotubes in another beaker, and dropwise adding an ethanol solution into the beaker; after the carbon nano tube is completely soaked, carrying out ultrasonic treatment on the carbon nano tube, wherein the working frequency is 20kHz, the ultrasonic power is 800W, the single ultrasonic time is 1min, the ultrasonic treatment is carried out again at the interval of 2min, and the total number of the ultrasonic treatment is 5 times, so that carbon nano tube slurry B is obtained;
s3, adding the carbon nanotube slurry B into the solution A, continuing to perform ultrasonic treatment for 1min at the working frequency of 20kHz and the ultrasonic power of 1000W, and then heating in a water bath to evaporate ethanol while stirring at the speed of 300r/min at 85 ℃ to obtain a paste C in which the carbon nanotube, the boric acid and the trihydroxypropane are uniformly mixed;
s4, transferring the paste C into a crucible and placing the crucible into a tube furnace; heating to 500 ℃ at a heating rate of 5 ℃/min under the atmosphere of nitrogen gas, preserving heat for 3 hours, and cooling along with the furnace to obtain boron oxide/amorphous carbon coated carbon nanotube powder;
s5, transferring the powder prepared in the step S4 into a high-pressure reaction kettle, wherein the apparent density is 0.1g/cm3Filling the whole kettle cavity, vacuumizing to 100Pa, introducing nitrogen into the kettle until the pressure in the kettle reaches 1atm, sealing the reaction kettle, heating to 1400 ℃ at the heating rate of 20 ℃/min, preserving the temperature for 1h, and naturally cooling to obtain the boron carbide coated carbon nanotube powder.
The prepared boron carbide-coated carbon nanotube composite was analyzed by a scanning electron microscope to obtain SEM photographs of different magnifications, as shown in fig. 1 and 2. It can be seen from the figure that boron carbide is uniformly coated on the surface of the carbon nanotube.
Example 2
S1, placing 40g of boric acid in a beaker, adding 25mL of trihydroxypropane into the beaker, uniformly stirring the boric acid by using a glass rod, heating the boric acid in a water bath to 85 ℃, and carrying out ultrasonic treatment on the boric acid with the working frequency of 20kHz, the ultrasonic power of 1400W and the ultrasonic time of about 5min to obtain a transparent solution A;
s2, placing 22g of carbon nanotubes in another beaker, and dropwise adding an ethanol solution into the beaker; after the carbon nano tube is completely soaked, carrying out ultrasonic treatment on the carbon nano tube, wherein the working frequency is 20kHz, the ultrasonic power is 800W, the single ultrasonic time is 2min, the ultrasonic treatment is carried out again at the interval of 2min, and the total number of the ultrasonic treatment is 10 times to obtain carbon nano tube slurry B;
s3, adding the carbon nanotube slurry B into the solution A, continuing to perform ultrasonic treatment for 2min at the working frequency of 20kHz and the ultrasonic power of 1000W, and then heating in a water bath to evaporate ethanol while stirring at the speed of 400r/min at the temperature of 75 ℃ to obtain a paste C in which the carbon nanotube, the boric acid and the trihydroxypropane are uniformly mixed;
s4, transferring the paste C into a crucible and placing the crucible into a tube furnace; heating to 600 ℃ at a heating rate of 10 ℃/min under the atmosphere of argon gas, preserving heat for 3 hours, and cooling along with a furnace to obtain boron oxide/amorphous carbon coated carbon nanotube powder;
s5, transferring the obtained powder into a high-pressure reaction kettle, wherein the apparent density is 0.15g/cm3Filling the whole kettle cavity, vacuumizing to 10Pa, and introducing argon into the kettle until the pressure in the kettle reaches 1 atm; and then sealing the reaction kettle, heating the reaction kettle to 1450 ℃ at the heating rate of 10 ℃/min, preserving the heat for 3h, and naturally cooling to obtain the boron carbide coated carbon nano tube powder.
Example 3
S1, putting 60g of boric acid in a beaker, adding 40mL of trihydroxypropane into the beaker, uniformly stirring the boric acid by using a glass rod, heating the boric acid in a water bath to 90 ℃, and carrying out ultrasonic treatment on the boric acid with the working frequency of 20kHz, the ultrasonic power of 1800W and the ultrasonic time of about 10min to obtain a transparent solution A;
s2, placing 22g of carbon nanotubes in another beaker, and dropwise adding an ethanol solution into the beaker; after the carbon nano tube is completely soaked, carrying out ultrasonic treatment on the carbon nano tube, wherein the working frequency is 20kHz, the ultrasonic power is 1000W, the single ultrasonic time is 5min, the ultrasonic treatment is carried out again at the interval of 2min, and the total number of times is 10 to obtain carbon nano tube slurry B;
s3, adding the carbon nanotube slurry B into the solution A, continuing to perform ultrasonic treatment for 2min at the working frequency of 20kHz and the ultrasonic power of 1800W, and then heating in a water bath to evaporate ethanol while stirring at the speed of 500r/min at 95 ℃ to obtain a paste C in which the carbon nanotube, the boric acid and the trihydroxypropane are uniformly mixed;
s4, transferring the paste C into a crucible and placing the crucible into a tube furnace; heating to 600 ℃ at a heating rate of 7 ℃/min under the atmosphere of argon gas, preserving heat for 3 hours, and cooling along with a furnace to obtain boron oxide/amorphous carbon coated carbon nanotube powder;
s5, transferring the obtained powder into a high-pressure reaction kettle, filling the whole kettle cavity, vacuumizing to 100Pa, and introducing argon into the kettle until the pressure in the kettle reaches 2 atm; and then sealing the reaction kettle, heating the reaction kettle to 1400 ℃ at the heating rate of 10 ℃/min, preserving the heat for 3h, and naturally cooling to obtain the boron carbide coated carbon nano tube powder.
The boron carbide coated carbon nanotube powder prepared in the examples 1, 2 and 3 and the 7075 aluminum alloy powder are respectively prepared into the carbon nanotube/boron carbide reinforced and toughened aluminum-based composite material according to the weight ratio of 10: 90. The preparation method comprises the following steps: ball-milling the raw materials on a light ball mill for 12 hours at the speed of 150r/min to obtain composite powder, and carrying out surface activation on the composite powder in a plasma activation sintering furnace, wherein the surface activation time is 30s, the activation voltage is 20kV, the activation current is 100A, and the vacuum degree is less than or equal to 10 Pa; and (3) quickly raising the temperature after surface activation, wherein the temperature raising rate is 100 ℃/min, the pressure is 20MPa, the temperature is raised to 530 ℃, the temperature is kept for 5min, and a sample obtained after sintering is subjected to heat treatment to obtain the carbon nano tube/boron carbide reinforced and toughened aluminum-based composite material. The results of the product part performance tests are shown in table 1.
Table 1 product part performance test results
| Item | Example 1 | Example 2 | Example 3 | 7075 aluminium alloy |
| Density (g/cm)3) | 2.713 | 2.722 | 2.734 | 2.810 |
| Hardness Value (HV) | 162 | 176 | 183 | 150 |
| Tensile strength (MPa) | 765 | 701 | 637 | 524 |
| Yield strength (MPa) | 602 | 588 | 569 | 455 |
As can be seen from Table 1, the boron carbide coated carbon nanotube powder of different embodiments has better reinforcing and toughening effects under the same addition amount, and the test performance of each product at room temperature is obviously improved compared with 7075 aluminum alloy.
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 (8)
1. A preparation method of a boron carbide coated carbon nanotube is characterized by comprising the following steps:
s1, mixing and stirring boric acid and trihydroxy propane uniformly, heating in a water bath, and carrying out ultrasonic treatment to completely dissolve boric acid in trihydroxy propane to obtain a transparent solution A;
s2, soaking the carbon nano tube in an ethanol solution, and then carrying out ultrasonic treatment to obtain carbon nano tube slurry B;
s3, adding the carbon nanotube slurry B prepared in the step S2 into the transparent solution A prepared in the step S1, uniformly mixing, performing ultrasonic treatment, and heating in a water bath while stirring to evaporate ethanol to obtain a paste C in which the carbon nanotube, the boric acid and the trihydroxypropane are uniformly mixed;
s4, placing the paste C prepared in the step S3 in an inert gas atmosphere, heating to 400-600 ℃ at a heating rate of 5-10 ℃/min, dehydrating boric acid, carbonizing trihydroxypropane, preserving heat for 2-3 hours, and cooling to obtain boron oxide/amorphous carbon coated carbon nanotube powder;
s5, loosely packing the boron oxide/amorphous carbon-coated carbon nanotube powder prepared in the step S4 in a high-pressure reaction kettle to fill the whole kettle cavity; vacuumizing the high-pressure reaction kettle to 0.1-100 Pa, and introducing inert gas to increase the pressure in the kettle to 1-2 atm; and then sealing the high-pressure reaction kettle, heating to 1400-1500 ℃ at the heating rate of 10-20 ℃/min, preserving the heat for 1-5 h, and naturally cooling to obtain the boron carbide coated carbon nanotube powder.
2. The method for producing a boron carbide-coated carbon nanotube according to claim 1, wherein in step S1, the molar ratio of boric acid to trimethylolpropane is (1.7-2.4): 1.
3. The method for preparing boron carbide-coated carbon nanotubes according to claim 1, wherein in step S1, the water bath temperature is 75 to 95 ℃; the ultrasonic treatment conditions were: the working frequency is 20kHz, the ultrasonic power is 1000-1800W, and the ultrasonic time is 5-10 min.
4. The method of claim 1, wherein in step S2, the carbon nanotubes are single-walled carbon nanotubes or multi-walled carbon nanotubes, each having a diameter of 10 to 200nm and a length of 5 to 20 μm.
5. The method for preparing boron carbide-coated carbon nanotubes as claimed in claim 1, wherein in step S2, the ultrasonic treatment conditions are: the working frequency is 20kHz, the ultrasonic power is 800-1000W, the single ultrasonic time is 1-5 min, and the ultrasonic is performed again at an interval of 2min, wherein the total time is 5-10 times.
6. The method for preparing boron carbide-coated carbon nanotubes as claimed in claim 1, wherein in step S3, the ultrasonic treatment conditions are: the working frequency is 20kHz, the ultrasonic power is 1000-1800W, and the ultrasonic time is 1-2 min.
7. The method for preparing boron carbide-coated carbon nanotubes as claimed in claim 1, wherein in step S3, the stirring speed is 300 to 500r/min and the water bath temperature is 75 to 95 ℃.
8. The method for producing boron carbide-coated carbon nanotubes as claimed in claim 1, wherein in step S5, the bulk density is 0.1 to 0.3g/cm based on the carbon nanotubes3。
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