CN111217364B - Rapid transfer method based on graphene adhesive tape - Google Patents
Rapid transfer method based on graphene adhesive tape Download PDFInfo
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- CN111217364B CN111217364B CN201811427260.1A CN201811427260A CN111217364B CN 111217364 B CN111217364 B CN 111217364B CN 201811427260 A CN201811427260 A CN 201811427260A CN 111217364 B CN111217364 B CN 111217364B
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Abstract
A rapid transfer method based on a graphene adhesive tape comprises the steps of preparing an adhesive tape solution to form an adhesive tape thin film; obtaining a graphene film; attaching the working surface of the film adhesive tape to a graphene film to obtain a graphene adhesive tape; floating the graphene adhesive tape on the surface of deionized water, and cleaning for 2-3 times; cleaning the surface of a required target substrate to prepare for transferring graphene; taking out the graphene adhesive tape from the deionized water, placing the graphene adhesive tape on a target substrate, completely attaching the graphene adhesive tape and the target substrate, and contacting the graphene with the target substrate; placing the graphene adhesive tape and the target substrate under an infrared baking lamp, and heating to soften the graphene adhesive tape; and after the moisture is completely evaporated, slowly tearing off the adhesive tape, and finishing the graphene transfer from the adhesive tape to the target substrate. The method has the advantages of low dependence on professional equipment, simple transfer process, complete transfer of graphene and long-term storage of graphene.
Description
Technical Field
The invention belongs to the field of graphene transfer, and particularly relates to a graphene flexible adhesive tape and a method for quickly transferring graphene based on the adhesive tape.
Background
The traditional graphene transfer technology is a wet transfer technology, and the specific transfer process is as follows: 1. dripping a small amount of polymethyl methacrylate (PMMA) on one surface of graphene/copper foil/graphene, and rotating at a high speed to form a layer of film to form PMMA/graphene/copper foil/graphene, wherein the PMMA/graphene/copper foil/graphene is used for avoiding the graphene from being damaged in the transfer process; 2. heating PMMA/graphene/copper foil/graphene at high temperature to cure PMMA; 3. removing the graphene on the back by using an oxygen plasma cleaner to obtain PMMA (polymethyl methacrylate)/graphene/copper foil, and avoiding the influence of the graphene on the back on a transfer result; 4. floating PMMA/graphene/copper foil on the surface of etching liquid, and etching a copper substrate to obtain a PMMA/graphene film; 5. repeatedly cleaning the PMMA/graphene film by using deionized water, removing impurities, and fishing up by using a target substrate to obtain a PMMA/graphene/target substrate; 6. naturally airing in the air, heating, and further removing residual moisture in the PMMA/graphene/target substrate; 7. and removing PMMA by using an organic good solvent such as acetone or dichloromethane, cleaning by using isopropanol, and blow-drying the surface by using nitrogen to obtain the graphene/target substrate sample, thereby completing the transfer.
The traditional graphene transfer technology and the coating method graphene transfer technology have the following defects:
1. impurities are remained, and the PMMA film is difficult to be completely dissolved by an organic solvent, so that the residues are generated, the electron mobility of the graphene is influenced, and the electrical property of the graphene electronic device is reduced.
2. The transfer is unstable, and each step in the complex operation flow may cause damage and defects of graphene, which seriously affects the effectiveness of the transfer result.
3. The target substrate is limited, most of organic substrates and flexible substrates are difficult to transfer due to the limitation of a transfer process, and meanwhile, the substrates with three-dimensional structures and rough surfaces cannot be completely transferred, so that the application of graphene is greatly limited.
4. The professional dependence is strong, the whole transfer process involves various reagents and equipment, the dependence on professional technologies and professional equipment is strong, and the development of downstream graphene industries is not facilitated.
5. The method has no storage property, the transferred graphene must be carried on a target substrate and cannot exist independently, so that the whole transfer process must be completed continuously, stepwise transfer cannot be realized, and no storage property exists.
6. The time is long, the process is complex, the complete graphene transfer once needs the time of nearly one day, the time is long, the number of transfer steps is large, the efficient application of the graphene is affected, and the application development of the graphene is not facilitated.
Disclosure of Invention
The invention aims to solve the problems of poor integrity, high dependence on professional technology and equipment, complicated transfer process, no storage property and the like in the graphene transfer technology; the graphene adhesive tape-based rapid transfer method has low dependence on professional equipment and simple transfer process, can completely transfer graphene and store the graphene for a long time, and comprises the following steps:
s1, preparing a tape solution, dripping the tape solution on a clean and flat smooth surface, and naturally airing to form a tape film; the smooth surface is a material with small surface roughness, such as a glass surface, and the like, and aims to obtain an adhesive tape with small surface roughness;
s2, obtaining a graphene film floating on the surface of the etching solution by using a coating method graphene transfer technology;
s3, taking the adhesive tape film off the smooth surface, taking the surface of the film adhesive tape in contact with the smooth surface as a working surface, and attaching the working surface to the graphene film to obtain the graphene adhesive tape; the graphene film is adhered to a working surface, and the graphene is transferred to the film adhesive tape from the etching solution;
s4, floating the graphene adhesive tape on the surface of deionized water, and cleaning for 2-3 times to remove ionic impurities on the back of the graphene adhesive tape;
s5, cleaning the surface of a needed target substrate to prepare for transferring graphene;
s6, taking out the graphene adhesive tape from the deionized water, placing the graphene adhesive tape on a target substrate, completely attaching the graphene adhesive tape and the target substrate, and contacting the graphene with the target substrate;
s7, placing the graphene adhesive tape and the target substrate under an infrared baking lamp, heating to soften the graphene adhesive tape, further improving the fit degree of the adhesive tape and the target substrate, and simultaneously evaporating water at high temperature to accelerate transfer; preferably, the temperature is gradually increased to about 60 degrees and then maintained.
And S9, after the moisture is completely evaporated, slowly tearing off the adhesive tape to finish the graphene transfer from the adhesive tape to the target substrate.
Further, in step S1, the adhesive tape solution is a PMMA/anisole solution, the mass fraction concentration of which is 4% to 8%, the concentration determines the viscosity of the solution, liquids with different viscosities have different flow properties when naturally dried, and the thicker the liquid with the higher concentration is, the thicker the obtained film is.
Alternatively, in step S1, the tape solution is a PS solution (polystyrene), or a PDMS solution (polydimethylsiloxane, silica gel), or a PC solution (polycarbonate).
Further, in step S2, ferric trichloride at a concentration of 1 mol/l, ferric nitrate at a concentration of 1 mol/l, or ammonium persulfate at a concentration of 0.1 mol/l is used as the etching solution.
Further, in step S5, the graphene tape is stored on the surface of the deionized water, so as to reduce the deposition of dust and impurities in the air and contaminate the graphene surface, and to avoid the curling of the tape itself and affecting the subsequent transfer quality. Thus, the graphene tape is completed. The graphene tape may be stored for 90 days or longer without destroying and affecting the quality of the graphene.
Further, in S6, when the target substrate is completely attached to the graphene tape, a weight is pressed on the PMMA graphene tape to attach the graphene to the target substrate.
The invention has the beneficial effects that:
1. a flat film with adhesiveness to graphene is formed by preparing an adhesive tape solution, the graphene is transferred after the graphene is adhered to a flat surface, and the adhesive tape is only contacted with the graphene from one surface, so that the integrity of the graphene is kept during transfer.
2. The dependence of graphene transfer on professional technology and equipment is weakened, and graphene can be transferred from the PMMA graphene adhesive tape to a required target substrate only by using an aqueous solution and a heat source.
3. Meanwhile, the PMMA graphene adhesive tape has storage performance of months, and the application efficiency of the PMMA graphene adhesive tape can be greatly improved.
4. The adhesive tape transfer technology can meet the transfer requirements of various target substrates, transfer uneven surfaces, three-dimensional surfaces and internal fine structures, and solve the problem that the target substrates are limited.
Drawings
Fig. 1 is an optical microscope picture of single layer graphene transferred onto a silica substrate after PMMA graphene tapes of the present invention are stored for 2 weeks and 1 month; wherein FIG. 1a is the storage period of 2 weeks and FIG. 1b is the storage period of 1 month.
Fig. 2 is a scanning electron microscope picture of single layer graphene transferred onto a silica substrate, wherein 2a is the original graphene appearance on the growth substrate prior to graphene transfer; 2b is a single-layer graphene scanning electron microscope picture transferred to a silicon dioxide substrate after the PMMA graphene adhesive tape is stored for 1 month; and 2c is a single-layer graphene scanning electron microscope picture transferred to a silicon dioxide substrate after the PMMA graphene adhesive tape is stored for 1 and a half months.
Detailed Description
The fast transfer technique based on graphene tape is specifically described below with reference to examples:
a rapid transfer method based on a graphene adhesive tape comprises the following steps:
1. 4 g of PMMA powder is dissolved in 46 g of anisole solution to obtain PMMA/anisole solution with the mass fraction of 8 percent.
2. And (3) dripping 2 ml of solution on the clean glass surface, and standing for more than 6 hours at normal temperature to obtain the cured PMMA adhesive tape.
3. And obtaining the graphene film floating on the surface of the ferric trichloride solution of 1 mol/L by using a coating method graphene transfer technology.
4. And (3) removing the PMMA adhesive tape from the surface of the glass sheet, attaching the PMMA adhesive tape to the graphene film from top to bottom, and transferring the graphene from the etching solution to the PMMA adhesive tape to obtain the PMMA graphene adhesive tape.
5. And (3) washing the PMMA graphene adhesive tape for 2-3 times by using deionized water to remove residual ionic impurities.
6. The PMMA graphene adhesive tape is taken out from the water surface, attached to a silicon dioxide substrate, padded with a layer of weighing paper for preventing the graphene from being polluted by a heavy object, and pressed on the adhesive tape by an iron block with a flat bottom surface.
7. And heating the PMMA graphene adhesive tape by using an infrared baking lamp to soften PMMA and accelerate the evaporation of water, wherein the surface temperature of the silicon dioxide substrate is about 65 ℃, and the heating time is about 20 minutes.
8. After the water had evaporated completely, the PMMA tape was slowly pulled off at a rate of about 1 cm/sec.
9. To this end, the graphene is transferred intact from the tape onto the silica substrate.
Claims (5)
1. A rapid transfer method based on a graphene adhesive tape comprises the following steps:
s1, preparing a tape solution, dripping the tape solution on a clean and flat smooth surface, and naturally airing to form a tape film; the smooth surface is a material with small surface roughness, and the purpose is to obtain an adhesive tape film with small surface roughness;
s2, obtaining a graphene film floating on the surface of the etching solution by using a coating method graphene transfer technology;
s3, taking the adhesive tape film off the smooth surface, taking the surface of the adhesive tape film in contact with the smooth surface as a working surface, and attaching the working surface to the graphene film to obtain the graphene adhesive tape; the graphene film is stuck on a working surface, and the graphene is transferred to the adhesive tape film from the etching solution;
s4, floating the graphene adhesive tape on the surface of deionized water, and cleaning for 2-3 times to remove ionic impurities on the back of the graphene adhesive tape;
s5, cleaning the surface of a needed target substrate to prepare for transferring graphene;
s6, taking out the graphene adhesive tape from the deionized water, placing the graphene adhesive tape on a target substrate, enabling the graphene adhesive tape to be completely attached to the target substrate, and enabling the graphene to be in contact with the target substrate;
s7, placing the graphene adhesive tape and the target substrate under an infrared baking lamp, gradually heating to 60 ℃, then keeping the temperature, heating to soften the graphene adhesive tape, further improving the bonding degree of the graphene adhesive tape and the target substrate, and simultaneously evaporating water at high temperature to accelerate transfer;
and S8, after the moisture is completely evaporated, slowly tearing off the adhesive tape film, and finishing the graphene transfer from the adhesive tape film to the target substrate.
2. The graphene tape-based rapid transfer method according to claim 1, wherein: in the step S1, the adhesive tape solution is PMMA/anisole solution, and the mass fraction concentration of the PMMA/anisole solution is 4% -8%.
3. The graphene tape-based rapid transfer method according to claim 1, wherein: in step S2, the etching solution is ferric trichloride with a concentration of 1 mol/l, ferric nitrate with a concentration of 1 mol/l, or ammonium persulfate with a concentration of 0.1 mol/l.
4. The graphene tape-based rapid transfer method according to claim 1, wherein: in step S5, the graphene tape is stored on the surface of deionized water.
5. The graphene tape-based rapid transfer method according to claim 1, wherein: in step S6, when the graphene adhesive tape and the target substrate are completely bonded, the weight is pressed on the graphene adhesive tape to bond the graphene and the target substrate.
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| CN201811427260.1A CN111217364B (en) | 2018-11-27 | 2018-11-27 | Rapid transfer method based on graphene adhesive tape |
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| CN201811427260.1A CN111217364B (en) | 2018-11-27 | 2018-11-27 | Rapid transfer method based on graphene adhesive tape |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102351175A (en) * | 2011-11-03 | 2012-02-15 | 东南大学 | High-quality transfer method of graphene prepared by chemical vapor deposition method |
| KR20130081028A (en) * | 2012-01-06 | 2013-07-16 | 전북대학교산학협력단 | Process for graphene based transparent electrode with no resistance change by curvature |
| WO2015197217A1 (en) * | 2014-06-25 | 2015-12-30 | Instytut Technologii Materialow Elektronicznych | Method of transferring a graphene film |
| CN106145098A (en) * | 2016-06-23 | 2016-11-23 | 无锡格菲电子薄膜科技有限公司 | A kind of with glued membrane be medium transfer Graphene method |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102351175A (en) * | 2011-11-03 | 2012-02-15 | 东南大学 | High-quality transfer method of graphene prepared by chemical vapor deposition method |
| KR20130081028A (en) * | 2012-01-06 | 2013-07-16 | 전북대학교산학협력단 | Process for graphene based transparent electrode with no resistance change by curvature |
| WO2015197217A1 (en) * | 2014-06-25 | 2015-12-30 | Instytut Technologii Materialow Elektronicznych | Method of transferring a graphene film |
| CN106145098A (en) * | 2016-06-23 | 2016-11-23 | 无锡格菲电子薄膜科技有限公司 | A kind of with glued membrane be medium transfer Graphene method |
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Inventor after: Zhao Pei Inventor after: Zhang Xuewei Inventor after: Zhang Yang Inventor after: Zheng Haoran Inventor after: Zhang Xuqing Inventor after: Ren Qiancheng Inventor after: Zhou Chuiying Inventor after: Wang Hongtao Inventor before: Zhao Pei Inventor before: Zhang Xuewei Inventor before: Zheng Haoran Inventor before: Zhang Xuqing Inventor before: Ren Qiancheng Inventor before: Zhou Chuiying Inventor before: Wang Hongtao |