CN104715927B - A kind of preparation method of the thin film capacitor based on graphene composite film - Google Patents
A kind of preparation method of the thin film capacitor based on graphene composite film Download PDFInfo
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- 239000010408 film Substances 0.000 title claims abstract description 143
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 87
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 86
- 239000003990 capacitor Substances 0.000 title claims abstract description 61
- 239000010409 thin film Substances 0.000 title claims abstract description 29
- 239000002131 composite material Substances 0.000 title claims abstract description 23
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 238000009413 insulation Methods 0.000 claims abstract description 43
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 19
- 238000001035 drying Methods 0.000 claims abstract description 18
- XMBWDFGMSWQBCA-UHFFFAOYSA-N hydrogen iodide Chemical compound I XMBWDFGMSWQBCA-UHFFFAOYSA-N 0.000 claims abstract description 15
- 229940071870 hydroiodic acid Drugs 0.000 claims abstract description 14
- 238000000576 coating method Methods 0.000 claims description 18
- 239000012528 membrane Substances 0.000 claims description 17
- 239000011248 coating agent Substances 0.000 claims description 16
- 239000007788 liquid Substances 0.000 claims description 5
- -1 polypropylene Polymers 0.000 claims description 5
- 239000004743 Polypropylene Substances 0.000 claims description 4
- 125000004494 ethyl ester group Chemical group 0.000 claims description 4
- 229920001155 polypropylene Polymers 0.000 claims description 4
- 230000009467 reduction Effects 0.000 claims description 4
- 229920006289 polycarbonate film Polymers 0.000 claims description 3
- 239000004793 Polystyrene Substances 0.000 claims description 2
- 229920002223 polystyrene Polymers 0.000 claims description 2
- 238000011084 recovery Methods 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 description 14
- 239000000463 material Substances 0.000 description 11
- 238000005516 engineering process Methods 0.000 description 9
- 230000000694 effects Effects 0.000 description 8
- 238000005457 optimization Methods 0.000 description 7
- 238000006722 reduction reaction Methods 0.000 description 7
- 239000011247 coating layer Substances 0.000 description 6
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- 229910052751 metal Inorganic materials 0.000 description 5
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- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 239000004411 aluminium Substances 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
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- 239000011701 zinc Substances 0.000 description 2
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- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
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Abstract
The invention discloses a kind of thin film capacitor preparation method based on graphene composite film, comprise the following steps：At 70~110 DEG C, concentration is coated on insulation film for 0.1~100mg/ml graphene oxide water solution, thickness is formed and is not less thanCoat；Then, it is that 30~120 DEG C of drying in oven solidify by film feeding temperature；Then, by film keep flattened state under with mass concentration be 1%~50% hydroiodic acid solution reaction；The time of reaction is 5~90 minutes；Then, film is obtained into the laminated film of graphene/insulation film in the drying in oven that temperature is 30~120 DEG C；By the reserved screen band of the laminated film of graphene/insulation film, then cut, wind, ultimately form thin film capacitor.Energy density, the power density of the obtained thin film capacitor based on graphene composite film are big, can further reduce the volume of capacitor, increase capacitance, reduce cost.
Description
Technical field
The invention belongs to thin film capacitor field, more particularly, to a kind of production of graphene composite film capacitor
Technology.
Background technology
Existing thin film capacitor is to make capacitor using the composite membrane film that metallizes, i.e. made by vacuum coating equipment
The heating fusing of aluminium, zinc or other metals, completes the coating metal to base film, forms electric capacity under the conditions of vacuum evaporation
The electrode layer of device.The base material of traditional thin film capacitor is generally polypropylene and polyester film, the thickness of thin of base material；In order to obtain
Larger electric capacity by material, it is necessary to roll long enough, and the thin film capacitor of acquisition can be used for handing over straight circuit.Thin film capacitor
And preparation method thereof shortcoming be that metal-coated structure is fine and close, impurity content big, the metallic diaphragm of coating under air extremely
Easily oxidation, causes metallic diaphragm quality and yield rate to reduce.Above-mentioned shortcomings influence huge to capacitor service life,
Easily very big damage is caused to base film in metallization process, reduction dielectric strength (base material thickness can reduce 1/4~1/5,
Have a strong impact on its dielectric strength).More seriously, metallization compound film capacitor is easy by environment temperature in work operation
With the influence of the factor such as humidity, reliable working operation is caused to substantially reduce.Under electric field action easily occur electrochemical reaction and
Air ionization, thus there is certain potential safety hazard.
The two-dimension periodic honeycomb lattice structure that graphene is made up of carbon hexatomic ring, is used as a kind of its application of new material
Still in continuous explore.Miniature graphene ultracapacitor is just because the effect of its super capacitor is attracted attention by the world, but this micro-
There is larger difference in the structure of type graphene ultracapacitor and thin film capacitor, ultracapacitor is to be based on electrochemical principle
Ultracapacitor, generally require cooperation electrolyte use, ultracapacitor storage energy in the electric charge of separation, for storing
The area of electric charge is bigger, electric charge that is isolating is more intensive, and its capacitance is bigger；Because resistance is big in ultracapacitor, often not
It can be used for alternating current circuit.
The content of the invention
It is multiple based on graphene it is an object of the invention to provide one kind for the drawbacks described above or Improvement requirement of prior art
The preparation method of the thin film capacitor of film is closed, wherein changing by the material to its crucial electrode layer, preparation technology parameter etc.
Enter, compared with prior art, method of the present invention can effectively solve the problem that metallization compound film capacitor metal-coated structure
It is not fine and close, the problem of impurity content is big, and damage of the processing technology to base material is reduced, the film prepared according to the inventive method
The property of capacitor is stable, service life is long.
To achieve the above object, according to one aspect of the present invention, there is provided a kind of film based on graphene composite film
The preparation method of capacitor, it is characterised in that comprise the following steps：
(1) at a temperature of 70 DEG C~110 DEG C, by the graphene oxide water solution that concentration is 0.1mg/ml~100mg/ml
It is coated on insulation film, forms thickness and be not less thanCoat；Coating speed is 3m/s~30m/s；
(2) insulation film with coat that step (1) is obtained is flattened；Then, this is had to the insulation of coat
Film is placed in the drying in oven that temperature is 30 DEG C~120 DEG C and solidified；The time of the drying is 5 minutes~60 minutes；
(3) film for obtaining step (2) is in the case where keeping flattened state, with the hydrogen iodine that mass concentration is 1%~50%
Acid solution is reduced；The described recovery time is 5 minutes~90 minutes；Then, it is 30 DEG C~120 DEG C in temperature by the film
Drying in oven, obtains the laminated film of graphene/insulation film；
(4) the reserved screen band of the laminated film for the graphene/insulation film for obtaining step (3), then cuts, winds, most
End form is into thin film capacitor.
As present invention further optimization, overlay film pressure is 1bar~10bar when being coated described in the step (1).
As present invention further optimization, the thickness of the coat in the step (1) is
As present invention further optimization, the insulation film in the step (1) is poly- ethyl ester, polypropylene, polyphenyl second
Any one in alkene and polycarbonate film, the thickness of insulation film is 4 microns~12 microns.
As present invention further optimization, it is to pass through to flatten the insulation film with coat in the step (2)
Insulation film with coat is transmitted what is carried out into membrane tension levelling device.
As present invention further optimization, the baking oven in the step (2) is convection oven.
As present invention further optimization, in the step (2) temperature for the drying time in 120 DEG C of baking oven not
More than 15 minutes.
As present invention further optimization, the hydroiodic acid solution reduction that mass concentration is 50% is used in the step (3)
Time be no more than 10 minutes.
By the contemplated above technical scheme of the present invention, compared with prior art, have the advantages that：
1. the thin film capacitor based on graphene composite film that the present invention is obtained, conventional films electricity is instead of using graphene
The metal (such as aluminium, zinc) of appearance, because graphene self-resistance rate is low, flexible property, obtained thin film capacitor energy
Density, power density are big.Also, the intensity of grapheme material is big, good toughness, its overlay film synthetic technology is simple；Due to using molten
The coating processes of liquid, reduce damage of the preparation process to base film (i.e. insulation film), it is ensured that the dielectric of insulation film
Intensity, effectively raises dielectric strength and the service life of capacitor, and favourable guarantor is provided for the performance of thin film capacitor
Barrier.
Because the specific surface area of grapheme material is high, compactness is good, the obtained thin-film capacitor based on graphene composite film
Energy density, the power density of device are big, can further reduce the volume of capacitor, increase capacitance, reduce cost.Graphene
Compound film production is environmentally safe using physics synthetic technology, and production capacitor is more cleaned.Thin relative to existing metallization
The use environment of membrane capacitance requires lower, and heatproof, heat-resisting, explosion-proof breakdown characteristics are stronger.Work operation in atmospheric environment
The remote ultra-traditional metallic film capacitor of graphene composite film thin film capacitor performance so that graphene composite film thin-film capacitor
Device is widely used field.
2. by being adjusted to the parameter in preparation technology, further ensure the thin-film electro based on graphene composite film
The quality of container.In the bifilm capacitor of graphene/insulation film, graphene, should be thin with insulation as electrode layer
Intermembranous to have stronger adhesive force, cover uniformly ensures good electric conductivity again.
It is controllable in order to form uniform thickness exemplified by graphene oxide water solution formation coat is coated on insulation film
Coat, the thickness of coat is not less than(can be more preferably ),
The concentration of graphene oxide water solution is 0.1mg/ml~100mg/ml；Coated temperature should be controlled between 70 DEG C~110 DEG C, temperature
Degree decides the state of graphene oxide water solution, and can influence infiltration and expansion of the graphene oxide water solution to insulation film
Dissipate, there is vital influence on the pattern of the coat of formation.During overlay film, overlay film pressure can also influence the coat to be formed
Quality, pressure is too small, coheres loosely, pressure is excessive, and coat may be caused to produce excessive defect, this hair with substrate material
Bright overlay film pressure is preferably 1bar~10bar, coat and insulation film to cohere effect good.Coat the speed of production pair of overlay film
Answer the time of contact of insulation film and graphene oxide water solution, and influenceed by graphene oxide water solution concentration, this hair
The speed of production of coating overlay film in bright is 3m/s~30m/s, at such speeds graphene oxide water solution and insulation film
Contact works well.The overlay film on insulation film in the present invention obtains the technique of coating layer, and coat film can be used directly
Machine is realized.
The stage of baking and curing is being carried out to the insulation film with coat, (is being led to by membrane tension levelling device
The sensor of jockey pulley is overregulated to adjust the flattening effect of film), film can be made to remain good profile pattern,
Ensure the planarization and uniformity of the graphene oxide coat after solidification.
Brief description of the drawings
Fig. 1 a are graphene two-dimensional structure schematic diagrames, and Fig. 1 b are graphene oxide water solutions；
Fig. 2 is the schematic flow sheet of the present invention；
Fig. 3 is the structural representation of coating processes of the present invention.
Implication in Fig. 3 representated by reference is as follows：1. film feeding；2. graphene oxide water solution proportioning device；3. apply
Cover roller；4. scraper；5. pressure roller；6. membrane tension leveling and drying；7. smooth roll；8. rubber rollers；9. reduction apparatus；10. drying dress
Put；11. winding.
Embodiment
In order to make the purpose , technical scheme and advantage of the present invention be clearer, it is right below in conjunction with drawings and Examples
The present invention is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, and
It is not used in the restriction present invention.
Embodiment 1
As shown in figure 3, being that 0.1mg/ml graphene oxide water solutions are poured into coating groove by 1000ml mass concentrations, apply
The control of machine speed of production is covered in 3m/s, and feeding 1 is capacitor membrane, by No. 2 and No. 3 transfer rollers that graphene oxide is water-soluble
Liquid is coated uniformly on film, to ensure that coating layer thickness is controllable and coating uniform, is repaiied by adjusting the angle and height of 4 scrapers
Positive graphene oxide thickness degree, control coat thickness existsThe adjustment of pressure roller 5 is adapted to pressure 3bar and completes graphene oxide
Keep laminated film that there is good flattening effect so as to baking and curing with the firm attachment of film, then by tension force levelling device 6,
And with drying unit, temperature control is sent to cut roll 7# and 8# that pressure is 2bar at 100 DEG C, by deflector roll and realizes holding exhibition
Level state, subsequently enter fill concentration be 40% reducing solution (such as：Hydroiodic acid etc.) the progress reduction reaction of device 9, herein also
During original, graphene oxide film and reducing solution are (such as：Hydroiodic acid etc.) react, graphene is reduced to by hydroiodic acid,
Graphene composite film product needed for obtaining, to remove 11 windings after 10 complete baking and curing again of film surface moisture,
Obtain the laminated film of graphene/insulation film.
Because coating machine is that graphene view picture is coated on capacitor membrane, and during production application it is root
The step of being also needed to according to the laminated film of the specification of capacitor, therefore above-mentioned graphene/insulation film by laser cutting.Pass through
Laser cutting, can be by the reserved screen band of laser cutting of the graphene on the laminated film of graphene/insulation film, for drawing electricity
The electrode of container.
After the completion of above process, then the laminated film of graphene/insulation film divided on small cutting machine by specification
Cut, then wind, so as to ultimately form thin film capacitor.
Insulation film (that is, capacitor membrane) in the present embodiment is poly- ethyl ester film 4 microns thick.
Embodiment 2
As shown in figure 3, being that 100mg/ml graphene oxide water solutions are poured into coating groove by 2000ml mass concentrations, apply
The control of machine speed of production is covered in 30m/s, feeding 1 is capacitor membrane, by No. 2 and No. 3 transfer rollers by graphene oxide water
Solution is coated uniformly on film, to ensure that coating layer thickness is controllable and coating uniform, by adjust the angle and height of 4 scrapers come
Graphene oxide thickness degree is corrected, control coat thickness existsThe adjustment of pressure roller 5 is adapted to pressure 4bar and completes graphite oxide
Alkene has good flattening effect to dry admittedly with the firm attachment of film, then by the holding laminated film of tension force levelling device 6
Change, and with drying unit, temperature control is sent to cut roll 7# and 8# that pressure is 2.5bar at 110 DEG C, by deflector roll and realized
Keep spreading, subsequently enter fill concentration be 50% reducing solution (such as：Hydroiodic acid etc.) 9 devices progress reduction reaction,
Again in this reduction process, graphene oxide film and reducing solution are (such as：Hydroiodic acid etc.) react, the graphene needed for obtaining
Laminated film product, to remove 11 windings after 10 complete baking and curing again of film surface moisture.
Insulation film (that is, capacitor membrane) in the present embodiment is 8 microns of thick polypropylene films.
Embodiment 3
As shown in figure 3, being that 50mg/ml graphene oxide water solutions are poured into coating groove by 2000ml mass concentrations, apply
The control of machine speed of production is covered in 15m/s, feeding 1 is capacitor membrane, by No. 2 and No. 3 transfer rollers by graphene oxide water
Solution is coated uniformly on film, to ensure that coating layer thickness is controllable and coating uniform, by adjust the angle and height of 4 scrapers come
Graphene oxide thickness degree is corrected, control coat thickness existsThe adjustment of pressure roller 5 is adapted to pressure 3.5bar and completes oxidation stone
Black alkene has good flattening effect to dry with the firm attachment of film, then by the holding laminated film of tension force levelling device 6
Solidification, and with drying unit, it is real that temperature control is sent to cut roll 7# and 8# that pressure is 2.5bar at 105 DEG C, by deflector roll
Now keep spreading, subsequently enter fill concentration be 45% reducing solution (such as：Hydroiodic acid etc.) 9 devices reduce it is anti-
Should, then in this reduction process, graphene oxide film and reducing solution are (such as：Hydroiodic acid etc.) react, the stone needed for obtaining
Black alkene laminated film product, to remove 11 windings after 10 complete baking and curing again of film surface moisture.
Insulation film (that is, capacitor membrane) in the present embodiment is 12 microns of thick polystyrene films.
Embodiment 4
As shown in figure 3, being that 0.1mg/ml graphene oxide water solutions are poured into coating groove by 1000ml mass concentrations, apply
The control of machine speed of production is covered in 3m/s, and feeding 1 is capacitor membrane, by No. 2 and No. 3 transfer rollers that graphene oxide is water-soluble
Liquid is coated uniformly on film；Coated temperature is 70 DEG C；To ensure that coating layer thickness is controllable and coating uniform, by adjusting 4 scrapers
Angle and height correct graphene oxide thickness degree, control coat thickness existsThe adjustment of pressure roller 5 is adapted to pressure
1bar completes graphene oxide and keeps laminated film to have good exhibition with the firm attachment of film, then by tension force levelling device 6
Flat effect is so as to baking and curing, and with drying unit, and temperature control is at 30 DEG C, and drying time is 60 minutes；Passed by deflector roll
It is sent to cut roll 7# and 8# that pressure is 2bar and realizes holding spreading, subsequently enters the reducing solution for filling that concentration is 10%
(such as：Hydroiodic acid etc.) 9 devices are carried out in reduction reaction, then this reduction process, and graphene oxide film and reducing solution are (such as：Hydrogen
Acid iodide etc.) react, the graphene composite film product needed for obtaining completes to dry again to remove film surface moisture by 10
11 winding, obtains the laminated film of graphene layer/insulation film after solidization.
Insulation film (that is, capacitor membrane) in the present embodiment is poly- ethyl ester film 12 microns thick.
Embodiment 5
As shown in figure 3, being that 5mg/ml graphene oxide water solutions are poured into coating groove by 1000ml mass concentrations, coat
The control of machine speed of production is in 25m/s, and feeding 1 is capacitor membrane, by No. 2 and No. 3 transfer rollers that graphene oxide is water-soluble
Liquid is coated uniformly on film；Coated temperature is 110 DEG C；To ensure that coating layer thickness is controllable and coating uniform, by adjusting 4 scrapers
Angle and height correct graphene oxide thickness degree, control coat thickness existsThe adjustment of pressure roller 5 is adapted to pressure
10bar completes graphene oxide and keeps laminated film to have good exhibition with the firm attachment of film, then by tension force levelling device 6
Flat effect is so as to baking and curing, and with drying unit, and temperature control is sent to pressure cutting for 2bar at 70 DEG C by deflector roll
Roller 7# and 8# realize keep spreading, subsequently enter fill concentration be 1% reducing solution (such as：Hydroiodic acid etc.) 9 devices enter
In row reduction reaction, then this reduction process, graphene oxide film and reducing solution are (such as：Hydroiodic acid etc.) react, obtain
Required graphene composite film product, to remove 11 windings after 10 complete baking and curing again of film surface moisture, is obtained
The laminated film of graphene/insulation film.
Insulation film (that is, capacitor membrane) in the present embodiment is 12 microns of thick polycarbonate films.
The graphene film capacitor of the production technology production of the graphene film capacitor of the present invention, the capacity of capacitor
It is the proportional relation of specific surface area and interfloor distance, i.e. c=(K* ε * S)/2 π * D), small volume, its energy density and power density
It is incomparable in the capacitor that the material having found makes in the past.Graphene composite film is made using physics synthetic technology to ring
Border is pollution-free, and production capacitor is more cleaned.Require lower in the use environment relative to existing metallic film capacitor, it is resistance to
Warm, heat-resisting, explosion-proof breakdown characteristics are stronger.Worked in atmospheric environment operation graphene composite film thin film capacitor performance it is remote
Ultra-traditional metallic film capacitor so that graphene composite film thin film capacitor is widely used field.
As it will be easily appreciated by one skilled in the art that the foregoing is merely illustrative of the preferred embodiments of the present invention, it is not used to
The limitation present invention, any modifications, equivalent substitutions and improvements made within the spirit and principles of the invention etc., it all should include
Within protection scope of the present invention.
Claims (5)
1. a kind of preparation method of the thin film capacitor based on graphene composite film, it is characterised in that comprise the following steps：
(1) at a temperature of 70 DEG C~110 DEG C, concentration is coated for 0.1mg/ml~100mg/ml graphene oxide water solution
On insulation film, forming thickness isCoat；Coating speed is 3m/s~30m/s；
The insulation film is any one in poly- ethyl ester, polypropylene, polystyrene and polycarbonate film, insulation film
Thickness is 4 microns~12 microns；
(2) insulation film with coat that step (1) is obtained is flattened；Then, this is had to the insulation film of coat
The drying in oven that temperature is 30 DEG C~120 DEG C is placed in solidify；The time of the drying is 5 minutes~60 minutes；
Wherein, by it is described with coat insulation film flattening be by by the insulation film with coat transmit into
What membrane tension levelling device was carried out；
(3) film for obtaining step (2) is molten for 1%~50% hydroiodic acid with mass concentration in the case where keeping flattened state
Liquid is reduced；The described recovery time is 5 minutes~90 minutes；Then, by the film in the baking oven that temperature is 30 DEG C~120 DEG C
Interior drying, obtains the laminated film of graphene/insulation film；
(4) the reserved screen band of the laminated film for the graphene/insulation film for obtaining step (3), then cuts, winds, most end form
Into thin film capacitor.
2. the preparation method of the thin film capacitor as claimed in claim 1 based on graphene composite film, it is characterised in that the step
Overlay film pressure is 1bar~10bar when being coated suddenly described in (1).
3. the preparation method of the thin film capacitor as claimed in claim 1 based on graphene composite film, it is characterised in that the step
Suddenly the baking oven in (2) is convection oven.
4. the preparation method of the thin film capacitor as claimed in claim 1 based on graphene composite film, it is characterised in that the step
Suddenly it is no more than 15 minutes for the drying time in 120 DEG C of baking oven in temperature in (2).
5. the preparation method of the thin film capacitor as claimed in claim 1 based on graphene composite film, it is characterised in that the step
Suddenly it is no more than 10 minutes for the time of 50% hydroiodic acid solution reduction with mass concentration in (3).
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| CN105236396A (en) * | 2015-09-01 | 2016-01-13 | 东华大学 | Preparation method of graphene oxide thin film |
| EP3151258A1 (en) * | 2015-09-30 | 2017-04-05 | Nawrocki, Piotr | Graphene capacitor, particularly for audio systems, and its use |
| CN106206015B (en) * | 2016-08-27 | 2018-03-02 | 安徽省宁国市海伟电子有限公司 | A kind of high temperature polypropylene metallized film |
| CN109961878B (en) * | 2017-12-22 | 2022-03-25 | 重庆元石盛石墨烯薄膜产业有限公司 | Method for setting functional layer of quantitative feeding transfer coating type graphene transparent conductive film substrate |
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| CN103337362A (en) * | 2013-04-24 | 2013-10-02 | 清华大学 | Nano capacitor and preparation method thereof |
| CN104219797A (en) * | 2014-09-10 | 2014-12-17 | 浙江碳谷上希材料科技有限公司 | Graphene electrothermal film |
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|---|---|---|---|---|
| US20100084697A1 (en) * | 2008-10-02 | 2010-04-08 | Kopp Thilo | Novel capacitors and capacitor-like devices |
| US8593783B2 (en) * | 2012-02-16 | 2013-11-26 | Elwha Llc | Graphene mounted on aerogel |
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| CN103337362A (en) * | 2013-04-24 | 2013-10-02 | 清华大学 | Nano capacitor and preparation method thereof |
| CN104219797A (en) * | 2014-09-10 | 2014-12-17 | 浙江碳谷上希材料科技有限公司 | Graphene electrothermal film |
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