CN106255238A - A kind of Graphene thermo electric material and application thereof - Google Patents
A kind of Graphene thermo electric material and application thereof Download PDFInfo
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- CN106255238A CN106255238A CN201610079331.8A CN201610079331A CN106255238A CN 106255238 A CN106255238 A CN 106255238A CN 201610079331 A CN201610079331 A CN 201610079331A CN 106255238 A CN106255238 A CN 106255238A
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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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Abstract
The invention provides a kind of Graphene thermo electric material and application thereof.A kind of Graphene thermo electric material, mainly it is made up of Graphene, other material with carbon elements and solvent, wherein Graphene is 0.5-10:1 with the weight ratio of other material with carbon elements, preferably 2-10:1, it is preferably 5-10:1, other material with carbon elements include the combination of one or more of carbon fiber, graphite, CNT, the preferred carbon fiber of other material with carbon elements.The Graphene thermo electric material of the present invention have energy-conservation, light, pliability is good, can large area uses, the most oxidizable, electrical and thermal conductivity performance is high, the advantage such as applied widely, can be used for manufacturing the multiple fields such as clothing, personal care, air equipment, armarium, domestic heating equipment, automobile.
Description
Technical field
The present invention relates to thermo electric material field, in particular to a kind of Graphene thermo electric material and application thereof.
Background technology
Day by day serious along with the constantly exhausted of the non-renewable resources such as coal, oil, natural gas and environmental pollution, grinds
Study carefully and develop renewable, green clean energy resource and supporting industrial goods thereof, article of everyday use seems the most urgent and important.Too
Sun energy, nuclear power, water power and wind-powered electricity generation replace non-renewable resources and generate heat under the overall background generated electricity, and numerous industrial goods and article of everyday use are also
Increasingly focus on energy-saving and emission-reduction.It addition, along with the demand of people's performance portable and wearable to product promotes, low energy consumption, light
Integrated product has shown huge market potential.
Graphene is as emerging material with carbon element, while there is electric-conductivity heat-conductivity high performance, have light, pliability good, can
Large area uses, the advantage such as the most oxidizable, has the far-infrared radiated property more highlighted than other material with carbon element, the heating made
Components and parts have the advantages that sendible temperature is high, thermal comfort is good, and therefore Graphene possesses the feature of excellent thermo electric material.But city
The energy saving of the thermo electric material made with Graphene on face is not the most fine.
In view of this, the special proposition present invention.
Summary of the invention
The first object of the present invention is to provide a kind of Graphene thermo electric material, and described Graphene thermo electric material has gently
Just, pliability good, can large area uses, the most oxidizable, electrical and thermal conductivity performance is high, the advantage such as applied widely, can be used for manufacturing
The multiple fields such as clothing, personal care, air equipment, armarium, household electronic products, heating equipment, automobile.
The second object of the present invention be to provide described Graphene thermo electric material as matrix surface electro-thermal coatings
Application, this application improves the comprehensive electric heating property of current material.
In order to realize the above-mentioned purpose of the present invention, spy by the following technical solutions:
A kind of Graphene thermo electric material, is mainly made up of Graphene, other material with carbon elements and solvent, wherein Graphene and other
The weight ratio of material with carbon element is 0.5-10:1, preferably 2-10:1, preferably 5-10:1, and other material with carbon elements include carbon fiber, graphite, carbon
The combination of one or more of nanotube, the preferred carbon fiber of other material with carbon elements.
As a example by carbon fiber, carbon fiber and Graphene belong to carbon-based material together, and the compatibility of the two and associativity are good, are difficult to oxygen
Change, good stability.For graphene/carbon fiber-incorporated slurry, carbon fiber has soft machinability, therefore with suitably
Ratio is mixed into carbon fiber can improve the machinability of Graphene so that it is be readily able to processing, it is easy to form membrane structure, the most again
Will not reduce the heat-conductivity conducting of Graphene, both can work in coordination with enhancing heat-conductivity conducting on the contrary, and this is and existing Graphene electricity
One of important difference of hot material, meanwhile, the introducing of carbon fiber can also reduce the cost of Graphene thermo electric material, can promote
Application；Solvent can good with optional dissolved degree, safe and harmless, reagent that the compatibility is good, consumption according to the actual requirements depending on.It addition,
When carbon fiber is combined in advance with matrix, Graphene, as slurry, provides a stable conduction can to the attachment of slurry
Supporter.
In like manner, other material with carbon element such as Graphene and graphite, CNT etc. is mixed and made into thermo electric material and can also reach above-mentioned
Technique effect.
Through inspection, the graphene conductive heat-conducting layer thermal conductivity of the present invention can reach more than 1000W/m k, and resistivity is 0.5
Ω/sq～5 Ω/sq, (1-5V) can work, compared with the energy-conservation 50%-70% of market Electric radiant Heating Film in lower voltage range.
High-temperature that the thermo electric material of the present invention is mainly used under the heating under lower pressure, especially 1-5V (room temperature～
130 DEG C) work, certainly, if the modifying agent of interpolation is reasonable, it is also possible to for hyperbaric heating.Its application process has multiple, both may be used
With by printing, scratch, spray, impregnate, the process combining such as pressing plays effect on the surface of other material, it is also possible to other
Material mixes together makes Electric radiant Heating Film, such as paper pulp.
It addition, above-mentioned thermo electric material can be used for multiple fields, both can be applicable to the heating folder of household goods medical, daily
Layer is it can also be used to warm, the warmhouse booth of building floor heating wall etc., it is possible to the naval vessels that are applied to work under low temperature environment, vehicle, aircraft
Deng pipeline, instrument, the deicing of parts.
Above-mentioned Graphene thermo electric material can also improve further:
Preferably, the concentration of described Graphene is 2mg/mL～200mg/mL.
First being that such concentration has enough viscosityes, solid difficulty is low, secondly at cost of material and conductive and heat-conductive
Higher cost performance, more preferably 50mg/mL～200mg/mL, 100mg/mL～150mg/mL can be obtained between property.
Preferably, one or more mixing during described solvent is water, hydrophilic solvent.The low cost of both solvents,
Safe and harmless, it is adaptable to multiple matrix, described hydrophilic solvent includes alcohols solvent, it is preferred that described alcohol is ethanol.
Preferably, described Graphene thermo electric material also includes dispersant, and dispersant can improve Graphene in the solution
Dispersion, it is ensured that the structure of solidification has homogeneous physicochemical property；Preferably, described dispersant is that phenylethylene-maleic anhydride is total to
Polyester, polyvinylpyrrolidone, polyethenoxy ether metacrylic acid ester, polyoxyethylene ether acrylate, polyethenoxy ether propylene
One or more mixing in acid esters, polyoxypropylene ether metacrylic acid ester.Above dispersant can reach to make slurry in water system
Solvent middle and high concentration and homodisperse effect.
Preferably, described Graphene thermo electric material also includes modifying agent, with satisfied different demands, such as, improves conduction, machine
The performances such as tool.
Preferably, one or more in far-infrared finishing agent, defoamer, adhesion promoter of described modifying agent；
One or more in titanium oxide, zirconium oxide, yittrium oxide, zinc oxide, aluminium oxide of described far-infrared finishing agent.
The normal emittance of above far-infrared finishing agent reaches more than 0.85, makes product have more excellent far infrared performance；
One or more in silicone oil, tallow amide, aluminium stearate of described defoamer.Above defoamer can increase
Add the mobility of slurry, carrier coats the uniformity and improves the heating uniformity of electro-thermal coatings.
Described adhesion promoter is selected from aminopropyl trimethoxysilane, polydimethylsiloxane, acrylic acid dicyclo penta 2
One or more in allyl ester monomer.Above adhesion promoter can make slurry more be firmly adhered on carrier.
Preferably, described Graphene is biomass Graphene.Described biomass Graphene is prepared by biomass；Preferably
The cellulose that described biomass Graphene is obtained by biomass is prepared.
The number of plies is more than 10 layers, and thickness is the cellular lamellar structure of the hexatomic ring of carbon, referred to as graphene nanometer sheet within 100nm
Layer；Being more than 10 layers with the number of plies that biomass are prepared for carbon source, thickness is the cellular lamellar structure of the hexatomic ring of carbon within 100nm,
It is referred to as biomass graphene nano lamella；The number of plies is the cellular lamellar structure of hexatomic ring of 1～10 layer of carbon, referred to as Graphene；With
Biomass are the cellular lamellar structure of the hexatomic ring that the number of plies is 1～10 layer of carbon prepared by carbon source, referred to as biomass Graphene.
Graphene of the present invention includes graphene nano lamella and Graphene, farther includes biomass graphene nano
Lamella and biomass Graphene.
Graphene of the present invention can be obtained by different preparation methoies, such as mechanical stripping method, epitaxial growth method, change
Learn vapor deposition method, graphite oxidation reducing process, it is also possible to be by biomass resource hydrothermal carbonization method, and in prior art
Graphene prepared by other method.But, which kind of method is all difficulty with preparing stricti jurise on a large scale in theory
Graphene, such as the Graphene that prior art prepares can exist some impurity element, carbon other homoatomic different
Body or the number of plies non-the monolayer even graphene-structured of multilamellar (such as 3 layers, 5 layers, 10 layers, 20 layers etc.), the present invention is utilized
Graphene also includes the Graphene on above-mentioned non-critical theory of meaning.
Preferably, the described biomass any a kind or the combination of at least 2 kinds in agriculture and forestry organic waste material and/or plant.
Preferably, any a kind or the combination of at least 2 kinds during described plant is needlebush and/or leaf wood.
Preferably, described agriculture and forestry organic waste material is corn stalk, corn cob, kaoliang stalk, megasse, bagasse, furfural dregs, xylose
Any a kind or the combination of at least 2 kinds in slag, wood flour, cotton stalk, shell and phragmites communis.
Preferably, described agriculture and forestry organic waste material is corn cob.
Except above-mentioned biomass are enumerated in addition to, biomass of the present invention can be that those skilled in the art can obtain
Any biomass resource known, the present invention does not continues to repeat.
Biomass Graphene of the present invention refers to the Graphene prepared with biomass for carbon source, concrete with biology
Matter is that carbon source prepares process this area of Graphene it has been reported that typical but non-limiting include CN104724699A, this
Bright repeat no more.
Preferably, described Graphene thermo electric material is tabular, column or fabric shape.
The shape of Graphene thermo electric material is mainly determined by its purposes, such as, when being used for making functional fabric, typically
For fabric shape；When for family or industrial heating, generally column, and it is generally tabular when the deicing of plant equipment.
It is of course also possible to according to actual techniques demand or aesthetic, be designed to arbitrary shape.
The preparation method that above Graphene thermo electric material makes sheet film shape may is that and mixed by all raw materials according to formula
Pulping, then shape and technique according to presetting are attached on carrier, final curing or dry.Can also be: first by carbon
Fiber and matrix slurry (referring mainly to paper pulp) carry out composite papermaking, then slurry Graphene and other auxiliary agents being mixed into is according in advance
If technique is attached on matrix, final curing or dry.
Graphene thermo electric material mentioned above, as the application of matrix surface electro-thermal coatings, is mainly used to improve material
Comprehensive electric heating property, make material on the basis of there is the advantages such as electrical and thermal conductivity performance is high, applied widely, also have light,
Pliability is good, can large area use, the advantage such as the most oxidizable.
Concrete application process can improve as follows:
Preferably, described electro-thermal coatings also includes the circuit layer of its surface printing.
The compatible materials of this structure is produced in enormous quantities, i.e. prints many height on large-area graphene conductive heat-conducting layer
Circuit, then cut into little element, and be more easy to realize quality control.It addition, in order to improve circuit layer leading on graphene layer
Electrical property, it is also possible to add modifying agent when making graphene layer and improve dispersion or the viscosity of Graphene.
Preferably, described electro-thermal coatings surface attachment phase-change material layers, first by Graphene thermo electric material and phase-change material
Combining, maximize favourable factors and minimize unfavourable ones, the advantage making full use of both, the thermo electric material of composition had both possessed the electric heating that Graphene is excellent
Can, possess again good heat storage performance.Secondly, the tectonic relationship being layering is used, it is to avoid the performance interference between material.
When electro-thermal coatings surface printing circuit layer, can be layer printed circuit board directly and phase change material contacts, it is also possible to
It is graphene layer and phase change material contacts, practical situation can be regarded and adjust.
Preferably, described phase-change material layers is made up of inorganic phase-changing material, organic phase change material goods polymeric phase change material；
Preferably, one or more in sodium sulfate class, sodium acetate class, calcium chloride, phosphoric acid salt of described inorganic phase-changing material,
Described organic phase change material selected from paraffin class, fatty acid or its lipid, higher aliphatic hydro carbons, alcohols, arene, amide-type and
One or more of polyhydroxy carbonic acid apoplexy due to endogenous wind, described polymeric phase change material TPO, polymeric polyalcohols, polyene alcohols, poly-
Olefin(e) acid class, polyamide-based in one or more.
In above material, the solid-solid phase transition material layer scope of application is wider, it is to avoid the flowing of solid-liquid phase change material liquid body
Restriction, and with polyalcohols solid-solid phase transition material layer as optimum, its cost is relatively low.
Preferably, encapsulate with insulant between described electro-thermal coatings and described phase-change material layers, described phase-change material layers
Surface with insulant encapsulate, setting up insulating protective layer is the safety in order to improve thermo electric material, in order to be directly used in people
Body.Insulating protective layer can use plastics or resinous material, different according to application, this insulant can add 1 ‰-
The oxytolerant heat-resistant agent of 3 ‰, it is preferable that described oxytolerant heat-resistant agent selected from diphenyl acrylate, 2,5-ditert-butylhydro quinone,
One or more in distearyl pentaerythritol diphosphite.
Preferably, described matrix surface is welded with circuit layer.Circuit position is set typically depending on application.
Preferably, described matrix includes the solid encasement needing to play thermal effect, it is preferred that described matrix includes knitting
Thing, building, Plastic, naval vessels, aircraft, deicing vehicle；Matrix be also according to material applications depending on, the compound of interlayer can be led to
Cross and print, scratch, spray, impregnate and the technique such as pressing realizes.
It addition, the application according to Graphene thermo electric material of the present invention is different, it has with the method for other Material cladding
Institute is different, the general following two method that uses:
Method one is printed on described graphene layer surface mainly for circuit layer, comprises the following steps:
Step A: according to the formula of described graphene conductive heat-conducting layer, all mixed raw materials are obtained Graphene slurry；
Step B: by described Graphene impregnating slurry, the surface of printing, spray or press to described base layer, dried shape
Become graphene layer；
Step C: at the surface printing circuit of described graphene layer, forms circuit layer；
Step D: described circuit layer surface impregnation, print, spray or pressing phase-change material, obtain product.
Preferably, impregnating, print, spray or after pressing phase-change material, it is additionally included in the surface encapsulation of phase-change material
Thermal insulation layer.
Preferably, the method being dried in step B is: dries or is vacuum dried.
Method two is welded on matrix mainly for circuit layer, comprises the following steps:
Step I: according to the formula of described graphene conductive heat-conducting layer, all mixed raw materials are obtained Graphene slurry；
Step II: at the surface printing circuit of matrix, forms circuit layer；
Step III: by described Graphene impregnating slurry, the surface of printing, spray or press to described matrix, dried shape
Become graphene layer；
Step IV: described graphene layer surface impregnation, print, spray or pressing phase-change material, obtain product.
Preferably, formed graphene layer step after and impregnate, print, spray or pressing phase-change material step it
Before also include: at the surface encapsulation insulating protective layer of described graphene layer.
Above two method all can be realized by conventional plant equipment, and flow process is simple, therefore easily realizes extensive
Produce.
Additionally also having a kind of situation is slurry and the matrix slurry (referring mainly to paper pulp) of Graphene thermo electric material to be blended in
Together, it is then cured into integrative-structure, forms Electric radiant Heating Film；Or carbon fiber is individually mixed with matrix slurry (referring mainly to paper pulp)
Solidify as carrier together, subsequently by Graphene thermo electric material slurry by being impregnated into matrix and being dried, form Electric radiant Heating Film.
The most only list the preparation method of Graphene thermo electric material spin-off, it is impossible to exhaustive, therefore the material of the present invention
Material is not to be limited in the range of use above.
Compared with prior art, the invention have the benefit that
(1) material softness can processing type strong；
(2) material conducts heat performance is excellent；
(3) material has good heat storage performance；
(4) material energy-saving environmental protection；
(5) materials application scope is wide；
(6) light portable；
(7) material preparation method is simple, production suitable for industrialized.
Accompanying drawing explanation
In order to be illustrated more clearly that the specific embodiment of the invention or technical scheme of the prior art, below will be to specifically
In embodiment or description of the prior art, the required accompanying drawing used is briefly described, it should be apparent that, in describing below
Accompanying drawing is some embodiments of the present invention, for those of ordinary skill in the art, before not paying creative work
Put, it is also possible to obtain other accompanying drawing according to these accompanying drawings.
The structure of the thermo electric material that Fig. 1 provides for the embodiment of the present invention 3；
The structure of a kind of thermo electric material that Fig. 2 provides for the present invention；
The structure of a kind of thermo electric material that Fig. 3 provides for the present invention；
The structure of the thermo electric material that Fig. 4 provides for the embodiment of the present invention 4；
Reference:
1-base layer；2-electrode；The thermally conductive layer of 3-graphene-containing
4-thermal insulation layer 5-phase-change material layers 6-insulating protective layer
7-circuit layer.
Detailed description of the invention
Below in conjunction with embodiment, embodiment of the present invention are described in detail, but those skilled in the art will
Understanding, the following example is merely to illustrate the present invention, and is not construed as limiting the scope of the present invention.In embodiment unreceipted specifically
Condition person, the condition advised according to normal condition or manufacturer is carried out.Agents useful for same or instrument unreceipted production firm person, be
Can be by the commercially available conventional products bought and obtain.
The percentage ratio of the various modifying agent added in Examples below refers both to relative to slurry total amount.
Prepare Graphene A:
First prepare cellulose:
(1) by after wheat straw comminution pretreatment, the dense formic acid for 80wt% of total acid and the organic acid solution pair of acetic acid are used
Wheat straw after process carries out steaming and decocting, and in the organic acid solution of the present embodiment, acetic acid is 1:12 with the mass ratio of formic acid, and is adding
Hydrogen peroxide (the H accounting for wheat straw raw material 1wt% is added before entering raw material2O2) as catalyst, control reaction temperature 120 DEG C, instead
Answering 30min, solid-liquid mass ratio is 1:10, and the reactant liquor obtained carries out solid-liquid separation for the first time；
(2) solid first time solid-liquid separation obtained adds the dense formic acid for 75wt% of total acid and the organic acid solution of acetic acid
Carrying out acid elution, the most above-mentioned total acid is dense for adding the peroxide accounting for wheat straw raw material 8wt% in the organic acid solution of 75wt%
Change hydrogen (H2O2) it is 1:12 as the mass ratio of catalyst and acetic acid with formic acid, controlling temperature is 90 DEG C, wash time 1h, solid-liquid
Mass ratio is 1:9, and reactant liquor carries out second time solid-liquid separation；
(3) collect the liquid obtained with second time solid-liquid separation for the first time, in 120 DEG C, under 301kPa, carry out High Temperature High Pressure
Evaporation, until being evaporated, using in the formic acid obtained and acetic acid vapor condensing reflux to the reactor of step (1) as cooking liquor, use
Steaming and decocting in step (1)；
(4) collecting the solid that second time solid-liquid separation obtains, and wash, controlling washing temperature is 80 DEG C, washing slurry
Dense for 6wt%, and the washing slurry obtained is carried out third time solid-liquid separation；
(5) collecting the liquid that third time solid-liquid separation obtains, carry out water, acid rectification, the mix acid liquor obtained is back to step
Suddenly be used for the steaming and decocting of step (1) in the reactor of (1) as cooking liquor, the Water circulation obtained washes water with water in step (5)；
(6) collect the third time solid that obtains of solid-liquid separation row filter of going forward side by side and obtain required screened stock cellulose.
Then Graphene is prepared with cellulose prepared as above for raw material:
(1) cellulose mixture of 1:1 in mass ratio and ferrous chloride, at 150 DEG C stirring carry out catalytic treatment 4h, be dried to
Presoma moisture 10wt%, obtains presoma；
(2)N2In atmosphere, with 3 DEG C/min speed, presoma is warming up to 170 DEG C, is incubated 2h, temperature programming afterwards to 400
DEG C, it is incubated 3h, is warming up to 1200 DEG C afterwards, after insulation 3h, obtain crude product；The heating rate of described temperature programming is 15 DEG C/min；
At (3) 55～65 DEG C, by crude product through sodium hydroxide solution that over-richness is 10%, 4wt% chlorohydric acid pickling after, water
Wash and obtain biomass Graphene, be designated as Graphene A.
Preparation biomass Graphene B:
Use the method for embodiment 10 in the patent of Publication No. CN104724696A, particularly as follows: collect straw, process dry
Shred into small pieces after Jing, be immersed in ethanol solution, at the uniform velocity stir 5 hours with the rotating speed of 100r/min；Then solution is shifted
To high speed centrifuge, rotating speed is set to 3000r/min, and centrifugation time is 20 minutes, takes off the broken sample of layer after terminating.Normal temperature and pressure
Under, broken sample is loaded in the Tissue Culture Dish of a diameter of 15cm, be placed in air inlet, regulate flow parameter, arranging wind speed is 6m/
S, air quantity is 1400m3/ h, keeps ventilation state 12 hours；Tube furnace is warmed up to 1300 DEG C, is passed through inert gas shielding, keeps
30 minutes；Dried broken sample is positioned in tube furnace, heats 5 hours, after being cooled to room temperature, obtain overburden ratio obvious
Biomass Graphene, is designated as Graphene B.
Prepare Graphene C:
Use the method for embodiment 1 in the patent of Publication No. CN105217621A, particularly as follows:
(1) by 2g graphite powder and 3g potassium dithionate, 3g phosphorus pentoxide and the mixing of 12mL concentrated sulphuric acid in reactor
System is reacted, stirs 4 hours under 80 DEG C of water bath condition, to forming dark blue solution, cooling, sucking filtration, obtain pre-oxygen after drying
The graphite changed；
(2) the graphite oxide 2g obtained by step (1) is taken in three-neck flask, dense with 150mL under conditions of ice-water bath
Sulfuric acid solution, is gradually added into the potassium permanganate of 25g, stirs 2 hours；
(3) three-neck flask of above-mentioned steps (2) is proceeded to oil bath, be warming up to 35 DEG C, stir 2 hours, continue stirring and press
30wt% hydrogen peroxide and the mixed solution of deionized water is added according to the amount that volume ratio is 1:15；Sucking filtration, divides by 4mL mass respectively
Number be 10% dilute hydrochloric acid and deionized water clean 1 time, centrifugal, obtain the graphene oxide aoxidized for the first time after drying；
(4) by the graphene oxide 2g of preparation in step (3) again under conditions of ice-water bath concentrated sulphuric acid with 50mL molten
Liquid is mixed in three-neck flask, is gradually added into the KMnO of 8g4, stir 1 hour；
(5) three-neck flask of above-mentioned steps (4) is proceeded to oil bath, be warming up to 40 DEG C, stir 1 hour, then proceed to heat up
To 90 DEG C, after stirring 1 hour, continue stirring and add 30wt% hydrogen peroxide and deionized water according to the amount that volume ratio is 1:7
Mixed solution, continue stirring 6 hours after cool down, sucking filtration, respectively with the dilute hydrochloric acid that 4mL mass fraction is 10% and deionized water
Clean 2 times, centrifugal, obtain the graphene oxide of size uniformity after drying, be designated as Graphene C.
Embodiment 1:
(1) by Graphene A and carbon fiber according to the ratio of 0.5:1, be equipped with the styrene of a certain amount of dispersant 1wt%-
Maleic anhydride ester, 0.1wt% silicone oil and the aminopropyl trimethoxysilane of 2wt% are also dissolved in ethanol, it is thus achieved that concentration is
The graphene composite material slurry of 2mg/mL.
(2) above-mentioned pulp spraying is applied to naval vessels ship pipeline, satellite antenna, the surface such as aircraft, automobile component, the most dry
Dry.
(3) it is dried complete heating film access low-voltage circuit by above-mentioned.
(4) in one layer of heat conduction protective layer of heating film surface spraying.
The pipeline of naval vessels that the present embodiment can be applicable to work under low temperature environment, vehicle, aircraft etc., instrument, parts
Deicing.(1～5V) purpose that surface is quickly heated can be realized under the conditions of small voltage.
Embodiment 2:
(1) Graphene A is mixed with the ratio uniform of 2:1 with carbon fiber, be equipped with the benzene second of a certain amount of dispersant 1wt%
Alkene-maleic anhydride ester, 0.1wt% silicone oil and the aminopropyl trimethoxysilane of 2wt% are also dissolved in ethanol, it is thus achieved that concentration
Graphene composite material slurry for 10mg/mL.
(2) above-mentioned pulp spraying is applied to naval vessels ship pipeline, satellite antenna, the surface such as aircraft, automobile component, the most dry
Dry.
(3) it is dried complete heating film access low-voltage circuit by above-mentioned.
(4) in one layer of heat conduction protective layer of heating film surface spraying.
The pipeline of naval vessels that the present embodiment can be applicable to work under low temperature environment, vehicle, aircraft etc., instrument, parts
Deicing.(1～5V) purpose that surface is quickly heated can be realized under the conditions of small voltage.
Embodiment 3
(1) Graphene A is combined with the ratio uniform of 3:1 with carbon fiber, adds the far-infrared finishing agent (oxygen of 0.5wt%
Change titanium), and add the aminopropyl trimethoxy silicon of 1wt% styrene-maleic anhydride copolymer ester, the silicone oil of 0.1wt% and 2%
Alkane, is well-dispersed in water, it is thus achieved that the slurry of 100mg/mL.
(2) at fabric lining two ends pressing welding copper chaff as electrode.
(3) slurry being coated uniformly on fabric lining surface and forms thickness is the film of 0.1mm, forms stone after drying or drying
Ink alkene radiation heating film.
(4) degasification, uses conductive plastic material once to encapsulate subsequently.
(5) cut, milling target, it is thus achieved that wiring solder joint, after wiring use insulant close contact.
(6) after phase-change material (sodium acetate) thin film that the outside stacking thickness of heat-conducting plastic is 0.5mm, insulating barrier is used to enter
The overall secondary encapsulation of row.
The Electric radiant Heating Film that the present embodiment acquisition has excellent far-infrared functional, heat storage capacity is good, energy-conservation, resistance is stable, favorably
Comfortable in health.Can be applicable to the heating interlayer of household goods medical, daily.
The product structure that this embodiment obtains is as it is shown in figure 1, include base layer 1 (i.e. fabric lining), electrode 2, graphitiferous
The thermally conductive layer 3 of alkene, thermal insulation layer 4, phase-change material layers 5, insulating protective layer 6.
On this basis, it is also possible to the lower surface at base layer 1 is symmetrical arranged thermal insulation layer 4, as shown in Figure 2；Or
Lower surface at base layer 1 is symmetrical arranged thermal insulation layer 4, phase-change material layers 5, as shown in Figure 3.
Embodiment 4:
(1) Graphene A is mixed with the ratio uniform of 5:1 with carbon fiber, be equipped with the polyvinyl pyrrole of a certain amount of 2wt%
Alkanone, the tallow amide of 0.05wt% and the polydimethylsiloxane of 1wt% are also dissolved in ethanol, it is thus achieved that concentration is 150mg/
The graphene composite material slurry of mL.
(2) making heat-resisting conductive paper by compound for the ratio of heat-resisting paper pulp and above-mentioned biomass Graphene slurry 1:1, thickness can
Regulate and control according to actual needs.
(3) copper slurry (silver slurry) is used to go out electrode and circuit at heat-resisting conductive paper surface printing.Then heating film makes complete.
(4) the polyalcohols solid-solid phase transition material thin film (tetramethylolmethane PE) selecting suitable phase transition temperature is fitted in heating
Film surface.
(5) degasification, subsequently use insulating barrier carry out overall package.
The heating film that the present embodiment obtains is light, and pliability is good, it is adaptable to little work voltage power supply, the suitable people of operating temperature
Body bears.Can be widely applied to clothing, personal care's wearable items.
This embodiment obtain product structure as shown in Figure 4, including the thermally conductive layer 3 of graphene-containing, circuit layer 7, phase
Change material layer 5, insulating protective layer 6.
Embodiment 5:
(1) by Graphene A and carbon fiber according to the ratio of 10:1, be equipped with 0.5wt% polyethenoxy ether acrylate,
The silicone oil of 0.1wt% and the aminopropyl trimethoxysilane of 2wt% are the most soluble in water, are subsequently added the far-infrared finishing of 0.1%
Agent (titanium oxide), it is thus achieved that concentration is the Graphene composite mortar of 100mg/mL.
(2) fabric lining, expanded material are sufficiently impregnated with in above-mentioned slurry, then pass through extruding or filtration, drying etc.
Processing step.
(3) then at the graphene layer surface spraying phase-change material (tetramethylolmethane PE) dried.
Above-mentioned fabric lining or expanded material are respectively applied to medicated clothing, the inner surface of implant or interlayer, can be according to reality
Border situation chooses whether external circuits.
The present embodiment applies far-infrared radiated property and the bacteriostasis property of biomass Graphene self, improve medicated clothing,
Performance is warmed up in body-sensing comfortableness and the warming increasing of the type products such as automotive seat.
Embodiment 6:
(1) Graphene B is mixed with the ratio uniform of 5:1 with carbon fiber, be equipped with the benzene second of a certain amount of dispersant 1wt%
Alkene-maleic anhydride ester, 0.1wt% silicone oil and the aminopropyl trimethoxysilane of 2wt% are also dissolved in ethanol, it is thus achieved that concentration
Graphene composite material slurry for 50mg/mL.
(2) above-mentioned pulp spraying is applied to naval vessels ship pipeline, satellite antenna, the surface such as aircraft, automobile component, the most dry
Dry.
(3) it is dried complete heating film access low-voltage circuit by above-mentioned.
(4) in one layer of heat conduction protective layer of heating film surface spraying.
The pipeline of naval vessels that the present embodiment can be applicable to work under low temperature environment, vehicle, aircraft etc., instrument, parts
Deicing.(1～5V) purpose that surface is quickly heated can be realized under the conditions of small voltage.
The present embodiment has the structure of similar embodiment 4.
Embodiment 7:
(1) Graphene C is mixed with the ratio uniform of 5:1 with carbon fiber, be equipped with a certain amount of dispersant 0.5wt% polyoxy
The acrylic acid DCPA monomer of vinyl Ether methacrylate, the aluminium stearate of 0.01wt% and 3% is the most soluble in water,
Obtain the graphene composite material slurry that concentration is 100mg/mL.
(2) in above-mentioned biomass Graphene slurry, the far-infrared finishing agent (aluminium oxide) of 3% is added, as conductive oil
Ink, by ink print on heat resistant plastice substrate.
(3) use copper slurry or silver slurry print electrode or direct pressing Copper Foil as electrode subsequently.
(4) degasification, uses conductive plastic material once to encapsulate subsequently.
(5) cut, milling target, it is thus achieved that wiring solder joint, after wiring use insulant close contact.
(6) solid-solid phase transition material (tetramethylolmethane PE) selecting suitable phase transition temperature is film adhered on heating film surface.
(7) degasification, subsequently use insulating barrier carry out overall package.
The heating Electric radiant Heating Film for building that the present embodiment acquisition has excellent far-infrared functional, heat storage capacity is good, energy-conservation.Have
Electric conversion efficiency is high, and radiant heat accounting example is big, the feature that sendible temperature is high, thermal comfort is good.Be applicable to build floor heating wall warm,
Warmhouse booth etc..
The present embodiment has the structure of similar embodiment 3.
Embodiment 8:
(1) Graphene A is mixed with the ratio uniform of 5:1 with graphite, be equipped with the polyvinylpyrrolidine of a certain amount of 2wt%
Ketone, the tallow amide of 0.05wt% and the polydimethylsiloxane of 1wt% are also dissolved in ethanol, it is thus achieved that concentration is 150mg/mL
Graphene composite material slurry.
(2) making heat-resisting conductive paper by compound for the ratio of heat-resisting paper pulp and above-mentioned biomass Graphene slurry 1:1, thickness can
Regulate and control according to actual needs.
(3) copper slurry (silver slurry) is used to go out electrode and circuit at heat-resisting conductive paper surface printing.Then heating film makes complete.
(4) the polyalcohols solid-solid phase transition material thin film (tetramethylolmethane PE) selecting suitable phase transition temperature is fitted in heating
Film surface.
(5) degasification, subsequently use insulating barrier carry out overall package.
The heating film that the present embodiment obtains is light, and pliability is good, it is adaptable to little work voltage power supply, the suitable people of operating temperature
Body bears.Can be widely applied to clothing, personal care's wearable items.
Embodiment 9:
(1) Graphene A is mixed with the ratio uniform of 5:1 with CNT, be equipped with the polyethylene pyrrole of a certain amount of 2wt%
Pyrrolidone, the tallow amide of 0.05wt% and the polydimethylsiloxane of 1wt% are also dissolved in ethanol, it is thus achieved that concentration is
The graphene composite material slurry of 150mg/mL.
(2) making heat-resisting conductive paper by compound for the ratio of heat-resisting paper pulp and above-mentioned biomass Graphene slurry 1:1, thickness can
Regulate and control according to actual needs.
(3) copper slurry (silver slurry) is used to go out electrode and circuit at heat-resisting conductive paper surface printing.Then heating film makes complete.
(4) the polyalcohols solid-solid phase transition material thin film (tetramethylolmethane PE) selecting suitable phase transition temperature is fitted in heating
Film surface.
(5) degasification, subsequently use insulating barrier carry out overall package.
The heating film that the present embodiment obtains is light, and pliability is good, it is adaptable to little work voltage power supply, the suitable people of operating temperature
Body bears.Can be widely applied to clothing, personal care's wearable items.
Above example 1 to 9 for mainly tabular or the thermo electric material of fabric shape, Coating combination mainly uses spraying
Technique, can also use process for pressing, but also can add thickening agent and reduce pressing difficulty during practical operation, and for column
The material of (i.e. electric wire), the sequencing of technique and auxiliary agent and condition that often step operation adds are referred to above-described embodiment, but
Associated methods between being every layer more preferably uses infusion process, such as, is impregnated in phase-change material by graphene layer, makes corresponding liquid
Physical ability is uniformly attached to graphene layer surface.
Experimental example
The electric heating property of graphene layer in the product that test above example 1-9 obtains, employing heating technique index (according to
GB/T4564-2008 nonmetal basal body infrared radiation heater general technical specifications detects), and compare with prior art, main
Comparative indices is wanted to have: electrical power density；Radiating surface electric-thermal radiation conversion ratio (requirement is not less than 50%)；Radiating surface temperature is uneven
Even degree (highest temperature and minimum temperature difference requirement are not more than 7 DEG C), the percentage ratio being used herein as the highest temperature and lowest temperature difference carrys out table
Show.Additionally heating-up time (being energized to the time of the highest temperature 90%, it is desirable to be not more than 10min) and resistivity are also entered by table 1 below
Go and compared.
Reference examples 1:
(1) carbon fiber and long fiber paper pulp are carried out papermaking directly as heating film according to the ratio of 3:7.
(2) it is dried complete heating film access low-voltage circuit by above-mentioned.
(3) in one layer of heat conduction protective layer of heating film surface pressing.
Table 1 test result
Wherein, embodiment 1-9 all realizes under voltage 1-5V.Reference examples 1 also records under 1-5V, and reference examples 2 is former
In patent not mentioned, reference examples 3 then could work under 220V or 380V voltage.By contrast, do not add the comparison of Graphene
Example 1 either resistance or non-uniform temperature degree are the most significantly higher, and electric radiation conversion efficiency ratio is relatively low；In reference examples 2
Parameter is less detailed, but can be seen that its energy saving is far below this patent；Reference examples 3 is to buy the product of enterprise, through actual measurement, adds
Hot degree of irregularity is higher, and running voltage is higher, and programming rate is the slowest.
Last it is noted that various embodiments above is only in order to illustrate technical scheme, it is not intended to limit；To the greatest extent
The present invention has been described in detail by pipe with reference to foregoing embodiments, it will be understood by those within the art that: it depends on
So the technical scheme described in foregoing embodiments can be modified, or the most some or all of technical characteristic is entered
Row equivalent；And these amendments or replacement, do not make the essence of appropriate technical solution depart from various embodiments of the present invention technology
The scope of scheme.
Claims (10)
1. a Graphene thermo electric material, it is characterised in that be mainly made up of Graphene, other material with carbon elements and solvent, Qi Zhongshi
Ink alkene is 0.5-10:1, preferably 2-10:1, preferably 5-10:1 with the weight ratio of other material with carbon elements, and other material with carbon elements include that carbon is fine
Dimension, graphite, the combination of one or more of CNT, the preferred carbon fiber of other material with carbon elements.
Graphene thermo electric material the most according to claim 1, it is characterised in that the concentration of described Graphene be 2mg/mL～
200mg/mL, preferably 50mg/mL～200mg/mL, preferably 100mg/mL～150mg/mL.
Graphene thermo electric material the most according to claim 1, it is characterised in that described solvent is water, hydrophilic solvent
One or more mixing, described hydrophilic solvent includes alcohols solvent, it is preferred that described alcohol is ethanol.
Graphene thermo electric material the most according to claim 1, it is characterised in that described Graphene thermo electric material also includes point
Powder, it is preferred that described dispersant is styrene-maleic anhydride copolymer ester, polyvinylpyrrolidone, polyoxyethylene ether methyl-prop
One in olefin(e) acid ester, polyoxyethylene ether acrylate, polyethenoxy ether acrylate, polyoxypropylene ether metacrylic acid ester or
Multiple mixing.
5. according to the Graphene thermo electric material described in any one of claim 1-4, it is characterised in that described Graphene thermo electric material
Also include modifying agent, it is preferred that described modifying agent is the one in far-infrared finishing agent, defoamer, adhesion promoter or many
Kind；It is highly preferred that described far-infrared finishing agent one in titanium oxide, zirconium oxide, yittrium oxide, zinc oxide, the aluminium oxide or
Multiple, one or more in silicone oil, tallow amide, aluminium stearate of described defoamer, described adhesion promoter selects
One or more in aminopropyl trimethoxysilane, polydimethylsiloxane, acrylic acid DCPA monomer.
6. the Graphene thermo electric material described in any one of claim 1-5 is as the application of matrix surface electro-thermal coatings.
Application the most according to claim 6, it is characterised in that described electro-thermal coatings also includes the circuit of its surface printing
Layer.
Application the most according to claim 6, it is characterised in that described electro-thermal coatings surface attachment phase-change material layers, preferably
, described phase-change material layers is made up of inorganic phase-changing material, organic phase change material or polymeric phase change material；It is highly preferred that institute
State one or more in sodium sulfate class, sodium acetate class, calcium chloride, phosphoric acid salt of inorganic phase-changing material, described organic
Phase-change material is selected from paraffin class, fatty acid or its lipid, higher aliphatic hydro carbons, alcohols, arene, amide-type and polyhydroxy carbon
One or more in acids, described polymeric phase change material TPO, polymeric polyalcohols, polyene alcohols, polyene acids, poly-
One or more in amide-type.
Application the most according to claim 8, it is characterised in that with absolutely between described electro-thermal coatings and described phase-change material layers
Edge material package, the surface insulant of described phase-change material layers encapsulates, it is preferred that in described insulant containing 1wt ‰-
The oxytolerant heat-resistant agent of 3wt ‰, it is highly preferred that described oxytolerant heat-resistant agent selected from diphenyl acrylate, 2,5-di-tert-butyl is to benzene
One or more in diphenol, distearyl pentaerythritol diphosphite.
10. according to the application described in any one of claim 6-9, it is characterised in that described matrix includes that needs play heating and make
Object, it is preferred that described matrix includes fabric, building, Plastic, naval vessels, aircraft, deicing vehicle；It is furthermore preferred that institute
State the complex method of matrix and described electro-thermal coatings selected from printing, scratch, spray, impregnating and pressing.
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