CN104495822B - The preparation method of a kind of graphene film coiled material and device - Google Patents
The preparation method of a kind of graphene film coiled material and device Download PDFInfo
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Abstract
The present invention relates to the preparation method of a kind of graphene film coiled material and device, belong to technical field of graphene preparation. The preparation method of graphene film coiled material includes: make Copper Foil thin slice overlap 0.1～1cm that growth has the Copper Foil thin slice of Graphene adjacent successively, adjacent; Conducting resinl is bonded in the overlapping of adjacent Copper Foil thin slice, Copper Foil thin slice is coupled together; The first soft objectives belt carrier negative charge is made by electrostatic generator; Side pressing by the first charged soft objectives carrier Yu Copper Foil thin slice; The second soft objectives belt carrier negative charge is made by electrostatic generator; Then by the opposite side pressing of the second charged soft objectives carrier Yu Copper Foil thin slice; Coiled material raw material utilizes electrochemical stripping method to peel off; In stripping process, the graphene layer of coiled material raw material separates formation coiled material primary product with copper foil layer, and described coiled material primary product include soft objectives carrier layer and graphene layer; Coiled material primary product obtain monolayer continuous graphite alkene film coil through last handling process.
Description
Technical field
The invention belongs to technical field of graphene preparation, the preparation method particularly relating to a kind of graphene film coiled material, and for preparing the device of monolayer 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 two dimensional crystal of only one atomic layers thick. Although single-layer graphene is just to be obtained by mechanical stripping graphite experimentally first for 2004, but owing to the character of its uniqueness excites the research interest of countless researcher, and obtains in a few years in past and study widely. Graphene has the power of excellence, heat, the character such as optical, electrical, is almost fully transparent, only has the absorptance of 2.3% at all band; Heat-conducting system is up to 5300W/m K, and under room temperature, its electron mobility is more than 15000cm2/ V s, and resistivity about 10-6Ω cm, for the material that resistivity is minimum in the world at present. And AndreGeim and KonstantinNovoselov also obtains 2010 years Nobel Prizes in physics because of its initiative work in Graphene. Graphene is not only suitable for basic physics research, have broad application prospects in fields such as display, the energy, detection, photoelectrons, such as molecular detector, thermal conductance/thermal interfacial material, field emission source, ultracapacitor, solaode, the rare lithium battery of graphite and integrated circuit, transparency conductive electrode etc. The applied research of Graphene has great market prospect, will bring revolutionary transformation to numerous research fields.
But the single-layer graphene of large-area high-quality grows in the metal catalytic substrate such as copper or nickel only by chemical vapour deposition (CVD) (CVD) method at present, need to be further diverted in other target substrate could use, and limited by CVD equipment and technique, the graphene film that existing CVD obtains is all smaller laminated structure, is unfavorable for the operation in subsequent production process and deposits.
Additionally, in existing method, in Graphene transfer process, a transforming growth has the Graphene of the Copper Foil thin slice side of Graphene, and growth has the Copper Foil thin slice utilization rate of Graphene to only have half, and production efficiency is low, and cost is high. If using binding agent in the process of transfer Graphene, impurity will be introduced in Graphene shifts, making graphene product performance and compatibility reduce, it is difficult to meet the demand of the industries such as quasiconductor.
Summary of the invention
The preparation method that the technical problem to be solved is to provide graphene film coiled material, is all smaller laminated structure to solve to utilize the graphene film that chemical vapour deposition technique obtains, is unfavorable for the operation in subsequent production process and deposits; In Graphene transfer process, a transforming growth has the Graphene of the Copper Foil thin slice side of Graphene, growth has the Copper Foil thin slice utilization rate of Graphene to only have half, production efficiency low cost is high, and use bonding mode transfer Graphene can introduce impurity in Graphene shifts, reduce graphene product performance and compatible problem.
The preparation method that the technical scheme is that a kind of graphene film coiled material, comprises the following steps:
Step 1, makes Copper Foil thin slice overlap 0.1～1cm that growth has the Copper Foil thin slice of Graphene adjacent successively, adjacent; The first soft objectives belt carrier negative charge is made by electrostatic generator; Then by the side pressing of the first charged soft objectives carrier Yu Copper Foil thin slice;
Step 2, is bonded in conducting resinl the overlapping of adjacent Copper Foil thin slice, is coupled together by Copper Foil thin slice; The second soft objectives belt carrier negative charge is made by electrostatic generator; Then by the another side surface pressing of the second charged soft objectives carrier Yu Copper Foil thin slice;
Soft objectives carrier forms coiled material raw material after rolling; Coiled material raw material includes the first soft objectives carrier layer, the first graphene layer, copper foil layer, the second graphene layer and the second soft objectives carrier layer;
Step 3, coiled material raw material utilizes electrochemical stripping method to peel off; In stripping process, the graphene layer of coiled material raw material separates formation coiled material primary product with copper foil layer, and described coiled material primary product include soft objectives carrier layer and graphene layer;
Step 4, coiled material primary product obtain monolayer continuous graphite alkene film coil through last handling process.
The preparation method of graphene film coiled material as above, it is preferable that the last handling process in step 4 is: coiled material primary product are sequentially placed in deionized water, hydrochloric acid, adulterant, deionized water and soak respectively 5～30 minutes, then dry up; Launch the coiled material primary product surface-coated one floor height molecule conductive protective film at graphene layer, on conductive polymer protecting film, then lay electrostatic protection film.
The preparation method of graphene film coiled material as above, it is preferable that step 3, first separates the first soft objectives carrier layer of coiled material raw material, the first graphene layer with copper foil layer, the second graphene layer, the second soft objectives carrier layer; Then the second soft objectives carrier layer, the second graphene layer are separated with copper foil layer.
The preparation method of graphene film coiled material as above, it is preferable that growth has the copper thickness of the Copper Foil thin slice of Graphene to be 5～500 μm.
The preparation method of graphene film coiled material as above, it is preferable that growth has the copper thickness of the Copper Foil thin slice of Graphene to be 25 μm.
The preparation method of graphene film coiled material as above, it is preferable that the material of described soft objectives carrier is the one in polyethylene terephthalate, Merlon, silicones and politef.
The invention has the beneficial effects as follows: graphene layer uses non-gluing mode with soft objectives carrier, it is possible to avoid introducing impurity in Graphene shifts, improve graphene product performance and compatibility, meet the demand of the industries such as quasiconductor, and reduce cost.Additionally, growth has the Copper Foil thin slice of Graphene to be linked together by conductive tape to peel off and be coated with formation continuous print Graphene coiled material after electroconductive polymer layer by electrochemistry bubbling in the present invention, it is simple to operation in subsequent production process and depositing. And the Graphene on Copper Foil two sides can be transferred, greatly improve the production efficiency of product.
For the preparation method realizing above-mentioned graphene film coiled material, the present invention also provides for a kind of equipment for preparing monolayer continuous graphite alkene film coil, comprising:
First electrostatic generator, is used for making soft objectives belt carrier negative charge;
Press fit device, for making growth have the Copper Foil thin slice of Graphene adjacent successively; And by the side pressing of charged soft objectives carrier Yu Copper Foil thin slice;
Conducting resinl laminating apparatus, for making adjacent Copper Foil thin slice connect without the side of Graphene conductive glue to Copper Foil thin slice; Soft objectives carrier forms coiled material raw material after rolling;
Coiled material raw material stripping off device, for being peeled off with copper foil layer by the graphene layer of coiled material raw material, forms coiled material primary product, and described coiled material primary product include soft objectives carrier layer, photocuring glue-line and graphene layer;
After-treatment device, for cleaning coiled material primary product, doping and armor coated obtain monolayer continuous graphite alkene film coil.
Coiled material raw material stripping off device includes:
Electrochemistry bubbling pond, holds electrolyte in described electrochemistry bubbling pond;
Coiled material feedstock device, is arranged on the side in described electrochemistry bubbling pond;
Copper foil layer coiler, including: metal roller bearing; Rustless steel roller, described rustless steel roller is arranged on described metal roller bearing; Motor, described motor drives rustless steel roller to rotate; Becket clevis, copper foil layer is clamped on rustless steel roller by described becket clevis; Described copper foil layer coiler electrically connects with power cathode;
The corrosion resistant plate electrically connected with positive source, corrosion resistant plate is using Graphene as anticorrosive coat; Described corrosion resistant plate is arranged on the inside in described electrochemistry bubbling pond, immerses electrolyte;
Second electrostatic generator, described second electrostatic generator is arranged on outside electrochemistry bubbling pond, for maintaining the negative charge that soft objectives carrier carries.
It is highly preferred that the electrostatic that electrostatic generator produces is that banding is uniformly distributed, and with electrostatic protection screening arrangement, it is prevented that affect other electronic equipments.
Equipment for preparing monolayer continuous graphite alkene film coil as above, further, the clamping degree of described becket clevis is adjustable.
Equipment for preparing monolayer continuous graphite alkene film coil as above, further, it is spiral closed reel that described coiled material primary product coiler includes cross section.
The invention has the beneficial effects as follows:
Rustless steel roller is using Graphene as anticorrosive coat, it is prevented that the corrosion of the electrolyte such as NaOH, increases the service life of equipment;
The coiled material raw material stripping off device optimizing design ensure that the high-quality of Graphene; Bubble, rustless steel roller idle running during the pulling force that the adhesion between Copper Foil and Graphene applies more than rustless steel pair of rollers Copper Foil is produced between Copper Foil and Graphene when peeling off; Rotating together with rustless steel roller drive Copper Foil when the pulling force that the adhesion between Copper Foil with Graphene applies less than rustless steel pair of rollers Copper Foil, said apparatus can better keep the integrity degree of coiled material primary product, it is prevented that ruptures in stripping process.
Accompanying drawing explanation
The press fit device schematic diagram that Fig. 1 provides for an embodiment of the present invention;
Coiled material raw material stripping off device that Fig. 2 provides for an embodiment of the present invention, after-treatment device schematic diagram.
In accompanying drawing, the list of parts representated by each label is as follows:
11, conveyer belt, 12, pressing cylinder, the 13, first electrostatic generator; 14, rolling cylinder, 21, electrochemistry bubbling pond, 22, coiled material feedstock device; 24, copper foil layer coiler, 25, corrosion resistant plate, 26, stationary fixture; 27, the second electrostatic generator, 31, coiled material primary product clean, doper, 32, protective layer coating unit; 82, coiled material raw material; 91, copper foil layer, 92, graphene layer, 93, soft objectives carrier.
Detailed description of the invention
Below in conjunction with accompanying drawing, principles of the invention and feature being described, example is served only for explaining the present invention, is not intended to limit the scope of the present invention.
The preparation method that the technical scheme is that a kind of graphene film coiled material, comprises the following steps:
Step 1, makes Copper Foil thin slice overlap 0.1～1cm that growth has the Copper Foil thin slice of Graphene adjacent successively, adjacent; Conducting resinl is bonded in the overlapping of adjacent Copper Foil thin slice, Copper Foil thin slice is coupled together; Utilize conducting resinl that growth has the purpose that the Copper Foil thin slice of Graphene connects be when carrying out subsequent electrochemical and peeling off, make Copper Foil thin slice form continuous print conductor, it is simple to continuously performing of electrochemical stripping.
Step 2, makes the first soft objectives belt carrier negative charge by electrostatic generator; Then by the side pressing of the first charged soft objectives carrier Yu Copper Foil thin slice; The second soft objectives belt carrier negative charge is made by electrostatic generator; Then by the opposite side pressing of the second charged soft objectives carrier Yu Copper Foil thin slice;
Soft objectives carrier forms coiled material raw material after rolling; Coiled material raw material includes the first soft objectives carrier layer, the first graphene layer, copper foil layer, the second graphene layer and the second soft objectives carrier layer successively;
Step 3, coiled material raw material utilizes electrochemical stripping method to peel off; In stripping process, the graphene layer of coiled material raw material separates formation coiled material primary product with copper foil layer, and described coiled material primary product include soft objectives carrier layer and graphene layer successively;
Step 4, coiled material primary product obtain monolayer continuous graphite alkene film coil through last handling process.
In said method, growth have the Graphene of the Copper Foil thin slice both sides of Graphene respectively with soft objectives carrier binder, peel off at twice during stripping, take full advantage of on Copper Foil the Graphene of growth, efficiency is doubled, reduce cost. Graphene layer and soft objectives carrier use non-gluing mode to adsorb, it is possible to avoid introducing impurity in Graphene shifts, improve graphene product performance and compatibility, meet the demand of the industries such as quasiconductor, and reduce cost. In the present invention, growth has the Copper Foil thin slice of Graphene to be linked together by conductive tape to peel off and be coated with formation continuous print Graphene coiled material after electroconductive polymer layer by electrochemistry bubbling, it is simple to operation in subsequent production process and depositing.
In one of the present invention embodiment more specifically, the last handling process in step 4 is: is sequentially placed in deionized water, hydrochloric acid, adulterant, deionized water by coiled material primary product and soaks respectively 5～30 minutes, then dries up; Launch the coiled material primary product surface-coated one floor height molecule conductive protective film at graphene layer, on conductive polymer protecting film, then lay electrostatic protection film.In a kind of specific embodiment, coiled material primary product are put into deionized water 5 minutes, hydrochloric acid 8 minutes, adulterant 20 minutes, deionized water 5 minutes, completes the cleaning of coiled material primary product. The mass concentration of hydrochloric acid used is 10%～20%. Described adulterant is selected from auric chloride, HNO3,HCL。
In one of the present invention embodiment more specifically, step 3, first the first soft objectives carrier layer of coiled material raw material, the first graphene layer are separated with copper foil layer, the second graphene layer, the second soft objectives carrier layer; Then the second soft objectives carrier layer, the second graphene layer are separated with copper foil layer. In stripping process, the graphene layer of coiled material raw material separates formation coiled material primary product with copper foil layer, and described coiled material primary product include soft objectives carrier layer and graphene layer. Namely a kind of coiled material primary product are the first soft objectives carrier layer, the first graphene layer. Another kind of coiled material primary product are two soft objectives carrier layer, the second graphene layer.
In one of the present invention embodiment more specifically, in step 1, growth has the copper thickness of the Copper Foil thin slice of Graphene to be 5～500 μm. It is more preferably 25 μm.
In one of the present invention embodiment more specifically, the material of described soft objectives carrier is the one in polyethylene terephthalate, Merlon, silicones and politef.
For the preparation method realizing above-mentioned graphene film coiled material, the embodiment of the present invention also provides for a kind of equipment for preparing monolayer continuous graphite alkene film coil, comprising:
Conducting resinl laminating apparatus, makes Copper Foil thin slice overlap 0.1～1cm that growth has the Copper Foil thin slice of Graphene adjacent successively, adjacent; Conducting resinl is bonded in the overlapping of adjacent Copper Foil thin slice, Copper Foil thin slice is coupled together; In specific implementation process, conducting resinl laminating apparatus includes Copper Foil thin slice feed arrangement, conveyer device, discharging device, feed arrangement supplies Copper Foil thin slice to conveyer device continuously, regulating feed speed makes the spacing between Copper Foil thin slice maintain setpoint distance (such as 0.5cm), and conducting resinl is bonded in the overlapping of adjacent Copper Foil thin slice by discharging device.
First electrostatic generator 13, for making the first soft objectives carrier, the second soft objectives belt carrier negative charge respectively;
Press fit device, for first by the side pressing of the first charged soft objectives carrier Yu Copper Foil thin slice; Then by the opposite side pressing of the second charged soft objectives carrier Yu Copper Foil thin slice;
As it is shown in figure 1, press fit device device includes conveyer belt 11, it is used for moving continuous print Copper Foil thin slice. The copper foil layer 91 of continuous print Copper Foil thin slice contacts with conveyer belt. Pressing cylinder 12, applies pressure and soft objectives carrier 93 and continuous Copper Foil thin slice has the one side pressing of graphene layer 92. Rolling cylinder 14, for forming coiled material raw material after being rolled by soft objectives carrier.
Coiled material raw material stripping off device, for being peeled off with copper foil layer by the graphene layer of coiled material raw material, forms coiled material primary product, and described coiled material primary product include soft objectives carrier layer, photocuring glue-line and graphene layer;
After-treatment device, is connected with coiled material raw material stripping off device, and coiled material primary product directly input after-treatment device, after-treatment device for coiled material primary product are cleaned, doping and armor coated obtain monolayer continuous graphite alkene film coil. As in figure 2 it is shown, after-treatment device includes the cleaning of coiled material primary product, doper 31 and protective layer coating unit 32.
As in figure 2 it is shown, be the coiled material raw material stripping off device of a kind of embodiment, comprising:
Electrochemistry bubbling pond 21, holds electrolyte in described electrochemistry bubbling pond; In specific implementation process, electrolyte 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, including: metal roller bearing; Rustless steel roller, described rustless steel roller is arranged on described metal roller bearing; Motor, described motor drives rustless steel roller to rotate; Becket clevis, copper foil layer is clamped on rustless steel roller by described becket clevis; Described copper foil layer coiler electrically connects with power cathode;
Stationary fixture 26, it is achieved coiled material raw material location in electrochemistry bubbling pond 21. Concrete, it is two adjacent cylinders, the suitable distance in interval between cylinder, enable coiled material raw material to pass through. What have already passed through stationary fixture realizes coiled material under electrochemical action, it is achieved graphene layer separates with copper foil layer, realizes further peeling off under the traction of copper foil layer coiler.
The corrosion resistant plate 25 electrically connected with positive source, corrosion resistant plate is using Graphene as anticorrosive coat; Described corrosion resistant plate is arranged on the inside in described electrochemistry bubbling pond, immerses electrolyte.
Second electrostatic generator 27, described second electrostatic generator is arranged on outside electrochemistry bubbling pond, for maintaining the negative charge that soft objectives carrier carries, the negative charge amount that soft objectives carrier carries determines the absorption affinity between Graphene and soft objectives carrier, in order to make demand when absorption affinity meets stripping, prevent Graphene from sticking on Copper Foil, it is necessary to make absorption affinity more than certain threshold value, namely require that the negative charge that soft objectives carrier carries is more than certain threshold value.
Equipment for preparing monolayer continuous graphite alkene film coil as above, further, the clamping degree of described becket clevis is adjustable. In a kind of specific embodiment, described becket clevis is elastic rubber ring, by selecting the elastic rubber ring of different-diameter deliberately to realize the different clamping degrees of Copper Foil.
Bubble, rustless steel roller idle running during the pulling force that the adhesion between Copper Foil and Graphene applies more than rustless steel pair of rollers Copper Foil is produced between Copper Foil and Graphene when peeling off; Rotating together with rustless steel roller drive Copper Foil when the pulling force that the adhesion between Copper Foil with Graphene applies less than rustless steel pair of rollers Copper Foil, said apparatus can better keep the integrity degree of coiled material primary product, it is prevented that ruptures in stripping process.
The foregoing is only presently preferred embodiments of the present invention, not in order to limit the present invention, all within the spirit and principles in the present invention, any amendment of making, equivalent replacement, improvement etc., should be included within protection scope of the present invention.
Claims (7)
1. the preparation method of a graphene film coiled material, it is characterised in that comprise the following steps:
Step 1, makes Copper Foil thin slice overlap 0.1～1cm that growth has the Copper Foil thin slice of Graphene adjacent successively, adjacent; Conducting resinl is bonded in the overlapping of adjacent Copper Foil thin slice, Copper Foil thin slice is coupled together;
Step 2, makes the first soft objectives belt carrier negative charge by electrostatic generator; Then by the side pressing of the first charged soft objectives carrier Yu Copper Foil thin slice; The second soft objectives belt carrier negative charge is made by electrostatic generator; Then by the opposite side pressing of the second charged soft objectives carrier Yu Copper Foil thin slice;
Soft objectives carrier forms coiled material raw material after rolling;Coiled material raw material includes the first soft objectives carrier layer, the first graphene layer, copper foil layer, the second graphene layer and the second soft objectives carrier layer;
Step 3, coiled material raw material utilizes electrochemical stripping method to peel off; Specifically: first the first soft objectives carrier layer of coiled material raw material, the first graphene layer are separated with copper foil layer, the second graphene layer, the second soft objectives carrier layer; Then the second soft objectives carrier layer, the second graphene layer are separated with copper foil layer;
Step 4, coiled material primary product obtain monolayer continuous graphite alkene film coil through last handling process.
2. the preparation method of graphene film coiled material according to claim 1, it is characterized in that, last handling process in step 4 is: is sequentially placed in deionized water, hydrochloric acid, adulterant, deionized water by coiled material primary product and soaks respectively 5～30 minutes, then dries up; Launch the coiled material primary product surface-coated one floor height molecule conductive protective film at graphene layer, on conductive polymer protecting film, then lay electrostatic protection film.
3. the preparation method of graphene film coiled material according to claim 1, it is characterised in that in step 1, growth has the copper thickness of the Copper Foil thin slice of Graphene to be 5～500 μm.
4. the preparation method of graphene film coiled material according to claim 3, it is characterised 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 graphene film coiled material according to claim 1, it is characterised in that the material of described soft objectives carrier is the one in polyethylene terephthalate, Merlon, silicones and politef.
6. the equipment being used for preparing monolayer continuous graphite alkene film coil, it is characterised in that including:
Conducting resinl laminating apparatus, for making adjacent Copper Foil thin slice connect the side of conductive glue to Copper Foil thin slice;
First electrostatic generator, for making the first soft objectives carrier, the second soft objectives belt carrier negative charge respectively;
Press fit device, for first by the side pressing of the first charged soft objectives carrier Yu Copper Foil thin slice; Then by the opposite side pressing of the second charged soft objectives carrier Yu Copper Foil thin slice;
Coiled material raw material stripping off device, for being peeled off with copper foil layer by the graphene layer of coiled material raw material, forms coiled material primary product, and described coiled material primary product include soft objectives carrier layer and graphene layer;
After-treatment device, for cleaning coiled material primary product, doping and armor coated obtain monolayer continuous graphite alkene film coil;
Described coiled material raw material stripping off device includes:
Electrochemistry bubbling pond, holds electrolyte in described electrochemistry bubbling pond;
Coiled material feedstock device, is arranged on the side in described electrochemistry bubbling pond;
Copper foil layer coiler, including: metal roller bearing; Rustless steel roller, described rustless steel roller is arranged on described metal roller bearing; Motor, described motor drives rustless steel roller to rotate; Becket clevis, copper foil layer is clamped on rustless steel roller by described becket clevis; Described copper foil layer coiler electrically connects with power cathode;
The corrosion resistant plate electrically connected with positive source, corrosion resistant plate is using Graphene as anticorrosive coat; Described corrosion resistant plate is arranged on the inside in described electrochemistry bubbling pond, immerses electrolyte;
Second electrostatic generator, described second electrostatic generator is arranged on outside electrochemistry bubbling pond, for maintaining the negative charge that soft objectives carrier carries.
7. the equipment for preparing monolayer continuous graphite alkene film coil according to claim 6, it is characterised in that the clamping degree of described becket clevis is adjustable.
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| CN106626556A (en) * | 2016-12-28 | 2017-05-10 | 镇江博昊科技有限公司 | Copper-based graphene composite film coil |
| CN110329818B (en) * | 2019-07-10 | 2020-07-28 | 郝影 | Graphene thin material coiling device |
| CN113148712A (en) * | 2020-12-31 | 2021-07-23 | 浙江大学台州研究院 | Film roll-to-roll production method |
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| KR101234180B1 (en) * | 2009-12-30 | 2013-02-18 | 그래핀스퀘어 주식회사 | Roll-to-roll doping method of graphene film and doped graphene film |
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