CN208158919U - Graphene heating film and graphene suitable for power battery pack heat membrane module - Google Patents
Graphene heating film and graphene suitable for power battery pack heat membrane module Download PDFInfo
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- CN208158919U CN208158919U CN201721925502.0U CN201721925502U CN208158919U CN 208158919 U CN208158919 U CN 208158919U CN 201721925502 U CN201721925502 U CN 201721925502U CN 208158919 U CN208158919 U CN 208158919U
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- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 160
- 238000010438 heat treatment Methods 0.000 title claims abstract description 75
- 239000012528 membrane Substances 0.000 title claims abstract description 31
- 239000002002 slurry Substances 0.000 claims abstract description 35
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- 239000000741 silica gel Substances 0.000 claims abstract description 30
- 229910002027 silica gel Inorganic materials 0.000 claims abstract description 30
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- XITRBUPOXXBIJN-UHFFFAOYSA-N bis(2,2,6,6-tetramethylpiperidin-4-yl) decanedioate Chemical compound C1C(C)(C)NC(C)(C)CC1OC(=O)CCCCCCCCC(=O)OC1CC(C)(C)NC(C)(C)C1 XITRBUPOXXBIJN-UHFFFAOYSA-N 0.000 description 1
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Classifications
-
- 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
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
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- Conductive Materials (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
This application involves technical field of graphene and heating element technical field, specifically disclose a kind of graphene heating film and a kind of graphene heating membrane module.The graphene heating film includes organic macromolecule-based film and the heating line at least one surface of the organic polymer basement membrane, and the heating line is by the way that graphene conductive slurry to be applied at least one described surface and be solidified to form.Graphene heating membrane module with heat conductive silica gel, graphene thermally conductive sheet, organic polymer insulating film and temperature sensor by combining the graphene heating film being made.High conductivity, high-termal conductivity, high mechanical strength and the high-flexibility of graphene is utilized in the graphene heating membrane module of the utility model, have many advantages, such as that heating voltage is low, heating speed is fast, electrothermal efficiency is high, heating surface uniformly, without rubescent red-hot phenomenon, can be windability good, soft, frivolous, conformal good.Suitable for providing heat source for power battery pack, influence of the low temperature charge and discharge to battery performance is solved.
Description
Technical field
This application involves technical field of graphene and heating element technical field, and in particular to a kind of graphene heating film
Membrane module is heated with a kind of graphene, is especially adapted for use in the graphene heating film and graphene heating film group of power battery pack
Part.
Background technique
The evident characteristic that electric automobile power battery charges at low temperature at present is that voltage rises rapidly, and is charged at low temperature
It will cause positive lithium and fall off that fast, cathode lithium insertion speed is slow, cause lithium metal accumulate generation dendrite at the electrode surface, easily wear out
Battery diaphragm makes battery short circuit, constitutes security risk.Therefore, under cryogenic, power battery is preferably heated so that battery
In room temperature state (20-30 DEG C) charge and discharge.
A kind of heating method is heated using PTC fever tablet.PTC fever tablet is semiconductive ceramic, the disadvantage is that weight
Amount is big, heating efficiency is low, volume size is big, without flexibility, hard crisp, inflexibility winding.Another way is using heating film
It is heated.The plane heater element that heating film is made of electrically insulating material with the heating resistor material encapsulated in it.Hair
Hotting mask needs to can be only achieved heating effect in very high voltage, radiation heat loss is very big, and heating circuit does not have since resistance is big
Good flexibility is easy open circuit in the process of bending, bad in terms of heat-resisting, wearability, moisture-proof and safety.
Graphene is a kind of flat film being made of carbon atom, and the connection between internal carbon atom is very flexible.Graphite
Its electron mobility is more than 15000cm to alkene at normal temperature2/ (Vs), thermal coefficient is up to 5300W/ (mK), and resistivity
Only about 10-6Ω cm, it is lower than copper or silver, it is the current the smallest material of world resistivity.Graphene is under the voltage lower than 12V
It is obtained with good heating effect.
Summary of the invention
To overcome problem of the prior art, the object of the present invention is to provide a kind of graphene heating films and a kind of graphene to add
Hotting mask component is particularly useful for the graphene heating membrane module of electric automobile power battery packet.
Therefore, in one aspect, the present invention provides a kind of graphene heating film, which includes organic high score
Subbase film and the heating line at least one surface of the organic polymer basement membrane, the heating line is by by graphene
Electrocondution slurry is applied at least one surface and is solidified to form.
Specifically, which includes the graphene 1-10 parts by weight of epoxy-functional, epoxy resin 4-15
Parts by weight, epoxy-modified siloxanes 2-6 parts by weight, epoxy active diluent 2-6 parts by weight and latent curing agent 0.1-0.8
Parts by weight.
Preferably, which also includes through silane coupler modified conductive black 5-20 parts by weight, resists
Wire drawing agent 0.2-1 parts by weight and 0.05-0.2 parts of antioxidant.
Specifically, which is PET film.
Specifically, which completed by way of spraying or silk-screen printing, preferably passes through silk-screen printing
Mode is completed.Spraying and screen printing technique in electrocondution slurry field application be it is known in the art that see, for example, with
Page 16 of Publication about Document：Li Jiang, Electric radiant Heating Film and silk-screen printing,《Silk-screen printing》, 01 phase in 1996.
Specifically, which completed by 100-150 DEG C of infrared heating 5-12 minutes.
On the other hand, the present invention provides a kind of graphene heating membrane module, and it includes root which, which heats membrane module,
According to the graphene heating film of first aspect present invention, the first heat conductive silica gel, the second heat conductive silica gel, the first graphene thermally conductive sheet,
Two graphene thermally conductive sheets, the first organic polymer insulating film and the second organic polymer insulating film, wherein first heat conductive silica gel
Positioned at the top of the graphene heating film, which is located at the top of first heat conductive silica gel, this first has
Machine polymer insulating film is located at the top of the first graphene thermally conductive sheet, which is located at the graphene heating film
Lower section, the second graphene thermally conductive sheet are located at the lower section of second heat conductive silica gel, which is located at should
The lower section of second graphene thermally conductive sheet.
Preferably, graphene heating membrane module further includes temperature sensor, and wherein the temperature sensor is located at first and leads
Between hot silica gel and the first graphene thermally conductive sheet, or between the second heat conductive silica gel and the second graphene thermally conductive sheet.
Preferably, which is commercially available sheet type temperature sensor, such as ultra-thin temperature sensors of high precision.
Preferably, first organic polymer insulating film and the second organic polymer insulating film are commercially available PE insulating film.
Preferably, the first graphene thermally conductive sheet and the second graphene thermally conductive sheet are commercially available graphene thermally conductive sheet.
Preferably, first heat conductive silica gel and the second heat conductive silica gel are commercially available heat conductive silica gel.
Preferably, first organic polymer insulating film and the second organic polymer insulating film are commercially available PE insulating film.
Beneficial effects of the present invention
The present invention, as host conductive agent, makes full use of the high conductivity of graphene, especially with this Shen using graphene
The ask someone graphene conductive slurry of exploitation produces graphene heating film, then by with heat conductive silica gel, graphene thermally conductive sheet and PE
Insulating film combination is made graphene heating membrane module, gained subassembly product after tested, operating voltage<12V, resistance are 3~5 Ω,
Cold insulation resistance>300M Ω, hot insulation resistance>3 DEG C of 200M Ω, temperature uniformity <, in addition maximum operation (service) temperature is 60
DEG C, have that heating voltage is low, heating speed is fast, electrothermal efficiency is high, heating surface uniformly, without rubescent red-hot phenomenon, energy-saving safe
Advantage.
Meanwhile the present invention makes full use of the high-termal conductivity of graphene.Graphene thermal conductivity is up to 4000-6600W/mK,
Compared with graphite and traditional heat-dissipating material, quick conductive characteristic that graphene has.Graphene heating membrane module of the invention is adopted
Use graphene thermally conductive sheet that quick conductive may be implemented as the transmitting medium of heat.
Moreover, graphene has high mechanical strength and high-flexibility, electric silica gel and PE insulating film softness are frivolous, manufactured
Graphene heats membrane module can be windability good, soft, frivolous, long service life.It can be according to being heated battery pack
Arbitrary shape bending, it is ensured that be in close contact with battery pack, guarantee the transmitting of maximum thermal energy, significantly save battery pack space and
The weight for reducing battery pack, improves the volume energy density and gravimetric energy density of battery pack.
By configuring ultra-thin high-accuracy temperature sensor, real time monitoring is heated in the temperature and power battery pack of membrane module
Portion's temperature can carry out humanized perforation, guarantee the stability of temperature, the peace of battery pack by the intelligent temperature controller on automobile
The convenience of full property and manipulation.Suitable for batteries of electric automobile packet, heat source is provided for battery pack, solves low temperature charge and discharge to battery
The influence of performance.
Detailed description of the invention
Fig. 1 is the schematic diagram of the graphene heating film of an embodiment according to the present invention.Appended drawing reference in figure is such as
Under：1- graphene heating film；2- heat conductive silica gel；3- graphene thermally conductive sheet；4-PE insulating film.
Specific embodiment
Below by specific embodiment and in conjunction with attached drawing, invention is further described in detail.
Graphene heating film of the invention includes organic macromolecule-based film and positioned at least the one of the organic polymer basement membrane
Heating line on a surface, the heating line is by the way that graphene conductive slurry to be applied at least one surface and solidify
And it is formed.
(I) component of the graphene conductive slurry
The graphene conductive slurry includes following components：The graphene 1-10 parts by weight of epoxy-functional, epoxy resin 4-
15 parts by weight, epoxy-modified siloxanes 2-6 parts by weight, epoxy active diluent 2-6 parts by weight and latent curing agent 0.1-
0.8 parts by weight.
Preferably, which is the epoxy resin with pi bond structure.It is highly preferred that the epoxy resin is with benzene
The epoxy resin of ring structure.It is more preferred still that the epoxy resin be bisphenol A type epoxy resin or bisphenol f type epoxy resin, especially
It is electron level bisphenol A type epoxy resin or bisphenol f type epoxy resin.Most preferably, which is bisphenol F type epoxy
Resin, because bisphenol f type epoxy resin has good high-temperature stability, to multiple materials such as metal, plastics, rubber, ceramics
With good adhesive property.
The graphene of the epoxy-functional is made by the way that graphene powder is carried out surface functionalization with the epoxy resin,
Wherein the weight ratio of the epoxy resin and the graphene powder is 1:4-3:1.Preferably, with Bisphenol F type epoxy resin by graphite
Alkene powder carries out surface functionalization.
The epoxy-modified siloxanes is, wherein asphalt mixtures modified by epoxy resin obtained by being modified siloxanes with the epoxy resin
The weight ratio of rouge and the siloxanes is 1:3-2:1, wherein the siloxanes is tetramethyl tetrahydro cyclotetrasiloxane, tetramethyl dihydro two
At least one of siloxanes, tetramethyl divinyl disiloxane or t etram-ethyltetravinylcyclotetrasiloxane.Preferably, it uses
Silicone powder is carried out surface functionalization by bisphenol f type epoxy resin.
Preferably, which also includes 5-20 parts by weight through silane coupler modified conductive black.
The silane coupler modified conductive black is, wherein silane obtained by being modified conductive black with silane coupling agent
Coupling agent accounts for the 0.8%-2.5% of the weight of the conductive black.Preferably, which is γ-(2,3- the third oxygen of epoxy)
Propyl trimethoxy silicane (KH560).
Preferably, the graphene conductive slurry also include 0.2-1 parts by weight the agent of tension silk and 0.05-0.2 parts of antioxygen
Agent.The tension silk agent can prevent the graphene conductive slurry from occurring wire drawing phenomenon in use, and the antioxidant
Help to prevent the oxidation of graphene conductive slurry.
Graphene used in the graphene conductive slurry is graphene powder well known in the art, preferably high conductivity
Graphene powder is less than in graphene powder preparation process using element dopings graphene, the numbers of plies of graphene powder such as N, B
5 layers.The available commercial quotient of this graphene is, for example, Xi Wang new material Science and Technology Co., Ltd. of Shenzhen, the hexa-atomic element in Changzhou
Limited liability company, Changzhou two dimension carbon Science and Technology Co., Ltd. etc..
Conductive black used in the graphene conductive slurry is conductive black well known in the art, such as Japanese lion princes and dukes
Take charge of the serial superconducting carbon black (Ketjenblack EC-300J and EC-600JD) of Ketjenblack (Ketjen black), the beauty of (LION)
The VXC series of conductive carbon black of Cabot Co., Ltd of state (CABOT) wins the production of wound Degussa (Evonik Degussa) company
PRINTEX XE2-B, PRINTEX L6, HIBLAXK 40B2 etc..
The epoxy active diluent is ethylene glycol diglycidylether, butanediol diglycidyl ether, 1,6- cyclohexandiol
Diglycidyl ether, tetrahydrophthalic acid 2-glycidyl ester, hexahydrophthalic acid 2-glycidyl ester, 1,2- hexamethylene two
At least one of alcohol diglycidyl ether or resorcinolformaldehyde resin.
The latent curing agent is group of the lanthanides boron trifluoride acetic acid complex compound La (BF3·C4H7O4)n、 Sm(BF3·C4H7O4)
n、Dy(BF3·C4H7O4)n、Er(BF3·C4H7O4) n or Yb (BF3·C4H7O4At least one of) n, wherein (BF3·
C4H7O4) n expression boron trifluoride acetic acid anion, n expression complexing coefficient.
The tension silk agent is at least one of nano-titanium dioxide, nano zine oxide, Nano carbon white.It is highly preferred that
The tension silk agent is A380 white carbon black.
The antioxidant is bis- (1- octyloxy -2,2,6,6- tetramethyl -4- piperidyl) sebacates, bis- (2,2,6,6-
Tetramethyl -4- piperidyl) sebacate, 4- [(the pungent sulfenyl -1,3,5- triazine -2- base of 4,6- bis-) amino] -2,6- di-t-butyl
At least one of phenol, dimethylsuccinic acid esters -4- hydroxyl -2,2,6,6- tetramethyl -4- piperidine alcohols.
(II) preparation method of the graphene conductive slurry
The preparation method of the graphene conductive slurry includes the following steps：
The epoxy-functional of graphene powder：Graphene powder is subjected to epoxy-functional with epoxy resin, wherein the ring
The weight ratio of oxygen resin and the graphene powder is 1:4-3:1；
Siloxanes it is epoxy-modified：Siloxanes is modified with epoxy resin, wherein the epoxy resin and the siloxanes
Weight ratio be 1:3-2:1；
Mixing：By surface functionalized graphene powder 1-10 parts by weight, through epoxy-modified siloxanes 2-6
Parts by weight, epoxy resin 4-15 parts by weight, epoxy active diluent 2-6 parts by weight and latent curing agent 0.1-0.8 weight
Part carries out low speed dispersion stirring, high speed dispersion stirring, vacuum defoamation, and the graphene conductive slurry is made.
Preferably, which is the epoxy resin with pi bond structure.It is highly preferred that the epoxy resin is with benzene
The epoxy resin of ring structure.It is more preferred still that the epoxy resin be bisphenol A type epoxy resin or bisphenol f type epoxy resin, especially
It is electron level bisphenol A type epoxy resin or bisphenol f type epoxy resin.Most preferably, which is bisphenol F type epoxy
Resin, because bisphenol f type epoxy resin has good high-temperature stability, to multiple materials such as metal, plastics, rubber, ceramics
With good adhesive property.
Preferably, the epoxy-functional step of the graphene powder includes by the graphene powder and epoxy resin anhydrous
In solvent, in 20-120 DEG C of temperature, power 500W-4800W, frequency is ultrasonic wave, the 300rpm- of 30KHz-120KHz
Concussion processing 1-8 hours under the rotation of 3500rpm, then vacuum filter is dry under conditions of being lower than 50 DEG C, removes solvent, system
The graphene of epoxy-functional is obtained, wherein the solvent is dehydrated alcohol, isopropanol, butanol, ethyl acetate, butyl acetate, acetic acid
One of pentyl ester, isoamyl acetate, isoamyl acetate, n-methyl-2-pyrrolidone (NMP) or several mixtures.
Preferably, the epoxy-modified step of the siloxanes includes by toluene, epoxy resin, catalyst platinum tetrachloride in logical nitrogen
15min is stirred under conditions of gas, wherein the weight ratio of toluene and the epoxy resin is 1.2:1-3.0:1, catalyst four
Platinum chloride accounts for the 0.008%-0.05% of weight epoxy, and gained mixture is then warming up to 70 DEG C in a nitrogen atmosphere,
It is added dropwise the 1 of toluene and siloxanes:1-5:1 mixed liquor 1h, the reaction was continued 6h, vacuum distillation remove toluene solvant, obtain epoxy and change
The siloxanes of property, wherein the siloxanes is tetramethyl tetrahydro cyclotetrasiloxane, tetramethyldihydrogendisiloxane, tetramethyl divinyl
At least one of base disiloxane or t etram-ethyltetravinylcyclotetrasiloxane.
It preferably, further include being changed conductive black in acidic aqueous solution with silane coupling agent before the mixing step
Property, wherein the silane coupling agent accounts for the 0.8%-2.5% of the weight of the conductive black；The mixing step includes being additionally added 5-20 weight
The modified conductive black for measuring part carries out mixing.Preferably, which is γ-(2,3- the third oxygen of epoxy) propyl three
Methoxy silane (KH560).
Preferably, which includes being additionally added the agent of tension silk and 0.05-0.2 parts anti-oxidant of 0.2-1 parts by weight
Agent carries out mixing.
Preferably, which carries out in contactless planet stirring vacuum defoamation all-in-one machine, the contactless row
The vacuum degree of planetary stirring vacuum deaeration all-in-one machine is -0.095MPa；When low speed dispersion stirring, revolution revolving speed is 100-
500rpm, the ratio between revolution and rotational velocity are 1:5-2:1, time 10min-120min；When high speed dispersion stirs, revolution revolving speed is
800-5000rpm, the ratio between revolution and rotational velocity are 1:2-3:1, time 15min-80min.
The graphene, the conductive black, the epoxy active diluent, the latent curing agent, the tension silk agent and this is anti-
Oxidant is as described in the first aspect of the invention.
Moreover, it is noted that carrying out ring to the graphene for the first aspect of the present invention and second aspect
The functionalized epoxy resin of oxygen carries out epoxy-modified epoxy resin to the siloxanes and as the master of the graphene conductive slurry
The epoxy resin of one of body component can be identical or can not be identical.Such as the graphene carries out the asphalt mixtures modified by epoxy resin of epoxy-functional
Rouge, the epoxy that one of epoxy-modified epoxy resin and the host component as the graphene conductive slurry are carried out to the siloxanes
Resin can be each independently bisphenol A type epoxy resin or bisphenol f type epoxy resin.
(III) preparating example of the graphene conductive slurry
Preparating example 1
In this preparating example, to graphene carry out epoxy-functional epoxy resin, siloxanes is carried out it is epoxy-modified
The epoxy resin of one of epoxy resin and host component as graphene conductive slurry is all made of bisphenol A type epoxy resin.It should
Bisphenol A type epoxy resin is purchased from Shenzhen Jia Dida Chemical Co., Ltd., model NPEL-128E.
By the 2g graphene powder (graphene of the high conductivity of Xi Wang new material Science and Technology Co., Ltd. of Shenzhen preparation
Powder), 3.5g bisphenol A type epoxy resin and 200g dehydrated alcohol be added in high speed rotation cavity testing machine.The high speed is revolved
Turn cavity testing machine and is configured with supersonic generator and heating constant-temperature equipment.By mixture at 20-120 DEG C, 1600rpm high speed is revolved
Turn and 2000W, frequency 80KHz ultrasonic wave under shake 1-8h hour, then vacuum filter is done under conditions of lower than 50 DEG C
It is dry, solvent is removed, the graphene powder of surface functionalization is made.
200g toluene, 80g bisphenol A type epoxy resin, 0.02g catalyst platinum tetrachloride are added in glass container,
Under the mixing speed of 200rpm, 15min is stirred under conditions of logical nitrogen.Then mixture is heated up in a nitrogen atmosphere
To 70 DEG C.The mixed liquor 1h of 80g toluene and 20g tetramethyl tetrahydro cyclotetrasiloxane is added dropwise using dropping funel.After being added dropwise,
The reaction was continued 6h, vacuum distillation remove toluene solvant, obtain epoxy-modified siloxanes.
Siloxanes epoxy-modified obtained by graphene powder surface-functionalized obtained by 10g, 4g, 10g is bis-
Phenol A type epoxy resin, 4g ethylene glycol diglycidylether, 0.5g La (BF3·C4H7O4) n, 0.5gA380 white carbon black and 0.1g
Bis- (1- octyloxy -2,2,6,6- tetramethyl -4- piperidyls) sebacates are added in glass container, in the stirring speed of 120rpm
It is stirred until homogeneous under degree.Then the contactless planet stirring vacuum defoamation one that vacuum degree is -0.095MPa is fed the mixture into
In body machine, low speed dispersion stirring is first carried out, revolution revolving speed is 100-500rpm, and the ratio between revolution and rotational velocity are 1:5-2:1,
Mixing time is 40min, and when then carrying out high speed dispersion stirring, revolution revolving speed is 800~5000rpm, revolution and rotational velocity
The ratio between be 1:2-3:1, mixing time 30min, then vacuum removal bubble, is made the graphene conductive slurry of this preparating example
Material.
Preparating example 2
In this preparating example, to graphene carry out epoxy-functional epoxy resin, siloxanes is carried out it is epoxy-modified
The epoxy resin of one of epoxy resin and host component as graphene conductive slurry is all made of bisphenol f type epoxy resin generation
For the bisphenol A type epoxy resin in preparating example 1, remaining is identical as preparating example 1.The bisphenol f type epoxy resin is purchased from deep
Jia Dida Chemical Co., Ltd. of ditch between fields city, model NPEF-170.
Preparating example 3
In this preparating example, the epoxy resin of epoxy-functional is carried out to graphene and siloxanes is carried out epoxy-modified
Epoxy resin is all made of the bisphenol A type epoxy resin in preparating example 1, one of host component as graphene conductive slurry
For epoxy resin using the bisphenol f type epoxy resin in preparating example 2, remaining is identical as preparating example 1.
Preparating example 4
In this preparating example, the epoxy resin of epoxy-functional is carried out to graphene and siloxanes is carried out epoxy-modified
Epoxy resin is all made of the bisphenol f type epoxy resin in preparating example 2, one of host component as graphene conductive slurry
For epoxy resin using the bisphenol A type epoxy resin in preparating example 1, remaining is identical as preparating example 1.
Preparating example 5-8
Preparating example 5-8 is corresponding with preparating example 1-4 respectively, but carries out what surface was modified to conductive black increasing
Step, and the modified conductive black in obtained surface is prepared into graphene conductive slurry together with remaining component.
Specifically, it using the conductive carbon black Ketjenblack EC-300J of Japanese lion princes and dukes department (LION), and uses
It is modified that KH560 silane coupling agent carries out surface to the conductive black.By 100g conductive carbon black Ketjenblack EC-300J and
1.2g KH560 silane coupling agent concentration be 0.5% dilute sulfuric acid aqueous solution in, 40~80 DEG C at a temperature of reaction 0.6~
2 hours, obtain the modified conductive black in surface.
For preparating example 5, by each component described in the resulting surface 20g modified conductive black and preparating example 1 into
Row is mixed, and wherein the graphene of epoxy-functional is changed to 1g by 10g, and presses described in preparating example 1 in contactless row
Low speed dispersion stirring, high speed dispersion stirring and vacuum defoamation are carried out in star stirring vacuum deaeration all-in-one machine, obtain graphene conductive
Slurry.
For preparating example 6, by each component described in the resulting surface 15g modified conductive black and preparating example 2 into
Row is mixed, and wherein the graphene of epoxy-functional is changed to 2.5g by 10g, and presses described in preparating example 1 contactless
Low speed dispersion stirring, high speed dispersion stirring and vacuum defoamation are carried out in planet stirring vacuum defoamation all-in-one machine, are obtained graphene and are led
Plasma-based material.
For preparating example 7, by each component described in the resulting surface 10g modified conductive black and preparating example 3 into
Row is mixed, and wherein the graphene of epoxy-functional is changed to 5g by 10g, and presses described in preparating example 1 in contactless row
Low speed dispersion stirring, high speed dispersion stirring and vacuum defoamation are carried out in star stirring vacuum deaeration all-in-one machine, obtain graphene conductive
Slurry.
For preparating example 8, each component described in the resulting surface 5g modified conductive black and preparating example 4 is carried out
It is mixed, wherein the graphene of epoxy-functional is changed to 7.5g by 10g, and presses described in preparating example 1 in contactless row
Low speed dispersion stirring, high speed dispersion stirring and vacuum defoamation are carried out in star stirring vacuum deaeration all-in-one machine, obtain graphene conductive
Slurry.
Illustrate that graphene heating film and graphene of the invention heat membrane module with embodiment below.These embodiments are to show
Example property, it must not believe that and be construed as limiting the invention.The scope of the present invention is limited only by the claims.
Embodiment 1
This example demonstrates that an embodiment of graphene heating film of the invention.
By any preparating example in " preparating example of (III) the graphene conductive slurry " above, stone is prepared
Black alkene electrocondution slurry.
PET polymeric membrane (being purchased from Dongguan City Sheng He Electron Material Co., Ltd, thickness 0.075-0.2mm) is chosen, is selected
Solar battery screen printer (is purchased from Shenzhen all-pass wire mark mechanical & electronic equipment corporation, Ltd), and first designs the heating of graphene heating film
Line map is fabricated to screen printing forme.
PET polymeric membrane is placed on the print station of solar battery screen printer, screen printing forme is fixed on screen frame, set
In the top of PET polymeric membrane, at a distance of 2-30 millimeters.Suitable graphene conductive slurry is added on silk screen, is scratched with scraper
Slurry is filled in it uniformly among mesh, and slurry is expressed to PET high score by screen mesh in the process of moving by scraper
On one surface of sub- film, heater circuit is printed out.It can depend on the needs and equally print out heater circuit on the other surface.
The PET polymeric membrane for having printed heater circuit is placed in infrared furnace, is carried out at 100-150 DEG C red
Outside line solidifies 5-12 minutes, and the graphene heating film of the present embodiment is made.
Embodiment 2
This example demonstrates that an embodiment of graphene heating membrane module of the invention.
Vacuum filling heat conductive silica gel (is purchased from Shenzhen Jia Feng Electron Material Co., Ltd), implements heat conductive silica gel package
Graphene heating film made from example 1 makes graphene heating film upper and lower surface respectively have one layer of electric silica gel, and every layer with a thickness of 0.08-
0.4mm.By ultra-thin temperature sensors of high precision (Wuxi Zhong Hui automotive electronics Co., Ltd) be placed in Upper conductive silica gel or under
On the surface of layer electric silica gel.Ultra-thin temperature sensors of high precision with a thickness of 0.2mm, temperature-measuring range is -40 DEG C to 100 DEG C,
Zero-power resistance is R25=10K Ω ± 0.5%, and material constant is B25/85=3370K ± 0.5%, reaction speed about 1s.
The graphene fever black upper and lower surface achieved above wrapped up with heat conductive silica gel is successively used into (the purchase of graphene thermally conductive sheet
(Foshan is purchased from from the supply of Xi Wang new material Science and Technology Co., Ltd. of Shenzhen, thickness 0.05mm-0.5mm) and PE insulating film
Nan Mu new material Co., Ltd of city, thickness 0.05-0.3mm) it clips, it is then placed within ultrasonic wave thermosol pressing curing and (is purchased from
Dongguan City Long Ke automation equipment Science and Technology Ltd.；Frequency 20KHZ, power 2000W, 100-150 DEG C of temperature, weld interval
0.5-10s), the graphene that the present embodiment is made heats membrane module.
Obtained graphene heating membrane module is according to GB/T 7287-2008《Infrared radiation heater test method》With
GB/T4208-2008《Waterproofing grade test method》It is tested for the property.Test item, test method and test result is as follows：
As seen from the above table, using grapheme material as host conductive agent, prepared graphene heats membrane module
Operating voltage<12V, resistance are 3-5 Ω, cold insulation resistance>300M Ω, hot insulation resistance>200M Ω, temperature uniformity
3 DEG C of <, in addition maximum operation (service) temperature is 60 DEG C, has that heating voltage is low, heating speed is fast, planar heating, energy-saving safe it is excellent
Point.
Use above specific example is expounded the present invention, is merely used to help understand the present invention, not to
The limitation present invention.The design of those skilled in the art according to the present invention can also be made and several simply push away
It drills, deform or replaces.These are deduced, deformation or alternative are also fallen into scope of the presently claimed invention.
Claims (10)
1. a kind of graphene heating film, which is characterized in that the graphene heating film include organic macromolecule-based film and be located at institute
The heating line at least one surface of organic polymer basement membrane is stated, the heating line is by applying graphene conductive slurry
It is added at least one described surface and is solidified to form.
2. graphene heating film according to claim 1, which is characterized in that the graphene conductive slurry includes epoxy official
Graphene 1-10 parts by weight, epoxy resin 4-15 parts by weight, the epoxy-modified siloxanes 2-6 parts by weight, epoxy-reactive of energyization
Diluent 2-6 parts by weight and latent curing agent 0.1-0.8 parts by weight.
3. graphene heating film according to claim 2, which is characterized in that the graphene conductive slurry also includes through silicon
The coupling agent modified conductive black 5-20 parts by weight of alkane, tension silk agent 0.2-1 parts by weight and 0.05-0.2 parts of antioxidant.
4. graphene heating film according to any one of claim 1-3, which is characterized in that the organic polymer basement membrane
For PET film, described apply is completed by way of silk-screen printing, and the solidification is by 100-150 DEG C of infrared heating
It 5-12 minutes completes.
5. a kind of graphene heats membrane module, which is characterized in that the graphene heating membrane module includes according to claim 1-4
Any one of described in graphene heating film, the first heat conductive silica gel, the second heat conductive silica gel, the first graphene thermally conductive sheet, the second stone
Black alkene thermally conductive sheet, the first organic polymer insulating film and the second organic polymer insulating film, wherein first heat conductive silica gel position
In the top of the graphene heating film, the first graphene thermally conductive sheet is located at the top of first heat conductive silica gel, described
First organic polymer insulating film is located at the top of the first graphene thermally conductive sheet, and second heat conductive silica gel is located at the stone
The lower section of black alkene heating film, the second graphene thermally conductive sheet are located at the lower section of second heat conductive silica gel, and described second is organic
Polymer insulating film is located at the lower section of the second graphene thermally conductive sheet.
6. graphene according to claim 5 heats membrane module, which is characterized in that the graphene heating membrane module also wraps
Include temperature sensor, wherein the temperature sensor between first heat conductive silica gel and the first graphene thermally conductive sheet or
Between second heat conductive silica gel and the second graphene thermally conductive sheet.
7. graphene according to claim 6 heats membrane module, which is characterized in that the temperature sensor is commercially available thin slice
Type temperature sensor.
8. graphene according to claim 6 or 7 heats membrane module, which is characterized in that the first graphene thermally conductive sheet
It is commercially available graphene thermally conductive sheet with the second graphene thermally conductive sheet.
9. graphene according to claim 6 or 7 heats membrane module, which is characterized in that first heat conductive silica gel and the
Two heat conductive silica gels are commercially available heat conductive silica gel.
10. graphene according to claim 6 or 7 heats membrane module, which is characterized in that first organic polymer is exhausted
Velum and the second organic polymer insulating film are commercially available PE insulating film.
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| CN112757724B (en) * | 2020-12-29 | 2022-05-20 | 杭州宜联研仿科技有限公司 | Preparation method of flexible metal-based graphene electrothermal material |
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