CN105692600B - A kind of preparation method of super soft light graphite alkene Electric radiant Heating Film - Google Patents
A kind of preparation method of super soft light graphite alkene Electric radiant Heating Film Download PDFInfo
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- C01B2204/00—Structure or properties of graphene
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Abstract
The invention discloses a kind of preparation method of super soft light graphite alkene Electric radiant Heating Film, the present invention assembles film forming using super large piece without fragment graphene oxide solution, and repairs graphene film Rotating fields at high temperature so that graphene film internal flaw is controlled preferably.Graphene film can realize the quick response to 1500 DEG C of high temperature 25 DEG C under 1V 10V in very short time 1s 10s, and temperature rate is 600 2000 DEG C of s‑1.Simultaneously there are many folds in this graphene Electric radiant Heating Film in itself, with fabulous flexibility, be applicable to various flexible devices.Therefore, this graphene Electric radiant Heating Film is simple in construction, can large area be prepared on a large scale, operating voltage safety, thermal conversion efficiency is high, and thermal conductivity is good, and response quickly, temperature can be controlled accurately, good toughness, can be used for different application environments.
Description
Technical field
The present invention relates to flexible electric heating material, more particularly to a kind of preparation method of super soft light graphite alkene Electric radiant Heating Film.
Background technology
It is most thin in known materials by two dimensional crystal material --- the graphene (graphene) that constitutes of single carbon atom layer
, it is referred to as the material of mystery, has started global research boom.Graphene has excellent electric property (electronics at room temperature
Mobility is up to 2 × 105cm2/ Vs), prominent heat conductivility (5000W/ (mK), extraordinary specific surface area (2630m2/ g), its
Young's modulus (1100GPa) and fracture strength (125GPa).Andre Geim and Konstantin Novoselov are because to stone
The contribution of black alkene research obtains Nobel prize for physics in 2010.The excellent electrical and thermal conductivity performance of graphene well beyond metal,
Graphene has the advantages that corrosion-and high-temp-resistant simultaneously, and its good mechanical performance and relatively low density more allow it to possess
The potentiality of thermo electric material field substituted metal.Because graphene large-scale processing is increasingly becoming reality, graphene film will replace gold
Belong to materials application in different fields.
Electrical resistor heating element in conventional electric heating system is typically using metal foil, film coating, resistance wire, wire netting etc.
Material.The use of most heating element heater is nichrome.However, for nichrome, still seeming in the following areas at present not
Foot：The density of nichrome is more than 8g/cm3, there is several millimeters thickness when using；Resistivity is low (~10-6 Ω/m), however it remains
Electric heating conversion efficiency low, the rate of heat addition is small, heating element heater does not have automatic constant-temperature and power back-off function so that electric heating system knot
Structure is complicated, the weak point such as thermal inertia is big；Ferrum-chromium-aluminum is Alfer, exist cold-shortness, 475 DEG C of fragility and 1000 DEG C with
On high-temperature brittleness, due to caused by high-temperature brittleness elevated temperature strength low to ultimately result in electric heating element service life short；Alloy can
Weldering property is very poor, and hardly possible is repaired.
And the graphene Electric radiant Heating Film reported at present has two kinds, one is graphene oxide Electric radiant Heating Film, using its resistance heating,
But its structural instability, there is very great fluctuation process in its heating for being, uncontrollable；Secondly being graphite film or the polyimides of firing
Film, but its flexibility is limited, will be damaged after the folding of finite number of time.
On the whole, current urgent need is developed stable, quick response, lightweight, high flexible and wide scope and fitted
Thermo electric material.
The content of the invention
The purpose of the present invention is to overcome the deficiencies in the prior art there is provided a kind of preparation side of super soft light graphite alkene Electric radiant Heating Film
Method.
The purpose of the present invention is achieved through the following technical solutions：A kind of preparation side of super soft light graphite alkene Electric radiant Heating Film
Method, step is as follows：
(1) by average-size of the concentration for 4-20mg/mL>100um graphene oxide water solution goes out from in-line
In the preparation facilities of mouth after continuously and smoothly's extrusion, stopped 10-100 seconds in solidification liquid or liquid nitrogen, be frozen into graphene oxide and coagulate
Glued membrane, graphene oxide gel film is put into -4~-20 DEG C of refrigerator and freezes snap frozen in 1-12h or liquid nitrogen.
(2) by step 1 freezing processing rear oxidation graphene aerogel film, high-temperature heat treatment is carried out in feeding high temperature furnace,
Processing mode is：400 DEG C first are warming up to 0.1-4 DEG C/min under atmosphere of inert gases, 0.5-1h is incubated, then in indifferent gas
1300 DEG C are warming up to 2-4 DEG C/min under body atmosphere, 1-4h is incubated, is then heated up under atmosphere of inert gases with 2-4 DEG C/min
To 3000 DEG C, 1-2h is incubated, you can obtain the pure graphene aerogel film of continuous ultralight rule orientating.
(3) after aerogel film high pressure is suppressed, pressure is 10-100MP, obtains uniform closely knit flexible graphene electric heating
Film.
Further, the rate of extrusion is between 4-20m/min.
Further, the temperature of described solidification liquid is 30-60 DEG C, by methanol, ethanol, ethyl acetate, n-butanol, second two
In alcohol, cyclohexanone, glycerine, butyl acetate, propane diols, n-propyl acetate, acetic acid, glycerine, isobutanol, methyl acetate etc.
It is one or more to be constituted according to any ratio.
Further, graphene oxide of the average-size more than 100um is obtained by the following method in the step 1：
(1) after the reaction solution dilution for the oxidized graphite flake for obtaining Modified-Hummer methods, enter in the mesh screen of 140 mesh
Row filtering, obtains filtration product；
(2) filtration product for obtaining step 1 in frozen water according to volume ratio 1：After 10 is well mixed, 2h is stood, is added dropwise
Enter hydrogen peroxide (H2O2Mass fraction for 30%), until the color of mixed liquor no longer changes, (potassium permanganate i.e. in mixed liquor is
Remove completely)；
(3) concentrated hydrochloric acid (concentration is 12mol/L) is added dropwise in the mixed liquor after being handled to step 2, until cotton-shaped oxygen
Graphite disappears, then goes out graphite oxide chip with the screen filtration of 140 mesh；
(4) the graphite oxide chip that step 3 is obtained is placed in shaking table, 20~80 turns/min, concussion washing so that oxidation
Graphite wafer is peeled off, and obtains the graphene oxide of no fragment super large piece, and average-size is more than 100um, and breadth coefficient is in 0.2-0.5
Between.
Further, the Modified-Hummer methods in the step 1 are specially：At -10 DEG C, potassium permanganate is filled
Point be dissolved in the concentrated sulfuric acid that mass fraction is 98%, stirring stopped after adding graphite, 60 revs/min of stirring 2h, low temperature (-
10-20 DEG C) under react 6-48h, obtain the oxidized graphite flake reaction solution of wide distribution；Described graphite, potassium permanganate and the concentrated sulfuric acid
Mass volume ratio is：1g：2-4g：30-40ml, the granularity of graphite is more than 150 μm.
Further, the mesh screen is the acidproof mesh screens such as titanium alloy.
Further, in the step 1, the reaction solution of oxidized graphite flake is diluted by diluents such as the concentrated sulfuric acids, dilute
The volume for releasing agent is 1-10 times of reaction solution volume.
The present invention has the advantage that compared with prior art：1) primary raw materials of graphene oxide is graphite, raw material
Wide material sources, be easy to get, it is with low cost；2) graphene film is carbon-based material, and density is only in 1.8-2.1g/cm3, light weight can be with
Large area is used；3) graphene film has fine toughness, can arbitrarily bend and keep good electric conductivity, there is high add
Work, is conducive to the demand of variously-shaped, various applications adapted to；4) graphene Electric radiant Heating Film has extremely low resistivity, ultrafast
The rate of heat addition, high thermal conductivity and quick heat radiating capability, almost without thermal inertia, other materials can be conducted heat to rapidly
Material；5) heat conduction is fast, and temperature is uniform and stable, and service life is long；6) graphene film thickness, area, shape and size can
Control, is applicable row wide；7) graphene Electric radiant Heating Film starts voltage and operating voltage is low, can be worked below human safety voltage；8)
Steady chemical structure of graphene Electric radiant Heating Film, applicable interval itself is extremely wide, all applicable from native country continent to the outer space；9) graphene
Electric radiant Heating Film cold resistance is very high, even if at very low temperature, still having flexible well and can work well.
Embodiment
A kind of super soft light graphite alkene Electric radiant Heating Film of the invention, is assembled by super large piece without fragment graphene oxide solution；
By 3000 DEG C of high-temperature process, its internal graphene film Rotating fields perfect reparation so that graphene Electric radiant Heating Film has high
Electrical conductivity, programming rate is exceedingly fast；Inside has the orientation of height, and graphene sheet layer is parallel with graphene film, and the degree of orientation reaches
More than 94%；Film surface and inside have many random stretchable folds so that it has very high flexibility and draftability；
High pressure briquetting process is have passed through, its structure is closely knit, but be due to that carbonaceous is relatively light in itself, therefore its density is relatively low；Film heat conduction itself
Property is good, therefore it has fabulous rate of temperature fall；By the pi-conjugated effects of π mutually overlap joint inside described graphene Electric radiant Heating Film, make
Obtaining it has good intensity；This body structure of film is extremely stable, and equalizing section compole is wide.
By the present invention in that with super large piece graphene oxide film forming, the wherein average-size of planar orientation is more than 100 μm
Graphene film important role during graphene film of the present invention is constituted, the present invention washes it in graphite oxide crystal
Before, the method separated using mesh screen is gone out chip separation.And using 10 times to be diluted with the frozen water of upper volume so that it is brilliant
Piece will not be destroyed because of the heat of solution of sulfuric acid.Washing is further shaken using shaking table so that graphene oxide layer is in stripping
From when avoid the broken of mechanical force.Further, the present invention also prepares graphene film by cryogenic conditions, in low temperature
Under, potassium permanganate oxidation is weaker, and the speed that its selfdecomposition produces oxygen is slow, therefore gas is to graphite oxide crystal
Fragmentation is just very weak so that the graphene oxide of big lamella is preserved.And do not have in course of reaction and cleaning process
Violent stirring and ultrasonic procedure, thus lamella there is no it is broken.In summary some, we have obtained the nothing of super large piece
The graphene oxide of fragment, average-size is more than 87um, and breadth coefficient is between 0.2-0.5, and shive content is less than 1%.
The preparation facilities used in the present invention exported with in-line is prior art, and it is rectangular parallelepiped structure, middle
In-line die orifice is provided with, described in-line die orifice is a runner become narrow gradually.The runner become narrow gradually can be effectively increased
Flow field is conducive to the formation of the regular orientation texture of graphene dispersion system to the active force of graphene film.
The present embodiment is served only for that the present invention is described further, it is impossible to be interpreted as the limit to the scope of the present invention
System, those skilled in the art makes some nonessential changes and adjustment according to the content of foregoing invention, belongs to the present invention
Protection domain.
Embodiment 1：The preparation of graphene oxide without fragment super large piece
Embodiment 1-1
(1) potassium permanganate is slowly added into the concentrated sulfuric acid quickly stirred, after after abundant dissolving, added at -10 DEG C
Graphite, 60 revs/min are slowly stirred stopping stirring after 2h, and 6h is reacted respectively at 20 DEG C, 50 DEG C, respectively obtain the oxygen of wide distribution
Graphite crystal；There is more fragment in the graphite oxide chip obtained at a temperature of two kinds, this causes its corresponding oxidation
Graphene equally has many fragments.
(2) (extension rate can be any multiple to the reaction solution diluting concentrated sulfuric acid obtained step 1, and the present embodiment is dilute
Release 10 times or so), and graphite oxide crystal filters out to the titanium alloy mesh screen of 150um apertures (140 mesh) (reaction solution is returned
Receive), and be poured slowly into the frozen water relative to 10 times of volumes of filtration product quickly stirred, 2h is stood, H2O2 is slowly added to, with
Except potassium permanganate unnecessary in dereaction, the appropriate hydrochloric acid of addition disappears until cotton-shaped graphite oxide, then uses titanium alloy mesh screen
(140 mesh) filters out graphite oxide chip；Shaking table slowly shakes washing, and the graphene oxide for obtaining no fragment super large piece is (average
Size is 87um, and 0.5) breadth coefficient is.Graphite, potassium permanganate and concentrated sulfuric acid mass volume ratio are：1g：2g：40ml, graphite
Granularity is 200um.
Washing obtained graphene oxide after the graphite oxide chip separation isolated after the lower reaction of 50 degree of high temperature equally has
Many fragments；Large stretch of graphene oxide Size Distribution more uniform concentration under low temperature after (20 DEG C) Reaction Separation, fragment contains
Amount is few.
Embodiment 1-2
Potassium permanganate is slowly added at -10 DEG C in the concentrated sulfuric acid quickly stirred, after after abundant dissolving, adds stone
Ink, 60 revs/min are slowly stirred stopping stirring after 2h, react 48h under low temperature (0 DEG C), obtain reaction solution；By reaction solution point
It is not diluted with the concentrated sulfuric acid of mass fraction more than 98%, mass fraction for 10% dilute sulfuric acid, then with 150um apertures
Graphite oxide crystal is filtered out (reaction solution recovery) by titanium alloy mesh screen, and be poured slowly into quickly stir relative to filtering
In the frozen water of 10 times of volumes of product, 2h is stood, H is slowly added to2O2, except potassium permanganate unnecessary in dereaction, to add in right amount
Hydrochloric acid disappears until cotton-shaped graphite oxide, then filters out graphite oxide chip with titanium alloy reticulated is sieved；Shaking table slowly shakes washing, obtains
To reaction product.Graphite, potassium permanganate and concentrated sulfuric acid mass volume ratio are：1：4g：30ml；The granularity of graphite is 500um.
Using diluting concentrated sulfuric acid, (average-size is 98um to the graphene oxide without fragment super large piece that reaction is obtained, distribution
Coefficient is diluted with dilute sulfuric acid 0.4), a large amount of fragments is contained in obtained product, Size Distribution coefficient is more than 100%.This is
It is highly exothermic due in dilute sulfuric acid dilution, destroy graphite oxide crystal.
Embodiment 1-3
Potassium permanganate is slowly added at -10 DEG C in the concentrated sulfuric acid quickly stirred, after after abundant dissolving, adds stone
Ink, 60 revs/min are slowly stirred stopping stirring after 2h, and 28h is reacted under low temperature (20 DEG C), and the graphite oxide for obtaining wide distribution is brilliant
Body；Reaction solution with diluting concentrated sulfuric acid and is filtered out into (reaction solution with the titanium alloy mesh screen in 150um apertures by graphite oxide crystal
Reclaim), and be poured slowly into respectively quickly stir relative in 5 times of volumes of filtration product, 8 times of volumes, the frozen water of 10 times of volumes,
2h is stood, H is slowly added to2O2, except potassium permanganate unnecessary in dereaction, to add appropriate hydrochloric acid until cotton-shaped graphite oxide
Disappear, then graphite oxide chip is filtered out with titanium alloy reticulated is sieved；Shaking table slowly shakes washing, obtains reaction product；Graphite, Gao Meng
Sour potassium is with concentrated sulfuric acid mass volume ratio：1：5g：34ml, the granularity of graphite is 2mm.
Experimental result shows, the frozen water of 5 times of volumes and 8 times of volumes can not the graphene film for obtaining size uniformity,
The graphene oxide of no fragment super large piece can be just obtained under 10 times of volumes, and (average-size is 92um, and breadth coefficient is 0.2).Thus
Understand, the amount of frozen water is too low, the heat of mixing will be caused to concentrate release, destroy crystal structure.
Embodiment 2：The graphene oxide without fragment super large piece prepared using embodiment 1 prepares flexible light weight graphite
Alkene Electric radiant Heating Film.
By graphene oxide (average-size the be 150um) aqueous solution of the certain density super large piece without fragment from a word
Continuously and smoothly in the preparation facilities (device is rectangular parallelepiped structure, and centre is provided with the in-line become narrow gradually a die orifice) of shape outlet
Enter solidification liquid for a period of time after extrusion, be frozen into graphene oxide gel film, be put into refrigerator in slow frost or liquid nitrogen
Snap frozen.Described concentration of the super large piece without fragment graphene oxide solution is between 100mg/mL.Described continuously and smoothly
The speed of solidification liquid is extruded into between 10m/min, temperature is 30 DEG C.Described solidification liquid is liquid nitrogen.Described solidification liquid
The middle residence time is 100 seconds.
High temperature is carried out with being obtained after freeze-drying or supercritical drying in graphite oxide aerogel film, feeding high temperature furnace
Heat treatment, processing mode is as shown in table 1~3, and after then its high pressure is suppressed, pressure is 50MP, obtains graphene Electric radiant Heating Film.
Table 1
Table 2
Table 3
From 1~table of table 3 as can be seen that being determined in terms of the performance of this material mainly has two, one material internal graphite oxide
Alkene chip architecture repair situation, i.e. functional group come off and high temperature under carbon conjugated structure reparation.Second, material internal orientation knot
The continuity of structure, i.e., the connectivity of internal lamellar structure.The two collective effect is to increase the performance of graphene film.
In table 1, compare A B C D E, A temperature is too low, is not enough to remove most of degradable functional group, causes the
Gas is largely quickly produced in two step pyroprocesses, and lamellar structure is torn at high temperature；E temperature is too high, and generation gas is too fast, and two
Person can cause deterioration in material properties.Have only at a temperature of BCD, functional group can slowly and thoroughly remove, to ensure material property.
Compare C F G H, F heating rates are too low, and gas release is excessively slow；H temperature-rise periods are too fast, and gas release is too fast, tear material
Expect internal structure, be unfavorable for forming conductive channel.Compare C I J K L M, I soaking times are too short, it is impossible to ensure most of official
The degraded that can be rolled into a ball；M insulating processes are long, can absorb the tar inside stove, are unfavorable for the lifting of performance.JKL due to avoid with
Upper 2 points, with good electric heating property and bending performance.
In table 2, compare A B C D E, A heating rates are too low to be not enough to form small gap structure, has a strong impact on electricity
Hot property.E programming rates are too high, can tear graphene interlayer structure so that graphene film electric heating property is deteriorated.Have BCD's only
, just can the capable continuity both ensured inside graphene film under programming rate.Compare C F G H, F temperature is too low so that steady
Fixed functional group can not be sufficiently disengaged from, and easily transition discharges gas during subsequently graphited, destruction graphene-structured
It is stable to be formed；H temperature is too high, has reached graphitization temperature, under conditions of now gas release, and its temperature is also not enough to maintain
The formation of conductive network, the micro- airbag structure now formed is imperfect；Compare C I J K L M, I soaking times are too short, stable
Functional group can not fully come off；M overlong times, the easy tar adsorption of graphene film, are unfavorable for the lifting of film properties；And CJK
Under the conditions of can both ensure fully coming off for stabilising functional group, the puzzlement of tar is avoided that again.
In table 3, compare A B C D E, A heating rates are too low, and it is excessively slow that most stabilising functional group comes off；E temperature-rise period mistakes
It hurry up, gas release and high-temperature expansion are too fast, are easily destroyed graphene-structured.In the case of only BCD, the structure on graphene
Could slowly it repair.Compare C F G H I, F outlet temperatures are too low, and graphene-structured repairs not perfect enough, so various property
Can be all very poor；I outlet temperatures are too high, and graphene can be vaporized；Repairing for graphene-structured could both be ensured at a temperature of CGH
It is multiple, it will not be vaporized and compare again.C J K L M, J soaking times are too low, and graphene-structured can not be repaired fully, when M is incubated
Between it is long, can also cause adsorb body of heater in tar, influence film electric heating and bending performance.
Claims (5)
1. a kind of preparation method of super soft light graphite alkene Electric radiant Heating Film, it is characterised in that step is as follows：
（1）By the average-size that concentration is 4-20mg/mL>100um graphene oxide water solution with in-line from exporting
After being extruded in preparation facilities with rate of extrusion 4-20m/min continuously and smoothlies, stopped 10-100 seconds in solidification liquid or liquid nitrogen, solidification
Into graphene oxide gel film, graphene oxide gel film is put into -4 ~ -20 DEG C of refrigerator and freezed in 1-12h or liquid nitrogen
Snap frozen；
（2）By step 1 freezing processing rear oxidation graphene aerogel film, send into high temperature furnace and carry out high-temperature heat treatment, handle
Mode is：400 DEG C first are warming up to 0.1-4 DEG C/min under atmosphere of inert gases, 0.5-1h is incubated, then in inert gas atmosphere
1300 DEG C are warming up to 2-4 DEG C/min under enclosing, 1-4h is incubated, is then warming up under atmosphere of inert gases with 2-4 DEG C/min
3000 DEG C, it is incubated 1-2h, you can obtain the pure graphene aerogel film of continuous ultralight rule orientating；
（3）After aerogel film high pressure is suppressed, pressure is 10-100MP, obtains uniform closely knit flexible graphene Electric radiant Heating Film；
Graphene oxide of the average-size more than 100 um is obtained by the following method in the step 1：
（1.1）After the reaction solution dilution for the oxidized graphite flake that Modified-Hummer methods are obtained, carried out in the mesh screen of 140 mesh
Filtering, obtains filtration product；
（1.2）The filtration product that step 1.1 is obtained is with frozen water according to volume ratio 1：After 10 is well mixed, 2h is stood, is added dropwise
Enter hydrogen peroxide, until the color of mixed liquor no longer changes；
（1.3）Concentrated hydrochloric acid is added dropwise in mixed liquor after being handled to step 1.2, until cotton-shaped graphite oxide disappearance, then uses
The screen filtration of 140 mesh goes out graphite oxide chip；
（1.4）The graphite oxide chip that step 1.3 is obtained is placed in shaking table, 20 ~ 80 turns/min, concussion washing so that oxidation
Graphite wafer is peeled off, and obtains the graphene oxide of no fragment super large piece, and average-size is more than 100 um, and breadth coefficient is in 0.2-
Between 0.5.
2. the method as described in claim 1, it is characterised in that the temperature of described solidification liquid is 30-60 DEG C, by methanol, second
Alcohol, ethyl acetate, n-butanol, ethylene glycol, cyclohexanone, glycerine, butyl acetate, propane diols, n-propyl acetate, acetic acid, isobutyl
It is one or more according to any ratio composition in alcohol, methyl acetate.
3. according to the method described in claim 1, it is characterised in that the Modified-Hummer methods in the step 1 are specific
For：At -10 DEG C, potassium permanganate is completely dissolved in the concentrated sulfuric acid that mass fraction is 98%, adds graphite, 60 revs/min are stirred
Mix and stop stirring after 2h, 6-48h is reacted in a low temperature of -10-20 DEG C, obtain the oxidized graphite flake reaction solution of wide distribution；It is described
Graphite, potassium permanganate and concentrated sulfuric acid mass volume ratio be：1 g：2-4g：30-40ml, the granularity of graphite is more than 150 μm.
4. according to the method described in claim 1, it is characterised in that the mesh screen is acidproof mesh screen.
5. according to the method described in claim 1, it is characterised in that in the step 1, the reaction solution of oxidized graphite flake passes through dense
Sulfuric acid is diluted, and the volume of the concentrated sulfuric acid is 1-10 times of reaction solution volume.
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| CN106185903B (en) * | 2016-07-15 | 2018-07-17 | 浙江大学 | A kind of method that ice crystal auxiliary prepares high flexibility graphene film |
| CN106332327A (en) * | 2016-08-19 | 2017-01-11 | 苏州思创源博电子科技有限公司 | Preparation method for composite graphene electrothermal film |
| EP3611130B1 (en) * | 2017-04-11 | 2022-12-14 | Hangzhou Gaoxi Technology Co., Ltd. | Preparation method for a flexible graphene film |
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| CN111944497B (en) * | 2019-05-16 | 2022-02-22 | 常州第六元素材料科技股份有限公司 | Graphene oxide composite carbon source mixture and preparation method thereof, graphene heat-conducting film and preparation method thereof |
| CN112210250A (en) * | 2020-09-29 | 2021-01-12 | 兰州大学 | Preparation method of graphene-based screen printing electrothermal ink |
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