CN111050433A - Flexible heating sheet and preparation method thereof - Google Patents
Flexible heating sheet and preparation method thereof Download PDFInfo
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- CN111050433A CN111050433A CN201911219773.8A CN201911219773A CN111050433A CN 111050433 A CN111050433 A CN 111050433A CN 201911219773 A CN201911219773 A CN 201911219773A CN 111050433 A CN111050433 A CN 111050433A
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Classifications
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- 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
- H05B3/146—Conductive polymers, e.g. polyethylene, thermoplastics
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/04—Carbon
- C08K3/041—Carbon nanotubes
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Nanotechnology (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Surface Heating Bodies (AREA)
- Resistance Heating (AREA)
Abstract
The invention belongs to the technical field of heat conduction materials, and particularly relates to a preparation method of a flexible heating sheet, which comprises the following steps: the method comprises the steps of obtaining carbon nanotube fiber bundles and a substrate, and arranging the carbon nanotube fiber bundles on the substrate according to a preset circuit diagram to obtain the substrate with the fiber circuit diagram; depositing a rubber mixed material on the surface of one side of the substrate on which the fiber circuit diagram is laid, so that the area of the fiber circuit diagram laid on the substrate except the end part of the carbon nano tube fiber bundle is fixedly sealed in the rubber mixed material, and forming a heating sheet on the substrate; wherein the rubber mixed material comprises rubber and a curing agent. The preparation method of the flexible heating sheet provided by the invention is simple in process flow, flexible and convenient to operate, and suitable for industrial large-scale production and application.
Description
Technical Field
The invention belongs to the technical field of heat conduction materials, and particularly relates to a flexible heating sheet and a preparation method thereof.
Background
The traditional heat conducting gasket basically takes silica gel or other high polymer materials as base materials, and the composite material is provided with a heat conducting channel by filling heat conducting materials, so that the heat conducting effect of the material is achieved. There are many kinds of conventional heat conductive materials, and examples thereof include a metal wire, a heat conductive powder, and a carbon material. The heat conducting powder is used as a heating sheet of the heat conducting material, the more the filled powder is, the more the powder particle size matching is reasonable, the more the heat conducting channels are, the higher the corresponding heat conducting coefficient of the material is, but with the more and more filled materials, the mechanical properties of the product, particularly the tensile strength, the compressibility and the like are greatly reduced, so that the application of the heat conducting powder in many occasions is limited, and meanwhile, the more the filled powder is, the density of the material is increased, and the heat conducting powder is obviously inconsistent with the light weight and the trend of user experience which are pursued at present. In addition, the metal wire is used as a heating sheet of the heat conduction material, the metal wire is used as an electric heating wire, the weight is heavy, the requirement of light weight of some heating equipment is not facilitated, the metal wire is easy to break, the safety performance is poor, the shape and the size of the heat source are limited, and the micro heat source is not facilitated to be manufactured. Carbon materials such as carbon nanotubes and graphene are used as heating sheets of heat conducting materials, and the carbon materials are not well dispersed in a matrix and are easy to agglomerate, so that the content of the carbon materials is low, the electrothermal conversion efficiency is low, and the application range of the electrothermal material is limited.
Disclosure of Invention
Problems to be solved by the invention
The invention aims to provide a preparation method of a flexible heating sheet, and aims to solve the technical problems of poor mechanical property, easiness in breaking, poor flexibility and plasticity, poor safety performance, low electrothermal conversion efficiency and the like of the conventional heating sheet.
Another object of the present invention is to provide a flexible heat generating sheet.
Means for solving the problems
In order to achieve the purpose of the invention, the technical scheme adopted by the invention is as follows:
a preparation method of a flexible heating sheet comprises the following steps:
the method comprises the steps of obtaining carbon nanotube fiber bundles and a substrate, and arranging the carbon nanotube fiber bundles on the substrate according to a preset circuit diagram to obtain the substrate with the fiber circuit diagram;
depositing a rubber mixed material on the surface of one side of the substrate on which the fiber circuit diagram is laid, so that the area of the fiber circuit diagram laid on the substrate except the end part of the carbon nano tube fiber bundle is fixedly sealed in the rubber mixed material, and forming a heating sheet on the substrate;
wherein the rubber mixed material comprises rubber and a curing agent.
Preferably, the substrate is provided with a plurality of detachable protrusions, and the detachable protrusions are used for providing path guidance for the carbon nanotube fiber bundle layout circuit diagram.
Preferably, the step of arranging the carbon nanotube fiber bundles on the substrate according to a preset circuit pattern includes: orderly winding the detachable bulges by the carbon nano tube fiber bundles according to a preset circuit diagram, and laying to form a carbon nano tube fiber circuit diagram; and/or the presence of a gas in the gas,
the end parts of the carbon nano tube fiber bundles are connected with the electrode plates and are communicated with an external circuit through the electrode plates.
Preferably, the step of depositing the rubber mixed material on the surface of the substrate on which the fiber circuit pattern is laid comprises: casting the rubber mixed material on the surface of one side of the substrate on which the fiber circuit diagram is arranged, so that the fiber circuit diagram is coated in the rubber mixed material, and the deposition thickness of the rubber mixed material is lower than the height of the detachable protrusion; and/or the presence of a gas in the gas,
the temperature of the curing treatment is 80-100 ℃.
Preferably, the mass ratio of the rubber to the curing agent in the rubber mixed material is (10-1): 1; and/or the presence of a gas in the gas,
the rubber is selected from: at least one of nitrile rubber, silicone rubber, polyisoprene rubber and ethylene propylene diene rubber; and/or the presence of a gas in the gas,
the curing agent is selected from: at least one of sulfur-containing compounds, metal oxides, peroxides, resins, quinones, and amines.
Preferably, the step of obtaining the carbon nanotube fiber bundle comprises:
obtaining a carbon nanotube array, pulling out a carbon nanotube film from the carbon nanotube array, and twisting the carbon nanotube film to obtain a carbon nanotube fiber;
and carrying out doubling treatment on the plurality of carbon nanotube fiber yarns to obtain the carbon nanotube fiber bundle.
Preferably, the carbon nanotube array is prepared by reacting for 5 to 10 minutes by a chemical vapor deposition method in a carbon source atmosphere at a temperature of 500 to 900 ℃; and/or the presence of a gas in the gas,
the step of pulling out the carbon nanotube film from the carbon nanotube array and then twisting the carbon nanotube film comprises: drawing a carbon nanotube film with the width of 0.1-20 cm from the carbon nanotube array, and twisting the carbon nanotube film according to the twist of 100-15000 tpm; and/or the presence of a gas in the gas,
the carbon nano tube fiber bundle is prepared by doubling 5-20 carbon nano tube fiber yarns.
Preferably, after the heat generating sheet is formed on the substrate, the method further includes: and dismantling the bulge on the substrate, removing the substrate, and then carrying out hot pressing treatment on the heating sheet to obtain the flexible heating sheet.
Preferably, the conditions of the hot pressing process include: hot pressing treatment is carried out under the conditions that the temperature is 100-300 ℃ and the pressure is 5-20 MPa.
Correspondingly, the invention also provides a flexible heating sheet, which is prepared by the method, the thickness of the flexible heating sheet is 1-3 mm, 0.1-0.6A of current is applied to the flexible heating sheet, and the temperature of the flexible heating sheet reaches 40-80 ℃ within 5 seconds.
Effects of the invention
The preparation method of the flexible heating sheet comprises the steps of firstly, arranging the carbon nano tube fiber bundles on the substrate to form a fiber circuit diagram, then depositing a mixed material of rubber and a curing agent on the surface of one side of the substrate on which the fiber circuit diagram is arranged, and fixedly sealing the area, except the end part of the carbon nano tube fiber bundle, of the fiber circuit diagram arranged on the substrate in the rubber mixed material, so that the heating sheet can be formed on the substrate. On one hand, the carbon nanotube fiber bundle is directly used as the heat conduction material of the heating sheet, and the carbon nanotube fiber bundle has the characteristics of excellent electric conductivity, mechanical property, high temperature resistance, corrosion resistance and the like due to the unique structure, so that the heating sheet has excellent electric heat conversion performance, uniform heating, good stability and long service life; on the other hand, the carbon nanotube fiber bundle is prepared by laying a heating circuit diagram on the substrate and then depositing rubber, the heating circuit diagram with any shape, size, hierarchical structure and the like can be laid according to the use and application requirements, the carbon nanotube fiber bundle is flexible in application and can meet different application requirements, and the carbon nanotube fiber bundle is small in size and light in weight, so that the preparation of a light and ultrathin flexible heating sheet is facilitated, the prepared heating sheet is good in flexibility and can be bent at will, and the application range is wide. The preparation method of the flexible heating sheet provided by the invention is simple in process flow, flexible and convenient to operate, and suitable for industrial large-scale production and application.
The flexible heating sheet provided by the invention is prepared by any method, and comprises a heating circuit distributed by carbon nanotube fiber bundles and a rubber material wrapping the heating circuit, wherein two ends of the carbon nanotube fiber bundles are respectively connected with electrode plates and are communicated with an external circuit through an electric heating sheet, so that electric heating conversion is realized. And (3) electrifying the flexible heating sheet with 0.1-0.6A of current, wherein the temperature of the flexible heating sheet reaches 40-80 ℃ within 5 seconds, the heating temperature is stable, the safety is high, and the heating is rapid. The flexible heating sheet provided by the invention has the advantages of high electric-heat conversion efficiency, uniform and stable heating, high flexibility, free bending, thin thickness of only 1-3 mm, light weight, strong practicability and convenient and flexible application.
Drawings
Fig. 1 is a schematic view of a flexible heat generating sheet provided in embodiment 1 of the present invention.
Fig. 2 is a schematic view of a flexible heat generating sheet provided in embodiment 2 of the present invention.
Detailed Description
In order to make the purpose, technical solution and technical effect of the embodiments of the present invention clearer, the technical solution in the embodiments of the present invention is clearly and completely described, and it is obvious that the described embodiments are a part of the embodiments of the present invention, but not all embodiments. All other embodiments obtained by a person of ordinary skill in the art without any inventive step in connection with the embodiments of the present invention shall fall within the scope of protection of the present invention.
In the description of the present invention, it is to be understood that the terms "first", "second" and the like are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or implying any number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include one or more of that feature. In the description of the present invention, "a plurality" means two or more unless specifically defined otherwise.
The weight of the related components mentioned in the description of the embodiments of the present invention may not only refer to the specific content of each component, but also represent the proportional relationship of the weight among the components, and therefore, the content of the related components is scaled up or down within the scope disclosed in the description of the embodiments of the present invention as long as it is in accordance with the description of the embodiments of the present invention. Specifically, the weight described in the description of the embodiment of the present invention may be a unit of mass known in the chemical industry field, such as μ g, mg, g, and kg.
The embodiment of the invention provides a preparation method of a flexible heating sheet, which comprises the following steps:
s10, obtaining a carbon nanotube fiber bundle and a substrate, and arranging the carbon nanotube fiber bundle on the substrate according to a preset circuit diagram to obtain the substrate with the fiber circuit diagram;
s20, depositing a rubber mixed material on the surface of one side of the substrate, where the fiber circuit diagram is arranged, so that the area, except the end part of the carbon nanotube fiber bundle, in the fiber circuit diagram arranged on the substrate is fixedly sealed in the rubber mixed material, and a heating sheet is formed on the substrate;
wherein the rubber mixed material comprises rubber and a curing agent.
The preparation method of the flexible heating sheet provided by the embodiment of the invention comprises the steps of firstly, arranging the carbon nano tube fiber bundles on the substrate to form a fiber circuit diagram, then, depositing a mixed material of rubber and a curing agent on the surface of one side of the substrate on which the fiber circuit diagram is arranged, and fixedly sealing the area, except the end part of the carbon nano tube fiber bundle, in the fiber circuit diagram arranged on the substrate in the rubber mixed material, so that the heating sheet can be formed on the substrate. On one hand, the embodiment of the invention directly adopts the carbon nanotube fiber bundle as the heat conduction material of the heating sheet, and the carbon nanotube fiber bundle has the characteristics of excellent electric conductivity, mechanical property, high temperature resistance, corrosion resistance and the like due to the unique structure, so that the heating sheet has excellent electric heat conversion performance, uniform heating, good stability and long service life; on the other hand, the heating sheet is prepared by laying the heating circuit diagram on the substrate by the carbon nano tube fiber bundle and then depositing rubber, the heating circuit diagram with any shape, size, hierarchical structure and the like can be laid according to the use and application requirements, different application requirements can be met in the aspect of flexible application, and the carbon nano tube fiber bundle is small in size and light in weight, so that the preparation of the light-weight and ultrathin flexible heating sheet is facilitated, the prepared heating sheet is good in flexibility and can be bent at will, and the application range is wide. The preparation method of the flexible heating sheet provided by the embodiment of the invention has the advantages of simple process flow, flexible and convenient operation and suitability for industrial large-scale production and application.
Specifically, in step S10, a carbon nanotube fiber bundle and a substrate are obtained, and the carbon nanotube fiber bundle is arranged on the substrate according to a preset circuit diagram, so as to obtain the substrate with the fiber circuit diagram. The heating material of the flexible heating sheet in the embodiment of the invention forms the heating circuit diagrams with different shapes, sizes, hierarchical structures and the like by arranging the circuit diagrams on the substrate, can arrange different circuit diagrams according to the actual requirements on the heating parts and the like of the heating sheet, meets different application requirements, and has flexible application and operation aspects. In some embodiments, the circuit diagram of the carbon nanotube fiber bundles arranged on the substrate may be in various shapes such as a labyrinth shape, a grid shape, etc., or a multi-layer circuit diagram may be arranged to form a multi-layer and multi-structure heating circuit diagram, so that the prepared heating sheet has a better heating effect.
In some embodiments, the step of obtaining carbon nanotube fiber bundles comprises:
s11, obtaining a carbon nanotube array, pulling out a carbon nanotube film from the carbon nanotube array, and twisting the carbon nanotube film to obtain a carbon nanotube fiber;
and S12, carrying out doubling treatment on the plurality of carbon nano tube fiber yarns to obtain the carbon nano tube fiber bundle.
According to the embodiment of the invention, the carbon nanotube fiber bundle is prepared by directly preparing the carbon nanotube fiber yarns from the carbon nanotube array with high crystallinity, high purity, good verticality and good uniformity, and then doubling the carbon nanotube fiber yarns to prepare the carbon nanotube fiber bundle, so that the prepared carbon nanotube fiber bundle has excellent conductivity, high strength, corrosion resistance, high temperature resistance, long service life, low probability of deformation at high temperature, light weight, small occupied space, flexibility, free bending, suitability for spinning into a carbon nanotube fiber net, excellent thermal conductivity for a heating sheet, light weight, high plasticity and the like.
In some embodiments, the carbon nanotube array is prepared by reacting for 5-10 minutes by a chemical vapor deposition method in a carbon source atmosphere at a temperature of 500-900 ℃; and then drawing a carbon nanotube film with the width of 0.1-20 cm from the carbon nanotube array, and twisting the carbon nanotube film according to the twist of 100-15000 tpm to obtain the carbon nanotube fiber. According to the embodiment of the invention, the carbon nanotube fiber yarns are reasonably controlled by reasonably controlling the film-drawing width in the carbon nanotube array, the diameter of the conventional carbon nanotube array substrate is usually about 8 inches at present, the maximum width of the drawable film is 20cm, but the utilization rate of the carbon nanotube array is low, and only a few meters of film can be drawn out of a disc; the smaller the width of the drawn film is, the higher the utilization rate of the carbon nanotube array is, so that the carbon nanotube fiber bundle is prepared by using a doubling mode more frequently. In addition, the carbon nanotube fiber is twisted and spun by the twist of 100 to 15000tpm, under the optimal twist, the carbon nanotubes are tightly cohered, the carbon nanotubes do not seriously deform in the axial direction of the fiber, the mechanical property of the carbon nanotube fiber is excellent, and the carbon nanotube fiber is suitable for the next processing and weaving. When the twist is too large, the carbon nanotube fiber can form a spiral shape, the carbon nanotube is seriously deformed in the axial direction of the fiber due to excessive twisting, and when the fiber is stressed in the axial direction, the bearing capacity of the carbon nanotube along the axial direction of the fiber is reduced due to the deformation, so that the integral mechanical property of the carbon nanotube fiber is reduced. When the twist is too small, the carbon nanotube film is not completely twisted, and the carbon nanotube film is still in a film state in some places or the carbon nanotubes are not tightly cohered and loosened to form weak nodes, so that the carbon nanotube film is firstly broken when the fiber is stressed. In some embodiments, a carbon nanotube film having a width of 0.1 cm, 2 cm, 5cm, 8 cm, 10 cm, 15 cm, 18 cm, or 20cm is drawn from a carbon nanotube array and spun into a carbon nanotube fiber filament using a twist that may be 100tpm, 1000tpm, 5000tpm, 10000tpm, or 15000 tpm.
In some embodiments, 5 to 20 carbon nanotube fibers are combined to obtain a carbon nanotube fiber bundle, so that the obtained carbon nanotube fiber bundle not only effectively ensures the spinnability of the carbon nanotube fiber bundle, but also can rapidly reach a preset temperature through a small current, and has good temperature stability. The more the carbon nanotube fiber is combined, the larger the cross-sectional area of the fiber bundle is, the smaller the resistance per unit length is, and the larger the current required to reach a certain temperature is.
In some embodiments, a catalyst layer is deposited on a substrate, the substrate is placed in a chemical vapor deposition reaction furnace, protective gas is introduced, the temperature is raised to 500-900 ℃, carbon source gas is introduced, and the reaction is carried out for about 5-10 min, so that a carbon nanotube array which grows uniformly is generated on the substrate; then pulling out a carbon nanotube film with the width of 0.1-20 cm from the carbon nanotube array, and twisting the carbon nanotube film according to the twist of 100-15000 tpm to prepare the carbon nanotube fiber; and then doubling 5-20 carbon nanotube fibers to obtain the carbon nanotube fiber bundle.
In some embodiments, the substrate is provided with a plurality of detachable projections, and the detachable projections are used for providing a path guide for the carbon nanotube fiber bundle routing circuit diagram. The detachable bulges arranged on the substrate are used for arranging the carbon nano tube fiber bundles into a circuit diagram, and the carbon nano tube fiber bundles are wound on the bulges to realize the arrangement of the carbon nano tube fiber bundles into the circuit diagram. In some embodiments, the removable protrusions on the base plate may be rivets or the like.
In some embodiments, the step of arranging the carbon nanotube fiber bundles on the substrate according to a predetermined pattern includes: and orderly winding the detachable bulges by the carbon nano tube fiber bundles according to a preset circuit diagram, and laying to form the carbon nano tube fiber circuit diagram. According to the embodiment of the invention, the carbon nanotube fiber bundle is orderly wound by the detachable bulges larger than the substrate, so that carbon nanotube fiber circuit diagrams with various patterns, shapes and layers, namely heating circuit diagrams, can be formed on the substrate.
In some embodiments, the ends of the carbon nanotube fiber bundles are each connected to an electrode pad, through which they communicate with an external circuit. In the embodiment of the invention, two ends of the carbon nanotube fiber bundle are respectively connected with the electrode plate through conductive silver paste and the like and then are arranged on the horizontal outer side of the substrate, the electrode plate is communicated with an external circuit, and the carbon nanotube fiber circuit diagram is conducted through the electrode plate, so that electrothermal conversion is realized.
In some embodiments, the step of depositing a rubber compound material on the surface of the substrate on which the fiber circuit pattern is laid comprises: and casting the rubber mixed material on the surface of one side of the substrate on which the fiber circuit diagram is arranged, so that the fiber circuit diagram is fixedly sealed in the rubber mixed material, and the deposition thickness of the rubber mixed material is lower than the height of the detachable protrusion. In some embodiments, the substrate with the fiber circuit diagram is placed in a mold, and then a rubber mixed material is cast on one side surface of the substrate with the fiber circuit diagram, so that the fiber circuit diagram is coated in the rubber mixed material, and the deposition thickness of the rubber mixed material is lower than the height of the detachable protrusion, thereby facilitating the detachment of the subsequent protrusion and facilitating the application of the heating sheet.
In some embodiments, the substrate with the fiber circuit diagram is placed in a mold, then a rubber mixed material is cast on the surface of one side of the substrate with the fiber circuit diagram, the fiber circuit diagram is wrapped in the rubber mixed material, the deposition thickness of the rubber mixed material is lower than the height of the detachable protrusion, then the rubber material is cured at the temperature of 80-100 ℃, a crude product of the heating sheet is formed on the substrate, and the heating sheet formed by curing at the temperature is not only beneficial to demolding, but also is not completely cured and shaped, so that the subsequent further processing is facilitated.
In some embodiments, the mass ratio of the rubber to the curing agent in the rubber mixed material is (10-1): 1, in the rubber mixed material, the mass ratio of the rubber to the curing agent enables the rubber mixed material to have better curing characteristics, the rubber can be crosslinked and cured at the curing temperature of 80-100 ℃, and the carbon nanotube fiber circuit diagram is wrapped in the rubber to form a heating sheet; and the rubber still has high flexibility after being cured, so that the heating sheet has excellent plasticity, can be bent at will, and is flexible and convenient to apply.
In some embodiments, the rubber is selected from: at least one of nitrile rubber, silicone rubber, polyisoprene rubber and ethylene propylene diene rubber. In some embodiments, the curing agent is selected from: at least one of sulfur-containing compounds, metal oxides, peroxides, resins, quinones, and amines. The rubber and the curing agent adopted by the embodiment of the invention can form a rubber body with good toughness and strong weather resistance after being combined with each other, so that the prepared heating sheet has excellent bending flexibility and long service life. In one embodiment, the amine-based curing agent may be 1, 2-ethylenediamine, propylenediamine, diethylenetriamine, triethylenetetramine, amine adducts thereof, m-phenylenediamine, diaminodiphenylmethane, diaminodiphenylsulfone, or the like; the resin curing agent can be polyurethane, epoxy resin, acrylate, etc. In one embodiment, the sulfur compound-containing curing agent can be thiuram disulfide or polysulfide, dithiodimorpholine, tetrathiodimorpholine, polysulfide polymer, alkylphenol monosulfide, alkylphenol disulfide, and the like. In one embodiment, the metal oxide curing agent may be zinc oxide, magnesium oxide, lead monoxide, lead tetraoxide, or the like. In one embodiment, the peroxide curing agent can be benzoyl peroxide, t-butyl peroxybenzoate, di-t-butyl peroxide, dicumyl peroxide, and the like. In one embodiment, the quinone curing agent may be p-quinone dioxime, dibenzoyl p-quinone dioxime, poly-p-nitrosobenzene, or the like.
In some embodiments, after forming the heat generating sheet on the substrate, the method further includes: and dismantling the bulge on the substrate, removing the substrate, and then carrying out hot pressing treatment on the heating sheet to obtain the flexible heating sheet. According to the embodiment of the invention, the detachable bulge on the substrate is removed, the cured and molded heating sheet is taken down from the substrate, and then the flexible heating sheet with a smooth surface is obtained through further hot pressing treatment, and meanwhile, in the hot pressing treatment process, the gap left by the bulge on the heating sheet can be softened and filled with rubber materials under heating, so that the flexible heating sheet is more complete and is more beneficial to application. In addition, when the heating sheet is applied, the heating sheet can be fixed on an object to be applied through a gap left by the protrusion on the heating sheet.
In some embodiments, the protrusions on the substrate are removed, and the heat generating sheet is subjected to a hot pressing treatment at a temperature of 100 ℃ to 300 ℃ and a pressure of 5MPa to 20MPa after the substrate is removed. The hot pressing condition can enable the heating sheet to form a more flat, compact and stable flexible heating sheet after being softened.
In some embodiments, the preparation method of the flexible heating sheet comprises the following steps:
s10, depositing a catalyst layer on a substrate, placing the substrate in a chemical vapor deposition reaction furnace, introducing protective gas, heating to 500-900 ℃, introducing carbon source gas, and reacting for about 5-10 min to generate a uniformly-grown carbon nanotube array on the substrate; then pulling out a carbon nanotube film with the width of 0.1-20 cm from the carbon nanotube array, and twisting the carbon nanotube film according to the twist of 100-15000 tpm to prepare the carbon nanotube fiber; then, doubling 5-20 carbon nanotube fibers to obtain carbon nanotube fiber bundles;
s20, winding and arranging the carbon nanotube fiber bundles into a carbon nanotube fiber circuit diagram by winding detachable bulges on the substrate, respectively connecting two ends of the carbon nanotube fiber bundles with electrode plates, and communicating with an external circuit through the electrode plates to obtain the substrate with the fiber circuit diagram;
s30, mixing rubber and a curing agent in a mass ratio of (10-1): 1, casting the rubber mixed material on one side surface of the substrate on which the fiber circuit diagram is arranged, so that the fiber circuit diagram is fixedly sealed in the rubber mixed material, wherein the deposition thickness of the rubber mixed material is lower than the height of the detachable protrusion, and curing is carried out at the temperature of 80-100 ℃ to form a heating sheet on the substrate;
s40, dismantling the bulge on the substrate, removing the substrate, and carrying out hot pressing treatment on the heating sheet under the conditions that the temperature is 100-300 ℃ and the pressure is 5-20 MPa to obtain the flexible heating sheet.
Correspondingly, the embodiment of the invention also provides a flexible heating sheet, which is prepared by the method, the thickness of the flexible heating sheet is 1-3 mm, the flexible heating sheet is electrified with 0.1-0.6A current, and the temperature of the flexible heating sheet reaches 40-80 ℃ within 5 seconds.
The flexible heating sheet provided by the embodiment of the invention is prepared by any method, and comprises a heating circuit distributed by carbon nanotube fiber bundles and a rubber material wrapping the heating circuit, wherein two ends of the carbon nanotube fiber bundles are respectively connected with electrode plates and are communicated with an external circuit through an electric heating sheet, so that electric-heat conversion is realized. And (3) electrifying the flexible heating sheet with 0.1-0.6A of current, wherein the temperature of the flexible heating sheet reaches 40-80 ℃ within 5 seconds, the heating temperature is stable, the safety is high, and the heating is rapid. The flexible heating sheet provided by the embodiment of the invention has the advantages of high electric-heat conversion efficiency, uniform and stable heating, high flexibility, free bending, thin thickness of only 1-3 mm, light weight, strong practicability and convenient and flexible application.
In order to make the above implementation details and operations of the present invention clearly understood by those skilled in the art and to make the advanced performance of the flexible heat generating sheet and the manufacturing method thereof according to the embodiments of the present invention obviously manifest, the above technical solutions are exemplified by a plurality of embodiments below.
Example 1
A flexible heating sheet includes the steps of:
① depositing catalyst layer on the substrate, placing in a chemical vapor deposition reaction furnace and introducing protective gas, heating to 700 deg.C, introducing carbon source gas, reacting for about 5min to generate uniformly grown carbon nanotube array on the substrate, pulling out a carbon nanotube film with a width of 7.5cm from the carbon nanotube array, twisting the film with a twist meter to obtain carbon nanotube fiber yarn with a twist of 1300tpm, and combining 10 carbon nanotube fiber yarns into a bundle of carbon nanotube fiber bundle to obtain the carbon nanotube fiber bundle.
② obtaining a template, installing nails in the holes of the template, positioning the electrode sheet on the pad, winding the single carbon nanotube fiber bundle according to the circuit diagram, as shown in figure 1, and bonding the head and the tail with the electrode sheet.
③ placing the template wound with carbon nanotube fiber bundle in a mold, pouring silicone rubber and curing agent on the template, and performing heat curing at 80 deg.C to form a heating sheet on the substrate.
④ moving the template and the rivet, and hot pressing the heating sheet at 120 deg.C and 5MPa to obtain the flexible heating sheet.
Example 2
A flexible heating sheet includes the steps of:
① depositing catalyst layer on the substrate, placing in a chemical vapor deposition reaction furnace, introducing protective gas, heating to 700 deg.C, introducing carbon source gas, reacting for about 5min to generate uniformly grown carbon nanotube array on the substrate, drawing out a carbon nanotube film with a width of 7.5cm from the carbon nanotube array, twisting the film with a twist meter to obtain carbon nanotube fiber yarn with a twist of 1300tpm, and combining 5 carbon nanotube fiber yarns into a carbon nanotube fiber bundle to obtain the carbon nanotube fiber bundle.
② obtaining a template, setting nails in the holes of the template, arranging electrode sheets on the pads, winding two carbon nanotube fiber bundles according to the circuit diagram, and bonding the head and the tail with the electrode sheets as shown in figure 2.
③ placing the template wound with carbon nanotube fiber bundle in a mold, pouring silicone rubber and curing agent on the template, and performing heat curing at 80 deg.C to form a heating sheet on the substrate.
④ moving the template and the rivet, and hot pressing the heating sheet at 100 deg.C and 5MPa to obtain the flexible heating sheet.
Further, in order to verify the advancement of the heat-generating flexible sheet prepared by the embodiment of the present invention, the embodiment of the present invention was subjected to a performance test.
Test example 1
In this test example, after applying current to the heat generating sheets prepared in examples 1 and 2, the temperature of the heat generating sheets prepared in examples 1 and 2 was measured by using a thermal imager, and the measurement results are shown in table 1 below:
TABLE 1
According to the test structure, the flexible heating sheet prepared in the embodiments 1 and 2 of the invention has the advantages of high heating rate and high thermal conductivity, and the temperature can be raised to about 50 ℃ within 5 seconds.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention are intended to be included within the scope of the present invention.
Claims (10)
1. The preparation method of the flexible heating sheet is characterized by comprising the following steps:
the method comprises the steps of obtaining carbon nanotube fiber bundles and a substrate, and arranging the carbon nanotube fiber bundles on the substrate according to a preset circuit diagram to obtain the substrate with the fiber circuit diagram;
depositing a rubber mixed material on the surface of one side of the substrate on which the fiber circuit diagram is laid, so that the area of the fiber circuit diagram laid on the substrate except the end part of the carbon nano tube fiber bundle is fixedly sealed in the rubber mixed material, and forming a heating sheet on the substrate;
wherein the rubber mixed material comprises rubber and a curing agent.
2. The method for manufacturing a flexible heating sheet according to claim 1, wherein the substrate is provided with a plurality of detachable projections, and the detachable projections are used for providing a path guide for the carbon nanotube fiber bundle routing diagram.
3. The method for manufacturing a flexible heating sheet according to claim 2, wherein the step of arranging the carbon nanotube fiber bundles on the substrate according to a predetermined pattern comprises: orderly winding the detachable bulges by the carbon nano tube fiber bundles according to a preset circuit diagram, and laying to form a carbon nano tube fiber circuit diagram; and/or the presence of a gas in the gas,
the end parts of the carbon nano tube fiber bundles are connected with the electrode plates and are communicated with an external circuit through the electrode plates.
4. A method for preparing a flexible heating sheet according to any one of claims 2 to 3, wherein the step of depositing a rubber mixture material on the surface of the side of the substrate on which the fiber circuit pattern is laid comprises: casting the rubber mixed material on one side surface of the substrate on which the fiber circuit diagram is arranged, so that the fiber circuit diagram is fixedly sealed in the rubber mixed material, and the deposition thickness of the rubber mixed material is lower than the height of the detachable protrusion; and/or the presence of a gas in the gas,
the temperature of the curing treatment is 80-100 ℃.
5. The method for preparing the flexible heating sheet according to claim 4, wherein the mass ratio of the rubber to the curing agent in the rubber mixed material is (10-1): 1; and/or the presence of a gas in the gas,
the rubber is selected from: at least one of nitrile rubber, silicone rubber, polyisoprene rubber and ethylene propylene diene rubber; and/or the presence of a gas in the gas,
the curing agent is selected from: at least one of sulfur-containing compounds, metal oxides, peroxides, resins, quinones, and amines.
6. A method for preparing a flexible heating sheet according to any one of claims 1 to 3 or 5, wherein the step of obtaining carbon nanotube fiber bundles comprises:
obtaining a carbon nanotube array, pulling out a carbon nanotube film from the carbon nanotube array, and twisting the carbon nanotube film to obtain a carbon nanotube fiber;
and carrying out doubling treatment on the plurality of carbon nanotube fiber yarns to obtain the carbon nanotube fiber bundle.
7. The method for preparing a flexible heating sheet according to claim 6, wherein the carbon nanotube array is prepared by reacting for 5 to 10 minutes by a chemical vapor deposition method in a carbon source atmosphere at a temperature of 500 to 900 ℃; and/or the presence of a gas in the gas,
the step of pulling out the carbon nanotube film from the carbon nanotube array and then twisting the carbon nanotube film comprises: drawing a carbon nanotube film with the width of 0.1-20 cm from the carbon nanotube array, and twisting the carbon nanotube film according to the twist of 100-15000 tpm; and/or the presence of a gas in the gas,
the carbon nano tube fiber bundle is prepared by doubling 5-20 carbon nano tube fiber yarns.
8. The method for manufacturing a flexible heat generating sheet according to claim 7, further comprising, after forming the heat generating sheet on the substrate, the steps of: and dismantling the bulge on the substrate, removing the substrate, and then carrying out hot pressing treatment on the heating sheet to obtain the flexible heating sheet.
9. The method for producing a flexible heat generating sheet according to claim 8, wherein the conditions of the heat press treatment include: hot pressing treatment is carried out under the conditions that the temperature is 100-300 ℃ and the pressure is 5-20 MPa.
10. A flexible heating sheet is characterized in that the flexible heating sheet is prepared by the method according to any one of claims 1 to 9, the thickness of the flexible heating sheet is 1 mm to 3 mm, 0.1A to 0.6A of current is applied to the flexible heating sheet, and the temperature of the flexible heating sheet reaches 40 ℃ to 80 ℃ within 5 seconds.
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