CN111565481A - Graphene and montmorillonite compounded flexible high-resistance high-temperature-resistant heating film and preparation method thereof - Google Patents

Graphene and montmorillonite compounded flexible high-resistance high-temperature-resistant heating film and preparation method thereof Download PDF

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CN111565481A
CN111565481A CN202010428811.7A CN202010428811A CN111565481A CN 111565481 A CN111565481 A CN 111565481A CN 202010428811 A CN202010428811 A CN 202010428811A CN 111565481 A CN111565481 A CN 111565481A
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graphene
montmorillonite
temperature
heating film
resistant
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王胜
郭玉芬
刘兆平
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Ningbo Graphene Innovation Center Co Ltd
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Ningbo Graphene Innovation Center Co Ltd
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    • HELECTRICITY
    • H05ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05BELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
    • H05B3/00Ohmic-resistance heating
    • H05B3/20Heating elements having extended surface area substantially in a two-dimensional plane, e.g. plate-heater
    • H05B3/34Heating elements having extended surface area substantially in a two-dimensional plane, e.g. plate-heater flexible, e.g. heating nets or webs
    • H05B3/36Heating elements having extended surface area substantially in a two-dimensional plane, e.g. plate-heater flexible, e.g. heating nets or webs heating conductor embedded in insulating material

Abstract

The application relates to a preparation method of a graphene and montmorillonite compounded flexible high-resistance high-temperature-resistant heating film, which comprises the following steps: s1: mixing the graphene conductive slurry and the expanded montmorillonite solution or slurry to obtain graphene and montmorillonite composite conductive slurry; and S2: and coating the graphene and montmorillonite composite conductive slurry on high-temperature-resistant cloth, drying, and annealing to obtain the graphene and montmorillonite composite flexible high-resistance high-temperature-resistant heating film. The application also relates to a graphene and montmorillonite compounded flexible high-resistance high-temperature-resistant heating film prepared by the method. The high temperature resistant heating film described herein has the characteristics of environmental protection, flexibility, high temperature resistance, and high electrical resistance.

Description

Graphene and montmorillonite compounded flexible high-resistance high-temperature-resistant heating film and preparation method thereof
Technical Field
The invention relates to the technical field of conductive paste and graphene, in particular to a flexible high-resistance high-temperature-resistant heating film compounded by graphene and montmorillonite and a preparation method thereof.
Background
At present, the electric heating films on the market comprise polyimide heating films, silicon rubber heating films, PET heating films, graphene heating films and the like. The first three of these heating films have low temperature resistance and can only be operated stably at temperatures below 200 ℃. The simple graphene heating film is usually used for far infrared heating, and the use temperature is below 100 ℃.
Chinese patent application publication No. CN110213845A reports a graphene high temperature resistant mica electric heating plate and a preparation method thereof, wherein a mica sheet and graphene are compounded by using organic silicon as a binder through a hot pressing method to form a sandwich structure of a graphene interlayer. Although the heating film prepared by the method has the advantages of high temperature resistance of 300 ℃, high heating efficiency and the like, the mica sheets in the heating film cause poor flexibility of the heating material, and the application of the heating material in certain occasions is limited. In addition, the use of organic silicon raises the environmental protection problem, and the sheet resistance of the single graphene heating film is lower, and the heating efficiency needs to be improved.
For this reason, there is a continuous need in the art to develop an environmentally friendly flexible high resistance high temperature resistant heating film and a method for preparing the same.
Disclosure of Invention
The application aims to provide a preparation method of an environment-friendly graphene and montmorillonite compounded flexible high-resistance high-temperature-resistant heating film, so that the technical problems in the prior art are solved. Specifically, the preparation method of the graphene-containing graphene and montmorillonite composite flexible high-resistance high-temperature-resistant heating film described herein includes mixing graphene conductive paste and expanded montmorillonite paste to obtain graphene and montmorillonite composite conductive paste, and coating the graphene and montmorillonite composite conductive paste on high-temperature-resistant cloth to obtain the flexible high-resistance high-temperature-resistant heating film.
It is another object of the present application to provide a flexible high-resistance high-temperature-resistant heating film prepared by the preparation method as described above.
In order to solve the above technical problem, the present application provides the following technical solutions.
In a first aspect, the present application provides a method for preparing a flexible high-resistance high-temperature-resistant heating film compounded by graphene and montmorillonite, which is characterized by comprising the following steps:
s1: mixing the graphene conductive slurry and the expanded montmorillonite solution or slurry to obtain graphene and montmorillonite composite conductive slurry; and
s2: and coating the graphene and montmorillonite composite conductive slurry on high-temperature-resistant cloth, drying, and annealing to obtain the graphene and montmorillonite composite flexible high-resistance high-temperature-resistant heating film.
In one embodiment of the first aspect, in step S1, the thickness of the graphene sheet in the graphene conductive paste is 1-3nm, and the sheet diameter is 1-10 um.
In one embodiment of the first aspect, in step S1, the graphene conductive paste has a sheet thickness of < 1.5nm and a sheet diameter of < 5 um.
In one embodiment of the first aspect, in step S1, the graphene conductive paste has a solid content of 2% to 6% by mass.
In one embodiment of the first aspect, in step S1, the swollen montmorillonite solution or slurry is prepared by: the swellable montmorillonite is dissolved in water and ultrasonically agitated for a first predetermined period of time.
In one embodiment of the first aspect, the power of the ultrasonic agitation is 100-500W; the first predetermined period of time is 0.5-5 h.
In one embodiment of the first aspect, the swellable montmorillonite is a sodium montmorillonite.
In one embodiment of the first aspect, the mass ratio of graphene to the swellable montmorillonite in the graphene conductive paste is 1: 0.5-1: 5.
in one embodiment of the first aspect, the high temperature resistant cloth is a high silica cloth or a glass fiber cloth.
In a second aspect, the present application provides a flexible high-resistance high-temperature-resistant heating film in which graphene and montmorillonite are compounded, which is prepared by the preparation method as described in the first aspect.
In one embodiment of the second aspect, the flexible high-resistance high-temperature-resistant heating film compounded by graphene and montmorillonite sequentially comprises a first graphene/montmorillonite composite film layer, a high-temperature-resistant cloth layer and a second graphene/montmorillonite composite film layer, and the high-temperature-resistant cloth layer is at least partially filled with the graphene and montmorillonite composite conductive paste.
In one embodiment of the second aspect, the first graphene/montmorillonite composite film layer or the second graphene/montmorillonite composite film layer is discontinuous.
Compared with the prior art, the beneficial effect of this application lies in:
(1) because no additional organic binder is needed, no organic solvent is used, and the used raw materials are all environment-friendly materials, the graphene and montmorillonite compounded flexible high-resistance high-temperature-resistant heating film and the preparation method thereof are all environment-friendly;
(2) the graphene and montmorillonite compounded flexible high-resistance high-temperature-resistant heating film does not use rigid materials, and the graphene film and the high-temperature-resistant cloth are both flexible, so that the finally obtained heating film is flexible;
(3) according to the graphene and montmorillonite compounded flexible high-resistance high-temperature-resistant heating film, the expanded montmorillonite is skillfully used as a binder and a heat-resistant resistance-increasing filler, so that the finally prepared heating film has excellent heat resistance and higher resistance, and can stably operate at the temperature of 400 ℃.
Drawings
The present application may be better understood by describing embodiments thereof in conjunction with the following drawings, in which:
fig. 1 shows a schematic view of a flexible high-resistance high-temperature-resistant heating film in which graphene and montmorillonite are compounded according to an embodiment of the present invention;
fig. 2 shows a scanning electron microscope picture of a surface of a first graphene/montmorillonite composite film of a flexible high-resistance high-temperature-resistant heating film composited by graphene and montmorillonite according to example 1 after annealing;
fig. 3 shows a scanning electron microscope picture of a surface of a second graphene/montmorillonite composite film of the graphene and montmorillonite compounded flexible high resistance high temperature resistant heating film according to example 1 after annealing;
fig. 4 shows a schematic diagram of a structure for testing a flexible heating film.
In the above drawings, reference numeral 100 denotes a first graphene/montmorillonite composite film layer, 200 denotes a high temperature-resistant cloth layer, 300 denotes a second graphene/montmorillonite composite film layer, 400 denotes the flexible heating film of fig. 1, 500 denotes a copper foil sheet as a heating film edge seal and a conductive connection of the heating film to a copper wire, and 600 denotes a copper wire.
Detailed Description
Unless otherwise defined, technical or scientific terms used herein in the specification and claims should have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. All numerical values recited herein as between the lowest value and the highest value are intended to mean all values between the lowest value and the highest value in increments of one unit when there is more than two units difference between the lowest value and the highest value.
In the following detailed description of the embodiments of the present invention, reference is made to the accompanying drawings, which are included to provide a further understanding of the invention, and in which is shown by way of illustration specific embodiments in which the invention may be practiced.
Definition of terms
Herein, the term "high temperature heating film" refers to an electrothermal film having an operating temperature of 300-450 ℃.
As used herein, the term "high resistance" refers to a square resistance of the heating film of 50 Ω/sq or more as measured by a four-probe.
As described above, the conventional electrical heating film generally operates at 200 ℃ or less, the graphene-based heating film generally operates at only 100 ℃, and the operating temperature of the graphene-based heating film can reach 300 ℃ by disposing mica sheets as insulating materials on both surfaces of the graphene film, but the mica sheets make the resulting heating film no longer flexible.
Therefore, the application aims to provide an environment-friendly graphene and montmorillonite compounded flexible high-resistance high-temperature-resistant heating film and a preparation method thereof. In one embodiment, the method for preparing the flexible high-resistance high-temperature-resistant cloth compounded by graphene and montmorillonite described herein comprises firstly compounding graphene sheets with inorganic montmorillonite having a lamellar structure to obtain graphene and montmorillonite compounded conductive slurry, and regulating and controlling the resistance of a graphene film through the insulating property of the montmorillonite. And then, taking high-temperature-resistant cloth (high-silica cloth or glass fiber cloth) as a substrate, coating the graphene and montmorillonite composite conductive slurry on the substrate, and obtaining the graphene composite heating film of the high-temperature-resistant substrate in one step under the condition of no binder.
In the embodiment, on one hand, montmorillonite is compounded with graphene, and the formed composite film is greatly reduced in conductivity and improved in heating resistance due to the obstruction of insulating montmorillonite. On the other hand, high-temperature-resistant high-silica cloth or glass fiber is used as a substrate, and in the coating process, the slurry partially permeates into the substrate, so that the interaction between the graphene composite membrane and the substrate is increased, and the graphene composite membrane and the substrate can be compounded without adding extra binder. The method has the advantages of simple process and environmental protection, and the prepared heating film has the advantages of high resistance and high temperature resistance, has certain flexibility and mechanical strength, and can realize 180-degree bending.
In a preferred embodiment, the preparation method of the graphene and montmorillonite compounded flexible high-resistance high-temperature-resistant heating film comprises the following steps:
(1) and (3) obtaining the dispersed graphene slurry with smaller size and sheet diameter by sanding the graphene conductive slurry with the solid content of 5-6%, wherein the solid content of the slurry is 2-4%.
(2) And (2) mixing the slurry obtained in the step (1) with montmorillonite powder or an ultrasonic montmorillonite solution under the stirring condition, mechanically stirring and mixing at a high speed, and then obtaining the graphene and montmorillonite composite conductive slurry in a sanding or emulsifying mode.
(3) And (3) coating the composite conductive slurry obtained in the step (2) on high-temperature-resistant cloth in a blade coating mode, drying at a certain temperature (80-100 ℃), and annealing in a muffle furnace at 350-450 ℃ to obtain the graphene composite montmorillonite heating film of the high-temperature-resistant flexible base cloth.
The total thickness of the obtained heating film is 50-300 um, the sheet resistance measured by four probes is 50-500 omega/sq, and the heating film is not broken after being bent for 500 times at 180 degrees.
In a preferred embodiment, the graphene paste may be a graphene conductive paste provided by ningbo ink science and technology ltd: the thickness of the lamella is 1-3nm, and the diameter of the lamella is 1-10 um. Preferably, the graphene slurry is sanded for 0.5-2h, the thickness of a sheet layer after sanding is less than 1.5nm, and the diameter of the sheet layer is less than 5 um.
In the heating film described herein, montmorillonite is the more critical component. Montmorillonite is a layered mineral composed of finely divided hydrous aluminosilicate, has a colloidal dispersion characteristic, and is usually produced as a mass or a soil-like aggregate. The montmorillonite can be seen as flaky crystal under an electron microscope, and the color is white gray, light blue or light red. When the temperature reaches 100-200 ℃, the montmorillonite gradually loses water. The dehydrated montmorillonite can also absorb water molecules or other polar molecules again. They can also swell and exceed several times their original volume when they absorb moisture. Most of domestic montmorillonite is calcium type montmorillonite. However, since it has a cation exchange structure, it can be modified with other cations such as sodium ion to obtain sodium type montmorillonite. In the present application, the montmorillonite is preferably sodium montmorillonite, mainly because sodium montmorillonite can continuously expand after absorbing water, and even can completely separate interlamination into a very thin single layer, thereby facilitating the intercalation of graphene into the interlamellar montmorillonite. And the interlayer spacing after the calcium type water absorption is increased to a certain value (2.14nm) and is not increased any more, so that the graphene is difficult to be accurately intercalated between the montmorillonite sheets, and the compounding of the graphene and the montmorillonite is not facilitated. In a preferred embodiment, the sodium montmorillonite is available from mitsubing technologies ltd, zhejiang, and has the product types: SD, high purity sodium montmorillonite.
In one embodiment, a montmorillonite solution or slurry mixed with the graphene conductive paste may be prepared by ultrasonic agitation. The power of the ultrasonic stirring is 100-500W. For example, the power of the ultrasonic agitation may be 100W, 120W, 150W, 180W, 200W, 250W, 300W, 350W, 400W, 450W, 500W, or a range or sub-range between any two of them. In one embodiment, the period of ultrasonic agitation is from 0.5 to 5 hours. For example, the period of ultrasonic agitation is 0.5h, 1h, 1.5h, 2h, 2.5h, 3h, 3.5h, 4h, 4.5h, 5h, or a range or subrange between any two of them.
In a preferred embodiment, the mass ratio of graphene to the swellable montmorillonite in the graphene conductive paste is 1: 0.5-1: 5.
in a preferred embodiment, the high temperature resistant cloth is a high silica cloth or a glass fiber cloth. In a preferred embodiment, the cloth thickness of the high temperature resistant cloth is 30-200um, preferably 30-100 um.
In a second aspect, the present application relates to a flexible high-resistance high-temperature-resistant heating film in which graphene and montmorillonite are compounded, which is prepared by the preparation method as described above. As shown in fig. 1, the flexible high-resistance high-temperature-resistant heating film compounded by graphene and montmorillonite described herein may sequentially include a first graphene/montmorillonite composite film layer 100, a high-temperature-resistant cloth layer 200, and a second graphene/montmorillonite composite film layer 300, wherein the high-temperature-resistant cloth layer 200 is at least partially filled with a graphene and montmorillonite composite conductive paste, which increases the adhesiveness between the graphene/montmorillonite composite film layer 100 and the base high-temperature-resistant cloth layer 200.
In a preferred embodiment, the first graphene/montmorillonite composite film layer 100 is uniformly continuous and the second graphene/montmorillonite composite film layer 300 is discontinuous. It will be understood by those skilled in the art that the terms "first" and "second" are used herein for the purpose of distinction only and are not particularly limited to the graphene/montmorillonite composite film layer. In a preferred embodiment, however, the first graphene/montmorillonite composite film layer is a composite film layer formed on the high-temperature-resistant cloth layer, and the second graphene/montmorillonite composite film layer is a composite film layer opposite to the first graphene/montmorillonite composite film layer and formed of graphene and montmorillonite composite conductive paste that has permeated through the high-temperature-resistant cloth.
The above-described preferred embodiments can be combined with each other to form new preferred embodiments of the present application, in keeping with the basic principles of the art.
Examples
The present application is further illustrated by the following examples, which are not intended to limit the scope of the invention. The experimental methods without specifying specific conditions in the following examples were selected according to the conventional methods and conditions, or according to the commercial instructions.
In the following examples, the scanning electron microscope pictures were obtained by means of a scanning electron microscope of the type Phenom Pro. In the following examples, montmorillonite is provided by Zhejiang san Ding science and technology Co., Ltd, and the product model is: SD, high purity sodium montmorillonite. The graphene conductive paste is provided by Ningbo ink science and technology Co.
Preparation examples
Example 1:
(1) mixing the graphene slurry with the solid content of 6% with solvent water, and sanding for 60min in a sanding mode (the conditions are that the rotating speed is 2000rpm, and the pump output flow is 40L/h), so that the graphene dispersion slurry with the solid content of 3% and the sheet thickness of less than 1.5nm and the sheet diameter of less than 5um is obtained.
(2) And (3) mixing 300g of the graphene slurry with 25g of montmorillonite powder under the stirring condition, mechanically stirring for 30min at the rotating speed of 3000rpm, then carrying out zirconium bead grinding for 30min, and carrying out vacuum defoaming to obtain the montmorillonite-graphene composite conductive slurry.
(3) And (3) coating the composite conductive slurry obtained in the step (2) on high-silica cloth in a blade coating mode, drying in an oven at 100 ℃, and then annealing in a muffle furnace at 450 ℃ to obtain the graphene composite montmorillonite heating film with the high-silica cloth substrate.
Fig. 2 shows a scanning electron microscope picture of the upper surface of the flexible high-resistance high-temperature-resistant heating film compounded of graphene and montmorillonite according to example 1 after annealing (i.e., the surface of the first graphene/montmorillonite composite film layer 100), and fig. 3 shows a scanning electron microscope picture of the lower surface of the flexible high-resistance high-temperature-resistant heating film compounded of graphene and montmorillonite according to example 1 after annealing (i.e., the surface of the second graphene/montmorillonite composite film layer 300). Referring to fig. 2, the upper surface of the heating film is flat and uniform, which indicates that the graphene and montmorillonite composite slurry has good dispersibility on the high temperature resistant cloth. Referring to fig. 3, there was a significant discontinuous film formed of the graphene/montmorillonite composite conductive paste on the lower surface of the heating film, indicating that the graphene/montmorillonite composite film was strongly bonded to the high silica cloth.
The total thickness of the heating film was measured to be about 90um, the sheet resistance was measured to be about 150 Ω/sq with four probes, and the film was not broken after being bent at 180 ° for 500 times.
Example 2:
(1) mixing the graphene slurry with the solid content of 6% with solvent water, and sanding for 60min in a sanding mode (the conditions are that the rotating speed is 2500rpm, and the pump output flow is 40L/h), so that the graphene dispersion slurry with the solid content of 3% and the sheet thickness of less than 1.5nm and the sheet diameter of less than 5um is obtained.
(2) And (3) mixing 300g of the graphene slurry with 27g of montmorillonite powder under the stirring condition, mechanically stirring for 30min at the rotating speed of 3000rpm, then carrying out zirconium bead grinding for 60min, and carrying out vacuum defoaming to obtain the montmorillonite-graphene composite conductive slurry.
(3) And (3) coating the composite conductive slurry obtained in the step (2) on glass fiber cloth in a blade coating mode, drying in an oven at 100 ℃, and then annealing in a muffle furnace at 450 ℃ to obtain the graphene composite montmorillonite heating film with the glass fiber cloth substrate.
The total thickness of the heating film was measured to be about 110um, the sheet resistance was measured to be about 105 Ω/sq with four probes, and the film was not broken after bending 500 times at 180 °.
Example 3:
(1) mixing the graphene slurry with the solid content of 6% with solvent water, and sanding for 120min in a sanding mode (the conditions are that the rotating speed is 2500rpm, and the pump output flow is 40L/h), so that the graphene dispersion slurry with the solid content of 3% and the sheet thickness of less than 1.5nm and the sheet diameter of less than 5um is obtained.
(2) And (3) mixing 300g of the graphene slurry with 45g of montmorillonite powder under the stirring condition, mechanically stirring for 30min at the rotating speed of 3000rpm, then carrying out zirconium bead grinding for 30min, and carrying out vacuum defoaming to obtain the montmorillonite-graphene composite conductive slurry.
(3) And (3) coating the composite conductive slurry obtained in the step (2) on high-silica cloth in a blade coating mode, drying in an oven at 80 ℃, and then annealing in a muffle furnace at 450 ℃ to obtain the graphene composite montmorillonite heating film with the high-silica cloth substrate.
The total thickness of the heating film was measured to be about 150um, the sheet resistance was measured to be about 450 Ω/sq with four probes, and the film was not broken after being bent 500 times at 180 °.
Example 4:
(1) 150g of graphene slurry with the solid content of 6 percent is mixed with montmorillonite solution (18g of montmorillonite +150g of deionized water) subjected to ultrasonic treatment (power: 300W, ultrasonic treatment time: 1h), the mixture is mechanically stirred for 30min at the rotating speed of 3000rpm and then is emulsified and dispersed for 30min at 5000rpm, and the composite conductive slurry of montmorillonite and graphene is obtained after vacuum defoaming.
(2) And (2) coating the composite conductive slurry obtained in the step (1) on high-silica cloth in a blade coating mode, drying in an oven at 100 ℃, and then annealing in a muffle furnace at 450 ℃ to obtain the graphene composite montmorillonite heating film with the high-silica cloth substrate.
The total thickness of the heating film was measured to be about 90um, the sheet resistance was measured to be about 150 Ω/sq with four probes, and the film was not broken after being bent at 180 ° for 500 times.
Comparative example 1:
taking the graphene slurry obtained in the step 1 of the embodiment 1, coating a film on a substrate high silica cloth in a blade coating mode, drying the substrate high silica cloth in an oven at 100 ℃, and then annealing the substrate high silica cloth in a muffle furnace at 450 ℃ to obtain a graphene heating film.
The total thickness of the graphene heating film is measured to be about 90um, the sheet resistance measured by a four-probe is about 500m omega/sq, and the graphene heating film is not broken after being bent for 500 times at 180 degrees.
Heating film test examples
The graphene heating films obtained in examples 1 to 4 and comparative example were cut to a thickness of 200 × 20x in terms of gauge (mm), and a heating film test structure as shown in FIG. 4 was fabricated, and then a voltage test was applied to copper wires 600 on both sides (DC voltage-stabilized power supply: output: DC 0-220V 0-10A). And (3) carrying out multipoint temperature measurement by using a thermocouple, keeping the temperature of the heating film at about 400 ℃ by adjusting voltage, running for 3 hours, repeatedly running for 3 times, and measuring the sheet resistance of the heating film by using the four probes again. The test results are shown in Table 1.
TABLE 1 results of the test of heating Properties of examples and comparative examples
Figure BDA0002499734790000091
In the embodiment, the heating temperature can reach 400 ℃ at rated voltage and below, the temperature difference is within +/-10 ℃, and the sheet resistance change is small after the operation is carried out for 3 times, which indicates that the heating film has good stability. In the comparative example, since the sheet resistance of the heating film is small, the temperature of the heating film still cannot reach more than 400 ℃ at the rated current of 10A, and thus the direct application to the heating film for high temperature is difficult.
The embodiments described above are intended to facilitate the understanding and appreciation of the application by those skilled in the art. It will be readily apparent to those skilled in the art that various modifications to these embodiments may be made, and the generic principles described herein may be applied to other embodiments without the use of the inventive faculty. Therefore, the present application is not limited to the embodiments herein, and those skilled in the art who have the benefit of this disclosure will appreciate that many modifications and variations are possible within the scope of the present application without departing from the scope and spirit of the present application.

Claims (10)

1. A preparation method of a flexible high-resistance high-temperature-resistant heating film compounded by graphene and montmorillonite is characterized by comprising the following steps:
s1: mixing the graphene conductive slurry and the expanded montmorillonite solution or slurry to obtain graphene and montmorillonite composite conductive slurry; and
s2: and coating the graphene and montmorillonite composite conductive slurry on high-temperature-resistant cloth, drying, and annealing to obtain the graphene and montmorillonite composite flexible high-resistance high-temperature-resistant heating film.
2. The preparation method according to claim 1, wherein in step S1, the thickness of the graphene sheet in the graphene conductive paste is 1-3nm, and the sheet diameter is 1-10 um.
3. The method according to claim 2, wherein in step S1, the graphene in the graphene conductive paste has a sheet thickness of < 1.5nm and a sheet diameter of < 5 um.
4. The preparation method according to claim 1, wherein in step S1, the graphene conductive paste has a solid content of 2% to 6% by mass.
5. The production method according to claim 1, wherein in step S1, the swollen montmorillonite solution or slurry is produced by: the swellable montmorillonite is dissolved in water and ultrasonically agitated for a first predetermined period of time.
6. The method according to claim 5, wherein the power of the ultrasonic agitation is 100-500W; the first preset time period is 0.5-5 h;
the swellable montmorillonite is sodium montmorillonite;
on the basis of mass, the mass ratio of the graphene in the graphene conductive paste to the expandable montmorillonite is 1: 0.5-1: 5.
7. the method according to any one of claims 1 to 6, wherein the high temperature-resistant cloth is a high silica cloth or a glass fiber cloth.
8. A flexible high-resistance high-temperature-resistant heating film in which graphene and montmorillonite are compounded, which is produced by the production method according to any one of claims 1 to 7.
9. The graphene and montmorillonite compounded flexible high-resistance high-temperature-resistant heating film according to claim 8, which comprises a first graphene/montmorillonite compounded film layer, a high-temperature-resistant cloth layer and a second graphene/montmorillonite compounded film layer in sequence, wherein the high-temperature-resistant cloth layer is at least partially filled with the graphene and montmorillonite compounded conductive paste.
10. The graphene and montmorillonite compounded flexible high resistance high temperature resistant heating film of claim 9, wherein the first graphene/montmorillonite composite film layer or the second graphene/montmorillonite composite film layer is discontinuous.
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Application publication date: 20200821