CN105898907A - Graphene heating film and preparation method thereof - Google Patents
Graphene heating film and preparation method thereof Download PDFInfo
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- CN105898907A CN105898907A CN201610409456.2A CN201610409456A CN105898907A CN 105898907 A CN105898907 A CN 105898907A CN 201610409456 A CN201610409456 A CN 201610409456A CN 105898907 A CN105898907 A CN 105898907A
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 183
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 178
- 238000010438 heat treatment Methods 0.000 title claims abstract description 74
- 238000002360 preparation method Methods 0.000 title claims abstract description 39
- 229910052751 metal Inorganic materials 0.000 claims abstract description 25
- 239000002184 metal Substances 0.000 claims abstract description 25
- 239000000853 adhesive Substances 0.000 claims abstract description 5
- 230000001070 adhesive effect Effects 0.000 claims abstract description 5
- 238000000034 method Methods 0.000 claims description 45
- 239000011159 matrix material Substances 0.000 claims description 26
- 238000006056 electrooxidation reaction Methods 0.000 claims description 21
- 229920002799 BoPET Polymers 0.000 claims description 19
- 239000003292 glue Substances 0.000 claims description 19
- 238000005260 corrosion Methods 0.000 claims description 18
- 230000007797 corrosion Effects 0.000 claims description 18
- 238000006243 chemical reaction Methods 0.000 claims description 14
- 150000001336 alkenes Chemical class 0.000 claims description 11
- 239000004575 stone Substances 0.000 claims description 10
- 238000000151 deposition Methods 0.000 claims description 9
- 239000007792 gaseous phase Substances 0.000 claims description 9
- 239000000126 substance Substances 0.000 claims description 9
- 239000002253 acid Substances 0.000 claims description 7
- 229910052756 noble gas Inorganic materials 0.000 claims description 7
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 claims description 6
- 229920000049 Carbon (fiber) Polymers 0.000 claims description 6
- 239000004917 carbon fiber Substances 0.000 claims description 6
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 6
- 239000004814 polyurethane Substances 0.000 claims description 6
- 229920002635 polyurethane Polymers 0.000 claims description 6
- 238000007761 roller coating Methods 0.000 claims description 6
- 238000005507 spraying Methods 0.000 claims description 6
- 239000004793 Polystyrene Substances 0.000 claims description 5
- 229920002223 polystyrene Polymers 0.000 claims description 5
- 230000001680 brushing effect Effects 0.000 claims description 4
- 239000004593 Epoxy Substances 0.000 claims 1
- 239000011347 resin Substances 0.000 claims 1
- 229920005989 resin Polymers 0.000 claims 1
- 238000012546 transfer Methods 0.000 abstract description 22
- 239000000758 substrate Substances 0.000 abstract description 15
- WABPQHHGFIMREM-UHFFFAOYSA-N lead(0) Chemical compound [Pb] WABPQHHGFIMREM-UHFFFAOYSA-N 0.000 abstract 1
- 239000010408 film Substances 0.000 description 179
- 239000010410 layer Substances 0.000 description 98
- 239000000243 solution Substances 0.000 description 31
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 13
- 239000011889 copper foil Substances 0.000 description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 10
- 239000010949 copper Substances 0.000 description 9
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 8
- 230000005611 electricity Effects 0.000 description 7
- 239000000463 material Substances 0.000 description 6
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 5
- 239000005030 aluminium foil Substances 0.000 description 5
- ORTQZVOHEJQUHG-UHFFFAOYSA-L copper(II) chloride Chemical compound Cl[Cu]Cl ORTQZVOHEJQUHG-UHFFFAOYSA-L 0.000 description 5
- 239000003822 epoxy resin Substances 0.000 description 5
- 229910052734 helium Inorganic materials 0.000 description 5
- 239000001307 helium Substances 0.000 description 5
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 5
- 229910052754 neon Inorganic materials 0.000 description 5
- GKAOGPIIYCISHV-UHFFFAOYSA-N neon atom Chemical compound [Ne] GKAOGPIIYCISHV-UHFFFAOYSA-N 0.000 description 5
- 229920000647 polyepoxide Polymers 0.000 description 5
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 4
- 229910052799 carbon Inorganic materials 0.000 description 4
- 230000008021 deposition Effects 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 239000007789 gas Substances 0.000 description 4
- 229910002804 graphite Inorganic materials 0.000 description 4
- 239000010439 graphite Substances 0.000 description 4
- 238000009413 insulation Methods 0.000 description 4
- 230000035484 reaction time Effects 0.000 description 4
- 229910052709 silver Inorganic materials 0.000 description 4
- 239000004332 silver Substances 0.000 description 4
- 239000002002 slurry Substances 0.000 description 4
- 229910052802 copper Inorganic materials 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 230000003628 erosive effect Effects 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 239000010409 thin film Substances 0.000 description 3
- 229910000831 Steel Inorganic materials 0.000 description 2
- 238000010304 firing Methods 0.000 description 2
- -1 graphite Alkene Chemical class 0.000 description 2
- 239000012528 membrane Substances 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 229920000307 polymer substrate Polymers 0.000 description 2
- 239000002356 single layer Substances 0.000 description 2
- 239000010959 steel Substances 0.000 description 2
- JPVYNHNXODAKFH-UHFFFAOYSA-N Cu2+ Chemical compound [Cu+2] JPVYNHNXODAKFH-UHFFFAOYSA-N 0.000 description 1
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 1
- 239000005977 Ethylene Substances 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 238000004026 adhesive bonding Methods 0.000 description 1
- 239000002390 adhesive tape Substances 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 239000003610 charcoal Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000005660 chlorination reaction Methods 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 229910001431 copper ion Inorganic materials 0.000 description 1
- 229910000365 copper sulfate Inorganic materials 0.000 description 1
- XTVVROIMIGLXTD-UHFFFAOYSA-N copper(II) nitrate Chemical compound [Cu+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O XTVVROIMIGLXTD-UHFFFAOYSA-N 0.000 description 1
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 description 1
- 238000005034 decoration Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000005485 electric heating Methods 0.000 description 1
- 230000005518 electrochemistry Effects 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 229920006389 polyphenyl polymer Polymers 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 230000000087 stabilizing effect Effects 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
- H05B3/00—Ohmic-resistance heating
- H05B3/10—Heating elements characterised by the composition or nature of the materials or by the arrangement of the conductor
- H05B3/12—Heating elements characterised by the composition or nature of the materials or by the arrangement of the conductor characterised by the composition or nature of the conductive material
- H05B3/14—Heating elements characterised by the composition or nature of the materials or by the arrangement of the conductor characterised by the composition or nature of the conductive material the material being non-metallic
- H05B3/145—Carbon only, e.g. carbon black, graphite
-
- 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
- H05B3/18—Heating elements characterised by the composition or nature of the materials or by the arrangement of the conductor the conductor being embedded in an insulating material
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2204/00—Structure or properties of graphene
- C01B2204/04—Specific amount of layers or specific thickness
-
- 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
- H05B2203/00—Aspects relating to Ohmic resistive heating covered by group H05B3/00
- H05B2203/013—Heaters using resistive films or coatings
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
Landscapes
- Carbon And Carbon Compounds (AREA)
Abstract
The invention provides a graphene heating film and a preparation method thereof. The graphene heating film is characterized by comprising a first insulated waterproof layer, an electrode layer, a heating film layer and a second insulated waterproof layer, wherein the first insulated waterproof layer, the electrode layer, the heating film layer and the second insulated waterproof layer are pasted into an integral structure; and the heating film layer is a graphene film. The preparation method of the graphene heating film comprises the following steps: (1) fabricating the graphene film; (2) covering the second insulated waterproof layer with a bonding adhesive; (3) bonding the second insulated waterproof layer and the graphene film into a whole; (4) removing a metal substrate on the graphene film; (5) pasting the electrode layer on the graphene film; (6) pasting the first insulated waterproof layer on the electrode layer; and (7) connecting the electrode layer and a lead wire. According to the graphene heating film and the preparation method thereof provided by the invention, the heating efficiency is high; large-area transferring of the graphene film can be achieved; the transfer time is short; and the transfer rate is high.
Description
Technical field
The present invention relates to material with carbon element technical field, especially relate to a kind of Graphene heating film and preparation thereof
Method.
Background technology
Electric-heating technology has the remarkable advantages such as clean energy resource, thermal conversion efficiency is high, Pavement design is convenient,
It is widely used in fields such as modern architecture, heating engineering, decorations.For traditional electricity
The inefficient shortcoming of heating technique, develops low resistance, high-termal conductivity, the high-performance of high heat-resistant stability
Charcoal base exothermic material is just becoming the inexorable trend of future development.
Graphene (Graphene) be a kind of be the cancellated carbon of hexagon by monolayer carbon atomic arrangement
The thin-film material that matter is novel.Electronics in single-layer graphene and hole carrier mobility are expected in temperature
For lower up to silicon 100 times.Graphene is the material of the thinnest rigid in known materials,
The performance of these excellences makes it have huge using value at electronics or even heating art.From 2004
The physicist An Deliehaimu of year Univ Manchester UK and Constantine's Nuo Woxiao love are from fixed
Since using adhesive tape to separate graphene film in graphite, graphene film is with its distinctive character
Through being increasingly becoming one of the most attracting material of field of new.
The graphenic surface defect that traditional graphene preparation method prepares is more, and graphene sheet layer is easy
Fold, curling, thus affect the performance of Graphene, and the Graphene table obtained after reduction
Face is almost without oxide group, thus its surface is hydrophobicity so that it is at water and some are common organic molten
Agent is easily reunited thus settles.
At present, the method preparing Graphene heating film has a lot, but wants to prepare large scale, electricity
Excellent performance, free of contamination graphene film are the most highly difficult.How main difficult point is graphene film
Preferably transfer in target substrate, prepare complete, without breakage, process stabilizing, reliably graphite
Alkene heating film.
Publication No. is that (patent name is: a kind of Graphene is thin for the Chinese patent of CN 102807208 A
Film transfer method;Filing date: 2012.08.01;) disclose a kind of graphene film transfer method,
Comprise the following steps:
(1) graphene film is attached directly in polymer substrate, is fluid by polymer treatment
State is also coated on graphene film and is solidified by polymer, makes graphene film and polymer substrate
Form covalent bond;(2) substrate corrosion fallen or pass through mechanical external force by graphene film and substrate
Separate, graphene film is come out near the one side of growth substrate, as making functional device
Significant surface.This graphene film transfer method is compared to traditional method, simple to operation, and can
It is attached on substrate in the way of making graphene film with covalent bond, difficult drop-off, and can use
The fresh one side of graphene film is as the ingredient of functional device, it is possible to be effectively improved functional device
Effect, be suitable for useful industrially.But, this graphene film transfer method cannot realize Graphene
The large-area transfer of film.
Notification number is that (patent name is: a kind of large area stone for the Chinese patent of CN 102592973 A
The transfer method of ink alkene;Filing date: 2012.03.02;) disclose a kind of large-area graphene
Transfer method, comprises the following steps:
(1) to the etchant solution of the graphene film spray metal in metallic substrates or by Metal Substrate
The end and graphene film dip a small amount of corrosion of metal solution;(2) then by metallic substrates and graphite
Alkene thin film is put in deionized water and is soaked, and washes away the etchant solution of remnants;(3) by metallic substrates and stone
Ink alkene thin film is immersed in the water, and makes the side contacted with graphene film have certain thickness water, puts into cold
Freeze room and make water freeze over;(4) ice of the side contacted with graphene film is separated, obtain graphite
Alkene ice sheet;(5) Graphene ice sheet is placed in target substrate, after ice-out, is achieved that Graphene
Transfer.The transfer method of the large-area graphene that this invention provides, using ice is that carrier method is simple,
Save the gluing in existing method, dissolve the step that metal, removing glue etc. are numerous and diverse;Avoid existing method
The pollution that Graphene is caused by middle organic gel residual and dissolving metal liquid, is suitable to graphene film extensive
Application and production.But the method for this employing ice cube transfer graphene film, relative to using chemistry
For the method peeled off, there is transfer time long, the shortcoming that the rate of transform is low.
Therefore, it is necessary to research and development one can realize the large-area transfer of graphene film, and transfer time is short,
The Graphene heating film preparation method that the rate of transform is high.
Summary of the invention
It is an object of the invention to provide a kind of efficiency of heating surface high, large-area turn of graphene film can be realized
Move, and transfer time is short, Graphene heating film that the rate of transform is high and preparation method thereof.
A kind of Graphene heating film that the present invention provides, including the first insulating waterproof layer, electrode layer, sends out
Hotting mask layer and the second insulating waterproof layer, the first insulating waterproof layer, electrode layer, heating film layer and second are exhausted
Edge waterproof layer is pasted and is structure as a whole, and described heating film layer is graphene film.
Preferably, described graphene film includes carbon fiber and Graphene, and wherein carbon fiber mass ratio is
40%-70%, the mass ratio of Graphene is 5%-15%.
Preferably, the thickness of described graphene film is 30-50 μm.
Preferably, described first insulating waterproof layer and the second insulating waterproof layer all use PVC film, PE
Film or PET film.
Preferably, the thickness of described first insulating waterproof layer and the second insulating waterproof layer is
0.2-0.6μm。
Preferably, described electrode layer is the two strip electrode bars being pasted onto on heating film layer, described two electricity
Pole bar is used to connect power supply by temperature control system.
Preferably, described two strip electrode bars are Copper Foil or silver slurry bar.
Preferably, described first insulating waterproof layer, electrode layer, heating film layer and the second insulating waterproof layer
Bonding glue be one or more in polyurethane, polystyrene, epoxy resin, acrylate.
Preferably, the thickness of described bonding glue is 150-280 μm.
A kind of Graphene heating film preparation method that the present invention provides, comprises the following steps that:
1), the making of graphene film, metal base surface use chemical gaseous phase depositing process prepare stone
Ink alkene film;
2) method, using spraying, brushing or roller coating covers bonding glue on the second insulating waterproof layer;
3) the second insulating waterproof layer that, will be covered with bonding glue is bonded as one with graphene film;
4), the method for mechanical stripping or electrochemical corrosion is used to remove the metallic matrix on graphene film,
Make the graphene film with insulating waterproof layer;
5), adhesive electrode layer on the graphene film being coated with the first insulating waterproof layer made;
6), on electrode layer, the first insulating waterproof layer is pasted;
7), electrode layer is connected with wire, is prepared as Graphene heating film.
Preferably, step 1) in, temperature be 25 DEG C, in normal pressure, noble gas, gnotobasis
Growth 15-20h, preparation a layer thickness is the graphene film of 30-50 μ m thick.
Preferably, step 3) in, it is 50 DEG C in temperature, in the environment of pressure is 50-150MPa,
Effect 2-5h, the second insulating waterproof layer that will be covered with bonding glue is bonded as one with graphene film.
Preferably, step 4) in, use the method for electrochemical corrosion to remove the metal on graphene film
Matrix, the temperature of corrosion reaction is 30-70 DEG C, and the time of corrosion is 3-10h, and etchant solution is Cu
Acid solution.
Preferably, step 6) in, utilize press 80 DEG C, act on 3-5h under the pressure of 300MPa,
Realize on electrode layer, paste the first insulating waterproof layer.
Preferably, step 2), step 3) and step 5) in, bonding glue is polyurethane, polyphenyl
One or more in ethylene, epoxy resin, acrylate.
Compared with prior art, the Graphene heating film that the present invention provides has the advantage that
(1) using graphene film as heating film, have thermal stability good, the long life is long,
The advantage that firing rate is fast;
(2) using graphene film as heating film, uniformity is more preferable, performance is more stable;
(3) good heat-insulation effect.
Compared with prior art, the Graphene heating film preparation method that the present invention provides has following excellent
Point:
(1) the large-area transfer of graphene film can be realized;
(2) graphene film is short for transfer time, and the rate of transform is high;
(3) in the manufacturing process of graphene film, select the convenient corrosion of metallic matrix, make Graphene
Film is peeled off convenient with metallic matrix ground.
(4) whole Graphene heating film preparation process is simple.
Accompanying drawing explanation
In order to be illustrated more clearly that the specific embodiment of the invention or technical scheme of the prior art, under
The accompanying drawing used required in detailed description of the invention or description of the prior art will be briefly described by face,
It should be evident that the accompanying drawing in describing below is some embodiments of the present invention, general for this area
From the point of view of logical technical staff, on the premise of not paying creative work, it is also possible to obtain according to these accompanying drawings
Obtain other accompanying drawing.
The structural representation of the Graphene heating film that Fig. 1 provides for the present invention;
The flow chart of the Graphene heating film preparation method that Fig. 2 provides for the present invention.
Reference:
1-the first insulating waterproof layer;2-electrode layer;
3-heating film layer;4-the second insulating waterproof layer.
Detailed description of the invention
Below in conjunction with accompanying drawing, technical scheme is clearly and completely described, it is clear that
Described embodiment is a part of embodiment of the present invention rather than whole embodiments.Based on this
Embodiment in bright, those of ordinary skill in the art are obtained under not making creative work premise
Every other embodiment, broadly fall into the scope of protection of the invention.
In describing the invention, it should be noted that term " " center ", " on ", D score, " left ",
Orientation or the position relationship of the instruction such as " right ", " vertically ", " level ", " interior ", " outward " are based on attached
Orientation shown in figure or position relationship, be for only for ease of description the present invention and simplify describe rather than
Instruction or the hint device of indication or element must have specific orientation, with specific azimuth configuration and
Operation, is therefore not considered as limiting the invention.Additionally, term " first ", " second ",
" the 3rd " is only used for describing purpose, and it is not intended that indicate or hint relative importance.
In describing the invention, it should be noted that unless otherwise clearly defined and limited, art
Language " is installed ", " being connected ", " connection " should be interpreted broadly, and connects, also for example, it may be fixing
Can be to removably connect, or be integrally connected;Can be to be mechanically connected, it is also possible to be electrical connection;
Can be to be joined directly together, it is also possible to be indirectly connected to by intermediary, can be two element internals
Connection.For the ordinary skill in the art, can understand that above-mentioned term is at this with concrete condition
Concrete meaning in invention.
The structural representation of the Graphene heating film that Fig. 1 provides for the present invention;Fig. 2 is that the present invention carries
The flow chart of the Graphene heating film preparation method of confession.
As it is shown in figure 1, a kind of Graphene heating film that the present invention provides, including the first insulating waterproof layer
1, electrode layer 2, heating film layer 3 and the second insulating waterproof layer 4, the first insulating waterproof layer 1, electrode
Layer 2, heating film layer 3 and the second insulating waterproof layer 4 are pasted and are structure as a whole, described heating film layer 3
For graphene film.
Compared with prior art, the Graphene heating film that the present invention provides has the advantage that
(1) using graphene film as heating film, have thermal stability good, the long life is long,
The advantage that firing rate is fast;
(2) using graphene film as heating film, uniformity is more preferable, performance is more stable;
(3) good heat-insulation effect.
Described graphene film includes carbon fiber and Graphene, and wherein carbon fiber mass ratio is 40%-70%,
The mass ratio of Graphene is 5%-15%.
The thickness of described graphene film is 30-50 μm.
Described first insulating waterproof layer 1 and the second insulating waterproof layer 4 all use PVC film, PE film or
PET film.
The thickness of described first insulating waterproof layer 1 and the second insulating waterproof layer 4 is 0.2-0.6 μm.
Described electrode layer 2 is the two strip electrode bars being pasted onto on heating film layer 3, described two strip electrode bars
It is used to connect power supply by temperature control system.
Described two strip electrode bars are Copper Foil or silver slurry bar.
Described first insulating waterproof layer 1, electrode layer 2, heating film layer 3 and the second insulating waterproof layer 4
Bonding glue be one or more in polyurethane, polystyrene, epoxy resin, acrylate.
The thickness of described bonding glue is 150-280 μm.
As in figure 2 it is shown, a kind of Graphene heating film preparation method that the present invention provides, including following work
Skill step:
1), the making of graphene film, metal base surface use chemical gaseous phase depositing process prepare stone
Ink alkene film;
2) method, using spraying, brushing or roller coating covers bonding on the second insulating waterproof layer 4 and uses
Glue;
3) the second insulating waterproof layer 4 that, will be covered with bonding glue is bonded as one with graphene film;
4), the method for mechanical stripping or electrochemical corrosion is used to remove the metallic matrix on graphene film,
Make the graphene film with insulating waterproof layer;
5), adhesive electrode layer 2 on the graphene film being coated with the first insulating waterproof layer 1 made;
6), on electrode layer 2, the first insulating waterproof layer 1 is pasted;
7), electrode layer 2 is connected with wire, is prepared as Graphene heating film.
Compared with prior art, the Graphene heating film preparation method that the present invention provides has following excellent
Point:
(1) the large-area transfer of graphene film can be realized;
(2) graphene film is short for transfer time, and the rate of transform is high;
(3) in the manufacturing process of graphene film, select the convenient corrosion of metallic matrix, make Graphene
Film is peeled off convenient with metallic matrix ground.
(4) whole Graphene heating film preparation process is simple.
The Graphene heating film preparation method that the present invention provides, concrete technology step is as follows:
1), the making of graphene film, metal base surface use chemical gaseous phase depositing process prepare stone
Ink alkene film;
Select to use chemical gaseous phase depositing process at metal base surface (such as aluminium foil, Copper Foil or nickel foil)
Prepare a layer graphene film, temperature be 25 DEG C, normal pressure, noble gas (such as helium, neon etc.),
Growing 15-20h in gnotobasis, preparation a layer thickness is the graphene film of 30-50 μ m thick.
2) method, using spraying, brushing or roller coating covers bonding on the second insulating waterproof layer 4 and uses
Glue;
Select one or more in polyurethane, polystyrene, epoxy resin and acrylate as viscous
Knot glue, use spraying, brush or roller coating method the second insulating waterproof layer 4 (as PVC film,
PE film or PET film) upper preparation a layer thickness is the tack coat about 150-280 μm.
3) the second insulating waterproof layer 4 that, will be covered with bonding glue is bonded as one with graphene film;
PVC film, PE film or PET film with tack coat is covered and has the metal of Graphene in growth
On matrix surface, it is 50 DEG C in temperature, in the environment of pressure is 50-150MPa, acts on 2-5h,
The second insulating waterproof layer 4 that will be covered with tack coat is bonded as one with graphene film.
4), the method for mechanical stripping or electrochemical corrosion is used to remove the metallic matrix on graphene film,
Make the graphene film with insulating waterproof layer;
It is by mechanically pulling off or the method for electrochemical corrosion, removes the metallic matrix on graphene film,
It is prepared as with PVC film, PE film or the graphene film of PET film;
Wherein, the temperature of electrochemical corrosion reaction is 30-70 DEG C, and the time of corrosion is 3-10h, rotten
Erosion solution is the acid solution of Cu.The time of corrosion reaction is rotten with the thickness of metallic matrix and electrochemistry
Erosion reaction temperature is relevant, is as the criterion eroding metallic matrix completely.
Etchant solution can be with the aqueous solution of selective chlorination copper liquor, copper sulfate solution or copper nitrate.
As a example by the solution of copper chloride, etching condition is as follows: copper chloride solution is 180-210g/L;Hydrochloric acid
Solution is 40-55g/L, and solution temperature is 30-45 DEG C;Electric current density is 2.1-7.8A/dm2.Whole
Electrochemical corrosion course is, on the Copper Foil of anode, copper betatopic becomes copper ion, and tough cathode ion obtains electric
Son becomes the process of metallic copper.
When copper chloride solution be 180g/L, hydrochloric acid solution be 45g/L, solution temperature be 30 DEG C time, electricity
Current density is 3.5A/dm2。
When copper chloride solution be 195g/L, hydrochloric acid solution be 50g/L, solution temperature be 40 DEG C time, electricity
Current density is 5A/dm2。
When copper chloride solution be 210g/L, hydrochloric acid solution be 55g/L, solution temperature be 45 DEG C time, electricity
Current density is 7.8A/dm2。
5), adhesive electrode layer 2 on the graphene film being coated with the first insulating waterproof layer 1 made;
Copper Foil or silver slurry bar conduction that width is 1-2cm is pasted at the two ends of the graphene film of preparation
Electrode.
6), on electrode layer 2, the first insulating waterproof layer 1 is pasted;
The side layer overlay thickness being not covered with the first insulating waterproof layer 1 on electrode layer 2 is
The PVC film of 0.2-0.6 μm, PE film or PET film, and be placed on the steel plate that thickness is 2cm thickness,
Utilize press temperature be 80 DEG C, pressure for 300MPa in the environment of, act on 3-5h, complete stone
The stickup of ink alkene film opposite side insulation waterproof membrane.
7), electrode layer 2 is connected with wire, is prepared as Graphene heating film.
Electrode layer 2 is connected with wire, is prepared as temperature any adjustable stone in the range of 30-110 DEG C
Ink alkene heating film.
In order to be illustrated more clearly that the technical scheme of Graphene heating film preparation method that the present invention provides,
It is described in further detail below in conjunction with embodiment.
Embodiment 1
1), select to use chemical gaseous phase deposition at metal base surface (such as aluminium foil, Copper Foil or nickel foil)
Method prepares a layer graphene film, temperature be 25 DEG C, normal pressure, noble gas be (such as helium, neon
Gas etc.), gnotobasis grows 15h, preparation a layer thickness is the graphene film of 30 μ m thick;
2) one or more in polyurethane, polystyrene, epoxy resin and acrylate, are selected to make
For bonding glue, use spraying, brush or the method for roller coating at the second insulating waterproof layer 4 (such as PVC
Film, PE film or PET film) upper preparation a layer thickness is the tack coat about 150-280 μm;
3), PVC film, PE film or the PET film covering with tack coat there is Graphene in growth
On matrix surface, it is 50 DEG C in temperature, in the environment of pressure is 50Pa, acts on 5h, will be covered with
Second insulating waterproof layer 4 of tack coat is bonded as one with graphene film;
4), it is by mechanically pulling off or the method for electrochemical corrosion, removes the Metal Substrate on graphene film
Body, is prepared as with PVC film, PE film or the graphene film of PET film;Electrochemical corrosion reaction
Temperature is 30 DEG C, and the time of corrosion is 10h, and etchant solution is the acid solution of Cu.Corrosion reaction
Time relevant with the thickness of metallic matrix and electrochemical corrosion reaction temperature, to erode metal completely
Matrix is as the criterion.
5), preparation graphene film two ends paste on width be 1-2cm Copper Foil or silver slurry bar lead
Electricity electrode;
6) the side layer overlay thickness, being not covered with the first insulating waterproof layer 1 on electrode layer 2 is
The PVC film of 0.2-0.6 μm, PE film or PET film, and be placed on the steel plate that thickness is 2cm thickness,
Utilize press temperature be 80 DEG C, pressure for 300MPa in the environment of, act on 3-5h, complete stone
The stickup of ink alkene film opposite side insulation waterproof membrane;
7), electrode layer 2 is connected with wire, is prepared as surface temperature any in the range of 30-110 DEG C
Adjustable Graphene heating film.
Embodiment 2
Embodiment 2 the difference is that only with embodiment 1, step 1), step 3) and step 4)
Difference, other steps are with embodiment 1).
1), select to use chemical gaseous phase deposition at metal base surface (such as aluminium foil, Copper Foil or nickel foil)
Method prepares a layer graphene film, temperature be 25 DEG C, normal pressure, noble gas be (such as helium, neon
Gas etc.), gnotobasis grows 17h, preparation a layer thickness is the graphene film of 38 μ m thick;
3), PVC film, PE film or the PET film covering with tack coat there is Graphene in growth
On matrix surface, it is 90 DEG C in temperature, in the environment of pressure is 50Pa, acts on 3.2h, will cover
The second insulating waterproof layer 4 having tack coat is bonded as one with graphene film;
4), it is by mechanically pulling off or the method for electrochemical corrosion, removes the Metal Substrate on graphene film
Body, is prepared as with PVC film, PE film or the graphene film of PET film, electrochemical corrosion reaction
Temperature is 40 DEG C, and the time of corrosion is 8.3h, and etchant solution is the acid solution of Cu.Corrosion reaction
Time relevant with the thickness of metallic matrix and electrochemical corrosion reaction temperature, to erode metal completely
Matrix is as the criterion.
Embodiment 3
Embodiment 3 the difference is that only with embodiment 1, step 1), step 3) and step 4)
Difference, other steps are with embodiment 1).
1), select to use chemical gaseous phase deposition at metal base surface (such as aluminium foil, Copper Foil or nickel foil)
Method prepares a layer graphene film, temperature be 25 DEG C, normal pressure, noble gas be (such as helium, neon
Gas etc.), gnotobasis grows 19h, preparation a layer thickness is the graphene film of 46 μ m thick;
3), PVC film, PE film or the PET film covering with tack coat there is Graphene in growth
On matrix surface, it is 120 DEG C in temperature, in the environment of pressure is 50Pa, acts on 4.1h, will cover
The second insulating waterproof layer 4 being stamped tack coat is bonded as one with graphene film;
4), it is by mechanically pulling off or the method for electrochemical corrosion, removes the Metal Substrate on graphene film
Body, is prepared as with PVC film, PE film or the graphene film of PET film, electrochemical corrosion reaction
Temperature is 60 DEG C, and the time of corrosion is 4.8h, and etchant solution is the acid solution of Cu.Corrosion reaction
Time relevant with the thickness of metallic matrix and electrochemical corrosion reaction temperature, to erode metal completely
Matrix is as the criterion.
Embodiment 4
Embodiment 4 the difference is that only with embodiment 1, step 1), step 3) and step 4)
Difference, other steps are with embodiment 1).
1), select to use chemical gaseous phase deposition at metal base surface (such as aluminium foil, Copper Foil or nickel foil)
Method prepares a layer graphene film, temperature be 25 DEG C, normal pressure, noble gas be (such as helium, neon
Gas etc.), gnotobasis grows 20h, preparation a layer thickness is the graphene film of 50 μ m thick;
3), PVC film, PE film or the PET film covering with tack coat there is Graphene in growth
On matrix surface, it is 50 DEG C in temperature, in the environment of 1 pressure is 50Pa, acts on 2h, will cover
The second insulating waterproof layer 4 having tack coat is bonded as one with graphene film;
4), it is by mechanically pulling off or the method for electrochemical corrosion, removes the Metal Substrate on graphene film
Body, is prepared as with PVC film, PE film or the graphene film of PET film, electrochemical corrosion reaction
Temperature is 70 DEG C, and the time of corrosion is 3h, and etchant solution is the acid solution of Cu.Corrosion reaction
Time relevant with the thickness of metallic matrix and electrochemical corrosion reaction temperature, to erode metal completely
Matrix is as the criterion.
The present invention uses uniform temperature and certain pressure intensity to process the graphene film generated so that stone
Complete performance and the temperature homogeneity of ink alkene heating film can be guaranteed.
The present invention can prepare different size of Graphene heating film according to the size of press.
The present invention in temperature for for 50 DEG C, pressure be in the environment of 50-150MPa under, act on 2-5h,
The graphene film of growth is processed, the Graphene heating film uniformity obtained more preferably, performance more
Stable, the temperature on surface can control within 5 DEG C.
The graphene film of preparation, by certain temperature, certain pressure, is applied by the present invention for a long time
Uniform power, makes the more firm of whole graphene film and PVC film, PE film or PET film bonding,
Can control the integrity of whole Graphene heating film well, the Graphene that the present invention provides simultaneously is sent out
Hotting mask preparation method, directly transfers to graphene film on PVC film, PE film or PET film, simplifies
Whole Graphene heating film prepares preparation flow.
Last it is noted that various embodiments above is only in order to illustrate technical scheme, rather than
It is limited;Although the present invention being described in detail with reference to foregoing embodiments, this area
Those of ordinary skill is it is understood that the technical scheme described in foregoing embodiments still can be entered by it
Row amendment, or the most some or all of technical characteristic is carried out equivalent;And these amendment or
Person replaces, and does not make the essence of appropriate technical solution depart from the model of various embodiments of the present invention technical scheme
Enclose.
Claims (10)
1. a Graphene heating film, it is characterised in that include the first insulating waterproof layer, electrode layer,
Heating film layer and the second insulating waterproof layer, the first insulating waterproof layer, electrode layer, heating film layer and second
Insulating waterproof layer is pasted and is structure as a whole, and described heating film layer is graphene film.
Graphene heating film the most according to claim 1, it is characterised in that described Graphene
Film includes carbon fiber and Graphene, and wherein carbon fiber mass ratio is 40%-70%, the quality of Graphene
Ratio is 5%-15%.
Graphene heating film the most according to claim 1, it is characterised in that described first exhausted
Edge waterproof layer and the second insulating waterproof layer all use PVC film, PE film or PET film.
4. according to the Graphene heating film described in claim 1,2 or 3, it is characterised in that described
Electrode layer is the two strip electrode bars being pasted onto on heating film layer, and described two strip electrode bars are used to by temperature
Degree control system connects power supply.
5. a Graphene heating film preparation method, it is characterised in that comprise the following steps that:
1), the making of graphene film, metal base surface use chemical gaseous phase depositing process prepare stone
Ink alkene film;
2) method, using spraying, brushing or roller coating covers bonding glue on the second insulating waterproof layer;
3) the second insulating waterproof layer that, will be covered with bonding glue is bonded as one with graphene film;
4), the method for mechanical stripping or electrochemical corrosion is used to remove the metallic matrix on graphene film,
Make the graphene film with insulating waterproof layer;
5), adhesive electrode layer on the graphene film being coated with the first insulating waterproof layer made;
6), on electrode layer, the first insulating waterproof layer is pasted;
7), electrode layer is connected with wire, is prepared as Graphene heating film.
Graphene heating film preparation method the most according to claim 5, it is characterised in that institute
State step 1) in, it is 25 DEG C in temperature, normal pressure, noble gas, aseptic environment grows 15-20h,
Preparation a layer thickness is the graphene film of 30-50 μ m thick.
Graphene heating film preparation method the most according to claim 5, it is characterised in that institute
State step 3) in, it is 50 DEG C in temperature, in the environment of pressure is 50-150MPa, acts on 2-5h,
The second insulating waterproof layer that will be covered with bonding glue is bonded as one with graphene film.
Graphene heating film preparation method the most according to claim 5, it is characterised in that institute
State step 4) in, use the method for electrochemical corrosion to remove the metallic matrix on graphene film, corrosion
The temperature of reaction is 30-70 DEG C, and the time of corrosion is 3-10h, and etchant solution is the acid solution of Cu.
Graphene heating film preparation method the most according to claim 5, it is characterised in that institute
State step 6) in, utilize press 80 DEG C, pressure for 300MPa in the environment of, act on 3-5h,
Realize on electrode layer, paste the first insulating waterproof layer.
Graphene heating film preparation method the most according to claim 5, it is characterised in that institute
State step 2), step 3) and step 5) in, bonding glue is polyurethane, polystyrene, epoxy
One or more in resin, acrylate.
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