CN105752963A - Foldable electrothermal film device based on graphene - Google Patents
Foldable electrothermal film device based on graphene Download PDFInfo
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- CN105752963A CN105752963A CN201610049028.3A CN201610049028A CN105752963A CN 105752963 A CN105752963 A CN 105752963A CN 201610049028 A CN201610049028 A CN 201610049028A CN 105752963 A CN105752963 A CN 105752963A
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- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
- H05B3/00—Ohmic-resistance heating
- H05B3/20—Heating elements having extended surface area substantially in a two-dimensional plane, e.g. plate-heater
- H05B3/34—Heating elements having extended surface area substantially in a two-dimensional plane, e.g. plate-heater flexible, e.g. heating nets or webs
- H05B3/36—Heating elements having extended surface area substantially in a two-dimensional plane, e.g. plate-heater flexible, e.g. heating nets or webs heating conductor embedded in insulating material
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2204/00—Structure or properties of graphene
- C01B2204/20—Graphene characterized by its properties
- C01B2204/22—Electronic properties
Abstract
The invention discloses a foldable electrothermal film device based on graphene.The foldable electrothermal film device comprises a heating element, protecting films and current intercepting bodies, wherein the heating element is a super-flexible graphene film obtained by subjecting large-piece even graphene oxide to solution film formation, chemical reduction, high-temperature reduction, high-pressure pressing and the like.The graphene film is formed by macroscopic multilayer-fold graphene with micro-scale folds through physical crosslinking, every two lamellas of the graphene film can slide relative to each other, and high flexibility is achieved.The graphene lamellas have few defects and are perfect in structure, extremely large in lamella crystalline area (about 100 micrometers) and compact in structure after the high-pressure pressing, and the electrothermal film prepared by the graphene film is super-high in conductivity and thermal conductivity.The super-flexible graphene electrothermal film can be repeatedly bent for more than 1200 times, the elongation at break of the electrothermal film is 12-18%, the conductivity of the electrothermal film is 8000-10600S/cm, and the thermal conductivity of the electrothermal film is 1800-2600W/mK.
Description
Technical field
The present invention relates to Novel heat-conducting device, particularly relate to a kind of collapsible electrothermal film device based on Graphene.
Background technology
2010, two professor Andre GeiM and Konstantin Novoselov of Univ Manchester UK obtained Nobel Prize in physics because being successfully separated out stable Graphene first, have started the upsurge that Graphene is studied by the whole world.Graphene has excellent electric property, and (under room temperature, electron 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).The electrical and thermal conductivity performance of Graphene excellence is well beyond metal, and Graphene has the advantage of corrosion-and high-temp-resistant simultaneously, and its good mechanical performance and relatively low density more allow it possess the potentiality at thermo electric material field substituted metal.
Macroscopic view assembles the main application form that the graphene film of graphene oxide or graphene nanometer sheet is nanoscale graphite alkene, and conventional preparation method is suction method, scrape embrane method, spin-coating method, spraying process and dip coating etc..By further high-temperature process, the defect of Graphene can be repaired, can effectively improve electric conductivity and the thermal conductance of graphene film, can be widely applied in smart mobile phone, intelligence hardware, panel computer, notebook computer contour radiating requirements accompanied electronic equipment with oneself.
But at present, the undersize of graphene oxide used own, and containing a lot of fragments so that it is not obtaining enough development in terms of heat conduction, heat conductivility is limited in 1400W/mK, it is impossible to meet the demand of rapid technological growth.And the deficiency of Design of Membrane Structure makes its flexibility be still not clear, limit its application in terms of flexible device.To this end, we have employed super large sheet graphene oxide assembles graphene film, considerably reduce edge phonon and dissipate, and at high temperature repair its damaged structure, provide path for its high heat conduction.It addition, perforating agent at high temperature drilling, define a lot of micro-air bag, obtain the graphene film of porous；After pressing, pore disappears, and membrane structure becomes fine and close, and its fold is retained simultaneously so that it has fabulous flexibility.
Summary of the invention
It is an object of the invention to overcome the deficiencies in the prior art, it is provided that a kind of collapsible electrothermal film device based on Graphene.
It is an object of the invention to be achieved through the following technical solutions: a kind of collapsible electrothermal film device based on Graphene; including heater element, protecting film and two bodies that dam; described protecting film is positioned at the both sides up and down of heater element, and two bodies that dam are connected with the two ends of heater element respectively；Described protecting film is PDMS film, and the body that dams is metal electrode；Heater element is Flexible graphene film, is prepared by the following method and obtains:
(1) more than the graphene oxide of 100 μm, average-size being configured to concentration is 6～30mg/mL graphene oxide water solution, adds the auxiliary agent of mass fraction 0.1-5% in the solution, and described auxiliary agent is inorganic salt, organic molecule or macromolecule；After ultrasonic disperse, it is poured on Die and mould plate and is dried into graphene oxide membrane, then reduce with reducing agent；
(2) graphene film after reducing first with the ramp to 500-800 DEG C of 0.1-1 DEG C/min, is incubated 0.5-2h under atmosphere of inert gases；
(3) with the ramp to 1000-1300 DEG C of 1-3 DEG C/min under atmosphere of inert gases, it is incubated 0.5-3h；
(4) with the ramp to 2500-3000 DEG C of 5-8 DEG C/min under atmosphere of inert gases, it is incubated 0.5-4h, after Temperature fall, i.e. can get porous graphene thin film.
(5) graphene film is under high pressure suppressed to obtain Flexible graphene film.
Further, described inorganic salt is selected from ammonium hydrogen carbonate, carbamide, thiourea, azodicarbonamide；Organic molecule is selected from glycerol, polyethylene glycol 200, PEG400；Macromolecule is selected from cellulose, gelatin, chitosan, aqueous polyurethane, acrylic emulsion etc..
Further, described reducing agent comprises hydrazine hydrate, amine, ascorbic acid, hydrogen iodide；Owing to hydrazine hydrate can make membrane material expand in reduction process, preferentially use hydrazine hydrate.
Further, described pressing process pressure is 50-200MP, and the time is 6-300h.
Further, in described step 1, the average-size graphene oxide more than 100um obtains by the following method:
(1), after the reactant liquor dilution of oxidized graphite flake Modified-Hummer method obtained, the mesh screen in 140 mesh filters, and obtains filtration product；
(2) filtration product step 1 obtained is after frozen water is according to volume ratio 1:10 mix homogeneously, stands 2h, is added dropwise over hydrogen peroxide (H2O2Mass fraction be 30%), until the color of mixed liquor no longer changes (i.e. potassium permanganate in mixed liquor is removed the most completely)；
(3) mixed liquor after step 2 processes is added dropwise over concentrated hydrochloric acid (concentration is 12mol/L), until cotton-shaped graphite oxide disappears, then goes out graphite oxide wafer with the screen filtration of 140 mesh；
(4) graphite oxide wafer step 3 obtained is placed in shaking table, 20～80 turns/min, and concussion washing so that graphite oxide wafer is peeled off, and obtains the graphene oxide without fragment super large sheet, average-size is more than 87um, and breadth coefficient is between 0.2-0.5.
Further, Modified-Hummer method in described step 1 is particularly as follows: at-10 DEG C, potassium permanganate is completely dissolved in the concentrated sulphuric acid that mass fraction is 98%, add graphite, stirring is stopped after 60 revs/min of stirring 2h, under low temperature (-10-20 DEG C), react 6-48h, obtain the oxidized graphite flake reactant liquor of wide distribution；Described graphite, potassium permanganate with concentrated sulphuric acid mass volume ratio is: 1g:2-4g:30-40ml, and the granularity of graphite is more than 150 μm.
Further, described mesh screen is the acidproof mesh screens such as titanium alloy.
Further, in described step 1, the reactant liquor of oxidized graphite flake is diluted by diluent such as concentrated sulphuric acids, and the volume of diluent is 1-10 times of reactant liquor volume.
By the present invention in that by super large sheet graphene oxide film forming, and allow under its mode at high temperature annealed, perfect reparation Graphene defect, and edge defect is preferably minimized, form perfect big conjugated structure, its conjugation size has even extended to the Graphene of full wafer, it is ensured that Graphene thermal conducting path unimpeded；Further by the temperature-rise period of three step independences so that the functional group of graphenic surface gradually disengages, and the auxiliary agent (perforating agent) being mixed between graphene film slowly decomposes, both of which discharges the most step by step, meanwhile, graphitizing process stepwise development, form the micro-air bag of Graphene；Use condition of high voltage to be compressed by micro-air bag further, form fold so that the deformation of graphene film is remembered, and gives the flexibility of its superelevation.And in the forming process of micro-air bag, the most stable functional group of graphenic surface comes off the most therewith, adds gas expansion under high temperature, thereby produces the graphene-structured being made up of 1-4 layer graphene sheet；Being successfully introduced into of the few Rotating fields of Graphene, is greatly improved the electrical and thermal conductivity performance of material.Super-high heat-conductive heat conductivity and flexible combination so that this heat conducting film has the widest application potential in terms of high frequency flexible electronic device.
Accompanying drawing explanation
Fig. 1 is the structural representation of device.
Detailed description of the invention
By the present invention in that by super large sheet graphene oxide film forming, wherein the average-size of planar orientation is more than graphene film important role during constituting graphene film of the present invention of 100 μm, the present invention, before graphite oxide crystal is washed, uses the way of mesh screen separation, chip separation is gone out.And using 10 times to be diluted with the frozen water of upper volume so that its wafer will not be destroyed because of the heat of solution of sulphuric acid.Use shaking table concussion washing further so that graphene oxide lamella avoids the broken of mechanical force peeling off when.Further, the present invention prepares graphene film also by cryogenic conditions, at low temperatures, potassium permanganate oxidation is more weak, the speed that its selfdecomposition produces oxygen is slow, and therefore gas is the most weak to the fragmentation of graphite oxide crystal so that the graphene oxide of big lamella is preserved.And course of reaction and cleaning process do not have violent stirring and ultrasonic procedure, therefore lamella there is no broken.Comprehensive above some, we have obtained the graphene oxide without fragment of super large sheet, and average-size is more than 87um, and breadth coefficient is between 0.2-0.5, and shive content is less than 1%.And the defect of graphene film is few, its ID/TG＜ 0.01.
Below in conjunction with the accompanying drawings and embodiment the invention will be further described.The present embodiment is served only for that the present invention is described further, it is impossible to being interpreted as limiting the scope of the invention, those skilled in the art makes some nonessential change and adjustment according to the content of foregoing invention, belongs to protection scope of the present invention.
Embodiment 1: use the graphene oxide without fragment super large sheet to prepare a kind of super Flexible graphene Electric radiant Heating Film.
The average-size graphene oxide more than 100um is configured to concentration is 6mg/mL graphene oxide water solution, add mass fraction 0.1 ammonium hydrogen carbonate in the solution, it is poured on after ultrasonic disperse on Die and mould plate and is dried into graphene oxide membrane, then reduce with hydrazine hydrate reduction agent；Graphene film after reduction the most progressively heats up 500 DEG C under atmosphere of inert gases, is incubated 2h；Under atmosphere of inert gases, progressively it is warmed up to 1000 DEG C, is incubated 3h；Under atmosphere of inert gases, progressively it is warmed up to 2500 DEG C, is incubated 4h, after Temperature fall, i.e. can get porous graphene thin film.After under high pressure being suppressed by graphene film, coating PDMS insulating protective layer in its both sides, constitute Electric radiant Heating Film, at the two ends of Electric radiant Heating Film difference fixed electrode, electrode is connected with Graphene Electric radiant Heating Film.
At described 500 DEG C, heating rate is 0.1 DEG C/min, and at 1000 DEG C, heating rate is 1 DEG C/min, less than 2500 DEG C, and heating rate is 5 DEG C/min.Described pressing process pressure is 200MP, and the time is 100h.
The film density obtained is 2.11g/cm3, it being resistant to repeatedly bend more than 1200 times, intensity is 80MP, and conductivity is 10600S/cm, and thermal conductivity is 2100W/mK.The structure of graphene film is the finest and close；After high temperature reduction, the internal graphene film containing the various numbers of plies of graphene film, and structure is the most perfect, and this lays the foundation for heat conduction.There is a lot of folds graphene membrane surface and inside, and this is that the flexibility of graphene film is laid a good foundation.The elongation at break of the graphene film of preparation has reached 16%, belongs to flexible fracture.After doubling repeatedly, conductivity variations is little, is maintained at about 10600S/cm, illustrates that it is flexible very well, and after repeatedly rolling, its performance can be recovered as before again, and this explanation, the Graphene macroscopic view that the graphene film that we prepare is real assembles.
Comparative example 1: shown in example 1 performed as described above, change its Elevated Temperature Conditions as follows:
Directly it is warmed up to 2500 DEG C with the speed of 100 DEG C/min, and reacts the identical time.The elongation at break of prepared film is 6%, and intensity is 20MP, and conductivity is 4000S/cm, and thermal conductivity is 1000W/mK.
Comparative example 2: shown in example 1 performed as described above, change the raw material of graphene oxide used by it, with shive content about 30% graphene oxide.The elongation at break of then prepared film is 7%, and intensity is 10MP, and conductivity is 3400S/cm, and thermal conductivity is 800W/mK.
Embodiment 2:.
The average-size graphene oxide more than 100um is configured to concentration is 30mg/mL graphene oxide water solution, add mass fraction 5% carbamide in the solution, it is poured on after ultrasonic disperse on Die and mould plate and is dried into graphene oxide membrane, then reduce with hydrogen iodide reducing agent；Graphene film after reduction carries out three step heat treatments according to the heat treatment mode shown in table 1～table 3 under atmosphere of inert gases；Porous graphene thin film is i.e. can get after Temperature fall.After under high pressure being suppressed by graphene film, coating PDMS insulating protective layer in its both sides, constitute Electric radiant Heating Film, at the two ends of Electric radiant Heating Film difference fixed electrode, electrode is connected with Graphene Electric radiant Heating Film.Described pressing process pressure is 200MP, and the time is 300h.
Table 1: first step Elevated Temperature Conditions
Table 2: second step Elevated Temperature Conditions
Table 3: the three step Elevated Temperature Conditions
From table 1～table 3 it can be seen that the performance of this material determines in terms of mainly having two, coming off and the reparation of carbon conjugated structure under high temperature of one material internal graphene oxide sheet structure repair situation, i.e. functional group.Its two, the seriality of material internal orientation texture, the i.e. connectivity of internal sheets Rotating fields.The two common effect is to increase the performance of graphene film.
As it can be seen from table 1 compare A1, B1, C1, D1, E1, the temperature of A1 is too low, is not enough to remove the functional group that major part is degradable, causes gas in second step pyroprocess the most quickly to produce, at high temperature tearing sheet Rotating fields；E1 temperature is too high, produces gas too fast, both can make deterioration in material properties.Having only at a temperature of B1, C1, D1, functional group can slowly and thoroughly remove, to ensure material property.Relatively C1, F1, G1, H1, F1 heating rate is too low, and gas release is the slowest；H1 temperature-rise period is too fast, and gas release is too fast, tears material internal structure, is unfavorable for forming conductive channel.Relatively C1, I1, J1, K1, L1, M1, I1 temperature retention time is too short, it is impossible to ensure the degraded of major part functional group；M1 insulating process is long, can absorb the tar inside stove, is unfavorable for the lifting of performance.C1, J1, K1, L1, owing to avoiding above 2 points, have good electric heating property and bending performance.
From Table 2, it can be seen that compare A2, B2, C2, D2, E2, too low being not enough to of A2 heating rate forms small gap structure, has a strong impact on electric heating property.E programming rate is too high, can tear Graphene interlayer structure so that graphene film electric heating property is deteriorated.Have only under the programming rate of B2, C2, D2, just can the capable seriality both ensured within graphene film.Relatively C2, F2, G2, H2, F2 temperature is too low so that stable functional group can not be sufficiently disengaged from, follow-up graphited during easy transition release gas, destroy the stable formation of graphene-structured；H2 temperature is too high, has reached graphitization temperature, and under conditions of now gas release, its temperature is also not enough to maintain the formation of conductive network, and the micro-airbag structure now formed is imperfect；Relatively C2, I2, J2, K2, L2, M2, I2 temperature retention time is too short, and stable functional group can not fully come off；M2 overlong time, the easy tar adsorption of graphene film, it is unfavorable for the lifting of film properties；And under the conditions of C2, J2, K2, both can ensure that fully coming off of stabilising functional group, it is avoided that again the puzzlement of tar.
From table 3 it is observed that compare A3, B3, C3, D3, E, A3 heating rate is too low, stabilising functional group come off the slowest；E temperature-rise period is too fast, and gas release and high-temperature expansion are too fast, are easily destroyed graphene-structured.Only in the case of B3, C3, D3, the structure on Graphene could be repaired slowly.Relatively C3, F3, G3, H3, I3, F3 outlet temperature is too low, and graphene-structured is repaired the most perfect, so various performance is the most very poor；I3 outlet temperature is too high, and Graphene can be vaporized；Could both ensure the reparation of graphene-structured at a temperature of C3, G3, H3, will not be vaporized again.Relatively C3, J3, K3, L3, M3, J3 temperature retention time is too low, and graphene-structured can not fully be repaired, and M3 temperature retention time is long, also can make to adsorb the tar in body of heater, affect electric heating and the bending performance of film.
Claims (8)
1. a collapsible electrothermal film device based on Graphene, it is characterised in that include heater element, guarantor
Cuticula and two bodies that dam, described protecting film is positioned at the both sides up and down of heater element, two dam body respectively with
The two ends of heater element are connected；Described protecting film is PDMS film, and the body that dams is metal electrode；Heater element
For Flexible graphene film, it is prepared by the following method and obtains:
(1) more than the graphene oxide of 100 μm, average-size being configured to concentration is 6～30mg/mL oxidations
Graphene aqueous solution, adds the auxiliary agent of mass fraction 0.1-5% in the solution, and described auxiliary agent is inorganic salt, has
The little molecule of machine or macromolecule；After ultrasonic disperse, it is poured on Die and mould plate and is dried into graphene oxide membrane, then use
Reducing agent reduces；
(2) by the graphene film after reduction under atmosphere of inert gases first with the ramp of 0.1-1 DEG C/min
To 500-800 DEG C, it is incubated 0.5-2h；
(3) with the ramp to 1000-1300 DEG C of 1-3 DEG C/min under atmosphere of inert gases, it is incubated 0.5-3h；
(4) with the ramp to 2500-3000 DEG C of 5-8 DEG C/min under atmosphere of inert gases, it is incubated 0.5-4h,
Porous graphene thin film is i.e. can get after Temperature fall.
(5) graphene film is under high pressure suppressed to obtain Flexible graphene film.
2. device as claimed in claim 1, it is characterised in that described inorganic salt is selected from ammonium hydrogen carbonate, urine
Element, thiourea, azodicarbonamide；Organic molecule is selected from glycerol, polyethylene glycol 200, PEG400；
Macromolecule is selected from cellulose, gelatin, chitosan, aqueous polyurethane, acrylic emulsion etc..
3. device as claimed in claim 1, it is characterised in that described reducing agent comprise hydrazine hydrate, amine,
Ascorbic acid, hydrogen iodide；Owing to hydrazine hydrate can make membrane material expand in reduction process, preferentially use hydration
Hydrazine.
4. device as claimed in claim 1, it is characterised in that described pressing process pressure is 50-200MP,
Time is 6-300h.
5. device as claimed in claim 1, it is characterised in that in described step 1, average-size is more than 100
The graphene oxide of um obtains by the following method:
(1) after the reactant liquor dilution of the oxidized graphite flake that Modified-Hummer method is obtained, in 140 mesh
Mesh screen filter, obtain filtration product；
(2) filtration product step 1 obtained is after frozen water is according to volume ratio 1:10 mix homogeneously, stands
2h, is added dropwise over hydrogen peroxide (H2O2Mass fraction be 30%), until the color of mixed liquor no longer changes (i.e.
Potassium permanganate in mixed liquor is removed the most completely)；
(3) mixed liquor after step 2 processes is added dropwise over concentrated hydrochloric acid (concentration is 12mol/L), until
Cotton-shaped graphite oxide disappears, then goes out graphite oxide wafer with the screen filtration of 140 mesh；
(4) graphite oxide wafer step 3 obtained is placed in shaking table, 20～80 turns/min, concussion washing,
Graphite oxide wafer being peeled off, obtains the graphene oxide without fragment super large sheet, average-size is more than 87um,
Breadth coefficient is between 0.2-0.5.
Device the most according to claim 5, it is characterised in that in described step 1
Modified-Hummer method is particularly as follows: at-10 DEG C, it is 98% that potassium permanganate is completely dissolved in mass fraction
Concentrated sulphuric acid in, add graphite, 60 revs/min stirring 2h after stop stirring, under low temperature (-10-20 DEG C)
Reaction 6-48h, obtains the oxidized graphite flake reactant liquor of wide distribution；Described graphite, potassium permanganate and concentrated sulphuric acid
Mass volume ratio is: 1g:2-4g:30-40ml, and the granularity of graphite is more than 150 μm.
Device the most according to claim 5, it is characterised in that described mesh screen is the acidproof mesh screens such as titanium alloy.
Device the most according to claim 5, it is characterised in that in described step 1, oxidized graphite flake
Reactant liquor is diluted by diluent such as concentrated sulphuric acids, and the volume of diluent is 1-10 times of reactant liquor volume.
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