CN115172578A - Carbon nitride/carbon nanotube composite film and preparation method and application thereof - Google Patents

Carbon nitride/carbon nanotube composite film and preparation method and application thereof Download PDF

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CN115172578A
CN115172578A CN202210774797.5A CN202210774797A CN115172578A CN 115172578 A CN115172578 A CN 115172578A CN 202210774797 A CN202210774797 A CN 202210774797A CN 115172578 A CN115172578 A CN 115172578A
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carbon
carbon nitride
composite film
nitride
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张云飞
李怡
刘辉
张桥
杜飞鹏
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Wuhan Institute of Technology
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    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
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    • H10N10/00—Thermoelectric devices comprising a junction of dissimilar materials, i.e. devices exhibiting Seebeck or Peltier effects
    • H10N10/80—Constructional details
    • H10N10/85—Thermoelectric active materials
    • H10N10/851—Thermoelectric active materials comprising inorganic compositions
    • H10N10/855—Thermoelectric active materials comprising inorganic compositions comprising compounds containing boron, carbon, oxygen or nitrogen
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B21/00—Nitrogen; Compounds thereof
    • C01B21/06—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron
    • C01B21/0605—Binary compounds of nitrogen with carbon
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00—Carbon; Compounds thereof
    • C01B32/15—Nano-sized carbon materials
    • C01B32/158—Carbon nanotubes
    • C01B32/168—After-treatment
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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    • C01P2004/01—Particle morphology depicted by an image
    • C01P2004/03—Particle morphology depicted by an image obtained by SEM
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
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    • C01P2004/00—Particle morphology
    • C01P2004/60—Particles characterised by their size
    • C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer

Abstract

The invention provides a carbon nitride/carbon nano tube composite film and a preparation method and application thereof. The carbon nitride/carbon nanotube composite film provided by the invention has the advantages of high conductivity, high Seebeck coefficient, high power factor and the like, has good flexibility, is easy to bend, and has good application prospect in the field of flexible wearable thermoelectric equipment.

Description

Carbon nitride/carbon nanotube composite film and preparation method and application thereof
Technical Field
The invention belongs to the technical field of composite materials, and relates to a carbon nitride/carbon nano tube composite film, and a preparation method and application thereof.
Background
Thermoelectric materials, also known as thermoelectric materials, are semiconductor functional materials that utilize the movement of carriers within a solid to achieve interconversion between thermal energy and electrical energy, have the advantages of small size, light weight, quiet operation, no need of conversion media and mechanical moving parts, etc., and are widely spotlighted as a novel energy material.
Thermoelectric conversion efficiency ZT = S of the material 2 Sigma T/kappa, wherein S, sigma, T and kappa are Seebeck coefficient, electric conductivity, absolute temperature and thermal conductivity coefficient respectively. The larger the ZT value, the higher the conversion efficiency. Therefore, an excellent thermoelectric material is required to have a large Seebeck coefficient, high electrical conductivity, and low thermal conductivity.
Inorganic materials have high Seebeck coefficient and conductivity, so that the inorganic materials are rapidly developed in the field of thermoelectric materials, and part of the inorganic materials are widely applied in the fields of thermocouple temperature control, semiconductor refrigeration and the like. Carbon nitride is a non-metallic semiconductor with tunable optoelectronic properties, high chemical stability, wide energy gap (forbidden band), low cost and easy synthesis, and is commonly used as a photocatalyst, a sensor and a photovoltaic material. However, the bulk carbon nitride has low quantum yield and high recombination rate of photo-generated electrons and holes, which limits practical application.
Disclosure of Invention
The composite film has good flexibility, excellent electrochemical performance and high power factor, and has good application prospect in the field of flexible wearable thermoelectric devices when used as a thermoelectric material.
In order to solve the technical problems, the technical scheme provided by the invention is as follows:
the carbon nitride/carbon nanotube composite film is obtained by compounding carbon nitride nanoparticles and carbon nanotubes.
According to the scheme, the carbon nitride nano particles are graphite phase carbon nitride, the particle size is 49-94 nm, the graphite phase carbon nitride structure is stable, and the carbon nitride nano particles have a layered structure similar to graphite.
According to the scheme, the preparation method of the carbon nitride nano-particles comprises the following steps: putting melamine into a ceramic crucible, taking nitrogen as a nitrogen source, heating to 500-600 ℃ at the speed of 2-4 ℃/min, and keeping the temperature for 2-6 h to obtain light yellow powder, and grinding the light yellow powder to obtain the carbon nitride nano-particles.
According to the scheme, the carbon nanotube is one or more of a single-walled carbon nanotube, a multi-walled carbon nanotube and a double-walled carbon nanotube, and is preferably a single-walled carbon nanotube.
According to the scheme, the mass fraction of carbon nitride in the carbon nitride/carbon nano tube composite film is 2.5-40%.
According to the scheme, the thickness of the carbon nitride/carbon nano tube composite film is 0.0008-0.0012 cm.
The invention also comprises a preparation method of the carbon nitride/carbon nano tube composite film, which comprises the following specific steps:
1) Ultrasonically dispersing a carbon nano tube in an organic solvent to obtain a carbon nano tube dispersion liquid;
2) Ultrasonically dispersing carbon nitride nano particles in an organic solvent to obtain carbon nitride dispersion liquid;
3) Mixing the carbon nano tube dispersion liquid obtained in the step 1) with the carbon nitride dispersion liquid obtained in the step 2), performing ultrasonic dispersion uniformly, then fully shearing by using a handheld homogenizer, performing reduced pressure filtration and washing to obtain a filter membrane, and finally performing vacuum drying on the obtained filter membrane to obtain the carbon nitride/carbon nano tube composite film.
According to the scheme, the organic solvent in the step 1) is the same as the organic solvent in the step 2), and is selected from one of absolute ethyl alcohol, dimethyl sulfoxide and N, N-dimethylformamide.
According to the scheme, the concentration of the carbon nano tube dispersion liquid in the step 1) is 0.7-1 mg/mL.
According to the scheme, the concentration of the carbon nitride dispersion liquid in the step 2) is 0.02-0.7 mg/mL.
According to the scheme, the mass ratio of the carbon nano tubes in the carbon nano tube dispersion liquid in the step 3) to the carbon nitride in the carbon nitride dispersion liquid is 1.4-40: 1.
according to the scheme, the ultrasonic dispersion time in the step 3) is 25-35 min, and the power is 100-200W.
According to the scheme, the shearing time in the step 3) is 2-7 min, the shearing speed is 3000-5000 rpm, and the power is 180-200W.
According to the scheme, in the step 3), the vacuum drying temperature is 45-80 ℃, the vacuum drying time is 4-24 hours, and the vacuum degree is 0.09-0.1 MPa.
The invention also comprises the application of the carbon nitride/carbon nano tube composite film in thermoelectric materials.
The invention adopts a thermal polymerization method to prepare graphite-phase carbon nitride, and disperses the graphite-phase carbon nitride in an organic solvent by an ultrasonic method to carry out ultrasonic shearing compounding with the carbon nano tube, thereby effectively improving the conductivity while improving the Seebeck coefficient and obviously improving the power factor.
The invention has the beneficial effects that: 1. the carbon nitride/carbon nanotube composite film provided by the invention has the advantages of high conductivity, high Seebeck coefficient, high power factor and the like, has good flexibility, is easy to bend, and has good application prospect in the field of flexible wearable thermoelectric equipment;
2. the preparation method disclosed by the invention is simple in steps, low in cost, green and environment-friendly, and good in repeatability.
Drawings
FIG. 1 is a FESEM image of carbon nitride nanoparticles used in embodiments of the present invention;
fig. 2 is an FESEM view of the carbon nitride/carbon nanotube composite film prepared in example 1.
Detailed Description
In order to make the technical solutions of the present invention better understood, the present invention is further described in detail with reference to the following examples.
The preparation method of the carbon nitride nano-particles used in the embodiment of the invention comprises the following steps: putting 5g of melamine into a ceramic crucible, introducing nitrogen as a protective atmosphere, heating to 550 ℃ at the speed of 2.41 ℃/min, and preserving heat for 4 hours at 550 ℃, wherein the obtained light yellow powder is ground to obtain carbon nitride nanoparticles with the particle size of 49-94 nm, the carbon nitride has a layered structure similar to graphite, and an FESEM image of the carbon nitride is shown in figure 1.
Comparative example 1
The preparation method of the carbon nano tube film comprises the following steps: ultrasonically dispersing 10mg of single-walled carbon nanotubes (the diameter is 1-3 nm, the length-diameter ratio is 5000-15000) in 10mL of absolute ethyl alcohol, wherein the ultrasonic dispersion time is 30 minutes, dispersing for 2 minutes by using a handheld homogenizer, carrying out suction filtration on a product, washing a filter cake by using absolute ethyl alcohol, and then carrying out vacuum drying on the obtained filter cake for 24 hours at the temperature of 60 ℃, wherein the vacuum degree of an oven is 0.1MPa, so that a carbon nanotube film is obtained, and the thickness of the film is 0.0008cm.
Example 1
A carbon nitride-doped carbon nanotube composite film is specifically prepared by the following steps:
1) Adding 7.8mg of single-walled carbon nanotubes (the diameter is 1-3 nm, the length-diameter ratio is 5000-15000) into 10mL of absolute ethyl alcohol, and performing ultrasonic dispersion for 30min to obtain a carbon nanotube dispersion liquid;
2) Adding 0.2mg of carbon nitride nano particles into 10mL of absolute ethyl alcohol, and performing ultrasonic dispersion for 30min to obtain a carbon nitride dispersion liquid;
3) Mixing the carbon nano tube dispersion liquid obtained in the step 1) with the carbon nitride dispersion liquid obtained in the step 2), performing ultrasonic dispersion for 30min with the power of 100W, shearing for 2min by using a handheld homogenizer with the shearing rotation speed of 5000rpm and the shearing power of 180W, performing reduced pressure filtration, washing a filter cake by using absolute ethyl alcohol to obtain a filter membrane, and finally performing vacuum drying on the obtained filter membrane at the temperature of 60 ℃ for 24h, wherein the vacuum degree of an oven is 0.1MPa, so that a carbon nitride/carbon nano tube composite film is obtained, the thickness of the film is 0.0010cm, and the mass fraction of carbon nitride in the composite film is 2.5%.
As shown in fig. 2, which is an FESEM image of the film sample prepared in this embodiment, it can be seen that the tube bundles of the carbon nanotubes in the composite film prepared in this embodiment are smooth and uniform, and the graphite-phase carbon nitride is perfectly attached to the surface of the tube bundles of the carbon nanotubes to form a uniform and stable composite structure, which is uniform and stable, and is beneficial to forming a composite film with a smooth surface, thereby effectively improving the Seebeck coefficient of the composite film.
Example 2
A carbon nitride-doped carbon nanotube composite film is specifically prepared by the following steps:
1) Ultrasonically dispersing 9.8mg of single-walled carbon nanotubes in 10mL of absolute ethyl alcohol to obtain a carbon nanotube dispersion liquid;
2) Ultrasonically dispersing 0.8mg of carbon nitride nano particles in 10mL of absolute ethyl alcohol to obtain a carbon nitride dispersion liquid;
3) Mixing the carbon nano tube dispersion liquid obtained in the step 1) with the carbon nitride dispersion liquid obtained in the step 2), performing ultrasonic dispersion for 30min with the ultrasonic power of 100W, shearing for 2min by using a handheld homogenizer with the shearing power of 180W, performing reduced pressure filtration, washing a filter cake by using absolute ethyl alcohol to obtain a filter membrane, and finally performing vacuum drying on the obtained filter membrane at 60 ℃ for 24h, wherein the vacuum degree of an oven is 0.1MPa, so that a carbon nitride/carbon nano tube composite film is obtained, the thickness of the film is 0.0011 cm, and the mass fraction of carbon nitride in the composite film is 7.5%.
Example 3
A carbon nitride-doped carbon nanotube composite film is specifically prepared by the following steps:
1) Ultrasonically dispersing 10mg of single-walled carbon nanotubes in 10mL of absolute ethyl alcohol to obtain a carbon nanotube dispersion liquid;
2) Ultrasonically dispersing 1.11mg of carbon nitride nano particles into 10mL of absolute ethyl alcohol to obtain a carbon nitride dispersion liquid;
3) Mixing the carbon nano tube dispersion liquid obtained in the step 1) with the carbon nitride dispersion liquid obtained in the step 2), performing ultrasonic dispersion for 30min, wherein the ultrasonic power is 100W, shearing for 2min by using a handheld homogenizer, wherein the shearing power is 180W, performing reduced pressure filtration, washing a filter cake by using absolute ethyl alcohol to obtain a filter membrane, and finally performing vacuum drying on the obtained filter membrane at 60 ℃ for 24h, wherein the vacuum degree of an oven is 0.1MPa, so that a carbon nitride/carbon nano tube composite film is obtained, the thickness of the film is 0.0013 cm, and the mass fraction of carbon nitride in the composite film is 10%.
Example 4
A carbon nitride-doped carbon nanotube composite film is specifically prepared by the following steps:
1) Ultrasonically dispersing 10mg of single-walled carbon nanotubes in 10mL of absolute ethyl alcohol to obtain a carbon nanotube dispersion liquid;
2) Ultrasonically dispersing 2.5mg of carbon nitride nano particles into 10mL of absolute ethyl alcohol to obtain a carbon nitride dispersion liquid;
3) Mixing the carbon nano tube dispersion liquid obtained in the step 1) with the carbon nitride dispersion liquid obtained in the step 2), performing ultrasonic dispersion for 30min, shearing for 2min by using a handheld homogenizer with the shearing power of 180W, performing reduced pressure filtration, washing a filter cake by using absolute ethyl alcohol to obtain a filter membrane, and finally performing vacuum drying on the obtained filter membrane at 60 ℃ for 24h, wherein the vacuum degree of an oven is 0.1MPa, so that a carbon nitride/carbon nano tube composite film is obtained, the thickness of the film is 0.00135 cm, and the mass fraction of carbon nitride in the composite film is 20%.
Example 5
A carbon nitride-doped carbon nanotube composite film is specifically prepared by the following steps:
1) Ultrasonically dispersing 10mg of single-walled carbon nanotubes in 10mL of absolute ethyl alcohol to obtain a carbon nanotube dispersion liquid;
2) Ultrasonically dispersing 4.29mg of carbon nitride nano particles into 10mL of absolute ethyl alcohol to obtain a carbon nitride dispersion liquid;
3) Mixing the carbon nano tube dispersion liquid obtained in the step 1) with the carbon nitride dispersion liquid obtained in the step 2), ultrasonically dispersing for 30min with the ultrasonic power of 100W, then shearing for 2min by a homogenizer in a handheld manner with the shearing power of 180W, then filtering under reduced pressure, washing a filter cake by absolute ethyl alcohol to obtain a filter membrane, and finally drying the obtained filter membrane in vacuum at 60 ℃ for 24h, wherein the vacuum degree of an oven is 0.1MPa, so that a carbon nitride/carbon nano tube composite film is obtained, the thickness of the film is 0.0018mm, and the mass fraction of carbon nitride in the composite film is 30%.
Example 6
A carbon nitride-doped carbon nanotube composite film is specifically prepared by the following steps:
1) Ultrasonically dispersing 10mg of single-walled carbon nanotubes in 10mL of absolute ethyl alcohol to obtain a carbon nanotube dispersion liquid;
2) Ultrasonically dispersing 6.67mg of carbon nitride nano particles into 10mL of absolute ethyl alcohol to obtain a carbon nitride dispersion liquid;
3) Mixing the carbon nano tube dispersion liquid obtained in the step 1) with the carbon nitride dispersion liquid obtained in the step 2), performing ultrasonic dispersion for 30min, wherein the ultrasonic power is 100W, shearing for 2min by using a handheld homogenizer, wherein the shearing power is 180W, performing reduced pressure filtration, washing a filter cake by using absolute ethyl alcohol to obtain a filter membrane, and finally performing vacuum drying on the obtained filter membrane at 60 ℃ for 24h, wherein the vacuum degree of an oven is 0.1MPa, so that a carbon nitride/carbon nano tube composite film is obtained, the thickness of the film is 0.0017 cm, and the mass fraction of carbon nitride in the composite film is 40%.
Example 7
A carbon nitride-doped carbon nanotube composite film is specifically prepared by the following steps:
1) Ultrasonically dispersing 7.8mg of single-walled carbon nanotubes in 10mL of dimethyl sulfoxide to obtain a carbon nanotube dispersion liquid;
2) Ultrasonically dispersing 0.2mg of carbon nitride nano particles in 10mL of dimethyl sulfoxide to obtain a carbon nitride dispersion liquid;
3) Mixing the carbon nano tube dispersion liquid obtained in the step 1) with the carbon nitride dispersion liquid obtained in the step 2), performing ultrasonic dispersion for 30min, wherein the ultrasonic power is 100W, shearing for 2min by using a handheld homogenizer, wherein the shearing power is 180W, performing reduced pressure filtration, washing a filter cake by using dimethyl sulfoxide to obtain a filter membrane, and finally performing vacuum drying on the obtained filter membrane at 60 ℃ for 24h, wherein the vacuum degree of an oven is 0.1MPa, so that a carbon nitride/carbon nano tube composite film is obtained, the thickness of the film is 0.0015 cm, and the mass fraction of carbon nitride in the composite film is 2.5%.
Thermoelectric performance parameters of the film samples prepared in comparative example 1 and examples 1-7 are shown in Table 1.
TABLE 1
Figure BDA0003726429320000061
As can be seen from Table 1, the conductivities of examples 1 to 6 showed a tendency of increasing and decreasing compared with comparative example 1, and the conductivity reached the maximum at example 1 and was 70256.5S/m; compared with the comparative example 1, the Seebeck coefficients of the examples 1 to 6 are basically improved; the power factor reached a maximum at example 1 of 163.0. Mu. W.m -1 ·K -2 。

Claims (10)

1. The carbon nitride/carbon nanotube composite film is characterized by being obtained by compounding carbon nitride nanoparticles and carbon nanotubes.
2. The carbon nitride/carbon nanotube composite film according to claim 1, wherein the carbon nitride nanoparticles are graphite phase carbon nitride and have a particle diameter of 49 to 94nm; the carbon nano tube is one or more of a single-wall carbon nano tube, a multi-wall carbon nano tube and a double-wall carbon nano tube.
3. The carbon nitride/carbon nanotube composite film according to claim 1, wherein the mass fraction of carbon nitride in the carbon nitride/carbon nanotube composite film is 2.5 to 40%.
4. A method for preparing the carbon nitride/carbon nanotube composite film according to any one of claims 1 to 3, which comprises the following steps:
1) Ultrasonically dispersing a carbon nano tube in an organic solvent to obtain a carbon nano tube dispersion liquid;
2) Ultrasonically dispersing carbon nitride nano particles in an organic solvent to obtain carbon nitride dispersion liquid;
3) Mixing the carbon nano tube dispersion liquid obtained in the step 1) with the carbon nitride dispersion liquid obtained in the step 2), ultrasonically dispersing uniformly, fully shearing by using a handheld homogenizer, filtering under reduced pressure, washing to obtain a filter membrane, and finally drying the obtained filter membrane in vacuum to obtain the carbon nitride/carbon nano tube composite film.
5. The method for preparing a carbon nitride/carbon nanotube composite film according to claim 4, wherein the organic solvent in step 1) is the same as the organic solvent in step 2), and is selected from one of absolute ethyl alcohol, dimethyl sulfoxide, and N, N-dimethylformamide.
6. The method for preparing a carbon nitride/carbon nanotube composite film according to claim 4, wherein the concentration of the carbon nanotube dispersion in the step 1) is 0.7 to 1mg/mL.
7. The method for preparing a carbon nitride/carbon nanotube composite film according to claim 4, wherein the concentration of the carbon nitride dispersion in the step 2) is 0.02 to 0.7mg/mL.
8. The method for preparing a carbon nitride/carbon nanotube composite film according to claim 4, wherein the mass ratio of the carbon nanotubes in the carbon nanotube dispersion liquid to the carbon nitride in the carbon nitride dispersion liquid in the step 3) is 1.4 to 40:1; step 3), the ultrasonic dispersion time is 25-35 min, and the power is 100-200W; in the step 3), the shearing time is 2-7 min, the shearing rotating speed is 3000-5000 rpm, and the power is 180-200W.
9. The method for preparing a carbon nitride/carbon nanotube composite film according to claim 4, wherein the vacuum drying temperature in step 3) is 45 to 80 ℃, the vacuum drying time is 4 to 24 hours, and the vacuum degree is 0.09 to 0.1MPa.
10. Use of the carbon nitride/carbon nanotube composite film according to any one of claims 1 to 3 for thermoelectric materials.
CN202210774797.5A 2022-07-01 2022-07-01 Carbon nitride/carbon nanotube composite film and preparation method and application thereof Pending CN115172578A (en)

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