CN103332682A - Method for superposed transfer of large-area graphene through using screen film and film covering machine - Google Patents

Method for superposed transfer of large-area graphene through using screen film and film covering machine Download PDF

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Publication number
CN103332682A
CN103332682A CN2013102899879A CN201310289987A CN103332682A CN 103332682 A CN103332682 A CN 103332682A CN 2013102899879 A CN2013102899879 A CN 2013102899879A CN 201310289987 A CN201310289987 A CN 201310289987A CN 103332682 A CN103332682 A CN 103332682A
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graphene
membrane screen
copper foil
laminating machine
target substrate
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CN2013102899879A
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CN103332682B (en
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吕鹏
张梓晗
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HEFEI VIGON MATERIAL TECHNOLOGIES Co Ltd
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HEFEI VIGON MATERIAL TECHNOLOGIES Co Ltd
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Abstract

The invention discloses a method for the superposed transfer of large-area graphene through using a screen film and a film covering machine. The method is characterized in that the method comprises the following steps: adhering the screen film to graphene on the upper surface of copper foil through using the film covering machine, etching away the copper foil to form a graphene/screen film composite layer, and allowing graphene to be separated from the screen film and to be released on a target substrate by utilizing the film covering machine. The method realizes the large area transfer of graphene through the screen film and the film covering machine, realizes the superposed transfer of a plurality of layers of graphene on the target substrate through repeating the above operation, and has the advantages of simplicity, easy operation, and low price of a used apparatus.

Description

A kind of method that shifts the big area Graphene with membrane screen and laminating machine stack
Technical field
The present invention relates to the transfer method of Graphene, especially relating to adds up shifts the method for big area Graphene.
Background technology
2004, Graphene was announced to the world splendidly, and caused a sensation the world.Nowadays the research temperature to Graphene does not still subtract.Prepare high-quality Graphene and be development and the progress of Graphene on synthetic, Graphene is really had breakthrough in Application Areas, so Graphene synthetic after how from the Copper Foil substrate the transfer that Graphene is harmless to get off also be an important link, because have only Graphene is transferred on the target substrate that is complementary with device, Graphene just can be advantageously applied to device, the final performance of device depends on the quality of the Graphene that obtains thus, therefore, the development and application of Graphene and prospect are inseparable with its transfer techniques.But the transfer techniques of Graphene is perfect not enough at present, and this has just limited application and the development of Graphene to a certain extent.The transfer method that with the Copper Foil is the Graphene of substrate mainly comprises: 1. " wet etching " transfer method: this method is difficult to shift than the big area Graphene, and comes off easily when shifting multilayer adding up; 2. " roll-to-roll " transfer method: it is remaining more serious that this method heat discharges the glue of adhesive tape, can destroy the performance of Graphene, higher to operator's technical requirements in addition, misoperation can make the Graphene part not discharge, the Graphene that causes shifting breaks, and influences the integrity of Graphene; When the multilayer that adds up shifts, because the phenomenon of remaining glue makes that how remaining the more glue of the number of plies that shifts is more many, the cleanliness factor of Graphene is had a significant impact; 3. " electrochemistry transfer " method, claim bubbling to send out again: this method can not shift the big area Graphene, and it will be as an end of electrode, and the integrity of transfer is bad; In addition, present method transfer Graphene that can not add up can only shift once; 4. " dry method transfer " method: this method is difficult to realize that larger area shifts, and dry method to shift maximum drawback be exactly that integrity is very poor, be difficult to obtain the more complete Graphene of big area; In addition, present method can not realize the transfer Graphene that adds up, and can only shift once).
Summary of the invention
The present invention is for avoiding above-mentioned existing in prior technology weak point, a kind of method with membrane screen and laminating machine stack transfer big area Graphene is provided, shifting Graphene in the hope of the repeatedly stack that can can't harm.
The present invention adopts following technical scheme for the technical solution problem:
The present invention superposes with membrane screen and laminating machine and shifts the method for big area Graphene, and its characteristics are to carry out as follows:
A, have the Copper Foil of Graphene to cut out to area upper surface growth to be not more than 100cm * 100cm, the membrane screen that area is not less than described Copper Foil covers the upper surface of described Copper Foil; Roller bearing with laminating machine pressurizes at described membrane screen, and membrane screen is sticked on the Graphene of Copper Foil upper surface, forms the composite structure of Copper Foil/Graphene/membrane screen;
B, the composite structure of described Copper Foil/Graphene/membrane screen is put into Copper Foil etching liquid etching up with described membrane screen, remove the Copper Foil substrate, form the composite bed of the Graphene/membrane screen that swims in Copper Foil etching liquid surface; Then the composite bed of described Graphene/membrane screen is transferred to clean also in the deionized water and at room temperature dried naturally, flash-off time is no less than 10 minutes.
C, with the composite bed of Graphene/membrane screen with Graphene towards being placed down on the target substrate, laminating machine is heated to 120 ℃-160 ℃, with the roller bearing of laminating machine with the composite bed of Graphene/membrane screen with target substrate roll extrusion be in the same place, Graphene separates with membrane screen and transfers on the target substrate, and it is 20-100 second that the roller bearing speed of adjustment laminating machine makes the time of roll extrusion process;
D, the target substrate of a layer graphene is arranged as the target substrate that shifts for the second time with transfer, repeating step a, b and c, at the layer graphene covering second layer Graphene of target substrate, and the like, until shifting the n layer graphene in target substrate, n is not more than 15.
The present invention superposes with membrane screen and laminating machine and shifts the method for big area Graphene, and its characteristics also are:
Described laminating machine is the laminating machine of silica gel roller bearing or the plastic packaging machine of silica gel roller bearing.
Described Copper Foil etching liquid is that mass concentration is the aqueous solution of the ammonium persulphate of 1%-20%.
Described target substrate is the silica-based end, silicon base, PET substrate or substrate of glass.
Compared with the prior art, beneficial effect of the present invention is embodied in:
1, the present invention has realized that by membrane screen and laminating machine the big area of Graphene shifts, and can shift multi-layer graphene in the target substrate stack by repetitive operation, the simple easy handling of method, and employed instrument is cheap;
2, the Graphene surface integrity of the inventive method transfer is good.
Description of drawings
Fig. 1 is the embodiment of the invention 1 shifts 1 layer graphene in the PET substrate photo;
Fig. 2 is the embodiment of the invention 2 shifts 12 layer graphenes at the silica-based end photo.
Embodiment
Embodiment 1
Present embodiment has shifted 1 layer of big area Graphene with membrane screen and laminating machine in PET substrate stack, and concrete steps are:
A, with upper surface growth have the Copper Foil of Graphene cut out to area be 7cm * 10cm, be the upper surface that the membrane screen of 8cm * 12cm covers Copper Foil with area; Roller bearing with laminating machine pressurizes at membrane screen, and membrane screen is sticked on the Graphene of Copper Foil upper surface, forms the composite structure of Copper Foil/Graphene/membrane screen; Copper Foil can be cut into any size as required.
B, the composite structure of described Copper Foil/Graphene/membrane screen is put into the aqueous solution etching that mass concentration is 10% ammonium persulphate down with the lower surface of Copper Foil, remove the Copper Foil substrate, form the composite bed of the Graphene/membrane screen that swims in Copper Foil etching liquid surface; It is clean and at room temperature dried in the air 20 minutes then the composite bed of Graphene/membrane screen to be transferred in the deionized water rinsing.
C, laminating machine is heated to 130 ℃, be rolled into together with composite bed and the PET substrate with Graphene/membrane screen of the roller bearing of laminating machine, the PET substrate contacts with Graphene, it is 60 seconds that the roller bearing speed of adjustment laminating machine makes the time of roll extrusion process, and Graphene separates with membrane screen and transfers in the PET substrate; Be illustrated in figure 1 as present embodiment has shifted a layer graphene in the PET substrate photo.
When needs when multi-layer graphene is shifted in PET substrate stack, the PET substrate of one layer graphene is arranged as the target substrate that shifts for the second time with transfer, repeating step a, b and c, layer graphene in the PET substrate covers second layer Graphene, and the like, until the Graphene that shifts the required number of plies in the PET substrate.The number of plies of Graphene can be selected arbitrarily as required on the target substrate, but can not surpass 15 layers, because when surpassing 15 layers, the performance of Graphene is subjected to very big influence.
Adopt present method Graphene can be transferred in the substrate of the silica-based end, silicon base, PET substrate, substrate of glass or other any one surfacings.
Embodiment 2
Present embodiment superposes at the silica-based end with membrane screen and laminating machine and has shifted 12 layers of big area Graphene, and concrete steps are:
A, with upper surface growth have the Copper Foil of Graphene cut out to area be 7cm * 12cm, be the upper surface that the membrane screen of 8cm * 14cm covers Copper Foil with area; Roller bearing with laminating machine pressurizes at membrane screen, and membrane screen is sticked on the Graphene of Copper Foil upper surface, forms the composite structure of Copper Foil/Graphene/membrane screen; Copper Foil can be cut into any size as required.
B, the composite structure of described Copper Foil/Graphene/membrane screen is put into the aqueous solution etching that mass concentration is 5% ammonium persulphate down with the lower surface of Copper Foil, remove the Copper Foil substrate, form the composite bed of the Graphene/membrane screen that swims in Copper Foil etching liquid surface; It is clean and at room temperature dried in the air 20 minutes to transfer in the deionized water water rinsing then.
C, laminating machine is heated to 140 ℃, be rolled into together with the roller bearing of laminating machine composite bed and the silica-based end with Graphene/membrane screen, the silica-based end, contact with Graphene, it is 80 seconds that the roller bearing speed of adjustment laminating machine makes the time of roll extrusion process, and Graphene separates with membrane screen and transfers at silica-based the end;
D, arranged as the silica-based end of shifting for the second time the silica-based end of a layer graphene with transfer, repeating step a, b and c, layer graphene at the silica-based end covers second layer Graphene, and the like, until shifting 12 layer graphenes at the silica-based end.Be illustrated in figure 2 as present embodiment shifts 12 layer graphenes at the silica-based end photo.

Claims (4)

1. one kind is shifted the method for big area Graphene with the stack of membrane screen and laminating machine, it is characterized in that carrying out as follows:
A, have the Copper Foil of Graphene to cut out to area upper surface growth to be not more than 100cm * 100cm, the membrane screen that area is not less than described Copper Foil covers the upper surface of described Copper Foil; Roller bearing with laminating machine pressurizes at described membrane screen, and membrane screen is sticked on the Graphene of Copper Foil upper surface, forms the composite structure of Copper Foil/Graphene/membrane screen;
B, the composite structure of described Copper Foil/Graphene/membrane screen is put into Copper Foil etching liquid etching up with described membrane screen, remove the Copper Foil substrate, form the composite bed of the Graphene/membrane screen that swims in Copper Foil etching liquid surface; Then the composite bed of described Graphene/membrane screen is transferred to clean also in the deionized water and at room temperature dried naturally, flash-off time is no less than 10 minutes;
C, with the composite bed of Graphene/membrane screen with Graphene towards being placed down on the target substrate, laminating machine is heated to 120 ℃-160 ℃, with the roller bearing of laminating machine with the composite bed of Graphene/membrane screen with target substrate roll extrusion be in the same place, Graphene separates with membrane screen and transfers on the target substrate, and it is 20-100 second that the roller bearing speed of adjustment laminating machine makes the time of roll extrusion process;
D, the target substrate of a layer graphene is arranged as the target substrate that shifts for the second time with transfer, repeating step a, b and c, at the layer graphene covering second layer Graphene of target substrate, and the like, until shifting the n layer graphene in target substrate, n is not more than 15.
2. according to claim 1 the stack with membrane screen and laminating machine shifted the method for big area Graphene, and it is characterized in that: described laminating machine is the laminating machine of silica gel roller bearing or the plastic packaging machine of silica gel roller bearing.
3. according to claim 1 the stack with membrane screen and laminating machine shifted the method for big area Graphene, and it is characterized in that: described Copper Foil etching liquid is that mass concentration is the aqueous solution of the ammonium persulphate of 1%-20%.
4. according to claim 1 the stack with membrane screen and laminating machine shifted the method for big area Graphene, and it is characterized in that: described target substrate is the silica-based end, silicon base, PET substrate or substrate of glass.
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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105621401A (en) * 2015-12-28 2016-06-01 中国科学院重庆绿色智能技术研究院 Multi-layer stacking and transferring method for graphene
CN105989911A (en) * 2015-02-10 2016-10-05 北京大学 Graphene and metal nanowire composite transparent and conductive plastic film, manufacturing method and application thereof
CN106587040A (en) * 2016-12-29 2017-04-26 浙江合特光电有限公司 Substrate transferring method of graphene film

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102774118A (en) * 2012-07-31 2012-11-14 无锡格菲电子薄膜科技有限公司 Method for transferring graphene film with static protective film as medium
CN102938373A (en) * 2012-10-22 2013-02-20 西安电子科技大学 Laminated transfer technology for graphene transparent conducting thin film and manufactured device thereby

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102774118A (en) * 2012-07-31 2012-11-14 无锡格菲电子薄膜科技有限公司 Method for transferring graphene film with static protective film as medium
CN102938373A (en) * 2012-10-22 2013-02-20 西安电子科技大学 Laminated transfer technology for graphene transparent conducting thin film and manufactured device thereby

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105989911A (en) * 2015-02-10 2016-10-05 北京大学 Graphene and metal nanowire composite transparent and conductive plastic film, manufacturing method and application thereof
CN105989911B (en) * 2015-02-10 2017-07-21 北京大学 A kind of graphene and metal nanometer line composite transparent conductive plastic film and preparation method and application
CN105621401A (en) * 2015-12-28 2016-06-01 中国科学院重庆绿色智能技术研究院 Multi-layer stacking and transferring method for graphene
CN105621401B (en) * 2015-12-28 2018-05-04 中国科学院重庆绿色智能技术研究院 A kind of graphene multiple-level stack transfer method
CN106587040A (en) * 2016-12-29 2017-04-26 浙江合特光电有限公司 Substrate transferring method of graphene film
CN106587040B (en) * 2016-12-29 2019-02-15 浙江合特光电有限公司 The substrate transfer method of graphene film

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