CN104495823A - Method and device for preparing single-layer continuous graphene film coiled material - Google Patents
Method and device for preparing single-layer continuous graphene film coiled material Download PDFInfo
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- CN104495823A CN104495823A CN201410782235.0A CN201410782235A CN104495823A CN 104495823 A CN104495823 A CN 104495823A CN 201410782235 A CN201410782235 A CN 201410782235A CN 104495823 A CN104495823 A CN 104495823A
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Abstract
The invention relates to a method and a device for preparing a single-layer continuous graphene film coiled material, and belongs to the technical field of graphene preparation. The method comprises the following steps: leading copper coil sheets on which graphene grows to be sequentially adjacent, overlapping adjacent copper coil sheets for 0.1-1cm, and adhering by means of conductive adhesive; charging negative charges on a flexible target carrier by virtue of an electrostatic generator; pressing the charged flexible target carrier with one side of the copper foil sheet; coiling the flexible target carrier to form a coil raw material which comprises a flexible target carrier layer, a graphene layer and a copper foil layer; stripping the coil raw material by utilizing an electrochemical stripping method, wherein the graphene layer and the copper foil layer in the coil raw material are separated in the stripping process to form a primary product of the coiled material, and the primary product of the coiled material comprises a flexible target carrier layer and a graphene layer; and carrying out post-treatment on the primary product of the coiled material to obtain the single-layer continuous graphene film coiled material.
Description
Technical field
The invention belongs to technical field of graphene preparation, particularly relate to a kind of preparation method of individual layer continuous graphite alkene film coil, and for the preparation of the device of individual layer continuous graphite alkene film coil; Achieve Graphene from the growth substrate of sheet to the seamless branches of the target substrate fast and low-cost of coiled material shape.
Background technology
Graphene is the hexagonal honey comb structure that carbon atom forms based on sp2 hydridization, the only two dimensional crystal of an atomic layers thick.Although single-layer graphene is just obtained by mechanically peel graphite experimentally first for 2004, the character due to its uniqueness excites the research interest of countless researcher, and obtains in a few years in the past and study widely.Graphene has excellent power, heat, the character such as optical, electrical, is almost completely transparent, only has the light absorption ratio of 2.3% in all wave band; Thermal conductivity is up to 5300W/mK, and under normal temperature, its electronic mobility is more than 15000cm
2/ Vs, and resistivity only about 10
-6Ω cm is the material that resistivity is minimum in the world at present.And Andre Geim and Konstant i n Novose l ov also obtains Nobel Prize in physics in 2010 because of its initiative work in Graphene.Graphene is not only applicable to basic physics research, have broad application prospects, as molecular detector, thermal conductance/heat interfacial material, field emission source, ultracapacitor, solar cell, the rare lithium cell of graphite and unicircuit, transparency conductive electrode etc. in fields such as display, the energy, detection, photoelectrons.The applied research of Graphene has great market outlook, will bring revolutionary transformation to numerous research field.
But the single-layer graphene of current large-area high-quality can only pass through chemical vapour deposition (CVD) method and grow in the substrate of the metal catalytic such as copper or nickel, need to transfer to further in other target substrate and could use, and by CVD equipment and process technology limit, the graphene film that existing CVD obtains is all the sheet structure that size is less, is unfavorable for operation in subsequent production process and deposits.
In addition, if use binding agent in the process of transfer Graphene, impurity will be introduced in Graphene transfer, make graphene product performance and compatible reduction, be difficult to the demand meeting the industries such as semi-conductor.
Summary of the invention
Technical problem to be solved by this invention is to provide the preparation method of individual layer continuous graphite alkene film coil, with solve utilize chemical Vapor deposition process to obtain graphene film be all the sheet structure that size is less, be unfavorable for operation in subsequent production process and deposit, and use bonding mode transfer Graphene can introduce impurity in Graphene transfer, reduce graphene product performance and compatible problem.
The technical scheme that the present invention solves the problems of the technologies described above is as follows: a kind of preparation method of individual layer continuous graphite alkene film coil, comprises the following steps:
Step 1, makes growth have the Copper Foil thin slice of Graphene adjacent successively, and adjacent Copper Foil thin slice overlap 0.1 ~ 1cm, is bondd by conductive resin;
Step 2, makes soft objectives belt carrier negative charge by electrostatic power unit; Then by the side pressing of charged soft objectives carrier and Copper Foil thin slice; Soft objectives carrier rolls rear formation coiled material raw material; Coiled material raw material comprises soft objectives carrier layer, graphene layer and copper foil layer successively;
Step 3, coiled material prepared using electrochemical stripping method is peeled off; In stripping process, the graphene layer of coiled material raw material is separated with copper foil layer and forms coiled material primary products, and described coiled material primary products comprise soft objectives carrier layer and graphene layer successively;
Step 4, coiled material primary products obtain individual layer continuous graphite alkene film coil through last handling process.
The preparation method of individual layer continuous graphite alkene film coil as above, further, the last handling process in step 4 is: coiled material primary products are put into deionized water, hydrochloric acid, doping agent, deionized water successively and soaks 5 ~ 30 minutes respectively, then dry up; Launch coiled material primary products at surface-coated one deck conductive polymer protective membrane of graphene layer, then on conductive polymer protective membrane, lay electrostatic protection film.
The preparation method of individual layer continuous graphite alkene film coil as above, further, in step 1, growth has the copper thickness of the Copper Foil thin slice of Graphene to be 25 ~ 500 μm.
The preparation method of individual layer continuous graphite alkene film coil as above, further, in step 1, growth has the copper thickness of the Copper Foil thin slice of Graphene to be 25 μm.
The preparation method of individual layer continuous graphite alkene film coil as above, further, the material of described soft objectives carrier is the one in polyethylene terephthalate, polycarbonate, silicone resin and tetrafluoroethylene.
The invention has the beneficial effects as follows: graphene layer and soft objectives carrier use non-gluing mode, can avoid introducing impurity in Graphene transfer, improve graphene product performance and compatibility, meet the demand of the industries such as semi-conductor, and reduce costs.In addition, in the present invention, growth has the Copper Foil thin slice of Graphene to be linked together by forming continuous print Graphene coiled material after the stripping of electrochemistry bubbling and coated with conductive macromolecule layer by conductive tape, is convenient to the operation in subsequent production process and deposits.
In order to realize the preparation method of above-mentioned individual layer continuous graphite alkene film coil, the present invention also provides a kind of equipment for the preparation of individual layer continuous graphite alkene film coil, and it comprises:
First electrostatic power unit, for making soft objectives belt carrier negative charge;
Press binding device, has the Copper Foil thin slice of Graphene adjacent successively for making growth; And by the side pressing of charged soft objectives carrier and Copper Foil thin slice;
Conductive resin laminating apparatus, for making adjacent Copper Foil thin slice connect to the opposite side of Copper Foil thin slice conductive glue; Soft objectives carrier rolls rear formation coiled material raw material; Coiled material raw material comprises soft objectives carrier layer, graphene layer and copper foil layer;
Coiled material raw material stripping off device, for the graphene layer of coiled material raw material and copper foil layer being peeled off, form coiled material primary products, described coiled material primary products comprise soft objectives carrier layer, photocuring glue-line and graphene layer;
After-treatment device, for cleaning coiled material primary products, doping and armor coatedly obtain individual layer continuous graphite alkene film coil.
As above for the preparation of the equipment of individual layer continuous graphite alkene film coil, further, coiled material raw material stripping off device comprises:
Electrochemistry bubbling pond, holds electrolytic solution in described electrochemistry bubbling pond;
Coiled material feedstock device, is arranged on the side in described electrochemistry bubbling pond;
Copper foil layer coiler, comprising: metal roller bearing; Stainless steel roller, described stainless steel roller is arranged on described metal roller bearing; Motor, described motor drives stainless steel roller to rotate; Metal ring clevis, copper foil layer is clamped on stainless steel roller by described metal ring clevis; Described copper foil layer coiler is electrically connected with power cathode;
The stainless steel plate be electrically connected with positive source, described stainless steel plate is arranged on the inside in described electrochemistry bubbling pond, immerses electrolytic solution;
Second electrostatic power unit, it is outside that described second electrostatic power unit is arranged on electrochemistry bubbling pond, for maintaining the negative charge that soft objectives carrier carries.
As above for the preparation of the equipment of individual layer continuous graphite alkene film coil, further, the clamping degree of described metal ring clevis is adjustable.
As above for the preparation of the equipment of individual layer continuous graphite alkene film coil, further, the electrostatic that described first electrostatic power unit and/or the second electrostatic power unit produce is that band shape is uniformly distributed, and with electrostatic protection shielding unit, prevents from affecting other electronicss.
The invention has the beneficial effects as follows:
Do not use viscose glue, do not introduce impurity, improve the quality of Graphene; The coiled material raw material stripping off device of optimization design ensure that the high quality of Graphene; Bubble is produced between Copper Foil and Graphene, stainless steel roller idle running when the bonding force between Copper Foil and Graphene is greater than the pulling force that stainless steel pair of rollers Copper Foil applies when peeling off; Rotate together with stainless steel roller drive Copper Foil when the bonding force between Copper Foil with Graphene is less than the pulling force of stainless steel pair of rollers Copper Foil applying, said apparatus better can keep the integrity degree of coiled material primary products, prevents from rupturing in stripping process.
Accompanying drawing explanation
The press binding device schematic diagram that Fig. 1 provides for an embodiment of the present invention;
Coiled material raw material stripping off device, after-treatment device schematic diagram that Fig. 2 provides for an embodiment of the present invention.
In accompanying drawing, the list of parts representated by each label is as follows:
11, conveying belt, 12, pressing cylinder, the 13, first electrostatic power unit; 14, rolling cylinder, 21, electrochemistry bubbling pond, 22, coiled material feedstock device; 24, copper foil layer coiler, 25, stainless steel plate, 26, stationary fixture; 27, the second electrostatic power unit, 31, the cleaning of coiled material primary products, doper, 32, protective layer coating unit; 82, coiled material raw material; 91, copper foil layer, 92, graphene layer, 93, soft objectives carrier.
Embodiment
Be described principle of the present invention and feature below in conjunction with accompanying drawing, example, only for explaining the present invention, is not intended to limit scope of the present invention.
The technical scheme that the present invention solves the problems of the technologies described above is as follows: a kind of preparation method of individual layer continuous graphite alkene film coil, comprises the following steps:
Step 1, makes growth have the Copper Foil thin slice of Graphene adjacent successively, and adjacent Copper Foil thin slice overlap 0.1 ~ 1cm, is bondd by conductive resin; Utilizing conductive resin to be when carrying out subsequent electrochemical and peeling off by growing the object having the Copper Foil thin slice of Graphene to connect, making Copper Foil thin slice form continuous print conductor, being convenient to carrying out continuously of electrochemical stripping.Concrete, such as neighbours growth has the overlapping dimension of the Copper Foil thin slice adjacent edge of Graphene to be set as distance 0.5cm, utilizes conductive resin to be linked together by Copper Foil thin slice.
Step 2, makes soft objectives belt carrier negative charge by electrostatic power unit; Then by the side pressing of charged soft objectives carrier and Copper Foil thin slice; Soft objectives carrier rolls rear formation coiled material raw material; Coiled material raw material comprises soft objectives carrier layer, graphene layer and copper foil layer successively;
Step 3, coiled material prepared using electrochemical stripping method is peeled off; In stripping process, the graphene layer of coiled material raw material is separated with copper foil layer and forms coiled material primary products, and described coiled material primary products comprise soft objectives carrier layer and graphene layer successively;
Step 4, coiled material primary products obtain individual layer continuous graphite alkene film coil through last handling process.
In aforesaid method, graphene layer and soft objectives carrier use non-gluing mode to adsorb, and can avoid introducing impurity in Graphene transfer, improve graphene product performance and compatibility, meet the demand of the industries such as semi-conductor, and reduce costs.In the present invention, growth has the Copper Foil thin slice of Graphene to be linked together by forming continuous print Graphene coiled material after the stripping of electrochemistry bubbling and coated with conductive macromolecule layer by conductive tape, is convenient to the operation in subsequent production process and deposits.
In one of the present invention more specifically embodiment, the last handling process in step 4 is: coiled material primary products are put into deionized water, hydrochloric acid, doping agent, deionized water successively and soaks 5 ~ 30 minutes respectively, then dry up; Launch coiled material primary products at surface-coated one deck conductive polymer protective membrane of graphene layer, then on conductive polymer protective membrane, lay electrostatic protection film.In a kind of specific embodiment, coiled material primary products are put into deionized water 5 minutes, hydrochloric acid 8 minutes, doping agent 20 minutes, deionized water 5 minutes, complete the cleaning of coiled material primary products.The mass concentration of hydrochloric acid used is 10% ~ 20%.Described doping agent is selected from gold trichloride, HNO
3, HCL.
In one of the present invention more specifically embodiment, in step 1, growth has the copper thickness of the Copper Foil thin slice of Graphene to be 25 ~ 500 μm.Be more preferably 25 μm.
In one of the present invention more specifically embodiment, described soft objectives carrier is polyethylene terephthalate carrier.
In order to realize the preparation method of above-mentioned individual layer continuous graphite alkene film coil, the embodiment of the present invention also provides a kind of equipment for the preparation of individual layer continuous graphite alkene film coil, and it comprises:
First electrostatic power unit 13, for making soft objectives belt carrier negative charge;
Press binding device, has the Copper Foil thin slice of Graphene adjacent successively for making growth; And by the side pressing of charged soft objectives carrier and Copper Foil thin slice;
As shown in Figure 1, press binding device device comprises conveying belt 11, for mobile continuous print Copper Foil thin slice.The copper foil layer 91 of continuous print Copper Foil thin slice contacts with conveying belt.Pressing cylinder 12, applies the one side pressing that soft objectives carrier 93 and continuous Copper Foil thin slice are had graphene layer 92 by pressure.Rolling cylinder 14, for rolling rear formation coiled material raw material by soft objectives carrier.
Conductive resin laminating apparatus, for making adjacent Copper Foil thin slice connect to the opposite side of Copper Foil thin slice conductive glue; Soft objectives carrier rolls rear formation coiled material raw material; Coiled material raw material comprises soft objectives carrier layer, graphene layer and copper foil layer; In specific implementation process, conductive resin laminating apparatus comprises Copper Foil thin slice feeding unit, e Foerderanlage, discharging device, feeding unit is continuously to e Foerderanlage supply Copper Foil thin slice, and conductive resin is bonded in the opposite side (one side be not namely connected with soft objectives carrier) of adjacent Copper Foil thin slice by discharging device.
Coiled material raw material stripping off device, for the graphene layer of coiled material raw material and copper foil layer being peeled off, form coiled material primary products, described coiled material primary products comprise soft objectives carrier layer, photocuring glue-line and graphene layer;
After-treatment device, be connected with coiled material raw material stripping off device, coiled material primary products directly input after-treatment device, and after-treatment device is used for coiled material primary products to clean, doping and armor coatedly obtain individual layer continuous graphite alkene film coil.As shown in Figure 2, after-treatment device comprises the cleaning of coiled material primary products, doper 31 and protective layer coating unit 32.
As shown in Figure 2, be a kind of coiled material raw material stripping off device of embodiment, it comprises:
Electrochemistry bubbling pond 21, holds electrolytic solution in described electrochemistry bubbling pond; In specific implementation process, electrolytic solution is selected from sodium hydroxide, sodium sulfate, potassium hydroxide etc.
Coiled material feedstock device 22, is arranged on the side in described electrochemistry bubbling pond; Coiled material raw material 82 is placed in coiled material feedstock device.
Copper foil layer coiler 24, comprising: metal roller bearing; Stainless steel roller, described stainless steel roller is arranged on described metal roller bearing; Motor, described motor drives stainless steel roller to rotate; Metal ring clevis, copper foil layer is clamped on stainless steel roller by described metal ring clevis; Described copper foil layer coiler is electrically connected with power cathode;
Stationary fixture 26, realizes the location of coiled material raw material in electrochemistry bubbling pond 21.Concrete, be two adjacent cylinders, the suitable distance in interval between cylinder, enables coiled material raw material pass through.That has passed stationary fixture realizes coiled material under electrochemical action, realizes graphene layer and is separated with copper foil layer, realizes further peeling off under the traction of copper foil layer coiler.
The stainless steel plate 25 be electrically connected with positive source, described stainless steel plate is arranged on the inside in described electrochemistry bubbling pond, immerses electrolytic solution.
Second electrostatic power unit 27, it is outside that described second electrostatic power unit is arranged on electrochemistry bubbling pond, for maintaining the negative charge that soft objectives carrier carries, the negative charge amount that soft objectives carrier carries determines the adsorptive power between Graphene and soft objectives carrier, demand when meeting stripping to make adsorptive power, prevent Graphene from sticking on Copper Foil, need to make adsorptive power be greater than certain threshold value, namely require that the negative charge that soft objectives carrier carries is greater than certain threshold value.
As above for the preparation of the equipment of individual layer continuous graphite alkene film coil, further, the clamping degree of described metal ring clevis is adjustable.In a kind of specific embodiment, described metal ring clevis is elastic rubber ring, by the different clamping degrees selecting the elastic rubber ring of different diameter can realize Copper Foil.
Bubble is produced between Copper Foil and Graphene, stainless steel roller idle running when the bonding force between Copper Foil and Graphene is greater than the pulling force that stainless steel pair of rollers Copper Foil applies when peeling off; Rotate together with stainless steel roller drive Copper Foil when the bonding force between Copper Foil with Graphene is less than the pulling force of stainless steel pair of rollers Copper Foil applying, said apparatus better can keep the integrity degree of coiled material primary products, prevents from rupturing in stripping process.
As above for the preparation of the equipment of individual layer continuous graphite alkene film coil; further; the electrostatic that described first electrostatic power unit and/or the second electrostatic power unit produce is that band shape is uniformly distributed, and electrostatic power unit, with electrostatic protection shielding unit, prevents from affecting other electronicss.
The foregoing is only preferred embodiment of the present invention, not in order to limit the present invention, within the spirit and principles in the present invention all, any amendment done, equivalent replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (9)
1. a preparation method for individual layer continuous graphite alkene film coil, is characterized in that, comprise the following steps:
Step 1, makes growth have the Copper Foil thin slice of Graphene adjacent successively, and adjacent Copper Foil thin slice overlap 0.1 ~ 1cm, is bondd by conductive resin;
Step 2, makes soft objectives belt carrier negative charge by electrostatic power unit; Then by the side pressing of charged soft objectives carrier and Copper Foil thin slice; Soft objectives carrier rolls rear formation coiled material raw material; Coiled material raw material comprises soft objectives carrier layer, graphene layer and copper foil layer;
Step 3, coiled material prepared using electrochemical stripping method is peeled off; In stripping process, the graphene layer of coiled material raw material is separated with copper foil layer and forms coiled material primary products, and described coiled material primary products comprise soft objectives carrier layer and graphene layer;
Step 4, coiled material primary products obtain individual layer continuous graphite alkene film coil through last handling process.
2. the preparation method of individual layer continuous graphite alkene film coil according to claim 1, it is characterized in that, last handling process in step 4 is: coiled material primary products are put into deionized water, hydrochloric acid, doping agent, deionized water successively and soaks 5 ~ 30 minutes respectively, then dry up; Launch coiled material primary products at surface-coated one deck conductive polymer protective membrane of graphene layer, then on conductive polymer protective membrane, lay electrostatic protection film.
3. the preparation method of individual layer continuous graphite alkene film coil according to claim 1, is characterized in that, in step 1, growth has the copper thickness of the Copper Foil thin slice of Graphene to be 25 ~ 500 μm.
4. the preparation method of individual layer continuous graphite alkene film coil according to claim 3, is characterized in that, in step 1, growth has the copper thickness of the Copper Foil thin slice of Graphene to be 25 μm.
5. the preparation method of individual layer continuous graphite alkene film coil according to claim 1, is characterized in that, the material of described soft objectives carrier is the one in polyethylene terephthalate, polycarbonate, silicone resin and tetrafluoroethylene.
6., for the preparation of an equipment for individual layer continuous graphite alkene film coil, it is characterized in that, comprising:
First electrostatic power unit, for making soft objectives belt carrier negative charge;
Press binding device, has the Copper Foil thin slice of Graphene adjacent successively for making growth; And by the side pressing of charged soft objectives carrier and Copper Foil thin slice;
Conductive resin laminating apparatus, for making adjacent Copper Foil thin slice connect to the opposite side of Copper Foil thin slice conductive glue; Soft objectives carrier rolls rear formation coiled material raw material; Coiled material raw material comprises soft objectives carrier layer, graphene layer and copper foil layer;
Coiled material raw material stripping off device, for the graphene layer of coiled material raw material and copper foil layer being peeled off, form coiled material primary products, described coiled material primary products comprise soft objectives carrier layer, photocuring glue-line and graphene layer;
After-treatment device, for cleaning coiled material primary products, doping and armor coatedly obtain individual layer continuous graphite alkene film coil.
7. the equipment for the preparation of individual layer continuous graphite alkene film coil according to claim 6, is characterized in that, coiled material raw material stripping off device comprises:
Electrochemistry bubbling pond, holds electrolytic solution in described electrochemistry bubbling pond;
Coiled material feedstock device, is arranged on the side in described electrochemistry bubbling pond;
Copper foil layer coiler, comprising: metal roller bearing; Stainless steel roller, described stainless steel roller is arranged on described metal roller bearing; Motor, described motor drives stainless steel roller to rotate; Metal ring clevis, copper foil layer is clamped on stainless steel roller by described metal ring clevis; Described copper foil layer coiler is electrically connected with power cathode;
The stainless steel plate be electrically connected with positive source, described stainless steel plate is arranged on the inside in described electrochemistry bubbling pond, immerses electrolytic solution;
Second electrostatic power unit, it is outside that described second electrostatic power unit is arranged on electrochemistry bubbling pond, for maintaining the negative charge that soft objectives carrier carries.
8. the equipment for the preparation of individual layer continuous graphite alkene film coil according to claim 7, is characterized in that, the clamping degree of described metal ring clevis is adjustable.
9. the equipment for the preparation of individual layer continuous graphite alkene film coil according to claim 7; it is characterized in that; the electrostatic that described first electrostatic power unit and/or the second electrostatic power unit produce is that band shape is uniformly distributed, and with electrostatic protection shielding unit, prevents from affecting other electronicss.
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| CN103288077A (en) * | 2013-06-28 | 2013-09-11 | 重庆墨希科技有限公司 | Method for rapidly and nondestructively transferring graphene |
| WO2014089437A1 (en) * | 2012-12-07 | 2014-06-12 | Graphene Frontiers, Llc | Method and apparatus for transfer of films among substrates |
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Patent Citations (4)
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| WO2013068521A1 (en) * | 2011-11-10 | 2013-05-16 | Deutsches Zentrum für Luft- und Raumfahrt e.V. | Device and method for mechanically thinning out blossom |
| WO2014089437A1 (en) * | 2012-12-07 | 2014-06-12 | Graphene Frontiers, Llc | Method and apparatus for transfer of films among substrates |
| CN102976318A (en) * | 2012-12-21 | 2013-03-20 | 重庆绿色智能技术研究院 | Reel-to-reel graphene preparation apparatus |
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