CN105752963B - A kind of foldable electrothermal film device based on graphene - Google Patents
A kind of foldable electrothermal film device based on graphene Download PDFInfo
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- CN105752963B CN105752963B CN201610049028.3A CN201610049028A CN105752963B CN 105752963 B CN105752963 B CN 105752963B CN 201610049028 A CN201610049028 A CN 201610049028A CN 105752963 B CN105752963 B CN 105752963B
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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
-
- 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 kind of foldable electrothermal film device based on graphene, including heater element, diaphragm and the body that dams；Wherein heater element is super soft graphene film, is obtained by super large piece uniform graphene oxide by steps such as solution film forming, electronation, high temperature reduction and high pressure compactings.Graphene film is made up of macroscopical multilayered fold graphene with micro-scale fold physical crosslinking, piece interlayer slip, therefore with high flexibility.Its graphene sheet layer perfect structure, lamella crystalline region greatly (100um or so) simultaneously seldom contains defective, and structure is closely knit after high pressure is suppressed, and the Electric radiant Heating Film prepared has the electric conductivity and thermal conductivity of superelevation.This super Flexible graphene Electric radiant Heating Film is resistant to bend repeatedly more than 1200 times, and elongation at break is 12 18%, and conductance is 8000 10600S/cm, and thermal conductivity is 1800 2600W/mK.
Description
Technical field
The present invention relates to novel heat-conducting device, more particularly to a kind of foldable electrothermal film device based on graphene.
Background technology
, two of Univ Manchester UK professor Andre GeiM and Konstantin Novoselov in 2010 because
Stable graphene is successfully separated out first and obtains Nobel Prize in physics, has started the upsurge that the whole world is studied graphene.
Graphene has excellent electric property, and (electron mobility is up to 2 × 10 at room temperature5cM2/ Vs), prominent heat conductivility (5000W/
(MK), extraordinary specific surface area (2630M2/ g), its Young's modulus (1100GPa) and fracture strength (125GPa).Graphene is excellent
Different electrical and thermal conductivity performance is well beyond metal, while graphene has the advantages that corrosion-and high-temp-resistant, and its good machinery
Performance and relatively low density more allow it to possess the potentiality in thermo electric material field substituted metal.
The graphene film of macroscopic view assembling graphene oxide or graphene nanometer sheet is the main application of nanoscale graphite alkene
Form, conventional preparation method is suction method, scrape embrane method, spin-coating method, spraying process and dip coating etc..At further high temperature
Reason, can repair the defect of graphene, can effectively improve the electric conductivity and thermal conductance of graphene film, can be widely applied to
Smart mobile phone, intelligence are with oneself in the high radiating requirements accompanied electronic equipment such as hardware, tablet personal computer, notebook computer.
But at present, undersize of graphene oxide used itself, and containing many fragments, make it in terms of heat conduction
Enough development are not obtained, heat conductivility is limited in 1400W/mK, it is impossible to meet the demand of rapid technological growth.And film
The deficiency of structure design causes its flexibility to be still not clear, and limits its application in terms of flexible device.Therefore, we employ
Super large piece graphene oxide assembles graphene film, considerably reduces edge phonon dissipation, and repair its breakage knot at high temperature
Structure, path is provided for its high heat conduction.In addition, perforating agent drilling at high temperature, forms many micro- air bags, obtains porous stone
Black alkene film；After pressing, stomata disappears, and membrane structure becomes fine and close, while its fold is retained so that it has fabulous soft
Property.
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 foldable electric heating membrane device based on graphene
Part.
The purpose of the present invention is achieved through the following technical solutions：A kind of foldable electric heating membrane device based on graphene
Part, including heater element, diaphragm and two bodies that dam, the diaphragm are located at the both sides up and down of heater element, and two dam
Body is connected with the two ends of heater element respectively；The diaphragm is PDMS films, and the body that dams is metal electrode；Heater element is flexibility
Graphene film, is prepared by the following method and obtains：
(1) graphene oxide that average-size is more than 100 μm is configured to concentration for 6~30mg/mL graphene oxide water
Solution, adds mass fraction 0.1-5% auxiliary agent in the solution, and the auxiliary agent is inorganic salts, organic molecule or macromolecule；It is super
After sound is scattered, it is poured on Die and mould plate and is dried into graphene oxide membrane, then reduced with reducing agent；
(2) graphene film after reduction is first warming up under atmosphere of inert gases with 0.1-1 DEG C/min speed
500-800 DEG C, it is incubated 0.5-2h；
(3) 1000-1300 DEG C is warming up to 1-3 DEG C/min speed under atmosphere of inert gases, is incubated 0.5-3h；
(4) 2500-3000 DEG C is warming up to 5-8 DEG C/min speed under atmosphere of inert gases, is incubated 0.5-4h, it is natural
Porous graphene film is can obtain after cooling.
(5) Flexible graphene film can be obtained by suppressing graphene film under high pressure.
Further, described inorganic salts are selected from ammonium hydrogen carbonate, urea, thiocarbamide, azodicarbonamide；Organic molecule is selected
From glycerine, polyethylene glycol 200, polyethylene glycol 400；Macromolecule is selected from cellulose, gelatin, chitosan, aqueous polyurethane, acrylic acid
Emulsion etc..
Further, described reducing agent includes hydrazine hydrate, amine, ascorbic acid, hydrogen iodide；Because hydrazine hydrate is in reduction
Process can cause membrane material to expand, preferentially using hydrazine hydrate.
Further, described pressing process pressure is 50-200MP, and the time is 6-300h.
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 87um, 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.
By the present invention in that with super large piece graphene oxide film forming, and allow under the mode that it anneals at high temperature, perfection is repaiied
Multiple graphene defect, and edge defect is preferably minimized, perfect big conjugated structure is formed, it is conjugated size and even extended to
The graphene of full wafer, it is ensured that graphene thermal conducting path it is unimpeded；Further pass through the temperature-rise period of three step independences so that stone
The functional group on black alkene surface is gradually disengaged, and the auxiliary agent (perforating agent) being mixed between graphene film is slowly decomposed, and both of which is with gas
Body form discharges step by step, meanwhile, graphitizing process stepwise development forms the micro- air bag of graphene；Further use condition of high voltage will
Micro- air bag is compressed, and forms fold so that the deformation of graphene film is remembered, and assigns the flexibility of its superelevation.And micro- air bag
Forming process in, graphenic surface the most stable functional group also comes off therewith, adds gas expansion under high temperature, thus produces
The graphene-structured that is made up of 1-4 layer graphene pieces；Being successfully introduced into for the few Rotating fields of graphene, is greatly improved material
Electrical and thermal conductivity performance.Super-high heat-conductive thermal conductivity and flexible combination so that the heat conducting film has in terms of high frequency flexible electronic device
Extremely wide application potential.
Brief description of the drawings
Fig. 1 is the structural representation of device.
Embodiment
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%.And stone
The defect of black alkene piece 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 be served only for being the present invention into
The explanation of one step, it is impossible to be interpreted as limiting the scope of the invention, those skilled in the art is according in foregoing invention
Appearance makes some nonessential changes and adjustment, belongs to protection scope of the present invention.
Embodiment 1：A kind of super Flexible graphene Electric radiant Heating Film is prepared using the graphene oxide without fragment super large piece.
The graphene oxide that average-size is more than 100um is configured to concentration for 6mg/mL graphene oxide water solutions,
The ammonium hydrogen carbonate of mass fraction 0.1 is added in solution, is poured on after ultrasonic disperse on Die and mould plate and is dried into graphene oxide membrane, so
Reduced afterwards with hydrazine hydrate reduction agent；Graphene film after reduction first progressively heats up 500 DEG C under atmosphere of inert gases, protects
Warm 2h；1000 DEG C are progressively warming up under atmosphere of inert gases, 3h is incubated；2500 are progressively warming up under atmosphere of inert gases
DEG C, it is incubated after 4h, Temperature fall and can obtain porous graphene film.After graphene film is suppressed under high pressure, its two
Side coats PDMS insulating protective layers, constitutes Electric radiant Heating Film, and fixed electrode, electrode and graphene Electric radiant Heating Film are distinguished at the two ends of Electric radiant Heating Film
It is connected.
Heating rate is 0.1 DEG C/min at described 500 DEG C, and heating rate is 1 DEG C/min at 1000 DEG C, 2500 DEG C with
Under, heating rate is 5 DEG C/min.Described pressing process pressure is 200MP, and the time is 100h.
Obtained film density is 2.11g/cm3, it is resistant to bend repeatedly more than 1200 times, intensity is 80MP, and conductance is
10600S/cm, thermal conductivity is 2100W/mK.The structure of graphene film is very fine and close；After high temperature reduction, contain inside graphene film
The graphene film of the various numbers of plies, and structure is all very perfect, and this lays the foundation for heat conduction.Graphene membrane surface and inside are all
There are many folds, this lays a good foundation for the flexibility of graphene film.The elongation at break of the graphene film of preparation reaches
16%, belong to flexible fracture.After doubling repeatedly, conductivity variations less, are maintained at 10600S/cm or so, illustrate that it is flexible
Very well, after and rolling repeatedly, its performance can be recovered as before again, this explanation, and the graphene film that we prepare is real graphite
Alkene macroscopic view assembles.
Comparative example 1：It is performed as described above shown in example 1, changes its Elevated Temperature Conditions as follows：
2500 DEG C are directly warming up to 100 DEG C/min speed, and reacts same time.The extension at break of prepared film
Rate is 6%, and intensity is 20MP, and conductance is 4000S/cm, and thermal conductivity is 1000W/mK.
Comparative example 2：It is performed as described above shown in example 1, changes the raw material of its graphene oxide used, it is left 30% with shive content
Right graphene oxide.Then the elongation at break of prepared film is 7%, and intensity is 10MP, and conductance is 3400S/cm, thermal conductivity
Rate is 800W/mK.
Embodiment 2：
The graphene oxide that average-size is more than 100um is configured to concentration for 30mg/mL graphene oxide water solutions,
The urea of mass fraction 5% is added in solution, is poured on after ultrasonic disperse on Die and mould plate and is dried into graphene oxide membrane, Ran Houyong
Hydrogen iodide reducing agent is reduced；Graphene film after reduction under atmosphere of inert gases according to the heat shown in 1~table of table 3 at
Reason mode carries out three step heat treatments；Porous graphene film is can obtain after Temperature fall.Graphene film is pressed under high pressure
After system, its both sides coat PDMS insulating protective layers, constitute Electric radiant Heating Film, Electric radiant Heating Film two ends distinguish fixed electrode, electrode with
Graphene Electric radiant Heating Film is connected.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 3:3rd step Elevated Temperature Conditions
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.
As it can be seen from table 1 comparing A1, B1, C1, D1, E1, A1 temperature is too low, is not enough to removing most of degradable
Functional group, cause gas in second step pyroprocess largely quickly to produce, lamellar structure torn at high temperature；E1 temperature mistakes
Height, generation gas is too fast, both can cause deterioration in material properties.Have only at a temperature of B1, C1, D1, functional group can slowly simultaneously
Thoroughly remove, to ensure material property.Compare C1, F1, G1, H1, F1 heating rates are too low, gas release is excessively slow；H1 liters
Warm process is too fast, and gas release is too fast, tears material internal structure, is unfavorable for forming conductive channel.Compare C1, I1, J1, K1,
L1, M1, I1 soaking times are too short, it is impossible to ensure the degraded of most of functional group；M1 insulating processes are long, can absorb inside stove
Tar, be unfavorable for the lifting of performance.C1, J1, K1, L1 are due to avoiding 2 points of the above, with good electric heating property and bending
Performance.
From Table 2, it can be seen that comparing A2, B2, C2, D2, E2, A2 heating rates are too low to be not enough to form small space
Structure, has a strong impact on electric heating property.E programming rates are too high, can tear graphene interlayer structure so that graphene film electric heating property
It is deteriorated.Have only under B2, C2, D2 programming rate, just can the capable continuity both ensured inside graphene film.Compare C2, F2,
G2, H2, F2 temperature are too low so that stable functional group can not be sufficiently disengaged from, and easily transition is released during subsequently graphited
Deflation body, the stable formation of destruction graphene-structured；H2 temperature is too high, has reached graphitization temperature, now gas release
Under the conditions of, its temperature is also not enough to maintain the formation of conductive network, and the micro- airbag structure now formed is imperfect；Compare C2, I2,
J2, K2, L2, M2, I2 soaking times are too short, and stable functional group can not fully come off；M2 overlong times, graphene film is easily inhaled
Attached tar, is unfavorable for the lifting of film properties；And can both ensure fully coming off for stabilising functional group under the conditions of C2, J2, K2, and energy
Avoid the puzzlement of tar.
From table 3 it is observed that comparing A3, B3, C3, D3, E, A3 heating rates are too low, the mistake that most stabilising functional group comes off
Slowly；E temperature-rise periods are too fast, and gas release and high-temperature expansion are too fast, are easily destroyed graphene-structured.Only B3, C3, D3 feelings
Under condition, the structure on graphene could be repaired slowly.Compare C3, F3, G3, H3, I3, F3 outlet temperatures are too low, graphene knot
Structure repairs not perfect enough, so various performances are all very poor；I3 outlet temperatures are too high, and graphene can be vaporized；C3, G3, H3's
At a temperature of could both ensure the reparation of graphene-structured, will not be vaporized again.Compare C3, J3, K3, L3, M3, J3 soaking times
Too low, graphene-structured can not be repaired fully, and M3 soaking times are long, can also to adsorb the tar in body of heater, influence film
Electric heating and bending performance.
Claims (7)
1. a kind of foldable electrothermal film device based on graphene, it is characterised in that cut including heater element, diaphragm and two
Fluid, the diaphragm is located 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；It is described
Diaphragm is PDMS films, and the body that dams is metal electrode；Heater element is Flexible graphene film, is prepared by the following method and obtains：
（1）The graphene oxide that average-size is more than 100 μm is configured to concentration for 6 ~ 30mg/mL graphene oxide water solutions,
Mass fraction 0.1-5% auxiliary agent is added in the solution, and the auxiliary agent is inorganic salts, organic molecule or macromolecule；Ultrasonic disperse
Afterwards, it is poured on Die and mould plate and is dried into graphene oxide membrane, is then reduced with reducing agent；
（2）Graphene film after reduction is first warming up to 500-800 under atmosphere of inert gases with 0.1-1 DEG C/min speed
DEG C, it is incubated 0.5-2h；
（3）1000-1300 DEG C is warming up to 1-3 DEG C/min speed under atmosphere of inert gases, 0.5-3h is incubated；
（4）2500-3000 DEG C is warming up to 5-8 DEG C/min speed under atmosphere of inert gases, 0.5-4h, Temperature fall is incubated
It can obtain porous graphene film afterwards；
（5）Graphene film is suppressed under high pressure can obtain Flexible graphene film；
Graphene oxide of the average-size more than 100 μm 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, breadth coefficient is between 0.2-0.5.
2. device as claimed in claim 1, it is characterised in that described inorganic salts are ammonium hydrogen carbonate；Organic molecule is selected from
Glycerine, urea, thiocarbamide, azodicarbonamide, acrylic emulsion；Macromolecule is selected from polyethylene glycol 200, polyethylene glycol 400, fiber
Element, gelatin, chitosan, aqueous polyurethane.
3. device as claimed in claim 1, it is characterised in that described reducing agent comprising hydrazine hydrate, amine, ascorbic acid,
Hydrogen iodide.
4. device as claimed in claim 1, it is characterised in that described pressing process pressure is 50-200MPa, and the time is 6-
300 h。
5. device according to claim 1, it is characterised in that the Modified-Hummer methods in the step 1.1 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.
6. device according to claim 1, it is characterised in that the mesh screen is the acidproof mesh screen of titanium alloy.
7. device according to claim 1, it is characterised in that in the step 1.1, the reaction solution of oxidized graphite flake passes through
Diluting concentrated sulfuric acid agent is diluted, and the volume of diluent is 1-10 times of reaction solution volume.
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| CN106947436B (en) | 2017-05-10 | 2022-10-14 | 中国科学院宁波材料技术与工程研究所 | Thermal interface material and preparation and application thereof |
| CN107454692A (en) * | 2017-07-14 | 2017-12-08 | 成都三乙医疗科技有限公司 | A kind of graphene heating plate |
| CN107651670B (en) * | 2017-10-13 | 2019-10-15 | 杭州高烯科技有限公司 | A kind of preparation method of no folding line elastic graphite alkene film |
| CN108521683B (en) * | 2018-05-15 | 2021-06-11 | 广西大学 | Nano-cellulose graphene oxide electric heating material and preparation method thereof |
| CN108966376B (en) * | 2018-07-10 | 2020-06-16 | 浙江大学 | Collapsible electric heat membrane device based on graphite alkene |
| CN108726509B (en) * | 2018-08-08 | 2021-06-22 | 内蒙古石墨烯材料研究院 | Graphene electrothermal film and preparation method and application thereof |
| CN109462900B (en) * | 2018-11-29 | 2021-07-13 | 牛墨石墨烯应用科技有限公司 | High-temperature graphene heating plate and preparation method thereof |
| CN109775697B (en) * | 2019-03-17 | 2020-08-18 | 杭州高烯科技有限公司 | High-conductivity foldable graphene film and preparation method and application thereof |
| CN110002438A (en) * | 2019-05-23 | 2019-07-12 | 科炭(厦门)新材料有限公司 | A kind of flexible, porous graphene film and its preparation method and application |
| CN114105125A (en) * | 2020-04-03 | 2022-03-01 | 常州富烯科技股份有限公司 | Method for preparing medium transmission core in heat pipe |
| CN112022686A (en) * | 2020-07-29 | 2020-12-04 | 烯旺新材料科技股份有限公司 | New application of graphene in amplitude improvement and channel following conduction of microvascular vasomotor |
| CN115087155B (en) * | 2022-07-21 | 2022-11-15 | 佛山(华南)新材料研究院 | Flexible skin-touch graphene electric heating sheet and manufacturing method thereof |
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