CN111807352B - Method for preparing graphene electrothermal film based on flexible porous fiber material - Google Patents

Method for preparing graphene electrothermal film based on flexible porous fiber material Download PDF

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CN111807352B
CN111807352B CN202010664776.9A CN202010664776A CN111807352B CN 111807352 B CN111807352 B CN 111807352B CN 202010664776 A CN202010664776 A CN 202010664776A CN 111807352 B CN111807352 B CN 111807352B
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graphene
porous fiber
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CN111807352A (en
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谭化兵
潘智军
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Anhui Aerospace and PMA Health Technology Co Ltd
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    • HELECTRICITY
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Abstract

The invention provides a method for preparing a graphene electrothermal film based on a flexible porous fiber material, which is characterized in that a laser-induced graphene method is adopted, an ultra-flexible self-supporting graphene conducting layer is directly prepared on the surface of the flexible porous material, then a PI flexible conducting electrode is introduced, and finally ultra-flexible packaging is carried out on the ultra-flexible self-supporting graphene conducting layer and a textile fabric, so that the ultra-flexible graphene electrothermal film is obtained.

Description

Method for preparing graphene electrothermal film based on flexible porous fiber material
Technical Field
The invention relates to a preparation method of an ultra-flexible graphene electrothermal film, in particular to a method for manufacturing the graphene electrothermal film by adopting a laser induction method, and belongs to the field of preparation methods of graphene electrothermal films.
Background
Graphene is a new strategic material, and in the industrial development process, the graphene electrothermal film is developed quickly, so that the production and manufacturing cost is low, and the production process is environment-friendly. Especially, graphite alkene electric heat membrane can launch can realize the far infrared of better resonance absorption effect with the human body, simultaneously still realize the face easily and generate heat, advantage such as fast generates heat, becomes the hot spot of the competitive research in current electric heat membrane field.
However, the current graphene electrothermal film is generally prepared by using graphene slurry or a Chemical Vapor Deposition (CVD) method, and the specific process is to attach a graphene conductive material to the surface of an insulating film, such as the surface of a PET or PI insulating film, and finally package the graphene conductive material by using PET or PI, so that the electrothermal film mainly has the following problems in the application process in the fields of physiotherapy protectors, heating clothes and the like: firstly, the whole electric heating film is hard, when in use, the electric heating film can generate sound due to the action of limbs and the like, and the experience effect is poor; secondly, because the electric heat membrane exists the restriction of packaging material totally, easy damage in the washing process influences normal use. Therefore, the graphene electrothermal film which is widely used in the field of health industry such as physical therapy protective equipment and clothes at present can not meet the requirements of high performance and high reliability due to self material reasons.
The statements in the background section are merely prior art as they are known to the inventors and do not, of course, represent prior art in the field.
Disclosure of Invention
The invention aims to solve one or more problems in the prior art, and provides a method for preparing a graphene electrothermal film based on a flexible porous fiber material, which comprises the following steps:
s1, utilizing laser induction to graphitize the part of the surface of the flexible porous fiber material, wherein the graphitized part forms a three-dimensional graphene layer;
s2: performing low-density compaction on the flexible porous fiber material with the graphitized surface obtained in the step S1 by using a roller press to obtain a graphene conductive film;
s3: compounding the graphene conductive film on the surface of the textile to form a textile/graphene conductive film compound;
s4: preparing a copper electrode flexible circuit board with a lead, and arranging a silver colloid electrode layer on the surface of a copper electrode which is to be in contact with a graphene layer on the graphene conductive film on the copper electrode flexible circuit board;
s5: attaching the copper electrode flexible circuit board with the silver colloid electrode layer after the treatment of S4 to the compound of the textile fabric/graphene conductive film obtained in S3, and attaching the silver colloid electrode layer and the graphene layer in an opposite position to form a structural member of the textile fabric/graphene conductive film/silver colloid electrode layer/copper electrode circuit board;
s6: and arranging the textile on the surface of the structural member of the textile/graphene conductive film/silver colloid electrode layer/copper electrode circuit board obtained in the step S5 to form a structure of the textile/graphene conductive film/silver colloid electrode layer/copper electrode circuit board/textile, namely the ultra-flexible graphene electrothermal film.
According to an aspect of the present invention, in the S1, the graphitized flexible porous fiber material has a bottom layer with a thickness of 2 ± 0.2 microns remained un-graphitized.
According to one aspect of the invention, the flexible porous fibrous material is selected from a wide variety of fibrous papers and fibrous cloths, preferably polyimide fibrous paper.
According to one aspect of the invention, the flexible porous fibrous material has a thickness of: 5-100 microns, preferably 20 microns.
According to one aspect of the present invention, the LIG laser source parameters are: the wavelength is 0.3-20 microns; power 2-20W, pulse time: 5-30 microseconds; the preferred conditions are: wavelength 10.6 microns, power 4.8W, pulse time 20 microseconds.
According to an aspect of the present invention, in the S2, a rolling pressure is 0.3 to 5Mpa, and a rolling speed is 0.5 to 5 m/min; preferably, the rolling pressure is 0.7MPa and the rolling speed is 2 m/min.
According to an aspect of the present invention, in the S3 and the S6, the textile is a knitted fabric, a fiber cloth, and a cotton cloth, preferably a low knitting density knitted fabric having excellent toughness.
According to an aspect of the present invention, in S3, the method for compounding the graphene conductive film on the surface of the textile includes: and hot-pressing and bonding the graphene conductive film and the textile together by using hot-melt adhesive as a bonding agent.
According to an aspect of the present invention, in S6, the step of disposing a textile on the surface of the structural member of the textile/graphene conductive film/silver colloid electrode layer/copper electrode circuit board obtained in S5 is performed by: hot-pressing and bonding the textile fabric and the structural member of the textile fabric/the graphene conductive film/the silver colloid electrode layer/the copper electrode circuit board together by using hot-melt adhesive as a bonding agent;
according to one aspect of the invention, the hot melt adhesives used in the two steps are EVA, TPU, PES or PA, preferably TPU.
According to one aspect of the present invention, in the S3, the thickness of the thermosol is 5 to 100 micrometers, preferably 20 micrometers thick.
According to one aspect of the present invention, in the S6, the thickness of the thermosol is 5 to 100 micrometers, preferably 20 micrometers thick.
According to an aspect of the present invention, in the S3, the hot pressing conditions are: the hot pressing temperature is 90-200 ℃, the hot pressing pressure is 0.3-2MPa, and the hot pressing time is 5-200S; the preferred conditions are: the hot pressing temperature is 150 ℃, the hot pressing pressure is 0.5MPa, and the hot pressing time is 30S.
According to one aspect of the invention, the parameters of the copper electrode flexible circuit board are as follows: and PI with the thickness of 20-50 microns is adopted to cover the copper film.
According to one aspect of the invention, a 20 micron thick PI copper film is used.
According to an aspect of the present invention, in S4, the method for providing the silver paste electrode layer on the surface of the copper electrode includes: and preparing the silver colloid electrode on the surface of the copper electrode by adopting a dispensing process.
According to one aspect of the inventionThe silver colloid adopts single-component silver colloid, and the volume resistivity is about 1-5 multiplied by 10-4Ω · cm, preferably 1X 10-4Ω·cm。
According to one aspect of the invention, the parameters for preparing the silver paste electrode are: curing at room temperature for 0.5-3 hours, preferably 2 hours.
The invention has the following effects:
according to the invention, a laser-induced graphene method is adopted, an ultra-flexible self-supporting graphene conducting layer is directly prepared on the surface of a flexible porous material, then a PI flexible conducting electrode is introduced, and finally ultra-flexible packaging is carried out on the PI flexible conducting electrode and a textile fabric, so that the ultra-flexible graphene electrothermal film is obtained. The obtained super-flexible graphene electrothermal film has the following characteristics:
1. the flexibility is good: the electric heating film is combined with the textile substrate, has super-soft characteristic and no abnormal sound, is particularly suitable for being applied to clothing products, and has the characteristic of no foreign body sensation to human bodies.
2. The performance is better: through washing test, the standard washing times can reach more than 50 times.
Drawings
FIG. 1 is a process flow diagram of a graphene electrothermal film;
FIG. 2 is a cross-sectional view of the graphene electrothermal film of the present invention;
101 is a porous fiber film (paper, cloth, cotton, etc.), 201 is a graphene film formed by an LIG process, 301 is a bottom layer packaging textile fabric, 302 is an upper layer packaging textile fabric, 401 is a copper electrode FPC (with terminal lead), and 402 is a copper electrode FPC; 501 external leads (wires), 601 and 602 adhesive layers, 701 silver paste electrodes, and 801 copper electrodes on the FPC.
Detailed Description
The present invention will be explained in more detail with reference to examples, which are provided only for illustrating the technical solutions of the present invention and are not intended to limit the spirit and scope of the present invention.
The embodiment of the invention provides a method for preparing a graphene electrothermal film based on a flexible porous fiber material. Referring to fig. 1, a-E are graphene electrothermal film process flows. A. Preparing a porous fiber membrane; B. preparing a graphene conducting layer by an LIG technology, and finishing a rolling compaction process; C. hot-pressing the graphene conductive layer to the surface of the textile fabric packaging layer; D. attaching a copper electrode FPC (including an external lead) to the surface of the graphene conductive film (including a silver adhesive dispensing process); E. and a complete graphene electrothermal film is packaged by adopting textile.
Several preferred embodiments of the method for preparing the graphene electrothermal film based on the flexible porous fiber material are detailed below in detail.
Example 1:
the method for preparing the graphene electrothermal film based on the flexible porous fiber material comprises the following steps:
1) a three-dimensional graphene conductive film pattern is prepared on the surface of polyimide porous fiber paper with the thickness of 10 microns by adopting an LIG (laser induced gelation) technology, and the bottom layer (about 2 microns thick) of the polyimide porous fiber paper with the surface covered with a graphene film is ensured not to be graphitized. The LIG uses a laser scanning device, the laser source is a carbon dioxide laser, the wavelength of the carbon dioxide laser is 10.6 microns, the power of the carbon dioxide laser is 4.8W, and the pulse time is 20 microseconds.
2) Carrying out rolling treatment on the graphene conductive film obtained in the step 1) by adopting a rolling machine, wherein the treatment conditions are as follows: the pressure is 0.6MPa, and the speed is 1.5 m/min;
3) with the graphene conductive film obtained in 2), adopt 20 microns thick TPU hot melt adhesive as the adhesive linkage, through the method of hot pressing, hot pressing to the looped fabric surface forms looped fabric/graphene composite structure, and the hot pressing condition is: the pressure is 0.6MPa, the temperature is 150 ℃, and the time is 30S;
4) preparing a silver colloid electrode on the surface of a copper electrode which is used for contacting with graphene on a prepared flexible circuit board (welded with an external lead wire) by a dispensing method, and pre-sticking the silver colloid electrode on the surface of a knitted fabric/graphene composite structure (pre-sticking TPU with the thickness of 10 microns on a copper-free electrode area of an FPC) to form a knitted fabric/graphene/silver electrode/copper electrode FPC composite structure;
5) adopt 20 microns thick TPU hot melt adhesive as the tie coat, carry out the pressfitting bonding with looped fabric/graphite alkene/silver electrode/copper electrode FPC integrated configuration and second floor encapsulation with looped fabric, the pressfitting condition is: the pressure is 0.6MPa, the temperature is 150 ℃, and the time is 30S, so that a knitted fabric/TPU/polyimide porous fiber paper/graphene/silver electrode/copper electrode FPC/TPU/knitted fabric structure, namely the super-flexible graphene electrothermal film is formed. The properties are shown in Table 1.
Example 2:
the method for preparing the graphene electrothermal film based on the flexible porous fiber material comprises the following steps:
1) a three-dimensional graphene conductive film pattern is prepared on the surface of polyimide porous fiber paper with the thickness of 10 microns by adopting an LIG (laser induced gelation) technology, and the bottom layer (about 2 microns thick) of the polyimide porous fiber paper with the surface covered with a graphene film is ensured not to be graphitized. The LIG uses a laser scanning device, the laser source is a carbon dioxide laser, the wavelength of the carbon dioxide laser is 10.6 microns, the power of the carbon dioxide laser is 4.8W, and the pulse time is 20 microseconds.
2) Carrying out rolling treatment on the graphene conductive film obtained in the step 1) by adopting a rolling machine, wherein the treatment conditions are as follows: the pressure is 0.6MPa, and the speed is 1.5 m/min;
3) in order to further improve the flexibility of the electric heating film, a laser cutting machine is adopted to cut the non-graphitized polyimide porous fiber paper on the surface of the graphene conductive film pattern;
4) with the graphene conductive film obtained in 3), adopt 20 microns thick TPU hot melt adhesive as the adhesive linkage, through the method of hot pressing, hot pressing to the looped fabric surface forms looped fabric/graphene composite structure, and the hot pressing condition is: the pressure is 0.6MPa, the temperature is 150 ℃, and the time is 30S;
5) preparing a silver colloid electrode on the surface of a copper electrode which is in contact with graphene on a prepared flexible circuit board (welded with an external lead) by a dispensing method, and pre-sticking the silver colloid electrode on the surface of a knitted fabric/graphene composite structure to form a knitted fabric/graphene/silver electrode/copper electrode FPC composite structure;
6) adopt 20 microns thick TPU hot melt adhesive as the tie coat, carry out the pressfitting bonding with looped fabric/graphite alkene/silver electrode/copper electrode FPC integrated configuration and second floor encapsulation with looped fabric, the pressfitting condition is: the pressure is 0.6MPa, the temperature is 150 ℃, and the time is 30S, so that a knitted fabric/TPU/polyimide porous fiber paper/graphene/silver electrode/copper electrode FPC/TPU/knitted fabric structure, namely the super-flexible graphene electrothermal film is formed. The properties are shown in Table 1.
Example 3:
the method for preparing the graphene electrothermal film based on the flexible porous fiber material comprises the following steps:
1) a three-dimensional graphene conductive film pattern is prepared on the surface of polyimide porous fiber paper with the thickness of 20 microns by adopting an LIG (laser induced gelation) technology, and the bottom layer (about 12 microns thick) of the polyimide porous fiber paper with the surface covered with a graphene film is ensured not to be graphitized. The LIG uses a laser scanning device, the laser source is a carbon dioxide laser, the wavelength of the carbon dioxide laser is 10.6 microns, the power of the carbon dioxide laser is 4.8W, and the pulse time is 20 microseconds.
2) Carrying out rolling treatment on the graphene conductive film obtained in the step 1) by adopting a rolling machine, wherein the treatment conditions are as follows: the pressure is 0.6MPa, and the speed is 1.5 m/min;
3) hot-pressing the graphene conductive film obtained in the step 2) to the surface of non-graphitized polyimide porous fiber paper by using a hot-pressing method through a TPU hot melt adhesive with the thickness of 20 microns to form a TPU/polyimide porous fiber paper/graphene composite structure, wherein the hot-pressing conditions are as follows: the pressure is 0.6MPa, the temperature is 150 ℃, and the time is 30S;
4) preparing a silver colloid electrode on the surface of a copper electrode which is in contact with graphene on a prepared flexible circuit board (welded with an external lead) by a dispensing method, and pre-sticking the silver colloid electrode on the surface of a TPU/polyimide porous fiber paper/graphene composite structure (pre-sticking 10 micron thick TPU on a FPC copper-free electrode area) to form a TPU/polyimide porous fiber paper/graphene/silver electrode/copper electrode FPC composite structure;
5) adopt 20 microns thick TPU hot melt adhesive as the tie coat, carry out the pressfitting bonding with TPU polyimide porous fiber paper/graphite alkene/silver electrode/copper electrode FPC integrated configuration and encapsulation with the looped fabric, the pressfitting condition is: the pressure is 0.6MPa, the temperature is 150 ℃, and the time is 30S, so that a TPU/polyimide porous fiber paper/graphene/silver electrode/copper electrode FPC/TPU/knitted fabric structure, namely the super-flexible graphene electrothermal film, is formed. The properties are shown in Table 1.
Example 4:
the method for preparing the graphene electrothermal film based on the flexible porous fiber material comprises the following steps:
1) a three-dimensional graphene conductive film pattern is prepared on the surface of polyimide porous fiber paper with the thickness of 20 microns by adopting an LIG (laser induced gelation) technology, and the bottom layer (about 12 microns thick) of the polyimide porous fiber paper with the surface covered with a graphene film is ensured not to be graphitized. The LIG uses a laser scanning device, the laser source is a carbon dioxide laser, the wavelength of the carbon dioxide laser is 10.6 microns, the power of the carbon dioxide laser is 4.8W, and the pulse time is 20 microseconds.
2) Carrying out rolling treatment on the graphene conductive film obtained in the step 1) by adopting a rolling machine, wherein the treatment conditions are as follows: the pressure is 0.6MPa, and the speed is 1.5 m/min;
3) in order to further improve the flexibility of the electric heating film, a laser cutting machine is adopted to cut the non-graphitized polyimide porous fiber paper on the surface of the graphene conductive film pattern;
4) hot-pressing the graphene conductive film obtained in step 3) to the surface of non-graphitized polyimide porous fiber paper by using a hot-pressing method through a TPU hot melt adhesive with the thickness of 20 microns to form a TPU/polyimide porous fiber paper/graphene composite structure, wherein the hot-pressing conditions are as follows: the pressure is 0.6MPa, the temperature is 150 ℃, and the time is 30S;
5) preparing a silver colloid electrode on the surface of a copper electrode which is in contact with graphene on a prepared flexible circuit board (welded with an external lead) by a dispensing method, and pre-sticking the silver colloid electrode on the surface of a TPU/polyimide porous fiber paper/graphene composite structure to form a TPU/polyimide porous fiber paper/graphene/silver electrode/copper electrode FPC composite structure;
6) adopt 20 microns thick TPU hot melt adhesive as the tie coat, carry out the pressfitting bonding with TPU polyimide porous fiber paper/graphite alkene/silver electrode/copper electrode FPC integrated configuration and encapsulation with the looped fabric, the pressfitting condition is: the pressure is 0.6MPa, the temperature is 150 ℃, and the time is 30S, so that a TPU/polyimide porous fiber paper/graphene/silver electrode/copper electrode FPC/TPU/knitted fabric structure, namely the super-flexible graphene electrothermal film, is formed. The properties are shown in Table 1.
Comparative example 1:
a double-sided PI-based graphene electrothermal film of the same size as in example 1. The properties are shown in Table 1.
The double-sided PI-based graphene electrothermal film has the following specific structure and materials:
1) the graphene electrothermal film structure is as follows: PI (lower layer)/copper electrode/graphene heating layer/PI (upper layer);
2) the graphene heating layer is an elastic conductive film made of Polyurethane (PU) composite graphene materials, wherein the mass percentage of polyurethane is 85%, and the mass percentage of graphene is 15%.
3) In the lower PI/copper electrode, the copper electrode is obtained by patterning a PI copper-clad film, the thickness of the PI is 13 microns, and the thickness of the copper electrode is 12 microns;
4) the upper layer PI is a PI covering film, and the total thickness is 20 micrometers.
The method comprises the following steps of putting the graphene electrothermal film into a pulsator washing machine for standard washing by adopting a standard washing test method, wherein the specific washing conditions are as follows:
1) the water injection amount is 25L;
2) 50mL of laundry detergent (blue moon);
3) each wash comprised a standard procedure of water flooding (3 times) -wash (1 time) -rinse (2 times) -dehydration (3 times); 4) the total wash time was 45 minutes.
And (4) judging the standard: the surface is not damaged after washing, and the resistance change rate is less than 10%.
Table 1:
serial number Sample (I) Can meet the standard washing times
1 Example 1 >50
2 Practice ofExample 2 >50
3 Example 3 >50
4 Example 4 >50
5 Comparative example 1 25
Finally, it should be noted that: although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that changes may be made in the embodiments and/or equivalents thereof without departing from the spirit and scope of the invention. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.

Claims (24)

1. A method for preparing a graphene electrothermal film based on a flexible porous fiber material is characterized by comprising the following steps:
s1, utilizing laser induction to graphitize the part of the surface of the flexible porous fiber material, wherein the graphitized part forms a three-dimensional graphene layer;
s2: performing low-density compaction on the flexible porous fiber material with the graphitized surface obtained in the step S1 by using a roller press to obtain a graphene conductive film;
s3: compounding the graphene conductive film on the surface of the textile to form a textile/graphene conductive film compound;
s4: preparing a copper electrode flexible circuit board with a lead, and arranging a silver colloid electrode layer on the surface of a copper electrode which is to be in contact with a graphene layer on the graphene conductive film on the copper electrode flexible circuit board;
s5: attaching the copper electrode flexible circuit board with the silver colloid electrode layer after the treatment of S4 to the compound of the textile fabric/graphene conductive film obtained in S3, and attaching the silver colloid electrode layer and the graphene layer in an opposite position to form a structural member of the textile fabric/graphene conductive film/silver colloid electrode layer/copper electrode circuit board;
s6: arranging a textile on the surface of the structural member of the textile/graphene conductive film/silver colloid electrode layer/copper electrode circuit board obtained in the step S5 to form a structure of the textile/graphene conductive film/silver colloid electrode layer/copper electrode circuit board/textile, namely the super-flexible graphene electrothermal film;
in the step S1, the flexible porous fiber material is polyimide fiber paper, and the graphitized flexible porous fiber material retains a bottom layer with a thickness of 2 ± 0.2 microns and is not graphitized; the LIG laser light source parameters are as follows: the wavelength is 0.3-20 microns; power 2-20W, pulse time: 5-30 microseconds.
2. The preparation method of the ultra-flexible graphene electrothermal film according to claim 1, wherein the thickness of the flexible porous fiber material is as follows: 5-100 microns.
3. The preparation method of the ultra-flexible graphene electrothermal film according to claim 1, wherein the thickness of the flexible porous fiber material is as follows: 20 microns.
4. The method for preparing the graphene electrothermal film based on the flexible porous fiber material as claimed in claim 1, wherein the LIG laser light source parameters are as follows: wavelength 10.6 microns, power 4.8W, pulse time 20 microseconds.
5. The method for preparing the graphene electrothermal film based on the flexible porous fiber material as claimed in claim 1, wherein in the S2, the rolling pressure is 0.3-5MPa, and the rolling speed is 0.5-5 m/min.
6. The method for preparing the graphene electrothermal film based on the flexible porous fiber material as claimed in claim 1, wherein in the step S2, the rolling pressure is 0.7MPa, and the rolling speed is 2 m/min.
7. The method for preparing the graphene electrothermal film based on the flexible porous fiber material according to claim 1, wherein in the S3 and the S6, the textile is knitted fabric, fiber cloth or cotton cloth.
8. The method for preparing the graphene electrothermal film based on the flexible porous fiber material as claimed in claim 1, wherein in the step S3, the method for compounding the graphene conductive film on the surface of the textile fabric is as follows: and hot-pressing and bonding the graphene conductive film and the textile together by using a hot melt adhesive as an adhesive.
9. The method for preparing the graphene electrothermal film based on the flexible porous fiber material according to claim 1, wherein in the step S6, the step of arranging the textile on the surface of the structural member of the textile/graphene conductive film/silver colloid electrode layer/copper electrode circuit board obtained in the step S5 is performed by: the hot melt adhesive is used as an adhesive to bond the textile fabric and the structural member of the textile fabric/graphene conductive film/silver adhesive electrode layer/copper electrode circuit board together in a hot-pressing manner.
10. The method for preparing the graphene electrothermal film based on the flexible porous fiber material according to claim 8 or 9, wherein the hot melt adhesive is EVA, TPU, PES or PA.
11. The method for preparing the graphene electrothermal film based on the flexible porous fiber material according to claim 10, wherein the hot melt adhesive is TPU.
12. The method for preparing the graphene electrothermal film based on the flexible porous fiber material as claimed in claim 8, wherein in the step S3, the thickness of the hot melt adhesive is 5-100 microns.
13. The method for preparing the graphene electrothermal film based on the flexible porous fiber material according to claim 12, wherein in the step S3, the thickness of the hot melt adhesive is 20 microns.
14. The method for preparing the graphene electrothermal film based on the flexible porous fiber material according to claim 9, wherein in the step S6, the thickness of the hot melt adhesive is 5-100 microns.
15. The method for preparing the graphene electrothermal film based on the flexible porous fiber material according to claim 14, wherein in the step S6, the thickness of the hot melt adhesive is 20 microns.
16. The method for preparing the graphene electrothermal film based on the flexible porous fiber material as claimed in claim 8, wherein in S3, the hot pressing conditions are as follows: the hot pressing temperature is 90-200 ℃, the hot pressing pressure is 0.3-2MPa, and the hot pressing time is 5-200S.
17. The method for preparing the graphene electrothermal film based on the flexible porous fiber material as claimed in claim 16, wherein in S3, the hot pressing conditions are as follows: the hot pressing temperature is 150 ℃, the hot pressing pressure is 0.5MPa, and the hot pressing time is 30S.
18. The method for preparing the graphene electrothermal film based on the flexible porous fiber material according to claim 1, wherein the parameters of the copper electrode flexible circuit board are as follows: and PI with the thickness of 20-50 microns is adopted to cover the copper film.
19. The method for preparing the graphene electrothermal film based on the flexible porous fiber material according to claim 18, wherein the parameters of the copper electrode flexible circuit board are as follows: the copper film was coated with PI 20 microns thick.
20. The method for preparing the graphene electrothermal film based on the flexible porous fiber material according to claim 1, wherein in the step S4, the method for arranging the silver colloid electrode layer on the surface of the copper electrode comprises the following steps: and preparing the silver colloid electrode on the surface of the copper electrode by adopting a dispensing process.
21. The method for preparing the graphene electrothermal film based on the flexible porous fiber material as claimed in claim 20, wherein the silver colloid is a single-component silver colloid with a volume resistivity of 1-5 x 10-4Ω·cm。
22. The method for preparing the graphene electrothermal film based on the flexible porous fiber material as claimed in claim 21, wherein the volume resistivity of the silver colloid is 1 x 10-4Ω·cm。
23. The method for preparing the graphene electrothermal film based on the flexible porous fiber material as claimed in claim 20, wherein parameters for preparing the silver colloid electrode are as follows: curing at room temperature for 0.5-3 hr.
24. The method for preparing the graphene electrothermal film based on the flexible porous fiber material as claimed in claim 23, wherein the curing time is 2 hours.
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CN111186833A (en) * 2020-03-10 2020-05-22 吉林大学 Porous graphene film prepared by laser processing method, preparation method and application thereof
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