CN104528694B - A kind of Graphene doping transfer method - Google Patents
A kind of Graphene doping transfer method Download PDFInfo
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- CN104528694B CN104528694B CN201410764269.7A CN201410764269A CN104528694B CN 104528694 B CN104528694 B CN 104528694B CN 201410764269 A CN201410764269 A CN 201410764269A CN 104528694 B CN104528694 B CN 104528694B
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Abstract
The present invention relates to Graphene production technical field, particularly relate to a kind of Graphene doping transfer method, comprise the following steps: step one, at growth graphenic surface coating macromolecule doping transfer medium；Step 2, is attached on target substrate surface by the Graphene pressing being coated with doping transfer medium obtained, and forms the composite construction being made up of successively target substrate, doping transfer medium, Graphene and growth substrate；Step 3, carries out pressure process process to described composite construction；Step 4, is heated the composite construction after carrying out pressure process process processing；Step 5, is easily separated process to the composite construction after heat treated, separates the growth substrate in composite construction.The invention has the beneficial effects as follows: select the macromolecular material with doping effect simultaneously as Graphene material for transfer and dopant material, high molecular stability feature is utilized to improve stably-doped property, save follow-up Graphene doping step, simplify Graphene production technology.
Description
Technical field
The present invention relates to Graphene production technical field, particularly relate to a kind of Graphene doping transfer method.
Background technology
Graphene is the two-dimension nano materials having now been found that in recent years, has numerous excellent properties.Wherein, high transmitance and the carrier mobility of superelevation so that it is industrial quarters can be enjoyed to pay close attention to as brand-new transparent conductive material.
Method prepared by the Graphene scale of existing maturation is chemical vapour deposition technique (CVD).CVD is prepared Graphene and is generally selected opaque metal as growth substrate, for instance Copper Foil, nickel foil etc..Will using as transparent conductive material, Graphene must be transferred into transparent substrates, and adulterates to reduce sheet resistance to it.Existing doping method is with little molecule for adulterant mostly, for instance ethylenediamine, nitric acid, gold chloride etc. so that it is physical absorption reaches doping purpose at graphenic surface.Small molecule dopant is weak with Graphene active force, volatile, causes that Graphene sheet resistance is continuously increased, seriously limit the practical application of Graphene in placement process.
Summary of the invention
The technical problem to be solved is to provide a kind of Graphene doping transfer method, simplifies production technology while improving Graphene electric performance stablity.
The technical scheme is that a kind of Graphene doping transfer method, it is characterised in that comprise the following steps:
Step one, at growth graphenic surface coating doping transfer medium；
Step 2, is attached on target substrate surface by the Graphene pressing being coated with doping transfer medium obtained, and forms the composite construction being made up of successively target substrate, doping transfer medium, Graphene and growth substrate；
Step 3, carries out pressure process process to described composite construction；
Step 4, is heated the composite construction after carrying out pressure process process processing；
Step 5, is easily separated process to the composite construction after heat treated, separates the growth substrate in composite construction.
On the basis of technique scheme, the present invention can also do following improvement.
nullFurther，Described step a kind of macromolecule doping transfer medium be the polymer containing cyano functional group side base and/or nitro functions side base and/or sulfonate functional groups side base and/or fluorine pendant groups and copolymer thereof，Such as: polyacrylonitrile (PAN) is dissolved in the mixture of dimethylformamide、Ethanol dissolves the mixture of NC Nitroncellulose、Cyanacrylate and methylmethacrylate copolymer are dissolved in the mixture of ethyl acetate、Poly-thereof (PSS) aqueous solution、Poly-perfluor-1，3-dioxol、CTFE one vinylidene fluoride copolymer、Poly-perfluoro capryl ethoxyethyl acrylate solution、The butyl acetate solution of perfluor nonyl ethoxyethyl acrylate-methacrylate copolymer、Perfluor-1，3-dioxol-vinylidene fluoride copolymer、Doping transfer medium perfluor-1，3-dioxol-trifluoro-ethylene copolymer solution、Perfluoro capryl ethoxyethyl acrylate-acrylic acid norborneol ester copolymer solution etc..
Further, the pressure that in described step 3, pressure process processes is 0.5MPa to 15MPa, and vacuum pressure is 0.1Pa to 200Pa.
Further, the pressure limit that in described step 3, pressure process processes is 2MPa to 8MPa, and vacuum pressure range is 0.1Pa to 10Pa.
Further, the time that in described step 3, pressure process processes is 0.5hr to 5hr.
Further, in described step 3, the pressure process process time is 2hr to 3hr.
Further, in described step 4, the temperature of heat treated is 50-200 DEG C, and heating treatment time is 5-400min.
Further, in described step 4, heat treatment temperature is 80-130 DEG C, and heating treatment time is 30-60min.
The invention has the beneficial effects as follows: select the macromolecular material with doping effect simultaneously as Graphene material for transfer and dopant material, high molecular stability feature is utilized to improve stably-doped property, save follow-up Graphene doping step, simplify Graphene production technology.
Accompanying drawing explanation
Fig. 1 is the flow chart of steps of the present invention；
Fig. 2 is the structural representation of heretofore described composite construction.
In accompanying drawing, the list of parts representated by each label is as follows:
1, target substrate, 2, doping transfer medium, 3, Graphene, 4, growth substrate 4.
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.
Embodiment one
The present embodiment comprises the following steps:
Step one, is dissolved in dimethylformamide by polyacrylonitrile (PAN), coats growth Graphene 3 surface by roll coating process；
Step 2, is coated with Graphene and the PET base pressing of polyacrylonitrile, forms the composite construction of PET/PAN/ Graphene/growth substrate；
Step 3, carries out pressure process process to described composite construction, and pressure is 0.5MPa, and vacuum pressure is 0.1Pa, and the time that pressure process processes is 5hr；
Step 4, is heated the composite construction after carrying out pressure process process processing, and the temperature of heat treated is 50 DEG C, and heating treatment time is 400min；
Step 5, is easily separated process to the composite construction after heat treated, separates the growth substrate 4 in composite construction.
Embodiment two
The present embodiment comprises the following steps:
Step one, ethanol dissolves NC Nitroncellulose, is coated on growth Graphene 3 surface；
Step 2, is attached on target substrate PET1 surface by Graphene 3 pressing being coated with NC Nitroncellulose 2 obtained, and forms the composite construction of PET/ NC Nitroncellulose/Graphene/growth substrate；
Step 3, carries out pressure process process to described composite construction, and pressure is 15MPa, and vacuum pressure is 200Pa, and the time that pressure process processes is 0.5hr；
Step 4, is heated the composite construction after carrying out pressure process process processing, and the temperature of heat treated is 50 DEG C, and heating treatment time is 400min；
Step 5, is easily separated process to the composite construction after heat treated, separates the growth substrate 4 in composite construction.
Embodiment three
The present embodiment comprises the following steps:
Step one, is dissolved in ethyl acetate by cyanacrylate and methylmethacrylate copolymer, is coated on growth Graphene 3 surface；
Step 2, Graphene 3 pressing being coated with cyanacrylate and methylmethacrylate copolymer 2 obtained is attached on target substrate PET1 surface, forms the composite construction of the composite construction of PET/ cyanacrylate copolymer/Graphene/growth substrate；
Step 3, carries out pressure process process to described composite construction, and pressure is 0.5MPa, and vacuum pressure is 200Pa, and the time that pressure process processes is 3hr；
Step 4, is heated the composite construction after carrying out pressure process process processing, and the temperature of heat treated is 50 DEG C, and heating treatment time is 400min；
Step 5, is easily separated process to the composite construction after heat treated, separates the growth substrate 4 in composite construction.
Embodiment four
The present embodiment comprises the following steps:
Step one, at poly-thereof (PSS) aqueous solution of growth Graphene 3 surface coating；
Step 2, is attached on target substrate PET1 surface by Graphene 3 pressing being coated with doping transfer medium PSS obtained, forms the composite construction of PET/PSS/ Graphene/growth substrate；
Step 3, carries out pressure process process to described composite construction, and pressure is 15MPa, and vacuum pressure is 0.1Pa, and the time that pressure process processes is 0.5hr；
Step 4, is heated the composite construction after carrying out pressure process process processing, and the temperature of heat treated is 50 DEG C, and heating treatment time is 400min；
Step 5, is easily separated process to the composite construction after heat treated, separates the growth substrate 4 in composite construction.
Embodiment five
The present embodiment comprises the following steps:
Step one, in poly-perfluor-1 of growth Graphene 3 surface coating, 3-dioxol is as doping transfer medium 2；
Step 2, poly-perfluor-1 that is coated with that will obtain, Graphene 3 pressing of 3-dioxol is attached on target substrate PET1 surface, forms poly-perfluor-1 of PET/, the composite construction of the composite construction of 3-dioxol/Graphene/growth substrate；
Step 3, carries out pressure process process to described composite construction, and pressure is 15MPa, and vacuum pressure is 0.1Pa, and the time that pressure process processes is 2hr；
Step 4, is heated the composite construction after carrying out pressure process process processing, and the temperature of heat treated is 50 DEG C, and heating treatment time is 400min；
Step 5, is easily separated process to the composite construction after heat treated, separates the growth substrate 4 in composite construction.
Embodiment six
The present embodiment comprises the following steps:
Step one, at growth Graphene 3 surface coating CTFE one vinylidene fluoride copolymer doping transfer medium 2；
Step 2, is attached on target substrate 1 surface by Graphene 3 pressing being coated with CTFE one vinylidene fluoride copolymer doping transfer medium 2 obtained, forms the composite construction of PET/ CTFE one vinylidene fluoride copolymer/Graphene/growth substrate
Step 3, carries out pressure process process to described composite construction, and pressure is 0.5MPa, and vacuum pressure is 0.1Pa, and the time that pressure process processes is 5hr；
Step 4, is heated the composite construction after carrying out pressure process process processing, and the temperature of heat treated is 200 DEG C, and heating treatment time is 5min；
Step 5, is easily separated process to the composite construction after heat treated, separates the growth substrate 4 in composite construction.
Embodiment seven
The present embodiment comprises the following steps:
Step one, at the poly-perfluoro capryl ethoxyethyl acrylate solution of growth Graphene 3 surface coating；
Step 2, Graphene 3 pressing that the surface obtained is coated with poly-perfluoro capryl ethoxyethyl acrylate solution is attached on target substrate 1 surface, forms the composite construction of the poly-perfluoro capryl ethoxyethyl acrylate/Graphene/growth substrate of PET/；
Step 3, carries out pressure process process to described composite construction, and pressure is 0.5MPa, and vacuum pressure is 0.1Pa, and the time that pressure process processes is 5hr；
Step 4, is heated the composite construction after carrying out pressure process process processing, and the temperature of heat treated is 200 DEG C, and heating treatment time is 5min；
Step 5, is easily separated process to the composite construction after heat treated, separates the growth substrate 4 in composite construction.
Embodiment eight
The present embodiment comprises the following steps:
Step one, at the butyl acetate solution of growth Graphene 3 surface coating perfluor nonyl ethoxyethyl acrylate-methacrylate copolymer；
Step 2, Graphene 3 pressing being coated with doping transfer medium perfluor nonyl ethoxyethyl acrylate-methacrylate copolymer 2 obtained is attached on target substrate PET1 surface, forms the composite construction of PET/ perfluor nonyl ethoxyethyl acrylate-methacrylate copolymer/Graphene/growth substrate
Step 3, carries out pressure process process to described composite construction, and pressure is 15MPa, and vacuum pressure is 200Pa, and the time that pressure process processes is 0.5hr；
Step 4, is heated the composite construction after carrying out pressure process process processing, and the temperature of heat treated is 200 DEG C, and heating treatment time is 5min；
Step 5, is easily separated process to the composite construction after heat treated, separates the growth substrate 4 in composite construction.
Embodiment nine
The present embodiment comprises the following steps:
Step one, at coating doping transfer medium perfluor-1, growth Graphene 3 surface, 3-dioxol-vinylidene fluoride copolymer；
Step 2, is attached on target substrate 1 surface by Graphene 3 pressing being coated with doping transfer medium 2 obtained, forms PET/ perfluor-1, the composite construction of 3-dioxol-vinylidene fluoride copolymer/Graphene/growth substrate；
Step 3, carries out pressure process process to described composite construction, and pressure is 0.5MPa, and vacuum pressure is 200Pa, and the time that pressure process processes is 3hr；
Step 4, is heated the composite construction after carrying out pressure process process processing, and the temperature of heat treated is 200 DEG C, and heating treatment time is 5min；
Step 5, is easily separated process to the composite construction after heat treated, separates the growth substrate 4 in composite construction.
Embodiment ten
The present embodiment comprises the following steps:
Step one, at coating doping transfer medium perfluor-1, growth Graphene 3 surface, 3-dioxol-trifluoro-ethylene copolymer solution；
Step 2, is attached on target substrate 1 surface by Graphene 3 pressing being coated with doping transfer medium 2 obtained, forms PET/ perfluor-1, the composite construction of 3-dioxol-trifluoro-ethylene copolymer/Graphene/growth substrate；
Step 3, carries out pressure process process to described composite construction, and pressure is 15MPa, and vacuum pressure is 0.1Pa, and the time that pressure process processes is 0.5hr；
Step 4, is heated the composite construction after carrying out pressure process process processing, and the temperature of heat treated is 200 DEG C, and heating treatment time is 5min；
Step 5, is easily separated process to the composite construction after heat treated, separates the growth substrate 4 in composite construction.
Embodiment 11
The present embodiment comprises the following steps:
Step one, at growth Graphene 3 surface coating doping transfer medium perfluoro capryl ethoxyethyl acrylate-acrylic acid norborneol ester copolymer solution；
Step 2, is attached on target substrate 1 surface by Graphene 3 pressing being coated with doping transfer medium 2 obtained, forms the composite construction of PET/ perfluoro capryl ethoxyethyl acrylate-acrylic acid norborneol ester copolymer/Graphene/growth substrate；The composite construction being made up of successively target substrate 1, doping transfer medium 2, Graphene 3 and growth substrate 4；
Step 3, carries out pressure process process to described composite construction, and pressure is 15MPa, and vacuum pressure is 0.1Pa, and the time that pressure process processes is 2hr；
Step 4, is heated the composite construction after carrying out pressure process process processing, and the temperature of heat treated is 200 DEG C, and heating treatment time is 5min；
Step 5, is easily separated process to the composite construction after heat treated, separates the growth substrate 4 in composite construction.
The present invention selects the macromolecular material with doping effect simultaneously as Graphene 3 material for transfer and dopant material, utilizes high molecular stability feature to improve stably-doped property, saves follow-up Graphene 3 and adulterate step, simplify Graphene 3 production technology.
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 (4)
1. a Graphene doping transfer method, it is characterised in that comprise the following steps:
Step one, in growth graphenic surface coating macromolecule doping transfer medium (2), described macromolecule doping transfer medium (2) is the polymer containing cyano functional group side base and/or nitro functions side base and/or sulfonate functional groups side base and/or fluorine pendant groups；
Step 2, the Graphene pressing being coated with doping transfer medium obtained is attached on target substrate surface, forms the composite construction being made up of successively target substrate (1), doping transfer medium (2), Graphene (3) and growth substrate (4)；
Step 3, carries out pressure process process to described composite construction, and the pressure that pressure process processes is 0.5MPa to 15MPa, and the process time that pressure process processes is 0.5hr to 5hr, and vacuum pressure is 0.1Pa to 200Pa；
Step 4, is heated the composite construction after carrying out pressure process process processing, and the temperature of described heat treated is 50-200 DEG C, and heating treatment time is 5-400min；
Step 5, is easily separated process to the composite construction after heat treated, separates the growth substrate (4) in composite construction.
2. a kind of Graphene doping transfer method according to claim 1, it is characterised in that the pressure limit that in described step 3, pressure process processes is 2MPa to 8MPa, and vacuum pressure range is 0.1Pa to 10Pa.
3. a kind of Graphene doping transfer method according to claim 1, it is characterised in that the process time that in described step 3, pressure process processes is 2hr to 3hr.
4. a kind of Graphene doping transfer method according to any one of claims 1 to 3, it is characterised in that in described step 4, the temperature of heat treated is 80-130 DEG C, and heating treatment time is 30-60min.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102826538A (en) * | 2012-09-17 | 2012-12-19 | 辽宁科技大学 | Method for preparing nitrogen-doped carbonaceous material by modifying polymer |
| 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 |
| CN103332680A (en) * | 2013-06-28 | 2013-10-02 | 重庆墨希科技有限公司 | Transferable graphene film and transfer method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102826538A (en) * | 2012-09-17 | 2012-12-19 | 辽宁科技大学 | Method for preparing nitrogen-doped carbonaceous material by modifying polymer |
| 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 |
| CN103332680A (en) * | 2013-06-28 | 2013-10-02 | 重庆墨希科技有限公司 | Transferable graphene film and transfer method thereof |
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