CN106276862B - A kind of device of roll-to-roll continuous transfer graphene - Google Patents
A kind of device of roll-to-roll continuous transfer graphene Download PDFInfo
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- CN106276862B CN106276862B CN201510237119.5A CN201510237119A CN106276862B CN 106276862 B CN106276862 B CN 106276862B CN 201510237119 A CN201510237119 A CN 201510237119A CN 106276862 B CN106276862 B CN 106276862B
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 94
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 92
- 239000000463 material Substances 0.000 claims abstract description 73
- 238000001035 drying Methods 0.000 claims abstract description 26
- 238000000034 method Methods 0.000 claims abstract description 22
- 239000000758 substrate Substances 0.000 claims abstract description 19
- 238000004140 cleaning Methods 0.000 claims abstract description 17
- 238000005868 electrolysis reaction Methods 0.000 claims abstract description 9
- 239000011159 matrix material Substances 0.000 claims abstract description 7
- 230000005587 bubbling Effects 0.000 claims abstract description 5
- 239000011888 foil Substances 0.000 claims description 14
- 239000002184 metal Substances 0.000 claims description 14
- 229910052751 metal Inorganic materials 0.000 claims description 14
- 239000003792 electrolyte Substances 0.000 claims description 13
- 239000002356 single layer Substances 0.000 claims description 6
- 238000005229 chemical vapour deposition Methods 0.000 claims description 5
- 239000000243 solution Substances 0.000 claims description 5
- 239000004831 Hot glue Substances 0.000 claims description 4
- 239000000853 adhesive Substances 0.000 claims description 4
- 230000001070 adhesive effect Effects 0.000 claims description 4
- 230000005540 biological transmission Effects 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- 238000004804 winding Methods 0.000 claims description 4
- 239000007864 aqueous solution Substances 0.000 claims description 3
- 230000001276 controlling effect Effects 0.000 claims description 3
- 239000002253 acid Substances 0.000 claims description 2
- 239000000654 additive Substances 0.000 claims description 2
- 230000000996 additive effect Effects 0.000 claims description 2
- 239000003513 alkali Substances 0.000 claims description 2
- 239000011248 coating agent Substances 0.000 claims description 2
- 238000000576 coating method Methods 0.000 claims description 2
- 229920001577 copolymer Polymers 0.000 claims description 2
- 229910002804 graphite Inorganic materials 0.000 claims description 2
- 239000010439 graphite Substances 0.000 claims description 2
- 239000003960 organic solvent Substances 0.000 claims description 2
- 238000003825 pressing Methods 0.000 claims description 2
- 230000001105 regulatory effect Effects 0.000 claims description 2
- 150000003839 salts Chemical class 0.000 claims description 2
- 238000000926 separation method Methods 0.000 claims description 2
- 239000004094 surface-active agent Substances 0.000 claims description 2
- 230000001360 synchronised effect Effects 0.000 claims description 2
- JTXMVXSTHSMVQF-UHFFFAOYSA-N 2-acetyloxyethyl acetate Chemical compound CC(=O)OCCOC(C)=O JTXMVXSTHSMVQF-UHFFFAOYSA-N 0.000 claims 1
- -1 graphite Alkene Chemical class 0.000 claims 1
- 238000004080 punching Methods 0.000 claims 1
- 239000007921 spray Substances 0.000 claims 1
- 238000004506 ultrasonic cleaning Methods 0.000 claims 1
- 238000005516 engineering process Methods 0.000 abstract description 6
- 230000002687 intercalation Effects 0.000 abstract description 6
- 238000009830 intercalation Methods 0.000 abstract description 6
- 230000015572 biosynthetic process Effects 0.000 abstract description 2
- 238000003786 synthesis reaction Methods 0.000 abstract description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 7
- 239000011889 copper foil Substances 0.000 description 7
- 239000007789 gas Substances 0.000 description 5
- 239000002390 adhesive tape Substances 0.000 description 4
- 229920002799 BoPET Polymers 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 150000001336 alkenes Chemical class 0.000 description 3
- 239000004820 Pressure-sensitive adhesive Substances 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 239000010410 layer Substances 0.000 description 2
- 239000004575 stone Substances 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 1
- 239000002202 Polyethylene glycol Substances 0.000 description 1
- LCJHLOJKAAQLQW-UHFFFAOYSA-N acetic acid;ethane Chemical compound CC.CC(O)=O LCJHLOJKAAQLQW-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 150000001721 carbon Chemical group 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 230000001413 cellular effect Effects 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 229920001223 polyethylene glycol Polymers 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000002023 wood Substances 0.000 description 1
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- Carbon And Carbon Compounds (AREA)
Abstract
It is specially a kind of to comprehensively utilize roll-to-roll technology and gas sparging intercalation technique continuously shifts the device of large-area graphene the present invention relates to the transfer device of graphene.The device includes material web, scrolling feed device, electrolysis bubbling device, cleaning device, drying device, tensile force adjusting device, scrolling material collecting device and control system, continuously shifts graphene in roll-to-roll mode.Device synthesis has used roll-to-roll technology and gas sparging intercalation technique, realizes the takeup type transfer of large-area graphene, while initial substrate is reusable.Device of the present invention is compatible with a variety of transfer medium films, the removing and transfer suitable for graphene and flexible substrate, it can also be used to transfer graphene to rigid matrix surface.
Description
Technical field:
The present invention relates to the transfer devices of graphene, specially a kind of to comprehensively utilize roll-to-roll technology and gas sparging intercalation
Technology continuously shifts the device of large-area graphene.
Background technique:
Graphene be by single layer of carbon atom it is tightly packed at bi-dimensional cellular shape crystal structure.The unique crystal knot of graphene
Structure makes it have excellent electricity, calorifics and mechanical property, it is expected in multi-functional nanometer electronic device, transparent conductive film, composite wood
The fields such as the gas sensors such as material, catalysis material are widely applied.Large area, high-quality graphene in acquisition different matrix
It is the premise and basis for realizing above-mentioned application.Currently, CVD method is the main side of controllable preparation large area, high-quality graphene
Method, the development of related process are also more perfect.However, how the large area of CVD growth, high-quality graphene to be efficiently transferred to
It is still the bottleneck for restricting graphene application in particular substrate.Therefore, the transfer method and dress of low cost, serialization are established
It sets for pushing the scale application of grapheme material to play an important role and meaning.
Chinese invention patent (patent No. ZL 201110154465.9) discloses a kind of lossless transfer graphene of low cost
Method.This method utilizes the principle of gas sparging intercalation, realizes nondestructively peeling and the transfer of graphene and initial substrate, initially
Matrix can repeatedly use, and significantly reduce the cost of transfer of graphene.However, lacking at present completely compatible with this method
Transfer device, limit application of the lossless transfer techniques of low cost in scale transfer graphene.
Summary of the invention:
The purpose of the present invention is to provide a kind of devices of roll-to-roll continuous transfer graphene, for realizing large area graphite
The low cost of alkene, serialization transfer.
The technical scheme is that
It is a kind of it is roll-to-roll it is continuous transfer graphene device, including material web, scrolling feed device, electrolysis bubbling device,
The components such as cleaning device, drying device, tensile force adjusting device, scrolling material collecting device and control system, in roll-to-roll mode
Continuous transfer graphene;
Material web is made a living the overlay film of initial substrate and graphene surface with graphene;The initial substrate of graphene includes
The foil or band of metal;Graphene is the graphene of the graphene grown using chemical vapor deposition method or separation method growth;
The overlay film on surface is the soft objectives matrix for shifting the deielectric-coating or graphene of graphene.
The device of the roll-to-roll continuous transfer graphene, scrolling feed device includes feeding roller and rotating device, is sent
Material roller is used to provide the power of rotation for winding and conveying material web, rotating device, and revolving speed and direction are by control system tune
Section.
The device of the described roll-to-roll continuous transfer graphene, electrolysis bubbling device include electrode, electrolytic cell and transmission shaft,
The connection of the cathode of material web and electrode, store in electrolytic cell electrolyte, the anode and electrolyte contacts of electrode, anode and cathode and
Electrolysis power connection;
Electrolyte includes the aqueous solution of the one or more of acid, alkali, salt, is added adjusts solution surface as needed
The additive of the properties such as power, viscosity.
The device of the roll-to-roll continuous transfer graphene, cleaning device use is washed away, sprayed, impregnating and ultrasonic wave is clear
The mode for the one or more washed cleans initial substrate and graphene film, for removing the attachment on surface;
Cleaning solution includes a combination of one or more combination of water, organic solvent and surfactant.
The device of the roll-to-roll continuous transfer graphene, drying device includes the drying equipments such as baking oven and blower, right
Initial substrate and graphene film are dried.
The device of the roll-to-roll continuous transfer graphene, tensile force adjusting device includes tensile force regulating roller and sensing
Device, for adjusting the tensile force of material web, to ensure that feeding is synchronous with rewinding.
The device of the roll-to-roll continuous transfer graphene, scrolling material collecting device includes material receiving roller and rotating device, is received
Material roller is used to provide the power of rotation for winding and tightening up material web, rotating device, and revolving speed and direction are by control system tune
Section.
The device of the roll-to-roll continuous transfer graphene, control system includes power supply, temperature controller, rotating device
Control program and equipment, power supply is rotating device, drying device and electrolytic process power supply in device, and temperature controller is used for
The temperature of drying device is adjusted, controls program and equipment for controlling rotating device and tensile force adjusting device.
The device of the roll-to-roll continuous transfer graphene, among different components using live-roller realization material web
Transmission.
The device of the roll-to-roll continuous transfer graphene, installs other transfer dresses additional before material receiving roller as needed
It sets, the graphene on overlay film surface is transferred in the target substrate of other flexibility or rigidities.
The features of the present invention and beneficial effect are:
1. device synthesis of the present invention has used roll-to-roll technology and gas sparging intercalation technique, large area stone is realized
Serialization, the takeup type transfer of black alkene, while initial substrate is reusable, the stripping suitable for graphene and flexible initial substrate
From and transfer.
2. a variety of transfer medium films such as device of the present invention and heat release adhesive tape, pressure sensitive adhesive tape, soft objectives matrix are equal
It is compatible, therefore flexible or rigid matrix surface can be transferred graphene to.
Detailed description of the invention:
Fig. 1 is the organigram of roll-to-roll continuous transfer graphene device.
In figure, 1 material web;2 feeding rollers;3 cathode;4 live-rollers;5 anodes;6 electrolytic cells;7 electrolyte;8 cleaning devices;9
Drying device;10 dance rollers;11 material receiving rollers I;12 material receiving rollers II;13 control systems;14 hot calenders.
Specific embodiment:
The present invention is described in further detail below by drawings and examples.
As shown in Figure 1, the device of the roll-to-roll continuous transfer graphene of the present invention specifically includes that material web 1, feeding roller 2, bears
Pole 3, live-roller 4, anode 5, electrolytic cell 6, electrolyte 7, cleaning device 8, drying device 9, dance roller 10, material receiving roller I 11,
Material receiving roller II 12 and control system 13 etc., specific structure is as follows:
The graphene surface adhesive transfer medium grown in metal foil forms material web 1, and one end of material web 1, which is wound in, to be sent
Expect on roller 2, the other end of material web 1 passes through cathode 3 and extends to 5 top of anode in the electrolyte 7 of electrolytic cell 6, and material web 1 is through being driven
Roller 4 separates two parts: metal foil and graphene/transfer medium.Wherein, metal foil is wound in material receiving roller I 11, winds in metal foil
In setting gradually cleaning device 8, drying device 9, dance roller 10 on the channel of material receiving roller I 11;Graphene/transfer medium volume
It is around in material receiving roller II 12, cleaning device 8 is set gradually on the channel that graphene/transfer medium is wound in material receiving roller II 12, is done
Dry device 9, dance roller 10.
Wherein, anode 5 and the material web 1 connecting with cathode 3 generate the water electrolysis in electrolyte 7 on 1 surface of material web
Hydrogen removes graphene from metal foil surface.Control system 13 includes the control journey of power supply, temperature controller, rotating device
Sequence and equipment, power supply are rotating device, drying device and electrolytic process power supply in device, and temperature controller is for adjusting drying
The temperature of device controls program and equipment for controlling rotating device and tensile force adjusting device.
In addition, when discharging adhesive tape and pressure sensitive adhesive tape as transfer medium using heat, it can be in drying device 9 and material receiving roller II 12
Between install additional hot calender 14.
Embodiment 1:
In the present embodiment, the method for roll-to-roll continuous transfer graphene is as follows: using copper foil as initial substrate, using poly-
Ethylene glycol terephthalate (PET) film is as transfer medium and target substrate, using hot melt adhesive (ethane-acetic acid ethyenyl ester
Copolymer) it is used as adhesive.Using CVD method, (in the present embodiment, copper foil, which can change nickel foil or other into, to be grown on copper foil
The metal foil of graphene) growth single-layer graphene.Using the cementation of hot melt adhesive, on the surface of graphene by PET film pressing,
Form material web 1.By the way of motor with reciprocating movement then material web 1 is separated material web wound on 2 surface of feeding roller,
Cathode 3, live-roller 4, cleaning device 8, drying device 9, dance roller 10 are sequentially passed through, respectively rolls up copper foil and PET film
It is wound on the surface of material receiving roller I 11 and material receiving roller II 12.
In transfer process, open feeding roller 2 and material receiving roller (material receiving roller I 11, material receiving roller II 12), make material web with 1~
The speed of 10cm/min transmits.Meanwhile 1 ampere of electric current is applied on cathode 3 and anode 5 using constant current mode, to being immersed in
Material band part in electrolyte 7 carries out electrolysis and is bubbled removing.Electrolyte is the NaOH aqueous solution of 1mol/L, and the container used is
Electrolytic cell 6, the operation temperature of electrolytic process is at 15~35 DEG C.Spray cleaning 8 and drying device 9 is opened, respectively to peeling away
Copper foil and single-layer graphene/PET film are cleaned and are dried.Cleaning solution is deionized water, and the temperature of drying device is set as
60℃.Copper foil after drying can be used for CVD growth graphene again wound on the surface of material receiving roller I 11.Single-layer graphene/PET
Winding film is on the surface of material receiving roller II 12, to complete the transfer of graphene.In order to shift multi-layer graphene, using single layer stone
Black alkene/PET is pressed together on graphene/copper foil surface as transfer medium, and repeating above-mentioned transfer process can be obtained the specific number of plies
Multi-layer graphene film.
Embodiment 2:
Difference from Example 1 is, in the present embodiment, the method for roll-to-roll continuous transfer graphene is as follows: using
Heat release adhesive tape installs hot calender 14 additional as transfer medium between drying device 9 and material receiving roller II 12.Transfer process
In, after obtained " graphene/heat discharges adhesive tape " composite membrane drying, hot calender 14 is first passed around, in 120 DEG C and 0.1MPa
Under the conditions of graphene is then transferred to glass surface, remaining heat release tape roll is around the surface of material receiving roller 12.
Embodiment the result shows that, the present invention continuously shifts the device of large-area graphene, be based on gas sparging Intercalation principle
Graphene is shifted, and realizes the transfer of serialization using roll-to-roll technology, has that structure is simple, transfer efficiency is high and cost of transfer
Low outstanding feature.
Claims (8)
1. a kind of device of roll-to-roll continuous transfer graphene, it is characterised in that: including material web, scrolling feed device, electrolysis
Bubbling device, cleaning device, drying device, tensile force adjusting device, scrolling material collecting device and control system, with roll-to-roll side
Formula continuously shifts graphene;
Material web is made a living the overlay film of initial substrate and graphene surface with graphene;The initial substrate of graphene includes metal
Foil or band;Graphene is the graphene of the graphene grown using chemical vapor deposition method or separation method growth;Surface
Overlay film be shift graphene deielectric-coating or graphene soft objectives matrix;
The graphene surface adhesive transfer medium grown in metal foil forms material web, and one end of material web is wound in feeding roller
On, the other end of material web passes through cathode and extends to anode top in the electrolyte of electrolytic cell, and material web separates two through live-roller
Point: metal foil and graphene/transfer medium;Wherein, metal foil is wound in material receiving roller I, is wound in the logical of material receiving roller I in metal foil
Cleaning device, drying device, dance roller are set gradually on road;Graphene/transfer medium is wound in material receiving roller II, in graphite
Alkene/transfer medium is wound on the channel of material receiving roller II and sets gradually cleaning device, drying device, dance roller;
Using pet film as transfer medium and target substrate, using hot melt adhesive ethylene-acetate second
Enoate copolymer grows single-layer graphene as adhesive, using CVD method on metal foil;Using the cementation of hot melt adhesive,
On the surface of graphene by pet film pressing, material web is formed;It will by the way of motor with reciprocating movement
Then material web separates material web wound on feeding roller surface, sequentially pass through cathode, live-roller, cleaning device, dry dress
It sets, dance roller, respectively by metal foil and pet film wound on material receiving roller I and material receiving roller II
Surface;
Tensile force adjusting device includes tensile force regulating roller and sensor, for adjusting the tensile force of material web, to ensure feeding
It is synchronous with rewinding;Control system includes the control program and equipment of power supply, temperature controller, rotating device, and power supply is in device
Rotating device, drying device and electrolytic process power supply, temperature controller is used to adjust the temperature of drying device, control program and
Equipment is for controlling rotating device and tensile force adjusting device.
2. the device of roll-to-roll continuous transfer graphene described in accordance with the claim 1, it is characterised in that: scrolling feed device packet
Feeding roller and rotating device are included, feeding roller is used to provide the power of rotation for winding and conveying material web, rotating device, turn
Speed and direction are adjusted by control system.
3. the device of roll-to-roll continuous transfer graphene described in accordance with the claim 1, it is characterised in that: electrolysis bubbling device packet
Include electrode, electrolytic cell and transmission shaft, the cathode of material web and electrode connects, store electrolyte in electrolytic cell, the anode of electrode with
Electrolyte contacts, anode and cathode are connect with electrolysis power;
Electrolyte includes the aqueous solution of the one or more of acid, alkali, salt, as needed be added adjust solution surface tension,
The additive of viscometric properties.
4. the device of roll-to-roll continuous transfer graphene described in accordance with the claim 1, it is characterised in that: cleaning device is using punching
It brushes, spray, impregnating and the mode of the one or more of ultrasonic cleaning cleans initial substrate and graphene film,
For removing the attachment on surface;Cleaning solution includes a combination of one or more combination of water, organic solvent and surfactant.
5. the device of roll-to-roll continuous transfer graphene described in accordance with the claim 1, it is characterised in that: drying device includes drying
Case and blower drying equipment, are dried initial substrate and graphene film.
6. the device of roll-to-roll continuous transfer graphene described in accordance with the claim 1, it is characterised in that: scrolling material collecting device packet
Material receiving roller and rotating device are included, material receiving roller is used to provide the power of rotation for winding and tightening up material web, rotating device, turn
Speed and direction are adjusted by control system.
7. the device of roll-to-roll continuous transfer graphene described in accordance with the claim 1, it is characterised in that: realized using live-roller
The transmission of material web among different components.
8. the device of roll-to-roll continuous transfer graphene described in accordance with the claim 1, it is characterised in that: as needed in rewinding
Other transfer devices are installed additional before roller, the graphene on overlay film surface are transferred in the target substrate of other flexibility or rigidities.
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