CN105898907A - Graphene heating film and preparation method thereof - Google Patents

Graphene heating film and preparation method thereof Download PDF

Info

Publication number
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
Authority
CN
China
Prior art keywords
film
graphene
layer
waterproof layer
heating film
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN201610409456.2A
Other languages
Chinese (zh)
Inventor
向联合
马磊
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Hangzhou Papabear Technology Co Ltd
Original Assignee
Hangzhou Papabear Technology Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Hangzhou Papabear Technology Co Ltd filed Critical Hangzhou Papabear Technology Co Ltd
Priority to CN201610409456.2A priority Critical patent/CN105898907A/en
Publication of CN105898907A publication Critical patent/CN105898907A/en
Pending legal-status Critical Current

Links

Classifications

    • 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
    • H05B3/10Heating elements characterised by the composition or nature of the materials or by the arrangement of the conductor
    • H05B3/12Heating 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
    • H05B3/14Heating 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
    • H05B3/145Carbon only, e.g. carbon black, graphite
    • 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
    • H05B3/10Heating elements characterised by the composition or nature of the materials or by the arrangement of the conductor
    • H05B3/18Heating 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
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B2204/00Structure or properties of graphene
    • C01B2204/04Specific amount of layers or specific thickness
    • HELECTRICITY
    • H05ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05BELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
    • H05B2203/00Aspects relating to Ohmic resistive heating covered by group H05B3/00
    • H05B2203/013Heaters using resistive films or coatings
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00Technologies relating to chemical industry
    • Y02P20/10Process 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

A kind of Graphene heating film and preparation method thereof
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.
CN201610409456.2A 2016-06-12 2016-06-12 Graphene heating film and preparation method thereof Pending CN105898907A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201610409456.2A CN105898907A (en) 2016-06-12 2016-06-12 Graphene heating film and preparation method thereof

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201610409456.2A CN105898907A (en) 2016-06-12 2016-06-12 Graphene heating film and preparation method thereof

Publications (1)

Publication Number Publication Date
CN105898907A true CN105898907A (en) 2016-08-24

Family

ID=56729203

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201610409456.2A Pending CN105898907A (en) 2016-06-12 2016-06-12 Graphene heating film and preparation method thereof

Country Status (1)

Country Link
CN (1) CN105898907A (en)

Cited By (22)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106304435A (en) * 2016-11-07 2017-01-04 泉州信和石墨烯研究院有限公司 A kind of waterproof Electric radiant Heating Film based on Graphene and production method thereof
CN106332329A (en) * 2016-10-21 2017-01-11 陕西长奇节能环保科技有限公司 Manufacturing method for mobile power infrared ray cushion
CN106793198A (en) * 2017-01-05 2017-05-31 梁宇 A kind of electric heating tape based on Graphene technology
CN106941736A (en) * 2017-03-20 2017-07-11 青岛华高墨烯科技股份有限公司 A kind of graphene electric heating film and preparation method thereof
CN107197545A (en) * 2017-06-20 2017-09-22 广西大学 Nano-cellulose graphene complex electrocaloric film and its green preparation process
CN107257589A (en) * 2017-04-24 2017-10-17 颜宏志 A kind of electric-heating thin film material and preparation method thereof
CN107635296A (en) * 2017-09-13 2018-01-26 合肥微晶材料科技有限公司 A kind of graphene nano silver wire composite and flexible heating membrane module
CN108248120A (en) * 2017-12-29 2018-07-06 无锡格菲电子薄膜科技有限公司 Graphene composite heating film
CN108337750A (en) * 2018-01-26 2018-07-27 上海华烯新材料科技有限公司 A kind of graphene heating film
CN108684091A (en) * 2018-07-31 2018-10-19 唐山建华科技发展有限责任公司 Graphene heating film and preparation method thereof
CN108738176A (en) * 2017-04-25 2018-11-02 青岛市琴岛电器有限公司 Graphene automobile heating cushion
CN108770096A (en) * 2018-08-20 2018-11-06 深圳市同益高新电子科技有限公司 A kind of preparation process of heating film
CN108903560A (en) * 2018-06-27 2018-11-30 四川省安德盖姆石墨烯科技有限公司 A kind of preparation method of graphene far infrared heating carpet
CN109041293A (en) * 2018-08-20 2018-12-18 深圳市同益高新电子科技有限公司 A kind of preparation method and application of electric heating film
CN109010967A (en) * 2018-07-10 2018-12-18 唐山德善中医药科技发展有限公司 A kind of suction cup
CN109156914A (en) * 2018-09-06 2019-01-08 崔淮路 A kind of warming interlayer housing with heating function
CN109774292A (en) * 2019-03-19 2019-05-21 中金态和(武汉)石墨烯研究院有限公司 A kind of preparation method of graphene composite heating film
CN109878165A (en) * 2019-03-01 2019-06-14 中金态和(武汉)石墨烯研究院有限公司 A kind of graphene composite heating film and its graphene composite heating film group
CN109927324A (en) * 2019-03-01 2019-06-25 中金态和(武汉)石墨烯研究院有限公司 A kind of three-layer co-extruded preparation method out of graphene composite heating film
CN110312333A (en) * 2019-07-25 2019-10-08 北京巡天探索科学研究院 Graphene intelligent chip
CN112999200A (en) * 2021-03-03 2021-06-22 张铿 Transdermal drug delivery layer
CN115209581A (en) * 2021-04-13 2022-10-18 深圳市为什新材料科技有限公司 Rigid heating film of electronic product and preparation method thereof

Citations (14)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102592973A (en) * 2012-03-02 2012-07-18 山东师范大学 Transfer method of large area graphene
CN102719877A (en) * 2011-06-09 2012-10-10 中国科学院金属研究所 Low-cost lossless transfer method of graphene
US20120267041A1 (en) * 2011-04-22 2012-10-25 Samsung Electronics Co., Ltd. Method of forming multi-layer graphene
CN102795619A (en) * 2012-09-04 2012-11-28 南开大学 Graphene thin film transferring method based on physical adsorption
CN102807208A (en) * 2012-08-01 2012-12-05 许子寒 Method for transferring graphene films
CN102883486A (en) * 2012-09-28 2013-01-16 江苏物联网研究发展中心 Graphene based transparent electric heating film and production method thereof
CN202799224U (en) * 2012-09-28 2013-03-13 江苏物联网研究发展中心 Transparent electric heating film based on graphene
CN103134100A (en) * 2011-11-25 2013-06-05 滕繁 Ultra-thin electrothermal film heating device for wall body and manufacture method thereof
US20140021195A1 (en) * 2010-02-12 2014-01-23 Research & Business Foundation Sungkyunkwan University Flexible transparent heating element using graphene and method for manufacturing the same
CN105082655A (en) * 2015-09-07 2015-11-25 杭州白熊科技有限公司 Novel carbon fiber heating membrane and preparation method and system thereof
CN105208692A (en) * 2015-10-10 2015-12-30 苏州聚宜工坊信息科技有限公司 Flexible heating film assembly and preparing method thereof
CN105304860A (en) * 2014-05-28 2016-02-03 福建省辉锐材料科技有限公司 Method for preparing graphene substrate electrode and battery and super capacitor
CN105506812A (en) * 2015-12-31 2016-04-20 白德旭 Graphene smart clothes
CN205902105U (en) * 2016-06-12 2017-01-18 杭州白熊科技有限公司 Graphite alkene heating film

Patent Citations (14)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20140021195A1 (en) * 2010-02-12 2014-01-23 Research & Business Foundation Sungkyunkwan University Flexible transparent heating element using graphene and method for manufacturing the same
US20120267041A1 (en) * 2011-04-22 2012-10-25 Samsung Electronics Co., Ltd. Method of forming multi-layer graphene
CN102719877A (en) * 2011-06-09 2012-10-10 中国科学院金属研究所 Low-cost lossless transfer method of graphene
CN103134100A (en) * 2011-11-25 2013-06-05 滕繁 Ultra-thin electrothermal film heating device for wall body and manufacture method thereof
CN102592973A (en) * 2012-03-02 2012-07-18 山东师范大学 Transfer method of large area graphene
CN102807208A (en) * 2012-08-01 2012-12-05 许子寒 Method for transferring graphene films
CN102795619A (en) * 2012-09-04 2012-11-28 南开大学 Graphene thin film transferring method based on physical adsorption
CN202799224U (en) * 2012-09-28 2013-03-13 江苏物联网研究发展中心 Transparent electric heating film based on graphene
CN102883486A (en) * 2012-09-28 2013-01-16 江苏物联网研究发展中心 Graphene based transparent electric heating film and production method thereof
CN105304860A (en) * 2014-05-28 2016-02-03 福建省辉锐材料科技有限公司 Method for preparing graphene substrate electrode and battery and super capacitor
CN105082655A (en) * 2015-09-07 2015-11-25 杭州白熊科技有限公司 Novel carbon fiber heating membrane and preparation method and system thereof
CN105208692A (en) * 2015-10-10 2015-12-30 苏州聚宜工坊信息科技有限公司 Flexible heating film assembly and preparing method thereof
CN105506812A (en) * 2015-12-31 2016-04-20 白德旭 Graphene smart clothes
CN205902105U (en) * 2016-06-12 2017-01-18 杭州白熊科技有限公司 Graphite alkene heating film

Cited By (27)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106332329A (en) * 2016-10-21 2017-01-11 陕西长奇节能环保科技有限公司 Manufacturing method for mobile power infrared ray cushion
CN106304435A (en) * 2016-11-07 2017-01-04 泉州信和石墨烯研究院有限公司 A kind of waterproof Electric radiant Heating Film based on Graphene and production method thereof
CN106304435B (en) * 2016-11-07 2019-03-26 泉州信和石墨烯研究院有限公司 A kind of waterproof Electric radiant Heating Film and its production method based on graphene
CN106793198A (en) * 2017-01-05 2017-05-31 梁宇 A kind of electric heating tape based on Graphene technology
CN106941736A (en) * 2017-03-20 2017-07-11 青岛华高墨烯科技股份有限公司 A kind of graphene electric heating film and preparation method thereof
CN107257589A (en) * 2017-04-24 2017-10-17 颜宏志 A kind of electric-heating thin film material and preparation method thereof
CN108738176A (en) * 2017-04-25 2018-11-02 青岛市琴岛电器有限公司 Graphene automobile heating cushion
CN107197545A (en) * 2017-06-20 2017-09-22 广西大学 Nano-cellulose graphene complex electrocaloric film and its green preparation process
CN107635296A (en) * 2017-09-13 2018-01-26 合肥微晶材料科技有限公司 A kind of graphene nano silver wire composite and flexible heating membrane module
CN107635296B (en) * 2017-09-13 2020-11-06 合肥微晶材料科技有限公司 Compound flexible heating film subassembly of graphite alkene silver nanometer line
CN108248120A (en) * 2017-12-29 2018-07-06 无锡格菲电子薄膜科技有限公司 Graphene composite heating film
CN108337750A (en) * 2018-01-26 2018-07-27 上海华烯新材料科技有限公司 A kind of graphene heating film
CN108903560A (en) * 2018-06-27 2018-11-30 四川省安德盖姆石墨烯科技有限公司 A kind of preparation method of graphene far infrared heating carpet
CN109010967A (en) * 2018-07-10 2018-12-18 唐山德善中医药科技发展有限公司 A kind of suction cup
CN108684091A (en) * 2018-07-31 2018-10-19 唐山建华科技发展有限责任公司 Graphene heating film and preparation method thereof
CN108684091B (en) * 2018-07-31 2024-05-10 黑龙江碳谷工贸有限公司 Graphene heating film and preparation method thereof
CN108770096A (en) * 2018-08-20 2018-11-06 深圳市同益高新电子科技有限公司 A kind of preparation process of heating film
CN109041293A (en) * 2018-08-20 2018-12-18 深圳市同益高新电子科技有限公司 A kind of preparation method and application of electric heating film
CN109156914B (en) * 2018-09-06 2021-05-04 安徽希飞科技有限公司 Warm-keeping interlayer coat with heating function
CN109156914A (en) * 2018-09-06 2019-01-08 崔淮路 A kind of warming interlayer housing with heating function
CN109927324A (en) * 2019-03-01 2019-06-25 中金态和(武汉)石墨烯研究院有限公司 A kind of three-layer co-extruded preparation method out of graphene composite heating film
CN109878165A (en) * 2019-03-01 2019-06-14 中金态和(武汉)石墨烯研究院有限公司 A kind of graphene composite heating film and its graphene composite heating film group
CN109774292A (en) * 2019-03-19 2019-05-21 中金态和(武汉)石墨烯研究院有限公司 A kind of preparation method of graphene composite heating film
CN110312333A (en) * 2019-07-25 2019-10-08 北京巡天探索科学研究院 Graphene intelligent chip
CN112999200A (en) * 2021-03-03 2021-06-22 张铿 Transdermal drug delivery layer
CN112999200B (en) * 2021-03-03 2024-04-09 北京昊澄生物科技有限公司 Transdermal drug delivery layer
CN115209581A (en) * 2021-04-13 2022-10-18 深圳市为什新材料科技有限公司 Rigid heating film of electronic product and preparation method thereof

Similar Documents

Publication Publication Date Title
CN105898907A (en) Graphene heating film and preparation method thereof
CN205902105U (en) Graphite alkene heating film
CN104846397B (en) One kind being used for electrochemical reduction CO2The electrode and its preparation method and application of formic acid processed
CN105734606B (en) A kind of SPE water electrolysis structure of ultra-thin membrane electrode and its preparation and application
CN107478697B (en) Rime shape metal organic frame composite micro-electrode and in-situ preparation method and application
CN107086306A (en) A kind of use graphene film as negative pole miniature thin-film lithium battery
CN102262989B (en) Method for manufacturing anodic aluminum oxide template and method for manufacturing field emission cathode array material by using template
JP2016508891A (en) Method and apparatus for transfer of film between substrates
CN102251232A (en) Method for preparing silver nanowire array in ordered porous alumina template
CN103342472A (en) Method for transferring graphene film
CN104716340B (en) A kind of preparation method of self-supporting Catalytic Layer
CN106653994B (en) A kind of single-layer electrodes type IPMC structure and its preparation process
CN104835872A (en) Flexible heterojunction film solar cell and preparation method thereof
CN105845463B (en) Preparation method based on three-dimensional grapheme/nickel hydroxide composite electrode material
CN102534742A (en) Titanium dioxide nano thin film composite material and constant-current preparation method thereof
CN108064120B (en) The preparation method and preparation facilities of a kind of flexible circuit or electrode
CN109465016A (en) A kind of palladium/graphene oxide/foam copper combination electrode and its preparation method and application
CN105702935A (en) Preparation method of multilayer anode with porous carbon composite material
CN108076591B (en) The preparation method and preparation facilities of a kind of flexible circuit or electrode
CN103606683A (en) Coiling-type germanium nanomaterial and preparation method thereof
CN107680707A (en) A kind of composition metal nano wire of core shell structure and preparation method and application
CN102732921B (en) Ionic liquid electrodeposition method for preparing three-dimensional ordered macroporous silicon-germanium and germanium-aluminum heterogeneous thin-film material
CN109728254A (en) A kind of technology of preparing of negative electrode of lithium ion battery porous copper foil
CN105761943A (en) Nickel tin alloy nano-pore array and preparation method thereof
CN108615892A (en) A kind of effective modification collector, preparation method and the usage for inhibiting the uncontrollable growth of lithium metal battery dendrite

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
C10 Entry into substantive examination
SE01 Entry into force of request for substantive examination
RJ01 Rejection of invention patent application after publication

Application publication date: 20160824

RJ01 Rejection of invention patent application after publication