CN115472330A - Carbon-based slurry, carbon film and preparation method thereof - Google Patents
Carbon-based slurry, carbon film and preparation method thereof Download PDFInfo
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- XROWMBWRMNHXMF-UHFFFAOYSA-J titanium tetrafluoride Chemical compound [F-].[F-].[F-].[F-].[Ti+4] XROWMBWRMNHXMF-UHFFFAOYSA-J 0.000 description 1
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/20—Conductive material dispersed in non-conductive organic material
- H01B1/24—Conductive material dispersed in non-conductive organic material the conductive material comprising carbon-silicon compounds, carbon or silicon
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B13/00—Apparatus or processes specially adapted for manufacturing conductors or cables
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
- H05B3/00—Ohmic-resistance heating
- H05B3/10—Heating elements characterised by the composition or nature of the materials or by the arrangement of the conductor
- H05B3/12—Heating elements characterised by the composition or nature of the materials or by the arrangement of the conductor characterised by the composition or nature of the conductive material
- H05B3/14—Heating elements characterised by the composition or nature of the materials or by the arrangement of the conductor characterised by the composition or nature of the conductive material the material being non-metallic
- H05B3/145—Carbon only, e.g. carbon black, graphite
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- Chemical & Material Sciences (AREA)
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- Spectroscopy & Molecular Physics (AREA)
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- Carbon And Carbon Compounds (AREA)
Abstract
The application relates to a carbon-based slurry, a carbon film and a preparation method thereof, wherein the carbon-based slurry comprises the following components in parts by weight: 10-40 parts of nano carbon material, 200-400 parts of binder and 5-20 parts of fluorinated titanium dioxide. The carbon-based slurry provided by the application has good antibacterial performance by adding the fluorinated titanium dioxide, and meanwhile, the titanium dioxide subjected to fluorination treatment effectively improves the hydrophobicity of the carbon film; the preparation method of the carbon film adopts a mode of firstly freezing and then heating, so that a plurality of micron-nanometer protrusions are formed on the surface of the carbon film, the size of the protrusions is far smaller than the diameter of a water drop at the millimeter level, the water drop cannot infiltrate the surface of the film, an ultra-hydrophobic layer is formed, the water contact angle of the ultra-hydrophobic layer is 165-175 degrees, the rolling angle is 5-15 degrees, and the nano carbon film material which can be electrically heated and has self-cleaning and antibacterial effects is provided.
Description
Technical Field
The application relates to the technical field of novel electric heating, in particular to carbon-based slurry, a carbon film and a preparation method thereof.
Background
The nano carbon film is manufactured by using nano carbon slurry as a heating base material, adopting a power control and coating process, utilizing a high-solid carbon-containing slurry dispersion technology, a high-adhesive-force carbon material compounding technology and a zero-leakage electric heating film design and preparation technology, and ensuring that the product has good stability in resistance and power. Under the action of an electric field, carbon molecular groups in the heating body generate Brownian motion, violent friction and impact occur among carbon molecules, the generated heat energy is transmitted outwards in the form of far infrared radiation and convection, and the heating mode is uniform, so that the nano carbon film is widely applied to heating equipment and heating equipment as an electrothermal film in the fields of physiotherapy instruments, automobile seats, steering wheels and the like.
In the related technology, the nano-carbon electrothermal film is mainly obtained by mixing, coating and drying a carbon-based material and an organic binder, and the nano-carbon electrothermal film has the problem of poor hydrophobic property in the actual use process, so that the service life of the product is very easy to shorten, and the application range of the product is limited. In addition, in the long-term use process, bacteria, stains and the like in the air are easy to deposit on the surface of the electrothermal film, and the heating performance and the cleanliness of the electrothermal film are affected.
Disclosure of Invention
The embodiment of the application provides a carbon-based slurry, a carbon film and a preparation method thereof, and aims to solve the problems of low antibacterial property and hydrophobic property of a nano-carbon electrothermal film in the related technology.
In a first aspect, the present application provides a carbon-based slurry comprising the following components by weight:
10-40 parts of nano carbon material, 200-400 parts of binder and 5-20 parts of fluorinated titanium dioxide.
In some embodiments, the fluorinated titanium dioxide is a rod-like crystal having a diameter of 100 to 300nm and a length of 1 to 3 μm.
In some embodiments, the nanocarbon material has a particle size of less than 100nm.
In some embodiments, the nanocarbon material comprises at least one of carbon nanotubes, carbon nanofibers, nanocarbon spheres, graphene, expanded graphite.
In some embodiments, the binder comprises at least one of N-methyl pyrrolidone, polyvinylidene fluoride, carboxymethyl cellulose, styrene butadiene rubber, polytetrafluoroethylene, polyacrylic acid.
In some embodiments, the binder consists of N-methyl pyrrolidone and polyvinylidene fluoride, and the mass ratio of the N-methyl pyrrolidone to the polyvinylidene fluoride is (12-6): 1.
in a second aspect, the present application provides a method for preparing a carbon thin film, comprising the steps of:
coating the carbon-based slurry on a substrate and standing;
freezing the base material coated with the carbon-based slurry at-30 to-18 ℃ for 3 to 8 hours;
then heat treatment is carried out for 5 to 8 hours at the temperature of between 100 and 150 ℃ to obtain the carbon film.
In some embodiments, the standing treatment time is 1 to 3 hours.
In a third aspect, the present application provides a carbon thin film prepared by the preparation method as described above;
the carbon film comprises a carbon film substrate and a super-hydrophobic layer coated on the surface of the carbon film substrate, wherein the super-hydrophobic layer is formed by fluorinated titanium dioxide which is arranged at intervals and embedded in the carbon film substrate, and the fluorinated titanium dioxide forms bulges on the surface of the carbon film substrate.
In some embodiments, the protrusions have a height of 100 to 300 μm, a diameter of 50 to 200 μm, and a pitch between adjacent protrusions of 300 to 500 μm.
The beneficial effect that technical scheme that this application provided brought includes: according to the carbon-based slurry provided by the application, the fluorinated titanium dioxide is added, so that the carbon-based slurry has good antibacterial performance, and meanwhile, the titanium dioxide subjected to fluorination effectively improves the hydrophobicity of a carbon film;
according to the preparation method of the carbon film, after the substrate is coated with the carbon-based slurry, the substrate is firstly subjected to freezing treatment for 3-8 hours at-30-18 ℃, gaps are formed on the surface of a carbon film substrate in the process, and then the substrate is subjected to heat treatment for 5-8 hours at 100-150 ℃, so that a binder on the surface of the carbon film is subjected to thermal decomposition at high temperature, fluorinated titanium dioxide is exposed, a plurality of micron-nanometer protrusions are formed on the surface of the carbon film by the uniformly dispersed fluorinated titanium dioxide, the size of the micron-nanometer protrusions is far smaller than the diameter of a water drop at a millimeter level, the surface of the carbon film cannot be soaked by the water drop, a super-hydrophobic layer is formed, the water contact angle of the super-hydrophobic layer is 165-175 degrees, the rolling angle is 5-15 degrees, and the prepared carbon film has good electric conductivity, antibacterial property and hydrophobic property, and has wide application prospects.
Drawings
In order to more clearly illustrate the technical solutions in the embodiments of the present application, the drawings required to be used in the description of the embodiments are briefly introduced below, and it is obvious that the drawings in the description below are only some embodiments of the present application, and it is obvious for those skilled in the art to obtain other drawings without creative efforts.
Fig. 1 is a schematic structural diagram of a carbon thin film provided in an embodiment of the present application;
in the figure: 1. a carbon film base; 2. a super-hydrophobic layer; 21. and (4) protruding.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present application clearer, the technical solutions in the embodiments of the present application will be clearly and completely described below in conjunction with the embodiments of the present application, and it is obvious that the described embodiments are some embodiments of the present application, but not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present application.
In a first aspect, an embodiment of the present application provides a carbon-based slurry, including the following components by weight:
10-40 parts of nano carbon material, 200-400 parts of binder and 5-20 parts of fluorinated titanium dioxide.
According to the carbon-based slurry, the carbon nanomaterial is used as the conductive functional body, so that the prepared carbon film has high conductivity, and the heat radiation function can be realized under the heating condition;
under ultraviolet irradiation, the titanium dioxide particles are chargedExcited from valence band to conduction band, generating electrons and holes simultaneously with O adsorbed on its surface 2 And H 2 The positive electrons and water molecules are combined to generate hydroxyl radicals which have strong oxidative decomposition capacity and can decompose most organic compounds and partial inorganic substances into nontoxic carbon dioxide and water, and negative electrons and oxygen are combined into active oxygen, namely super-oxidative ions, so that the super-oxidative ions have strong oxidative decomposition capacity, can damage cell membranes of bacteria and solidify proteins of the bacteria, can decompose harmful compounds released on bacterial corpses while killing the bacteria, and show excellent antibacterial performance; under the irradiation of ultraviolet light, a large amount of-OH is distributed on the surface of the titanium dioxide particles after a series of reactions, and the-OH is used as a hydrophilic group to improve the hydrophilicity of the titanium dioxide particles, so that the hydrophilicity of the carbon film is improved.
In some embodiments, the method of making the fluorinated titania may include the steps of:
mixing titanium dioxide powder with a trifluoroacetic acid aqueous solution, stirring in a water bath at 60 ℃ for 1h, standing for 12h, drying at 80 ℃, cooling to room temperature, and performing heat treatment at 300 ℃ to volatilize residual trifluoroacetic acid to obtain fluorinated titanium dioxide.
It should be noted that the micro-nano-scale protrusions described herein refer to protrusions having a height of micro-size or nano-size and a diameter of nano-size or nano-size.
The carbon thin film with high conductivity, strong antibacterial property and super-hydrophobicity can be prepared by optimizing the formula of the carbon-based slurry, if the content of the nano carbon materials is too low, the nano carbon materials cannot be in complete contact with each other to form a conductive path, so that the resistance of the carbon thin film is too high, the power of the carbon thin film is too low, the heat radiation effect cannot meet the use requirement easily, the resistance of the carbon thin film is further reduced along with the increase of the content of the nano carbon materials, when the nano carbon materials are in full contact with each other to reach a saturated state, the resistance is not obviously changed any more, and meanwhile, the carbon thin film is not uniformly heated due to the fact that the content is too high and the agglomeration phenomenon easily occurs.
If the content of the binder is too low, the uniform dispersion and binding effects on the nano-carbon material and the fluorinated titanium dioxide cannot be achieved, and if the content of the binder is too high, the dispersion degree of the nano-carbon material and the fluorinated titanium dioxide is too high, and micron-nanometer level protrusions are difficult to form in subsequent links.
If the content of the fluorinated titanium dioxide is too low, the fluorinated titanium dioxide cannot play a strong antibacterial role, and meanwhile, the content of the fluorinated titanium dioxide is too small, so that the fluorinated titanium dioxide is excessively dispersed in the carbon film, the distance is too large, the formation of protrusions with the interval of micron or nanometer sizes is not facilitated, water drops can possibly intrude into the carbon film from gaps among the protrusions, and the carbon film does not have super-hydrophobicity.
In some embodiments, the fluorinated titanium dioxide is a rod-like crystal having a diameter of 100 to 300nm and a length of 1 to 3 μm.
It should be noted that the super-hydrophobic layer has the super-hydrophobic performance mainly due to two key factors, one of which is: forming a plurality of bulges on the surface of the carbon film, wherein the sizes of the bulges are in a micron or nanometer level, and the second step is as follows: the distance between adjacent bulges is in nanometer or micrometer level, the minimum diameter of a water drop in nature is usually 1-2mm due to the action of surface tension, and the water drop cannot infiltrate the bulges and cannot enter the bulge gaps into the carbon film due to the fact that the size of the bulges and the bulge gaps is far smaller than the diameter of the water drop by controlling the sizes of the bulges and the bulge gaps to be in micrometer or nanometer level, so that super-hydrophobicity is realized;
if the size of the protrusions is in a micron or nanometer level and the distance between adjacent protrusions is in a millimeter level, the protrusions are distributed too dispersedly, the distance between the protrusions is too large, the diameter size of water drops is achieved, and the water drops can be caused to directly infiltrate the carbon film between the gaps of the protrusions and cannot play a good hydrophobic role;
if the distance between the protrusions is in the micrometer or nanometer level and the size of the protrusions is too large to reach the millimeter level, water drops may directly infiltrate the protrusions, and a good hydrophobic effect cannot be achieved.
The applicant discovers through research that in the subsequent process of heating and decomposing the binder, rod-shaped fluorinated titanium dioxide crystals with the length of 1-3 microns can protrude out of the carbon nano-material to form protrusions, the fluorinated titanium dioxide on the surface layer can effectively decompose organic matters and bacteria on the surface of the carbon film, the antibacterial performance is improved, and the micrometer-nanometer level protrusions can be obtained within the range by controlling the diameter of the fluorinated titanium dioxide to be 100-300 nm and easily causing the protrusion structure to be too large if the diameter of the fluorinated titanium dioxide is too large, so that the formation of a super-hydrophobic layer is not facilitated.
In some embodiments, the nanocarbon material has a particle size of less than 100nm.
If the particle size distribution of the nanocarbon material is too large, the conductive performance tends to be lowered, and therefore, the particle size of the nanocarbon material is preferably less than 100nm.
In some embodiments, the nanocarbon material comprises at least one of carbon nanotubes, carbon nanofibers, nanocarbon spheres, graphene, expanded graphite.
In some embodiments, the binder comprises at least one of N-methyl pyrrolidone, polyvinylidene fluoride, carboxymethyl cellulose, styrene butadiene rubber, polytetrafluoroethylene, polyacrylic acid.
The binder mainly plays a role in dispersing and binding the nanocarbon material and the fluorinated titanium dioxide.
In some embodiments, the binder consists of N-methyl pyrrolidone and polyvinylidene fluoride, and the mass ratio of the N-methyl pyrrolidone to the polyvinylidene fluoride is (12-6): 1.
in the research of the applicant, the binder formed by compounding the N-methyl pyrrolidone and the polyvinylidene fluoride can further improve the hydrophobicity of the carbon film.
In a second aspect, an embodiment of the present application provides a method for preparing a carbon thin film, including the following steps:
coating the carbon-based slurry on a substrate and standing;
freezing the base material coated with the carbon-based slurry at-30 to-18 ℃ for 3 to 8 hours;
then heat treatment is carried out for 5 to 8 hours at the temperature of between 100 and 150 ℃ to obtain the carbon film.
After the carbon-based slurry is coated on the substrate, the substrate is frozen at-30 ℃ to-18 ℃ for 3-8 h, a gap is formed on the surface of the carbon film substrate in the process, and then heat treatment is carried out at 100-150 ℃ for 5-8 h, so that a binder on the surface of the carbon film is thermally decomposed at high temperature, fluorinated titanium dioxide is exposed, a plurality of micron-nanometer protrusions are formed on the surface of the uniformly dispersed fluorinated titanium dioxide on the surface of the carbon film, the size of the micron-nanometer protrusions is far smaller than the diameter of a water drop at the millimeter level, the water drop cannot infiltrate the surface of the carbon film, a super-hydrophobic layer is formed, the water contact angle of the super-hydrophobic layer is 165-175 degrees, and the rolling angle is 5-15 degrees.
Specifically, the substrate is a flexible substrate, and the flexible substrate commonly used in the art, such as cloth, PE film, etc., may be used as the flexible substrate, and is not particularly limited herein.
In a preferred embodiment, the process parameters for applying the carbon-based slurry to a substrate are: scraper gap: 3-8 mm, moving speed: 20 to 45m/h.
In a preferred embodiment, the method for preparing the carbon-based slurry includes:
preparing a binder: dissolving polyvinylidene fluoride in N-methyl pyrrolidone, and stirring at the stirring speed of 1000-4000 r/min for 1-3 h;
preparing a fluoridized titanium dioxide dispersion liquid: weighing fluorinated titanium dioxide powder, dissolving the fluorinated titanium dioxide powder in an ethylene glycol dimethyl ether solvent, and carrying out ultrasonic treatment for 10-30 min at the temperature of 40-70 ℃ for 24h at room temperature to obtain a fluorinated titanium dioxide dispersion liquid;
preparing carbon-based slurry: the nano-carbon material, the titanium fluoride dioxide dispersion liquid and the binder are centrifugally dispersed and mixed uniformly under the vacuum condition, and the technological parameters are as follows: the vacuum degree is-0.1 Mpa-0.08 Mpa, the stirring speed is 2000 r/min-4500 r/min during centrifugal dispersion, the centrifugal speed is 3000-5000 r/min, and the stirring time is 4-8 h.
In some embodiments, the standing treatment time is 1 to 3 hours.
The standing treatment process aims to preliminarily solidify the carbon-based slurry, and make hydrophobic fluorinated titanium dioxide enriched on the surface of the slurry, so that the antibacterial property of the carbon film can be improved on one hand, and the subsequent formation of micron-nanometer protrusions is facilitated on the other hand.
In a third aspect, the present application provides a carbon thin film prepared by the preparation method as described above;
the carbon film comprises a carbon film substrate 1 and a super-hydrophobic layer 2 coated on the surface of the carbon film substrate, wherein the super-hydrophobic layer 2 is formed by fluorinated titanium dioxide which is arranged at intervals and embedded in the carbon film substrate 1, and protrusions 21 are formed on the surface of the carbon film substrate 1 by the fluorinated titanium dioxide.
According to the method, the bulge with the micro-nano structure on the surface is prepared by controlling the freezing temperature and time and the heat treatment temperature and time of the carbon-based slurry and matching and cooperating the conditions, and the thickness of the carbon film is 1-5 mm.
In some embodiments, the protrusions 21 have a height of 100 to 300 μm, a diameter of 50 to 200 μm, and a pitch between adjacent protrusions 21 is 300 to 500 μm.
The protrusions with the size of micron level or nanometer level can be prepared under the conditions, if the heating time or temperature is lower than the range of the application, the decomposition ratio of the binder is insufficient, the micron-nanometer level protrusions cannot be formed, if the heating time or temperature is too high, the binder is decomposed too much, the toughness of the carbon film is affected, the bonding strength of the nano carbon material and the fluorinated titanium dioxide is not high, and the phenomena of powder removal and the like are easy to occur.
In a preferred embodiment, the frozen material is preferably air dried at 100 ℃ for 8h and then 150 ℃ for 5h.
The decomposition ratio of the binder can be further ensured, so that micron-nanometer protrusions are formed on the surface of the carbon film.
The present application will be further described with reference to specific examples.
Example 1
This example is intended to illustrate a carbon-based slurry, a carbon thin film and a method for preparing the same disclosed in the present application, and includes the following steps:
101: preparing a binder: dissolving 50g of polyvinylidene fluoride powder in a 2 LN-methyl pyrrolidone solvent, and stirring for 3h at a stirring speed of 2000r/min to obtain a binder;
102: preparing a fluoridized titanium dioxide dispersion liquid: weighing 2g of titanium dioxide fluoride powder, dissolving the titanium dioxide fluoride powder in 20mL of ethylene glycol dimethyl ether solvent, and carrying out ultrasonic treatment for 30min at the temperature of 70 ℃ for stirring at room temperature for 24h to obtain a titanium dioxide fluoride dispersion liquid;
103: 30 parts of a nano carbon material, 10 parts of fluorinated titanium dioxide dispersion liquid and 200 parts of a binder are taken, and are centrifugally dispersed and uniformly mixed under a vacuum condition, wherein the process parameters are as follows: the vacuum degree is minus 0.1Mpa to 0.08Mpa, the stirring speed is 4500r/min during centrifugal dispersion, the centrifugal speed is 5000r/min, and the stirring time is 8h, so as to obtain the carbon-based slurry:
104: coating the carbon-based slurry on a PE film, and standing for 2 hours;
105: freezing the PE film coated with the carbon-based slurry at-30 ℃ for 8h;
106: and (4) after freezing, drying the mixture for 6 hours at 120 ℃ by hot air to obtain the carbon film with the super-hydrophobic layer on the surface.
Example 2
This example is used to illustrate a carbon-based slurry, a carbon thin film and a method for preparing the same disclosed in the present application, and includes the following steps:
101: preparing a binder: weighing 25g of carboxymethyl cellulose and 25g of styrene butadiene rubber, uniformly mixing, dissolving in 2L of water, and stirring for 3 hours at a stirring speed of 2000r/min to obtain a binder;
102: preparing a fluoridized titanium dioxide dispersion liquid: weighing 2g of titanium dioxide fluoride powder, dissolving the titanium dioxide fluoride powder in 20mL of ethylene glycol dimethyl ether solvent, and carrying out ultrasonic treatment for 30min at the temperature of 70 ℃ for stirring at room temperature for 24h to obtain a titanium dioxide fluoride dispersion liquid;
103: 30 parts of a nano carbon material, 10 parts of fluorinated titanium dioxide dispersion liquid and 200 parts of a binder are taken, and are centrifugally dispersed and uniformly mixed under a vacuum condition, wherein the process parameters are as follows: the vacuum degree is minus 0.1Mpa to 0.08Mpa, the stirring speed is 4500r/min during centrifugal dispersion, the centrifugal speed is 5000r/min, and the stirring time is 8h, so as to obtain the carbon-based slurry:
104: coating the carbon-based slurry on a PE film, and standing for 2 hours;
105: freezing the PE film coated with the carbon-based slurry at-30 ℃ for 8h;
106: and (4) after freezing, drying the mixture for 6 hours at 120 ℃ by hot air to obtain the carbon film with the super-hydrophobic layer on the surface.
Example 3
This example is intended to illustrate a carbon-based slurry, a carbon thin film and a method for preparing the same disclosed in the present application, and includes the following steps:
101: preparing a fluoridized titanium dioxide dispersion liquid: weighing 2g of titanium dioxide fluoride powder, dissolving the titanium dioxide fluoride powder in 20mL of glycol dimethyl ether solvent, and carrying out ultrasonic treatment for 30min at the temperature of 70 ℃ for 24h at room temperature to obtain titanium dioxide fluoride dispersion;
102: 30 parts of a nano carbon material, 10 parts of fluorinated titanium dioxide dispersion liquid and 200 parts of polytetrafluoroethylene binder are taken, and are centrifugally dispersed and uniformly mixed under the vacuum condition, wherein the process parameters are as follows: the vacuum degree is minus 0.1Mpa to 0.08Mpa, the stirring speed is 4500r/min during centrifugal dispersion, the centrifugal speed is 5000r/min, and the stirring time is 8h, so as to obtain the carbon-based slurry:
103: coating the carbon-based slurry on a PE film, and standing for 2 hours;
104: freezing the PE film coated with the carbon-based slurry at-30 ℃ for 8h;
105: and (4) after freezing, drying the mixture for 6 hours at 120 ℃ by hot air to obtain the carbon film with the super-hydrophobic layer on the surface.
Example 4
This example is intended to illustrate a carbon-based slurry, a carbon thin film and a method for preparing the same disclosed in the present application, and includes the following steps:
101: preparing a fluoridized titanium dioxide dispersion liquid: weighing 2g of titanium dioxide fluoride powder, dissolving the titanium dioxide fluoride powder in 20mL of ethylene glycol dimethyl ether solvent, and carrying out ultrasonic treatment for 30min at the temperature of 70 ℃ for stirring at room temperature for 24h to obtain a titanium dioxide fluoride dispersion liquid;
102: 30 parts of a nano carbon material, 10 parts of fluorinated titanium dioxide dispersion liquid and 200 parts of polyacrylic acid binder are taken, and are centrifugally dispersed and uniformly mixed under a vacuum condition, wherein the process parameters are as follows: the vacuum degree is minus 0.1Mpa to 0.08Mpa, the stirring speed is 4500r/min during centrifugal dispersion, the centrifugal speed is 5000r/min, and the stirring time is 8h, so as to obtain the carbon-based slurry:
103: coating the carbon-based slurry on a PE film, and standing for 2 hours;
104: freezing the PE film coated with the carbon-based slurry at-30 ℃ for 8h;
105: and (4) after freezing, drying the mixture for 6 hours by hot air at 120 ℃ to obtain the carbon film with the super-hydrophobic layer on the surface.
Example 5
This example is intended to illustrate a carbon-based slurry, a carbon thin film and a method for preparing the same disclosed in the present application, and includes the following steps:
101: preparing a binder: dissolving 50g of polyvinylidene fluoride powder in a 2 LN-methyl pyrrolidone solvent, and stirring for 3h at a stirring speed of 2000r/min to obtain a binder;
102: preparing a fluoridized titanium dioxide dispersion liquid: weighing 2g of titanium dioxide fluoride powder, dissolving the titanium dioxide fluoride powder in 20mL of glycol dimethyl ether solvent, and carrying out ultrasonic treatment for 30min at the temperature of 70 ℃ for 24h at room temperature to obtain titanium dioxide fluoride dispersion;
103: 30 parts of nano carbon material, 10 parts of fluorinated titanium dioxide dispersion liquid and 200 parts of binder are taken, and are centrifugally dispersed and uniformly mixed under the vacuum condition, and the process parameters are as follows: the vacuum degree is minus 0.1Mpa to 0.08Mpa, the stirring speed is 4500r/min during centrifugal dispersion, the centrifugal speed is 5000r/min, and the stirring time is 8h, so that the carbon-based slurry is obtained:
104: coating the carbon-based slurry on a PE film, and standing for 2 hours;
105: freezing the PE film coated with the carbon-based slurry at-30 ℃ for 8h;
106: and (3) after freezing, drying the mixture by hot air at 100 ℃ for 8h, and then drying the mixture by hot air at 150 ℃ for 5h to obtain the carbon film with the super-hydrophobic layer on the surface.
Comparative example 1
This comparative example is illustrative of a carbon-based slurry, a carbon thin film, and a method of making the same disclosed herein, comprising the steps of:
101: preparing a binder: dissolving 50g of polyvinylidene fluoride powder in a 2 LN-methyl pyrrolidone solvent, and stirring for 3h at a stirring speed of 2000r/min to obtain a binder;
102: 30 parts of nano carbon material and 10 parts of binder are taken, and are centrifugally dispersed and uniformly mixed under the vacuum condition, wherein the technological parameters are as follows: the vacuum degree is minus 0.1Mpa to 0.08Mpa, the stirring speed is 4500r/min during centrifugal dispersion, the centrifugal speed is 5000r/min, and the stirring time is 8h, so that the carbon-based slurry is obtained:
104: coating the carbon-based slurry on a PE film, and standing for 2 hours;
105: freezing the PE film coated with the carbon-based slurry at-30 ℃ for 8h;
106: after freezing, the mixture is dried by hot air at 120 ℃ for 6 hours to obtain the carbon film.
Comparative example 2
This comparative example is illustrative of a carbon-based slurry, a carbon thin film, and a method of making the same disclosed herein, comprising the steps of:
101: preparing a binder: dissolving 50g of polyvinylidene fluoride powder in a 2 LN-methyl pyrrolidone solvent, and stirring for 3h at a stirring speed of 2000r/min to obtain a binder;
102: preparing a fluorinated titanium dioxide dispersion liquid: weighing 2g of titanium dioxide fluoride powder, dissolving the titanium dioxide fluoride powder in 20mL of glycol dimethyl ether solvent, and carrying out ultrasonic treatment for 30min at the temperature of 70 ℃ for 24h at room temperature to obtain titanium dioxide fluoride dispersion;
103: taking 30 parts of a nano carbon material, 3 parts of fluorinated titanium dioxide dispersion liquid and 200 parts of a binder, and carrying out centrifugal dispersion and uniform mixing under a vacuum condition, wherein the process parameters are as follows: the vacuum degree is minus 0.1Mpa to 0.08Mpa, the stirring speed is 4500r/min during centrifugal dispersion, the centrifugal speed is 5000r/min, and the stirring time is 8h, so as to obtain the carbon-based slurry:
104: coating the carbon-based slurry on a PE film, and standing for 2 hours;
105: freezing the PE film coated with the carbon-based slurry at-30 ℃ for 8h;
106: after freezing, the mixture is dried by hot air at 120 ℃ for 6 hours to obtain the carbon film.
Comparative example 3
This comparative example is illustrative of a carbon-based slurry, a carbon thin film, and a method of making the same disclosed herein, comprising the steps of:
101: preparing a binder: dissolving 50g of polyvinylidene fluoride powder in a 2 LN-methyl pyrrolidone solvent, and stirring for 3h at a stirring speed of 2000r/min to obtain a binder;
102: preparing a fluoridized titanium dioxide dispersion liquid: weighing 2g of titanium dioxide fluoride powder, dissolving the titanium dioxide fluoride powder in 20mL of ethylene glycol dimethyl ether solvent, and carrying out ultrasonic treatment for 30min at the temperature of 70 ℃ for stirring at room temperature for 24h to obtain a titanium dioxide fluoride dispersion liquid;
103: 30 parts of a nano carbon material, 25 parts of fluorinated titanium dioxide dispersion liquid and 200 parts of a binder are taken, and are centrifugally dispersed and uniformly mixed under a vacuum condition, wherein the process parameters are as follows: the vacuum degree is minus 0.1Mpa to 0.08Mpa, the stirring speed is 4500r/min during centrifugal dispersion, the centrifugal speed is 5000r/min, and the stirring time is 8h, so as to obtain the carbon-based slurry:
104: coating the carbon-based slurry on a PE film, and standing for 2 hours;
105: freezing the PE film coated with the carbon-based slurry at-30 ℃ for 8h;
106: after freezing, the mixture is dried by hot air at 120 ℃ for 6 hours to obtain the carbon film.
Comparative example 4
This comparative example is for comparative illustration of the carbon-based slurry, the carbon thin film and the method for preparing the same disclosed in the present application, and includes the steps of:
101: preparing a binder: dissolving 50g of polyvinylidene fluoride powder in a 2 LN-methyl pyrrolidone solvent, and stirring for 3h at a stirring speed of 2000r/min to obtain a binder;
102: preparing a fluorinated titanium dioxide dispersion liquid: weighing 2g of titanium dioxide fluoride powder, dissolving the titanium dioxide fluoride powder in 20mL of ethylene glycol dimethyl ether solvent, and carrying out ultrasonic treatment for 30min at the temperature of 70 ℃ for stirring at room temperature for 24h to obtain a titanium dioxide fluoride dispersion liquid;
103: 30 parts of a nano carbon material, 10 parts of fluorinated titanium dioxide dispersion liquid and 200 parts of a binder are taken, and are centrifugally dispersed and uniformly mixed under a vacuum condition, wherein the process parameters are as follows: the vacuum degree is minus 0.1Mpa to 0.08Mpa, the stirring speed is 4500r/min during centrifugal dispersion, the centrifugal speed is 5000r/min, and the stirring time is 8h, so as to obtain the carbon-based slurry:
104: coating the carbon-based slurry on a PE film, and standing for 2 hours;
105: and (3) drying the PE film coated with the carbon-based slurry by hot air at 120 ℃ for 6 hours to obtain the carbon film.
Comparative example 5
This comparative example is illustrative of a carbon-based slurry, a carbon thin film, and a method of making the same disclosed herein, comprising the steps of:
101: preparing a binder: dissolving 50g of polyvinylidene fluoride powder in a 2 LN-methyl pyrrolidone solvent, and stirring for 3h at a stirring speed of 2000r/min to obtain a binder;
102: preparing a fluoridized titanium dioxide dispersion liquid: weighing 2g of titanium dioxide fluoride powder, dissolving the titanium dioxide fluoride powder in 20mL of ethylene glycol dimethyl ether solvent, and carrying out ultrasonic treatment for 30min at the temperature of 70 ℃ for stirring at room temperature for 24h to obtain a titanium dioxide fluoride dispersion liquid;
103: 30 parts of a nano carbon material, 10 parts of fluorinated titanium dioxide dispersion liquid and 200 parts of a binder are taken, and are centrifugally dispersed and uniformly mixed under a vacuum condition, wherein the process parameters are as follows: the vacuum degree is minus 0.1Mpa to 0.08Mpa, the stirring speed is 4500r/min during centrifugal dispersion, the centrifugal speed is 5000r/min, and the stirring time is 8h, so that the carbon-based slurry is obtained:
104: coating the carbon-based slurry on a PE film, and standing for 2 hours;
105: and (3) freezing the PE film coated with the carbon-based slurry at-30 ℃ for 8h to obtain the carbon film.
Comparative example 6
This comparative example is for comparative illustration of the carbon-based slurry, the carbon thin film and the method for preparing the same disclosed in the present application, and includes the steps of:
101: preparing a binder: dissolving 50g of polyvinylidene fluoride powder in a 2 LN-methyl pyrrolidone solvent, and stirring for 3h at a stirring speed of 2000r/min to obtain a binder;
102: preparing a fluorinated titanium dioxide dispersion liquid: weighing 2g of titanium dioxide fluoride powder, dissolving the titanium dioxide fluoride powder in 20mL of glycol dimethyl ether solvent, and carrying out ultrasonic treatment for 30min at the temperature of 70 ℃ for 24h at room temperature to obtain titanium dioxide fluoride dispersion;
103: 30 parts of a nano carbon material, 10 parts of fluorinated titanium dioxide dispersion liquid and 200 parts of a binder are taken, and are centrifugally dispersed and uniformly mixed under a vacuum condition, wherein the process parameters are as follows: the vacuum degree is minus 0.1Mpa to 0.08Mpa, the stirring speed is 4500r/min during centrifugal dispersion, the centrifugal speed is 5000r/min, and the stirring time is 8h, so as to obtain the carbon-based slurry:
104: coating the carbon-based slurry on a PE film, and standing for 2 hours;
105: freezing the PE film coated with the carbon-based slurry at 0 ℃ for 8h;
106: and (4) after freezing, drying the mixture for 6 hours by hot air at 120 ℃ to obtain the carbon film with the super-hydrophobic layer on the surface.
Comparative example 7
This comparative example is used for comparative illustration of the carbon-based slurry, the carbon thin film and the method for preparing the same disclosed in the present application, and includes the following steps:
101: preparing a binder: dissolving 50g of polyvinylidene fluoride powder in a 2 LN-methyl pyrrolidone solvent, and stirring for 3h at a stirring speed of 2000r/min to obtain a binder;
102: preparing a fluoridized titanium dioxide dispersion liquid: weighing 2g of titanium dioxide fluoride powder, dissolving the titanium dioxide fluoride powder in 20mL of ethylene glycol dimethyl ether solvent, and carrying out ultrasonic treatment for 30min at the temperature of 70 ℃ for stirring at room temperature for 24h to obtain a titanium dioxide fluoride dispersion liquid;
103: 30 parts of nano carbon material, 10 parts of fluorinated titanium dioxide dispersion liquid and 200 parts of binder are taken, and are centrifugally dispersed and uniformly mixed under the vacuum condition, and the process parameters are as follows: the vacuum degree is minus 0.1Mpa to 0.08Mpa, the stirring speed is 4500r/min during centrifugal dispersion, the centrifugal speed is 5000r/min, and the stirring time is 8h, so as to obtain the carbon-based slurry:
104: coating the carbon-based slurry on a PE film, and standing for 2 hours;
105: freezing the PE film coated with the carbon-based slurry at-50 ℃ for 8h;
106: and (4) after freezing, drying the mixture for 6 hours at 120 ℃ by hot air to obtain the carbon film with the super-hydrophobic layer on the surface.
Comparative example 8
This comparative example is used for comparative illustration of the carbon-based slurry, the carbon thin film and the method for preparing the same disclosed in the present application, and includes the following steps:
101: preparing a binder: dissolving 50g of polyvinylidene fluoride powder in a 2 LN-methyl pyrrolidone solvent, and stirring for 3h at a stirring speed of 2000r/min to obtain a binder;
102: preparing a fluoridized titanium dioxide dispersion liquid: weighing 2g of titanium dioxide fluoride powder, dissolving the titanium dioxide fluoride powder in 20mL of ethylene glycol dimethyl ether solvent, and carrying out ultrasonic treatment for 30min at the temperature of 70 ℃ for stirring at room temperature for 24h to obtain a titanium dioxide fluoride dispersion liquid;
103: 30 parts of a nano carbon material, 10 parts of fluorinated titanium dioxide dispersion liquid and 200 parts of a binder are taken, and are centrifugally dispersed and uniformly mixed under a vacuum condition, wherein the process parameters are as follows: the vacuum degree is minus 0.1Mpa to 0.08Mpa, the stirring speed is 4500r/min during centrifugal dispersion, the centrifugal speed is 5000r/min, and the stirring time is 8h, so as to obtain the carbon-based slurry:
104: coating the carbon-based slurry on a PE film, and standing for 2 hours;
105: freezing the PE film coated with the carbon-based slurry at-30 ℃ for 8h;
106: and (4) after the freezing is finished, drying the mixture for 6 hours by hot air at the temperature of 80 ℃ to obtain the carbon film with the super-hydrophobic layer on the surface.
Comparative example 9
This comparative example is for comparative illustration of the carbon-based slurry, the carbon thin film and the method for preparing the same disclosed in the present application, and includes the steps of:
101: preparing a binder: dissolving 50g of polyvinylidene fluoride powder in a 2 LN-methyl pyrrolidone solvent, and stirring for 3h at a stirring speed of 2000r/min to obtain a binder;
102: preparing a fluoridized titanium dioxide dispersion liquid: weighing 2g of titanium dioxide fluoride powder, dissolving the titanium dioxide fluoride powder in 20mL of glycol dimethyl ether solvent, and carrying out ultrasonic treatment for 30min at the temperature of 70 ℃ for 24h at room temperature to obtain titanium dioxide fluoride dispersion;
103: 30 parts of nano carbon material, 10 parts of fluorinated titanium dioxide dispersion liquid and 200 parts of binder are taken, and are centrifugally dispersed and uniformly mixed under the vacuum condition, and the process parameters are as follows: the vacuum degree is minus 0.1Mpa to 0.08Mpa, the stirring speed is 4500r/min during centrifugal dispersion, the centrifugal speed is 5000r/min, and the stirring time is 8h, so as to obtain the carbon-based slurry:
104: coating the carbon-based slurry on a PE film, and standing for 2 hours;
105: freezing the PE film coated with the carbon-based slurry at-30 ℃ for 8h;
106: and (4) after freezing, drying the mixture for 6 hours at 180 ℃ by hot air to obtain the carbon film.
Performance testing
The following performance tests were performed on the carbon thin films prepared in examples 1 to 5 and comparative examples 1 to 9, and the results are filled in table 1.
Resistance: measuring the sheet resistance of the carbon film sample by using a four-point measuring method, and using a point-shaped tip as a probe by using a four-probe measuring method;
antibacterial activity: according to JISZ2801:2012 'antibacterial effect of antibacterial test method of antibacterial processed product' and selecting staphylococcus aureus as test strain for detection;
hydrophobicity: static water contact angle and sliding angle measurements were performed on the carbon films.
TABLE 1
According to table 1, by combining the test data of the examples 1 to 5 and the test data of the comparative example 1, the resistance of the carbon thin film prepared by the formula and the preparation method of the carbon thin film prepared by the examples 1 to 5 is more than 4.0 Ω, and the carbon thin film has good electric heating performance, and compared with the comparative example 1 without adding fluorinated titanium dioxide, the carbon thin film has greatly improved antibacterial activity and hydrophobic performance, wherein the antibacterial activity value can reach more than 5.0, the contact reaches more than 165 °, the rolling angle is 5 °, and the super-hydrophobic requirement is met, so that the antibacterial property and the hydrophobic property of the carbon thin film can be obviously improved by the cooperation of the fluorinated titanium dioxide and the rest components;
combining the test data of example 1 and comparative examples 2-3, the amount of the fluorinated titania added in comparative example 2 is below the range of the present application, compared to example 1, the antibacterial activity is sharply reduced to 2.0, the water contact angle is reduced to 150 °, the rolling angle is increased to 15 °, which indicates that comparative example 2 is significantly inferior to example 1 in both antibacterial activity and hydrophobicity, and the amount of the fluorinated titania added in comparative example 3 is above the range of the present application, which is not favorable for forming micron-nanometer protrusions, so that the water contact angle is reduced to a certain extent, the water rolling angle is increased to 10 °, which indicates that comparative example 3 is inferior to example 1 in hydrophobicity, and the present application controls the amount of the fluorinated titania added to be within 5-20 parts, so that the carbon thin film has both high antibacterial activity and strong hydrophobicity;
combining the test data of the example 1 and the test data of the comparative examples 4-5, the freezing treatment operation is not performed in the comparative example 4, the heat treatment operation is not performed in the comparative example 5, the water contact angles of the carbon films prepared by the freezing treatment and the heat treatment are only 55 degrees and 60 degrees, which are obviously lower than 175 degrees of the example 1, and the method is proved that the freezing treatment and the high-temperature heat treatment are combined in the preparation process of the carbon film, so that the micron-nanometer protrusions can be formed, and the hydrophobicity of the carbon film can be obviously improved;
combining the test data of the example 1 and the comparative examples 6 to 7, the temperature of the freezing treatment in the comparative example 6 is higher than the application range, the temperature of the freezing treatment in the comparative example 7 is lower than the application range, the water contact angles of the carbon films prepared by the two are only 55 degrees and 90 degrees, and are obviously lower than 175 degrees of the carbon films prepared by the example 1, and the application proves that the temperature of the freezing treatment is controlled between-30 ℃ and-18 ℃, so that the micron-nanometer protrusions can be formed on the surface of the carbon film, and the formation of the micron-nanometer protrusions is not facilitated due to the over-high temperature or the over-low temperature;
combining the test data of example 1 and comparative examples 8-9, the temperature in the heat treatment of comparative example 8 is lower than the range of the application, the temperature in the heat treatment of comparative example 9 is higher than the range of the application, the water contact angles of the carbon films prepared by the two are only 85 degrees and 95 degrees, and are significantly lower than 175 degrees of example 1, which shows that the temperature in the heat treatment of the application is controlled between 100 ℃ and 150 ℃, so that the micron-nanometer protrusions can be formed on the surface of the carbon film, and the temperature is too high or too low, which is not beneficial to the formation of the micron-nanometer protrusions.
The above description is merely exemplary of the present application and is presented to enable those skilled in the art to understand and practice the present application. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the application. Thus, the present application is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (10)
1. A carbon-based slurry is characterized by comprising the following components in parts by weight:
10-40 parts of nano carbon material, 200-400 parts of binder and 5-20 parts of fluorinated titanium dioxide.
2. The carbon-based slurry according to claim 1, wherein the fluorinated titanium dioxide is a rod-like crystal having a diameter of 100 to 300nm and a length of 1 to 3 μm.
3. The carbon-based slurry according to claim 1, wherein the nanocarbon material has a particle size of less than 100nm.
4. The carbon-based slurry according to claim 1, wherein the nanocarbon material comprises at least one of carbon nanotubes, carbon nanofibers, nanocarbon spheres, graphene, and expanded graphite.
5. The carbon-based slurry according to claim 1, wherein the binder comprises at least one of N-methyl pyrrolidone, polyvinylidene fluoride, carboxymethyl cellulose, styrene-butadiene rubber, polytetrafluoroethylene, polyacrylic acid.
6. The carbon-based slurry according to claim 5, wherein the binder comprises N-methyl pyrrolidone and polyvinylidene fluoride, and the mass ratio of the N-methyl pyrrolidone to the polyvinylidene fluoride is (12-6): 1.
7. the preparation method of the carbon film is characterized by comprising the following steps:
coating the carbon-based slurry according to any one of claims 1-6 onto a substrate, standing;
freezing the base material coated with the carbon-based slurry at-30 ℃ to-18 ℃ for 3-8 h;
then heat treatment is carried out for 5 to 8 hours at the temperature of between 100 and 150 ℃ to obtain the carbon film.
8. The method for preparing a carbon thin film according to claim 7, wherein the standing treatment time is 1 to 3 hours.
9. A carbon thin film produced by the production method according to any one of claims 7 to 8;
the carbon film comprises a carbon film substrate (1) and a super-hydrophobic layer (2) coated on the surface of the carbon film substrate (1), wherein the super-hydrophobic layer (2) is formed by fluorinated titanium dioxide which is arranged at intervals and embedded in the carbon film substrate (1), and protrusions (21) are formed on the surface of the carbon film substrate (1) by the fluorinated titanium dioxide.
10. The carbon thin film according to claim 9, wherein the protrusions (21) have a height of 100 to 300 μm, a diameter of 50 to 200 μm, and a pitch between adjacent protrusions (21) of 300 to 500 μm.
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