CN108289345A - Preparation method, graphene Electric radiant Heating Film, electrothermal device and the application of graphene Electric radiant Heating Film - Google Patents
Preparation method, graphene Electric radiant Heating Film, electrothermal device and the application of graphene Electric radiant Heating Film Download PDFInfo
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- CN108289345A CN108289345A CN201810085202.9A CN201810085202A CN108289345A CN 108289345 A CN108289345 A CN 108289345A CN 201810085202 A CN201810085202 A CN 201810085202A CN 108289345 A CN108289345 A CN 108289345A
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- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
- H05B3/00—Ohmic-resistance heating
- H05B3/02—Details
- H05B3/03—Electrodes
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- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
- H05B3/00—Ohmic-resistance heating
- H05B3/10—Heater elements characterised by the composition or nature of the materials or by the arrangement of the conductor
- H05B3/12—Heater 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—Heater 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
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- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
- H05B3/00—Ohmic-resistance heating
- H05B3/20—Heating elements having extended surface area substantially in a two-dimensional plane, e.g. plate-heater
Abstract
The present invention provides a kind of preparation method of graphene Electric radiant Heating Film, graphene Electric radiant Heating Film, electrothermal device and applications, are related to electrothermal film technology field.Graphene electrophoresis slurry uniform deposition is mainly formed graphene conductive polymeric membrane by the preparation method on the metallic substrate by electrophoresis process, using etching, overlay film obtains graphene Electric radiant Heating Film, the electric heating film thickness obtained using electrophoresis process is uniform, and lot stability is high and heating temperature is uniform；Meanwhile electrode and graphene conductive polymeric membrane are integrally formed, and can avoid the electrode overheating point problem caused by the later stage is laid with by the way of electrode at present.In addition, the preparation method is simple, easily operated, production foundation is provided for industrial production.The present invention also provides the graphene Electric radiant Heating Films obtained using above-mentioned preparation method.The present invention also provides electrothermal devices, including above-mentioned graphene Electric radiant Heating Film, due to advantage possessed by graphene Electric radiant Heating Film itself so that the electrothermal device has good heating property.
Description
Technical field
The present invention relates to electrothermal film technology fields, in particular to a kind of preparation method of graphene Electric radiant Heating Film, graphite
Alkene Electric radiant Heating Film, electrothermal device and application.
Background technology
Since graphene is prepared in first time in 2004, graphene is known as " king of new material ", " dark fund ", it is
It is only the quasi- two dimensional crystal of the monatomic number of plies or several monoatomic layers by a kind of thickness being made of completely the carbon atom of SP2 hydridization
There are material the excellent properties such as highly conductive, high intensity, high heat conduction, these excellent performances of graphene it to be made to be led in electrical heating
Domain shows good application prospect.Graphene electric-heating technology based on graphene Electric radiant Heating Film has environmentally protective, hot turn
Change efficient, far-infrared physiotherapy and the advantages that Pavement design facilitates, it is wide in fields such as modern architecture, heating engineering and decorations
General application.
Currently, there are mainly two types of the preparation methods of graphene Electric radiant Heating Film, one is the method by chemical vapor deposition come
Obtain transparent graphene Electric radiant Heating Film, but this method and process it is complicated, it is of high cost, large scale Electric radiant Heating Film, non-bending resistance can not be made
Folding；Another kind is that macromolecule resin and graphene powder are configured to graphene slurry, then passes through printing, spraying or blade coating
Method obtain graphene Electric radiant Heating Film, as patent No. CN 201510635047.X disclose a kind of system of graphene heater
Film-forming resin, diluent, graphene, auxiliary agent are first uniformly mixed and obtain graphene resin mixture liquor by Preparation Method, this method, then
Graphene conductive layer is formed on film-forming carrier in a manner of coating, obtains being carried by graphene conductive layer and film forming after then drying
The heater of body composition.It was susceptible at there are the temperature uniformities relatively low, electrode of graphene heating film made from this method
The shortcomings of hot spot, poor batch volume Stability of Resistivity.Therefore a kind of graphene electricity that fever is uniform, safe and stable is developed
Hotting mask is current urgent problem to be solved.
In view of this, special propose the present invention.
Invention content
First of the present invention is designed to provide a kind of preparation method of graphene Electric radiant Heating Film, by using electrophoresis process
The graphene electric heating film thickness being prepared is uniform, and lot stability is high and heating temperature is uniform, improves existing graphene hair
Hotting mask product thickness is uneven, the technical problem that lot stability is poor and heating temperature uniformity is relatively low.
Second object of the present invention is to provide a kind of graphene Electric radiant Heating Film, and the graphene electric heating film thickness is uniform, batch
Secondary stability is high and heating temperature is uniform.
Third object of the present invention is to provide a kind of electrothermal device.
Fourth object of the present invention is to provide a kind of preparation method of graphene Electric radiant Heating Film, graphene Electric radiant Heating Film or electricity
The application of thermal device.
In order to realize that the above-mentioned purpose of the present invention, spy use following technical scheme：
The present invention provides a kind of preparation method of graphene Electric radiant Heating Film, includes the following steps；
(a) graphene electrophoresis slurry is formed into graphene conductive high score on the metallic substrate by electrophoresis process uniform deposition
Sub- film；
(b) metal substrate is etched into electrode；
(c) the electrode overlay film after etching step (b), obtains graphene Electric radiant Heating Film.
Further, the graphene electrophoresis slurry is the electrophoresis slurry containing graphene, and the electrophoresis slurry includes third
Olefin(e) acid class electrophoresis slurry, pure phenolic electrophoresis slurry, polybutadiene electrophoresis slurry, epoxy resin electrophoresis slurry or polyurethane
Any one in class electrophoresis slurry；
Preferably, the solid content of graphene is 1~10%, preferably 1~8% in the graphene electrophoresis slurry, into one
Step preferably 1.5~6%.
Further, the graphene conductive polymeric membrane thickness is at 10~100 μm, preferably 12~60 μm, further
Preferably 15~25 μm.
Further, the metal substrate is metal copper foil or metal aluminum foil, and excellent is metallic copper of the thickness at 10~50 μm
Foil or metal aluminum foil；
Preferably, in step (a) electrophoresis process, power-on voltage be 50~120V, preferably 80~120V, further preferably
For 85~115V；
Preferably, in step (a) electrophoresis process, electrophoresis time is 10~60s, preferably 10~50s, further preferred 10
~30s.
Further, the etching technics in step (b) employed in etching process is laser engraving or chemical etching；
Preferably, the etching technics in step (b) employed in etching process is chemical etching；
Preferably, the etching liquid in the chemical etching process is copper chloride, iron chloride, ferric nitrate, ammonium persulfate or double
In oxygen water any one or at least two combination.
Further, in step (b), metal substrate is etched into the textured electrode of tool；
Preferably, the lines includes any one in interdigitated lines, arc lines or parallel lines.
Further, the coating technique employed in step (c) coating process is hot pressing overlay film；
Preferably, the film covered in step (c) coating process includes that polyester film, Kapton, polyethylene are thin
In film, silicon rubber film, polypropylene film, polyamide film or Teflon film any one or at least two combination；
Preferably, the thickness of the film covered in step (c) coating process be 50~175 μm, preferably 50~160 μm,
Further preferably 60~150 μm.
The present invention also provides a kind of graphene Electric radiant Heating Films, are prepared into using the preparation method of above-mentioned graphene Electric radiant Heating Film
It arrives.
The present invention also provides a kind of electrothermal devices, including above-mentioned graphene Electric radiant Heating Film.
The present invention also provides the preparation method of above-mentioned graphene Electric radiant Heating Film, graphene Electric radiant Heating Film or electrothermal devices to add in electricity
Application in hot field.
Compared with prior art, the preparation method of graphene Electric radiant Heating Film provided by the invention and graphene Electric radiant Heating Film and electric heating
Device has the advantages that：
(1) the present invention provides a kind of preparation methods of graphene Electric radiant Heating Film, mainly by electrophoresis process by graphene
Electrophoresis slurry uniform deposition forms graphene conductive polymeric membrane on the metallic substrate, and using etching, overlay film obtains graphene
Electric radiant Heating Film, the electric heating film thickness obtained using electrophoresis process is uniform, and lot stability is high and heating temperature is uniform；Meanwhile electrode
It is integrally formed with graphene conductive polymeric membrane, it can be to avoid the electrode overheating caused by the later stage is laid with by the way of electrode at present
Point problem.
(2) preparation method of graphene Electric radiant Heating Film provided by the invention, metal substrate is etched into different lines
Electrode adjusts the power of Electric radiant Heating Film by the design of different electrode lines；In addition, the preparation method is simple, easily operated,
Production foundation is provided for industrial production.
(3) the present invention provides graphene Electric radiant Heating Films, are made by above-mentioned preparation method, graphene electric heating film thickness is equal
Even, lot stability is high and heating temperature is uniform.
(4) the present invention provides electrothermal devices, including above-mentioned graphene Electric radiant Heating Film, by graphene Electric radiant Heating Film institute itself
It has the advantage that so that the electrothermal device has good heating property.
(5) the present invention also provides the applications of the preparation method of graphene Electric radiant Heating Film, graphene Electric radiant Heating Film or electrothermal device.
It is excellent possessed by preparation method and graphene Electric radiant Heating Film obtained and electrothermal device itself in view of above-mentioned graphene Electric radiant Heating Film
Gesture so that it has good application in field of electric heating.
Description of the drawings
It, below will be to specific in order to illustrate more clearly of the specific embodiment of the invention or technical solution in the prior art
Embodiment or attached drawing needed to be used in the description of the prior art are briefly described, it should be apparent that, in being described below
Attached drawing is some embodiments of the present invention, for those of ordinary skill in the art, before not making the creative labor
It puts, other drawings may also be obtained based on these drawings.
Fig. 1 is to form graphene conductive polymeric membrane on the metallic substrate；
Fig. 2 is electrode；
Fig. 3 is graphene Electric radiant Heating Film.
Icon：1- metal substrates；2- graphene conductive polymeric membranes；3- electrodes；4- films.
Specific implementation mode
Embodiment of the present invention is described in detail below in conjunction with embodiment, but those skilled in the art will
Understand, the following example is merely to illustrate the present invention, and is not construed as limiting the scope of the invention.It is not specified in embodiment specific
Condition person carries out according to conventional conditions or manufacturer's recommended conditions.Reagents or instruments used without specified manufacturer is
The conventional products that can be obtained by commercially available purchase.
According to the first aspect of the invention, a kind of preparation method of graphene Electric radiant Heating Film is provided, is included the following steps；
(a) graphene electrophoresis slurry forms graphene conductive macromolecule on the metallic substrate by electrophoresis process uniform deposition
Film；
(b) metal substrate is etched into electrode；
(c) the electrode overlay film after etching step (b), obtains graphene Electric radiant Heating Film.
From existing different using chemical vapor deposition method and printing, the method for spraying or blade coating, present invention offer
Graphene Electric radiant Heating Film preparation method mainly by electrophoresis process by graphene electrophoresis slurry uniform deposition in metal substrate
Upper formation graphene conductive polymeric membrane, using etching, overlay film obtains graphene Electric radiant Heating Film.It is obtained using electrophoresis process
Electric heating film thickness is uniform, and lot stability is high and heating temperature is uniform；Meanwhile electrode and graphene conductive polymeric membrane one at
Type, can be to avoid the electrode overheating point problem caused by the later stage pastes by the way of electrode at present.
Specifically, electrophoresis process is to keep the particles such as the graphene being suspended in electrophoresis slurry and resin fixed using extra electric field
To migrating and being deposited on metal substrate surface to form graphene conductive polymeric membrane, it is formed by graphene conductive macromolecule
Film main component is graphene and resin.By the electrophoresis process make graphene electrophoresis slurry can uniform deposition in metal substrate
On 1, the higher graphene conductive polymeric membrane 2 of uniformity is formed, it is specific as shown in Figure 1.
The selection of electrophoresis slurry (electrophoretic paint) is also critically important in electrophoresis process, concerning in formed graphene conductive height
The performance of molecular film, and then influence the performance of graphene Electric radiant Heating Film.As a kind of preferred embodiment of the present invention, the graphene
Electrophoresis slurry be the electrophoresis slurry containing graphene, electrophoresis slurry include acrylic compounds electrophoresis slurry, pure phenolic electrophoresis slurry,
Any one in polybutadiene electrophoresis slurry, epoxy resin electrophoresis slurry or polyurethanes electrophoresis slurry.Electrophoresis slurry
Anodic electrophoresis slurry and ability cathode electrophoresis slurry can be divided into, selected with specific reference to needs of production.
As a kind of preferred embodiment of the present invention, the solid content of graphene is 1~10% in graphene electrophoresis slurry,
Preferably 1~8%, further preferably 1.5~6%.
In the present invention, the solid content of graphene refers to the mass fraction that graphene accounts for entire graphene electrophoresis slurry.Stone
The black typical but non-limiting solid content of alkene is 1%, 2%, 3%, 4%, 5%, 6%, 7%, 8%, 9% or 10%.
It should be noted that graphene should limit in a specific range in graphene electrophoresis slurry, graphite just can ensure that
Alkene has good compatibility with electrophoresis slurry, while graphene electrophoresis slurry also has excellent electric conductivity.Graphene is solid
Content is too low, is unfavorable for the raising of electric conductivity, and graphene solid content is excessively high, since graphene oil suction is high, electrophoresis can be caused to starch
Expect that viscosity is excessively high, while the excessively high graphene electrophoresis adhesion of slurry that also results in of graphene solid content declines.
As a kind of preferred embodiment of the present invention, graphene conductive polymeric membrane thickness is at 10~100 μm, preferably
It is 12~60 μm, further preferably 15~25 μm.
Typical but non-limiting graphene conductive polymeric membrane thickness is 10 μm, 12 μm, 15 μm, 18 μm, 20 μm, 25 μ
M, 30 μm, 35 μm, 40 μm, 45 μm, 50 μm, 55 μm, 60 μm, 65 μm, 70 μm, 75 μm, 80 μm, 85 μm, 90 μm, 95 μm or 100
μm。
It is graphene electric heating film quality in the thickness and uniformity of the graphene conductive polymeric membrane that metal substrate surface is formed
The important indicator of amount.Pass through the restriction to graphene conductive polymeric membrane thickness so that graphene Electric radiant Heating Film has certain soft
Property and good mechanical performance.
As a kind of preferred embodiment of the present invention, in step (a) electrophoresis process, used power-on voltage is 50-
120V, preferably 80-120V, further preferably 85-115V.Typical but non-limiting power-on voltage be 50V, 55V, 60V,
65V, 70V, 75V, 80V, 85V, 90V, 95V, 100V, 105V, 110V, 115V or 120V.
Electrophoresis time used by electrophoresis process is 10-60s, preferably 10-50s, further preferred 10-30s.It is typical
But unrestricted electrophoresis time is 10s, 15s, 20s, 25s, 30s, 35s, 40s, 45s, 50s, 55s or 60s.
Pass through the restriction to the technological parameters such as power-on voltage, electrophoresis time in electrophoresis process so that be formed by graphene
Conducting polymer film has good quality.
As a kind of preferred embodiment of the present invention, metal substrate is metal copper foil or metal aluminum foil.Metal copper foil is
A kind of the moon matter electrolysis material, one layer thin be deposited on circuit board substrate layer, continuous metal foil, it leads as PCB's
Electric body.It is easy to be bonded in insulating layer, receives printing protective layer, circuit patterns are formed after corrosion.Metal aluminum foil electric conductivity with
Heat dissipation effect is only second to copper foil, can be attached to various different substrate materials, possesses wider temperature use scope.
Preferably, metal substrate thickness is 10~50 μm of metal copper foil or metal aluminum foil, more preferable thickness is 25~
40 μm of metal copper foil.The typical but non-limiting thickness of metal substrate be 10 μm, 15 μm, 20 μm, 25 μm, 30 μm, 35 μm,
40 μm, 45 μm or 50 μm.
Pass through to metal substrate it is specific restriction and optimization so that graphene conductive polymeric membrane be more easy to uniform deposition in
Metal substrate surface.
The metal substrate 1 that the surface that step (a) obtains is formed to graphene conductive polymeric membrane 2 performs etching, and is had
There is the electrode 3 of specific lines, it is specific as shown in Figure 2.
As a kind of preferred embodiment of the present invention, the etching technics in step (b) employed in etching process includes
Chemical etching or laser engraving.Chemical etching is the technology by materials'use chemical reaction or physical shock effect and removal.Swash
Light engraving is using based on Numeric Control Technology, and laser is process medium.Rapidoprint irradiates the fusing of lower moment in laser engraving
With the physical modification of gasification, laser engraving can be made to achieve the purpose that processing.
Preferably, the etching technics in step (b) employed in etching process is chemical etching.By to etching technics
It limits, ensures excellent anisotropic etching.
It is further preferred that etching liquid in chemical etching process be copper chloride, iron chloride, ferric nitrate, ammonium persulfate or
In hydrogen peroxide any one or at least two combination.Above-mentioned etching liquid all has good etching selection for metal substrate
Property.
As a kind of preferred embodiment of the present invention, electrode lines includes interdigitated lines, arc lines or parallel line
Any one in road, preferably interdigitated lines.
The present invention can adjust the power of Electric radiant Heating Film, easy to operate, side by the design of above-mentioned different electrode lines
Just.
Electrode 3 after step (b) is etched covers film 4, obtains graphene Electric radiant Heating Film, specific as shown in Figure 3.As this
A kind of preferred embodiment of invention, the coating technique in step (c) employed in coating process are hot pressing overlay film；
Preferably, the film covered in coating process in step (c) includes polyester film, Kapton, polyethylene
In film, silicon rubber film, polypropylene film, polyamide film or Teflon film any one or at least two group
It closes, preferably polyester film and polyamide film.
Preferably, the thickness of the film covered in coating process in step (c) is 50~175 μm, preferably 50~160 μ
M, further preferably 60~150 μm.
The typical but non-limiting thickness of film covered be 50 μm, 55 μm, 60 μm, 70 μm, 80 μm, 90 μm, 100 μm,
110 μm, 120 μm, 130 μm, 140 μm, 150 μm, 160 μm, 170 μm or 175 μm.
The preparation method of the graphene Electric radiant Heating Film of the above-mentioned offer of the present invention is simple, easily operated, is provided for industrial production
Produce foundation.
According to the second aspect of the invention, a kind of graphene Electric radiant Heating Film is additionally provided, using above-mentioned graphene Electric radiant Heating Film
Preparation method be prepared.It is uniform by graphene electric heating film thickness made from above-mentioned preparation method, lot stability it is high and
Heating temperature is uniform.
According to the third aspect of the present invention, a kind of electrothermal device, including above-mentioned graphene Electric radiant Heating Film are additionally provided, by
The advantage possessed by graphene Electric radiant Heating Film itself so that the electrothermal device has good heating property.
According to the fourth aspect of the present invention, the preparation method of above-mentioned graphene Electric radiant Heating Film and obtained is additionally provided
The application of graphene Electric radiant Heating Film and electrothermal device in electric fever field.
The advantage of preparation method and graphene Electric radiant Heating Film obtained in view of above-mentioned graphene Electric radiant Heating Film so that it is in electricity
There is good application in fever field.
With reference to specific embodiment and comparative example, the invention will be further described.
Embodiment 1
A kind of preparation method of graphene Electric radiant Heating Film provided in this embodiment, includes the following steps：
(a) under 100V voltages, in the electrophoresis tank for being placed with polyurethane graphene electrophoresis slurry (graphene solid content is 4%)
(50 μm of copper foils do metal substrate to middle preparation electro-deposition 30cm × 30cm graphene conductive polymers film, control graphene high score
Proton conducting membrane thickness is 25 μm), film baking temperature is 120 DEG C, baking time 20min；
(b) by the copper foil substrate of above-mentioned graphene conductive polymer film by chemical etching (etching liquid is copper chloride) at
Interdigitated copper electrode；
(c) it is 75 μm by thickness by laminating machine and the polyester film with hot melt adhesive is layed onto and above-mentioned obtains graphene high score
Proton conducting membrane two sides is to get to graphene Electric radiant Heating Film.
Embodiment 2
The preparation method of a kind of graphene Electric radiant Heating Film provided in this embodiment, in addition to using graphene electrophoresis in step (a)
Slurry is epoxy resin-matrix graphene electrophoresis slurry, remaining is same as Example 1.
Embodiment 3
The preparation method of a kind of graphene Electric radiant Heating Film provided in this embodiment, in addition to using graphene electrophoresis in step (a)
Slurry is polybutadiene graphene electrophoresis slurry, remaining is same as Example 1.
Embodiment 4
The preparation method of a kind of graphene Electric radiant Heating Film provided in this embodiment, in addition in step (a) graphene electrophoresis slurry
Graphene solid content is 5.4%, remaining is same as Example 1.
Embodiment 5
The preparation method of a kind of graphene Electric radiant Heating Film provided in this embodiment, in addition in step (a) graphene electrophoresis slurry
Graphene solid content is 10%, remaining is same as Example 1.
Embodiment 6
The preparation method of a kind of graphene Electric radiant Heating Film provided in this embodiment, in addition in step (a) graphene electrophoresis slurry
Graphene solid content is 12%, remaining is same as Example 1.
Embodiment 7
The preparation method of a kind of graphene Electric radiant Heating Film provided in this embodiment, in addition in step (a) graphene electrophoresis slurry
Graphene solid content is 0.8%, remaining is same as Example 1.
Embodiment 8
The preparation method of a kind of graphene Electric radiant Heating Film provided in this embodiment, in addition to graphene conductive high score in step (a)
Sub- film thickness control is 80 μm, remaining is same as Example 1.
Embodiment 9
The preparation method of a kind of graphene Electric radiant Heating Film provided in this embodiment, in addition to graphene conductive high score in step (a)
Sub- film thickness control is 10 μm, remaining is same as Example 1.
Embodiment 10
A kind of preparation method of graphene Electric radiant Heating Film provided in this embodiment, in addition in step (b) by chemical etching at
Parallel lines copper electrode, remaining is same as Example 3.
Embodiment 11
The preparation method of a kind of graphene Electric radiant Heating Film provided in this embodiment, in addition to the etching work employed in step (b)
Skill is laser engraving, remaining is same as Example 3.
Embodiment 12
The preparation method of a kind of graphene Electric radiant Heating Film provided in this embodiment, in addition to the thickness of the film covered in step (c)
Degree is 75 μm, remaining is same as Example 3.
Comparative example 1
A kind of preparation method for graphene Electric radiant Heating Film that this comparative example provides, includes the following steps：
It is 75 μm in thickness in a manner of coating by polyurethane graphene conductive slurry (graphene solid content is 4%) to gather
Ester film forms graphene conductive layer, is then 120 DEG C in baking temperature, after baking time is dry under conditions of being 20min,
Graphene conductive layer surface sticks parallel lines copper electrode, is 75 μm by thickness finally by laminating machine and carries the poly- of hot melt adhesive
Graphene Electric radiant Heating Film is obtained after ester film overlay film.
Comparative example 2
The preparation method for a kind of graphene Electric radiant Heating Film that this comparative example provides, in addition to graphene solid content to be adjusted to
5.4%, remaining step is identical as comparative example 1.
Comparative example 3
A kind of preparation method for graphene Electric radiant Heating Film that this comparative example provides, includes the following steps：
After using deionized water, acetone to clean successively after the upper surface polishing treatment of copper foil, naturally dry.It then will be adjacent
Graphite cake is stacked up with 20 μm interval (square of interval graphite cake material is realized) distance with copper foil and to be formed 6 layers of structure
Carrier.Ready carrier is put into reacting furnace, and seals reacting furnace, is evacuated to successively using vacuum pump, molecular pump
10-3Pa then heats to 1000 DEG C, respectively with flow 20sccm (sccm refers to 25 DEG C, under atmospheric pressure it is per minute with vertical
The flow of square centimetre of meter) and 500sccm be passed through hydrogen and argon gas, after keeping the temperature 30 minutes, methane is passed through with flow 200sccm, 15
Terminate ventilation after minute and is cooled down with 15 DEG C/min.Etc. being cooled to room temperature taking-up carrier, using fixture to graphite cake and copper foil point
From obtaining the graphene film with copper foil.Applying thickness on the graphene surface of the graphene film with copper foil is
500nm glue-line layers, thickness are 75 μm of PET film adhered on above-mentioned band glue-line, and then by chemical etching, (etching liquid is
Copper chloride) at interdigitated copper electrode, last yet another face paste closes the PET film that thickness is 50 μm, obtains chemical vapor deposition
Transparent graphene heating film prepared by method.
Further to verify the effect of above-described embodiment and comparative example, ad hoc following experimental example.
Experimental example 1
Above-described embodiment and the obtained graphene Electric radiant Heating Film of comparative example are powered test under 220V voltages, specifically detection
The results are shown in Table 1.
The performance test results for the graphene Electric radiant Heating Film that 1 each embodiment and comparative example of table provides
It is obtained using graphene electric heating membrane preparation method provided in an embodiment of the present invention it can be seen from data in table 1
Graphene Electric radiant Heating Film overall performance is better than the graphene Electric radiant Heating Film that the preparation method provided using comparative example is obtained.
Specifically, embodiment 2 and embodiment 3 are the control experiment of embodiment 1, three is the difference is that step (a)
Employed in graphene electrophoresis slurry it is different.The type of graphene electrophoresis slurry is different it can be seen from data in table 1 so that
The main component of formed graphene conductive polymeric membrane is different, and then causes the performance of graphene Electric radiant Heating Film different.
Embodiment 4-7 is the control experiment of embodiment 1, and several persons are the difference is that graphene in graphene electrophoresis slurry
Solid content is different.As can be seen from Table 1, in the range of graphene solid content of the present invention limits, graphene electric heating film surface
Temperature is uniform, has good comprehensive performance.
Embodiment 8 and 9 is the control experiment of embodiment 1.With 25 μm of graphene conductive polymeric membrane thickness in embodiment 1
Difference, graphene conductive polymeric membrane thickness is 80 μm in embodiment 8, and graphene conductive polymeric membrane thickness is in embodiment 9
10μm.Graphene conductive polymeric membrane thickness is smaller it can be seen from data in table 1, and graphene Electric radiant Heating Film surface temperature difference is smaller.
In the preparation method for the graphene Electric radiant Heating Film that comparative example 1 and comparative example 2 provide, graphene conductive layer is to use
What conventional coating method was formed, and parallel lines copper electrode be after be routed to graphene conductive layer surface.By that can be seen in table 1
Go out, the preparation method of comparative example 1 and 2, it is in uneven thickness that conventional coating method be easy to cause Electric radiant Heating Film, and then leads to Electric radiant Heating Film table
Face non-uniform temperature degree is larger, while the method for tradition laying electrode be easy to cause at electrode points and heat spot occurs.
Comparative example 3 is the transparent graphene heating film prepared using chemical vapour deposition technique.It can be seen by data in table 1
Go out, although its at electrode without heat spot, Electric radiant Heating Film surface temperature difference is larger, this illustrates Electric radiant Heating Film surface temperature unevenness
It increases.And whole preparation process is also complex, cost is higher.
In conclusion graphene electric heating film thickness made from the preparation method of the graphene Electric radiant Heating Film provided through the invention
Uniformly, lot stability is high and heating temperature is uniform；Meanwhile electrode and graphene conductive polymeric membrane are integrally formed, and can be kept away
Exempt from the electrode overheating point problem caused by the later stage is laid with by the way of electrode at present.
Finally it should be noted that：The above embodiments are only used to illustrate the technical solution of the present invention., rather than its limitations；To the greatest extent
Present invention has been described in detail with reference to the aforementioned embodiments for pipe, it will be understood by those of ordinary skill in the art that：Its according to
So can with technical scheme described in the above embodiments is modified, either to which part or all technical features into
Row equivalent replacement；And these modifications or replacements, various embodiments of the present invention technology that it does not separate the essence of the corresponding technical solution
The range of scheme.
Claims (10)
1. a kind of preparation method of graphene Electric radiant Heating Film, which is characterized in that include the following steps：
(a) graphene electrophoresis slurry forms graphene conductive polymeric membrane on the metallic substrate by electrophoresis process uniform deposition；
(b) metal substrate is etched into electrode；
(c) the electrode overlay film after etching step (b), obtains graphene Electric radiant Heating Film.
2. preparation method according to claim 1, which is characterized in that the graphene electrophoresis slurry is to contain graphene
Electrophoresis slurry, the electrophoresis slurry include acrylic compounds electrophoresis slurry, pure phenolic electrophoresis slurry, polybutadiene electrophoresis slurry
Any one in material, epoxy resin electrophoresis slurry or polyurethanes electrophoresis slurry；
Preferably, the solid content of graphene is 1~10%, preferably 1~8% in the graphene electrophoresis slurry, further excellent
It is selected as 1.5~6%.
3. preparation method according to claim 1, which is characterized in that the graphene conductive polymeric membrane thickness be 10~
100 μm, preferably 12~60 μm, further preferably 15~25 μm.
4. according to the preparation method described in claim 1-3 any one, which is characterized in that the metal substrate is metal copper foil
Or metal aluminum foil, the metal copper foil or metal aluminum foil that preferably thickness is 10~50 μm；
Preferably, in step (a) electrophoresis process, power-on voltage is 50~120V, preferably 80~120V, further preferably 85
~115V；
Preferably, in step (a) electrophoresis process, electrophoresis time be 10~60s, preferably 10~50s, further preferred 10~
30s。
5. according to the preparation method described in claim 1-3 any one, which is characterized in that adopted in step (b) etching process
Etching technics is laser engraving or chemical etching；
Preferably, the etching technics employed in step (b) etching process is chemical etching；
Preferably, the etching liquid that the chemical etching process uses is copper chloride, iron chloride, ferric nitrate, ammonium persulfate or dioxygen
In water any one or at least two combination.
6. according to the preparation method described in claim 1-3 any one, which is characterized in that in step (b), metal substrate is carved
Lose into the textured electrode of tool；
Preferably, the lines includes any one in interdigitated lines, arc lines or parallel lines.
7. according to the preparation method described in claim 1-3 any one, which is characterized in that adopted in step (c) coating process
Coating technique is hot pressing overlay film；
Preferably, the film covered in step (c) coating process includes polyester film, Kapton, polyethylene film, silicon
In rubber film, polypropylene film, polyamide film or Teflon film any one or at least two combination；
Preferably, the thickness of the film covered in step (c) coating process be 50~175 μm, preferably 50~160 μm, into one
Preferably 60~150 μm of step.
8. a kind of graphene Electric radiant Heating Film, which is characterized in that using the graphene Electric radiant Heating Film described in claim 1-7 any one
Preparation method is prepared.
9. a kind of electrothermal device, which is characterized in that including graphene Electric radiant Heating Film according to any one of claims 8.
10. the preparation method of the graphene Electric radiant Heating Film described in claim 1-7, graphene Electric radiant Heating Film according to any one of claims 8 or
Application of the electrothermal device in field of electric heating described in claim 9.
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| CN109152114A (en) * | 2018-10-26 | 2019-01-04 | 烟台市秀春来壁纸有限公司 | A kind of graphene Electric radiant Heating Film and preparation method thereof |
| CN109413774A (en) * | 2018-10-31 | 2019-03-01 | 宁波石墨烯创新中心有限公司 | A kind of graphene Electric radiant Heating Film, preparation method and electric heating products |
| CN109874187A (en) * | 2019-01-29 | 2019-06-11 | 鸿纳（东莞）新材料科技有限公司 | A kind of graphene heating film and its compounding method |
| CN110267372A (en) * | 2019-05-07 | 2019-09-20 | 宁波石墨烯创新中心有限公司 | A kind of graphene electric heating composite members and its manufacturing method |
| CN112812687A (en) * | 2020-12-30 | 2021-05-18 | 杭州吉华高分子材料股份有限公司 | Preparation method of graphene electrothermal film containing in-situ polymerization insulating coating |
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| CN112812687B (en) * | 2020-12-30 | 2021-11-30 | 杭州吉华高分子材料股份有限公司 | Preparation method of graphene electrothermal film containing in-situ polymerization insulating coating |
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