CN106672955A - Method for transferring graphene film with non-planar special-shaped structure - Google Patents
Method for transferring graphene film with non-planar special-shaped structure Download PDFInfo
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- CN106672955A CN106672955A CN201611096740.5A CN201611096740A CN106672955A CN 106672955 A CN106672955 A CN 106672955A CN 201611096740 A CN201611096740 A CN 201611096740A CN 106672955 A CN106672955 A CN 106672955A
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 159
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 158
- 238000000034 method Methods 0.000 title claims abstract description 30
- 239000003292 glue Substances 0.000 claims abstract description 83
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 79
- 239000000741 silica gel Substances 0.000 claims abstract description 79
- 229910002027 silica gel Inorganic materials 0.000 claims abstract description 79
- 229910052751 metal Inorganic materials 0.000 claims abstract description 20
- 239000002184 metal Substances 0.000 claims abstract description 20
- 239000011248 coating agent Substances 0.000 claims abstract description 17
- 238000000576 coating method Methods 0.000 claims abstract description 17
- 238000001035 drying Methods 0.000 claims abstract description 5
- 239000010408 film Substances 0.000 claims description 135
- 239000011159 matrix material Substances 0.000 claims description 84
- 238000005530 etching Methods 0.000 claims description 30
- 229910052739 hydrogen Inorganic materials 0.000 claims description 30
- 239000001257 hydrogen Substances 0.000 claims description 30
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 30
- 125000000304 alkynyl group Chemical group 0.000 claims description 22
- 229920002554 vinyl polymer Polymers 0.000 claims description 21
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 20
- 239000007788 liquid Substances 0.000 claims description 19
- 238000012546 transfer Methods 0.000 claims description 18
- 239000010409 thin film Substances 0.000 claims description 17
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 16
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 15
- -1 graphite alkene Chemical class 0.000 claims description 15
- 239000007789 gas Substances 0.000 claims description 14
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 14
- 238000007711 solidification Methods 0.000 claims description 13
- 230000008023 solidification Effects 0.000 claims description 13
- 229910052802 copper Inorganic materials 0.000 claims description 10
- 239000010949 copper Substances 0.000 claims description 10
- 125000004122 cyclic group Chemical group 0.000 claims description 10
- 230000005855 radiation Effects 0.000 claims description 10
- 238000006243 chemical reaction Methods 0.000 claims description 8
- 238000000926 separation method Methods 0.000 claims description 8
- 238000005229 chemical vapour deposition Methods 0.000 claims description 7
- 150000001875 compounds Chemical class 0.000 claims description 7
- 229910052759 nickel Inorganic materials 0.000 claims description 7
- 229910052697 platinum Inorganic materials 0.000 claims description 7
- 238000013459 approach Methods 0.000 claims description 5
- QXLPXWSKPNOQLE-UHFFFAOYSA-N methylpentynol Chemical compound CCC(C)(O)C#C QXLPXWSKPNOQLE-UHFFFAOYSA-N 0.000 claims description 5
- 229960002238 methylpentynol Drugs 0.000 claims description 5
- KSLSOBUAIFEGLT-UHFFFAOYSA-N 2-phenylbut-3-yn-2-ol Chemical compound C#CC(O)(C)C1=CC=CC=C1 KSLSOBUAIFEGLT-UHFFFAOYSA-N 0.000 claims description 4
- 229910002804 graphite Inorganic materials 0.000 claims description 4
- 239000010439 graphite Substances 0.000 claims description 4
- 239000000463 material Substances 0.000 claims description 3
- 238000006555 catalytic reaction Methods 0.000 claims description 2
- XYFCBTPGUUZFHI-UHFFFAOYSA-N Phosphine Chemical compound P XYFCBTPGUUZFHI-UHFFFAOYSA-N 0.000 claims 2
- 239000003795 chemical substances by application Substances 0.000 claims 2
- 239000005977 Ethylene Substances 0.000 claims 1
- 229910000073 phosphorus hydride Inorganic materials 0.000 claims 1
- 230000001629 suppression Effects 0.000 claims 1
- 238000000151 deposition Methods 0.000 abstract description 3
- 239000000758 substrate Substances 0.000 abstract 3
- 230000007547 defect Effects 0.000 abstract 1
- 229920002545 silicone oil Polymers 0.000 description 29
- 150000002431 hydrogen Chemical class 0.000 description 15
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 14
- 229910052799 carbon Inorganic materials 0.000 description 13
- 238000010030 laminating Methods 0.000 description 13
- 238000003756 stirring Methods 0.000 description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 13
- 239000008367 deionised water Substances 0.000 description 12
- 229910021641 deionized water Inorganic materials 0.000 description 12
- 239000000126 substance Substances 0.000 description 12
- 238000001291 vacuum drying Methods 0.000 description 12
- 238000010792 warming Methods 0.000 description 12
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 description 10
- 230000035484 reaction time Effects 0.000 description 8
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 5
- 229910001870 ammonium persulfate Inorganic materials 0.000 description 5
- 229910017604 nitric acid Inorganic materials 0.000 description 5
- MCAPDUSPBSEQQO-UHFFFAOYSA-N O1[SiH2]O[SiH2]O[SiH2]O[SiH2]1.CC=C Chemical compound O1[SiH2]O[SiH2]O[SiH2]O[SiH2]1.CC=C MCAPDUSPBSEQQO-UHFFFAOYSA-N 0.000 description 4
- 239000003112 inhibitor Substances 0.000 description 4
- 150000003057 platinum Chemical class 0.000 description 4
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 3
- 150000001336 alkenes Chemical class 0.000 description 3
- 239000003054 catalyst Substances 0.000 description 3
- FBAFATDZDUQKNH-UHFFFAOYSA-M iron chloride Chemical compound [Cl-].[Fe] FBAFATDZDUQKNH-UHFFFAOYSA-M 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 229910052710 silicon Inorganic materials 0.000 description 3
- 239000010703 silicon Substances 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 230000008021 deposition Effects 0.000 description 2
- 239000004575 stone Substances 0.000 description 2
- PAWQVTBBRAZDMG-UHFFFAOYSA-N 2-(3-bromo-2-fluorophenyl)acetic acid Chemical compound OC(=O)CC1=CC=CC(Br)=C1F PAWQVTBBRAZDMG-UHFFFAOYSA-N 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 238000005234 chemical deposition Methods 0.000 description 1
- 238000002242 deionisation method Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000000686 essence Substances 0.000 description 1
- 239000011888 foil Substances 0.000 description 1
- 108010025899 gelatin film Proteins 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- MRNHPUHPBOKKQT-UHFFFAOYSA-N indium;tin;hydrate Chemical compound O.[In].[Sn] MRNHPUHPBOKKQT-UHFFFAOYSA-N 0.000 description 1
- 239000004973 liquid crystal related substance Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- XAKYZBMFCZISAU-UHFFFAOYSA-N platinum;triphenylphosphane Chemical class [Pt].C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1 XAKYZBMFCZISAU-UHFFFAOYSA-N 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2204/00—Structure or properties of graphene
- C01B2204/20—Graphene characterized by its properties
- C01B2204/22—Electronic properties
Landscapes
- Carbon And Carbon Compounds (AREA)
- Laminated Bodies (AREA)
Abstract
The invention relates to the technical field of graphene transparent conductive films, and provides a method for transferring a graphene film with a non-planar special-shaped structure. The method comprises the following steps: duplicating a metal substrate C which has the same shape with a special-shaped structural part A of a graphene film to be transferred; growing a graphene film on the metal substrate C, meanwhile, coating the surface of a graphene film layer with peeling glue, and depositing a silica gel layer on the surface of the peeling glue after drying and curing; forming a special-shaped structural part B after the metal substrate C is etched completely, wherein the special-shaped structural part B has an attaching shape corresponding to the special-shaped structural part A; attaching one side, provided with the graphene film, of the special-shaped structural part B to a corresponding surface of the deformed structural part A, separating the peeling glue and the silica gel layer in the special-shaped structural part B from the graphene film, and attaching the graphene film to the special-shaped structural part A. By adopting the method, the defect that only the graphene film can be transferred to a two-dimensional planar structure in the prior art is overcome, and the application range of the graphene film is enlarged.
Description
Technical field
The present invention relates to transparent graphene conductive film technical field, more particularly to a kind of on-plane surface polymorphic structure Graphene
The transfer method of thin film.
Background technology
Graphene film has a light transmission of excellent electric conductivity and superelevation, and because of its ultra-thin and flexible characteristic such as flexible
Can so as to transparent conductive film can be prepared into, be expected to become the substitution material of the tin indium oxide for commonly using at present, be applied to
The fields such as touch screen, liquid crystal display, transparency electrode, electrode of solar battery and electromagnetic shielding.
Generally, the graphene film that continuous, transparent, electrical conductivity is high and area is big can be prepared using chemical deposition,
Graphene prepared by the method is attached to metal foil surface, therefore, how by its is lossless, efficient, be easily transferred to
In destination carrier, can become realize the key of graphene film industrialization.At present, the transfer techniques of graphene film are general only
Can be shifted in two-dimension plane structure, so as to limit development and the range of application of graphene film industry.
The content of the invention
In sum, it is an object of the invention to provide a kind of transfer method of on-plane surface polymorphic structure graphene film,
Aim to solve the problem that the problem that graphene film cannot be shifted on on-plane surface polymorphic structure in prior art.
The present invention is achieved in that the transfer method of on-plane surface polymorphic structure graphene film, and it comprises the steps：
Step one, prepares the anisotropic approach part A shape identical metallic matrix C with graphene film to be transferred；
Step 2, by chemical vapour deposition technique the metallic matrix C surface deposited graphite alkene thin film；
Step 3, in the metallic matrix C there is the side of graphene film to coat one layer of stripping glue, and dry solidification；
Step 4, in the metallic matrix C there is the side deposition of the stripping glue to be solidified by silica gel presoma drying
The layer of silica gel formed after process；
Step 5, the metallic matrix C in step 4 is placed in etching liquid, is removed and is obtained after the metallic matrix C
Special-shaped structural part B；
Step 6, under negative pressure of vacuum environment, has graphene film according to ratcheting shape by the special-shaped structural part B
Side is fitted on the special-shaped structural part A, and under separation condition, graphene film is separated with the stripping glue, and removes institute
State stripping glue and the layer of silica gel so that be covered with graphene film on special-shaped structural part A.
Compared with prior art, the transfer method of the on-plane surface polymorphic structure graphene film that the present invention is provided, by multiple
Make the special-shaped structural part A shape identical metallic matrix C with graphene film to be transferred；And grow graphite on metallic matrix C
Alkene thin film, meanwhile, glue is peeled off in the surface-coated of the graphene film layer, deposit one on the surface of the stripping glue after dry solidification
Layer layer of silica gel, the layer of silica gel is solidify to form by silica gel presoma drying, and layer of silica gel is used as the supporting layer for peeling off glue；Work as metal
After matrix C is fully etched, special-shaped structural part B is formed, special-shaped structural part B has the laminating shape corresponding with anisotropic approach part A
Shape；There is the side of graphene film to be attached at special-shaped structural part A corresponding surfaces special-shaped structural part B according to ratcheting shape
On, and under the conditions of particular separation, the stripping glue in special-shaped structural part B and layer of silica gel are separated, graphene film is then attached at
On special-shaped structural part A, graphene film can only be transferred to the shortcoming of two-dimension plane structure more than to overcome prior art, so as to
Expand the range of application of graphene film.
Specific embodiment
In order that the objects, technical solutions and advantages of the present invention become more apparent, with reference to embodiments, to the present invention
It is further elaborated.It should be appreciated that specific embodiment described herein is not used to only to explain the present invention
Limit the present invention.
A kind of transfer method of on-plane surface polymorphic structure graphene film that the present invention is provided, it comprises the steps：
Step S01, prepares the anisotropic approach part A shape identical metallic matrix C with graphene film to be transferred；
Step S02, by chemical vapour deposition technique metallic matrix C surface deposited graphite alkene thin film；
Step S03, in metallic matrix C there is the side of graphene film to coat one layer of stripping glue, and dry solidification；
Step S04, in the metallic matrix C there is the side deposition of the stripping glue to be solidified by silica gel presoma drying
The layer of silica gel formed after process；
Step S05, the metallic matrix C in step 4 is placed in etching liquid, to be removed and obtain polymorphic structure after metallic matrix C
Part B；
Step S06, under negative pressure of vacuum environment, the side that the special-shaped structural part B has graphene film is fitted in
On the special-shaped structural part A, under separation condition, graphene film with it is described stripping glue separate, and remove it is described stripping glue and
The layer of silica gel so that be covered with graphene film on special-shaped structural part A.
Further, the material of metallic matrix C is copper or nickel, and the fusing point of copper and mickel can bear more than 1050 DEG C
The hot environment of chemical vapour deposition reaction.
Further, in step S02, the method for chemical vapour deposition technique is：Using methane and hydrogen as working gas,
Temperature be 1000~1050 DEG C, negative pressure pressure be 1~50Pa under conditions of, react 10~40min.Wherein, reaction temperature can
For 1000 DEG C, 1005 DEG C, 1010 DEG C, 1015 DEG C, 1020 DEG C, 1025 DEG C, 1030 DEG C, 1035 DEG C, 1040 DEG C, 1045 DEG C and
1050 DEG C, negative pressure pressure can be 1Pa, 5Pa, 10Pa, 15Pa, 20Pa, 25Pa, 30Pa, 35Pa, 40Pa, 45Pa and 50Pa.
During chemical vapour deposition reaction, in 10~30sccm, the flow of hydrogen is 5~20sccm to the flow of methane.
Further, in step S03, it is 10 μm, 15 μ that the coating thickness for peeling off glue is 10~100 μm, i.e. coating thickness
m、20μm、25μm、30μm、35μm、40μm、45μm、50μm、55μm、60μm、65μm、70μm、75μm、80μm、85μm、90μm
And 100 μm.Peel off glue and play a part of carrier, i.e., after metal basal board C is possible to determine when the sample has been completely etched, the graphene film on its surface
Can stick on stripping glue, be easy to transfer.
Preferably, it can be foamed glue or ultraviolet glue to peel off glue.Wherein, foamed glue is that high temperature peels off glue, is had at normal temperatures
Viscosity, loses viscosity after heating；Ultraviolet glue be then under ultraviolet light solidification after, lose viscosity.Above two peels off glue coating
Dry solidification is needed after graphene film, its condition of cure is to be 80~90 DEG C in temperature to toast 5~15min.
Further, in step S04, silica gel presoma includes the following component of following parts by weight：
Wherein, the weight proportion of containing hydrogen silicone oil can be 1 part, 2 parts, 3 parts, 4 parts, 5 parts, 6 parts, 7 parts, 8 parts, 9 parts and 10
Part, the weight proportion of inhibitor can be 0.1 part, 0.2 part, 0.3 part, 0.4 part and 0.5 part, and the weight proportion of catalyst can be
0.1 part, 0.11 part, 0.12 part, 0.13 part, 0.14 part, 0.15 part, 0.16 part, 0.17 part, 0.18 part, 0.19 part and 0.2
Part.Specifically, by 100 parts of vinyl silicone oil, 1~10 part of containing hydrogen silicone oil, 0.1~0.5 part of inhibitor and 0.1~
1~5min is stirred in 0.2 part of catalysis in the planetary stirring machine that rotating speed is 1500~2000r/min.Wherein, vinyl silicone oil
, in 300~5000cps, containing hydrogen silicone oil range of viscosities is in 50~500cps for range of viscosities.The condition of cure of silica gel presoma is 40
~60 DEG C of bakings are until be fully cured.Here, the effect of layer of silica gel is to play a part of to carry support to peeling off glue, is easy to turn
Move.
Specifically, inhibitor is 1- acetenyl -1- Hexalin, methylpentynol, 3- phenyl-ethyl acetylene -3-
Any one or a few in alcohol and methyl ethylene cyclotetrasiloxane.Preferably, inhibitor is 1- acetenyl -1- hexamethylenes
Alcohol.
Specifically, catalyst be platinum-vinyl siloxane coordination compound, double (alkynyls) (cyclic diolefine alkynyl) platinum complex and
Any one or a few in double (alkynyls) double (triphenylphosphine) platinum complexes.Preferably, catalyst is platinum-vinyl siloxane
Coordination compound.
Further, in step S05, the concentration of etching liquid is 0.1~1mol.Specifically, metallic matrix C is placed in into etching
In liquid, until its metal part is completely dissolved in etching liquid, special-shaped structural part B is obtained, and by anisotropic approach part submergence deionization
Repeatedly rinsed in water, every time the time of rinsing is 30~60min, then be placed on baking in the environment that temperature is 40~50 DEG C
Dry 2~4h.
Specifically, etching liquid was any one or a few in Liu Suan An ﹑ iron chloride or nitric acid.
Specifically, in step S06, when peel off glue be foamed glue when, its separation condition be temperature range be 120~
Heated at 150 DEG C, i.e., temperature range can be 120 DEG C, 125 DEG C, 130 DEG C, 135 DEG C, 140 DEG C 145 DEG C and 150 DEG C, will
Special-shaped structural part A and special-shaped structural part B after laminating is positioned over together temperature range to be heated under 120~150 DEG C of environment,
Foamed glue is separated because being lost viscosity by high temperature with graphene film, so as to realize that foamed glue is thin from Graphene with layer of silica gel
Film is removed, i.e., graphene film is transferred on special-shaped structural part A.
Specifically, in step 6, when it is ultraviolet glue to peel off glue, its separation condition is to be in the amount of radiation of ultraviolet
300~800mJ/cm2Under radiated, i.e., the amount of radiation of ultraviolet can be 300mJ/cm2、350mJ/cm2、400mJ/cm2、
450mJ/cm2、500mJ/cm2、550mJ/cm2、600mJ/cm2、650mJ/cm2、700mJ/cm2、750mJ/cm2And 800mJ/
cm2, it is 300~800mJ/cm by the amount of radiation that the special-shaped structural part A and special-shaped structural part B after laminating is positioned over together ultraviolet2
Under radiated, ultraviolet glue loses viscosity because being irradiated by ultraviolet, and separates with graphene film, so as to realize ultraviolet glue with
Layer of silica gel is removed from graphene film, i.e., graphene film is transferred on special-shaped structural part A.
It is described in detail below in conjunction with realization of the specific embodiment to the present invention.
Embodiment 1
1) growth of graphene film
Prepared and special-shaped structural part A shape identical metallic matrix C using metallic copper, metallic matrix C is placed in into chemical gas
In phase cvd furnace, 1000 DEG C are warming up to, negative pressure pressure is 1Pa, and hydrogen flowing quantity is 5sccm, and methane flow is 10sccm, during reaction
Between be 10min, the superficial growth of metallic matrix C goes out a layer graphene thin film.
2) graphene film is transferred to on-plane surface special-shaped structural part
There is the foamed glue that the side coating thickness of graphene film is 100 μm in metallic matrix C, in 90 DEG C of bakings
15min solidifies.By 100 parts of vinyl silicone oil, 10 parts of containing hydrogen silicone oil, 0.5 part of 1- acetenyl -1- Hexalin and 0.2
Part platinum-vinyl siloxane coordination compound mixed under rotating speed 2000r/min before 5min obtains silica gel by planetary stirring machine
Body is driven, silica gel presoma is coated on foamed glue, and in 60 DEG C of bakings until being fully cured to form layer of silica gel.Will be with silica gel
The metallic matrix C of layer is immersed in the Ammonium persulfate. that concentration is 1mol/L, until copper metal basal board C completes etching and obtains abnormity
Structural member B, then special-shaped structural part B is immersed in into rinsing three times in deionized water, 60min is rinsed every time to remove etching liquid, so
Dry 4h in 50 DEG C of vacuum drying oven afterwards.0.5h is kept under condition of negative pressure, special-shaped structural part B is had into graphene film
Side fits in the corresponding sides of special-shaped structural part A, to discharge the air between graphene film and special-shaped structural part A, so
The special-shaped structural part A and special-shaped structural part B after laminating is placed in 150 DEG C of environment afterwards, until foamed glue loses viscosity, completely from
Graphene film surface comes off, and removes together with layer of silica gel, and so, graphene film is then transferred on special-shaped structural part A.
Embodiment 2
1) growth of graphene film
Prepared and special-shaped structural part A shape identical metallic matrix C using metallic copper, metallic matrix C is placed in into chemical gas
In phase cvd furnace, 1025 DEG C are warming up to, negative pressure pressure is 25Pa, and hydrogen flowing quantity is 10sccm, and methane flow is 20sccm, reaction
Time is 25min, and the superficial growth of metallic matrix C goes out a layer graphene thin film.
2) graphene film is transferred to on-plane surface special-shaped structural part
There is the foamed glue that the side coating thickness of graphene film is 60 μm in metallic matrix C, at 85 DEG C 10min is toasted
Solidification.By 100 parts of vinyl silicone oil, 8 parts of containing hydrogen silicone oil, 0.3 part of 1- acetenyl -1- Hexalin and 0.15 part
Platinum-vinyl siloxane coordination compound mixes 3min under rotating speed 1800r/min and obtains silica gel presoma by planetary stirring machine,
Silica gel presoma is coated on foamed glue, and in 50 DEG C of bakings until being fully cured to form layer of silica gel.By with layer of silica gel
Metallic matrix C is immersed in the Ammonium persulfate. that concentration is 0.5mol/L, until copper metal basal board C completes etching obtains special-shaped knot
Component B, then special-shaped structural part B is immersed in into rinsing three times in deionized water, 45min is rinsed every time to remove etching liquid, then
3h is dried in 45 DEG C of vacuum drying oven.0.7h is kept under condition of negative pressure, special-shaped structural part B is had into the one of graphene film
Side fits in the corresponding sides of special-shaped structural part A, to discharge the air between graphene film and special-shaped structural part A, then
Special-shaped structural part A and special-shaped structural part B after laminating is placed in 135 DEG C of environment, until foamed glue loses viscosity, completely from stone
Black alkene film surface comes off, and removes together with layer of silica gel, and so, graphene film is then transferred on special-shaped structural part A.
Embodiment 3
1) growth of graphene film
Prepared and special-shaped structural part A shape identical metallic matrix C using metallic copper, metallic matrix C is placed in into chemical gas
In phase cvd furnace, 1050 DEG C are warming up to, negative pressure pressure is 50Pa, and hydrogen flowing quantity is 20sccm, and methane flow is 30sccm, reaction
Time is 40min, and the superficial growth of metallic matrix C goes out a layer graphene thin film.
2) graphene film is transferred to on-plane surface special-shaped structural part
There is the foamed glue that the side coating thickness of graphene film is 100 μm in metallic matrix C, in 90 DEG C of bakings
15min solidifies.By 100 parts of vinyl silicone oil, 10 parts of containing hydrogen silicone oil, 0.5 part of 1- acetenyl -1- Hexalin and 0.2
Part platinum-vinyl siloxane coordination compound mixed under rotating speed 2000r/min before 5min obtains silica gel by planetary stirring machine
Body is driven, silica gel presoma is coated on foamed glue, and in 60 DEG C of bakings until being fully cured to form layer of silica gel.Will be with silica gel
The metallic matrix C of layer is immersed in the Ammonium persulfate. that concentration is 1mol/L, until copper metal basal board C completes etching and obtains abnormity
Structural member B, then special-shaped structural part B is immersed in into rinsing three times in deionized water, 60min is rinsed every time to remove etching liquid, so
Dry 4h in 50 DEG C of vacuum drying oven afterwards.1h is kept under condition of negative pressure, special-shaped structural part B is had into the one of graphene film
Side fits in the corresponding sides of special-shaped structural part A, to discharge the air between graphene film and special-shaped structural part A, then
Special-shaped structural part A and special-shaped structural part B after laminating is placed in 150 DEG C of environment, until foamed glue loses viscosity, completely from stone
Black alkene film surface comes off, and removes together with layer of silica gel, and so, graphene film is then transferred on special-shaped structural part A.
Embodiment 4
1) growth of graphene film
Prepared and special-shaped structural part A shape identical metallic matrix C using metallic copper, metallic matrix C is placed in into chemical gas
In phase cvd furnace, 1000 DEG C are warming up to, negative pressure pressure is 1Pa, and hydrogen flowing quantity is 5sccm, and methane flow is 10sccm, during reaction
Between be 10min, the superficial growth of metallic matrix C goes out a layer graphene thin film.
2) graphene film is transferred to on-plane surface special-shaped structural part
There is the ultraviolet glue that the side coating thickness of graphene film is 10 μm in metallic matrix C, at 80 DEG C 5min is toasted
Solidification.By 100 parts of vinyl silicone oil, 1 part of containing hydrogen silicone oil, 0.1 part of methylpentynol and 0.1 part
Platinum-vinyl siloxane coordination compound mixes 1min under rotating speed 1500r/min and obtains silica gel presoma by planetary stirring machine,
To be coated in ultraviolet glue with silica gel presoma, and in 40 DEG C of bakings until being fully cured to form layer of silica gel.Will be with silica gel
The metallic matrix C of layer is immersed in the Ammonium persulfate. that concentration is 0.1mol/L, until copper metal basal board C completes etching obtains different
Shape structural member B, then special-shaped structural part B is immersed in into rinsing three times in deionized water, 30min is rinsed every time to remove etching liquid,
Then 2h is dried in 40 DEG C of vacuum drying oven.Under condition of negative pressure, special-shaped structural part B had into the side patch of graphene film
Together in the corresponding sides of special-shaped structural part A, to discharge the air between graphene film and special-shaped structural part A, then will patch
Special-shaped structural part A and special-shaped structural part B after conjunction is placed in UV radiation dose 300mJ/cm2In environment, until ultraviolet glue loses
Viscosity, comes off completely from graphene film surface, and removes together with layer of silica gel, and so, graphene film is then transferred to abnormity
On structural member A.
Embodiment 5
1) growth of graphene film
Prepared and special-shaped structural part A shape identical metallic matrix C using metallic copper, metallic matrix C is placed in into chemical gas
In phase cvd furnace, 1025 DEG C are warming up to, negative pressure pressure is 25Pa, and hydrogen flowing quantity is 10sccm, and methane flow is 20sccm, reaction
Time is 25min, and the superficial growth of metallic matrix C goes out a layer graphene thin film.
2) graphene film is transferred to on-plane surface special-shaped structural part
There is the ultraviolet glue that the side coating thickness of graphene film is 60 μm in metallic matrix C, at 85 DEG C 10min is toasted
Solidification.By 100 parts of vinyl silicone oil, 8 parts of containing hydrogen silicone oil, 0.3 part of methylpentynol and 0.15 part
Double (alkynyls) (cyclic diolefine alkynyl) platinum complex mixes 3min under rotating speed 1800r/min and obtains silica gel by planetary stirring machine
Presoma, by silica gel presoma in ultraviolet glue, and in 50 DEG C of bakings until being fully cured to form layer of silica gel.Will be with layer of silica gel
Metallic matrix C be immersed in concentration be 0.5mol/L iron chloride in, until copper metal basal board C completes etching obtains special-shaped knot
Component B, then special-shaped structural part B is immersed in into rinsing three times in deionized water, 45min is rinsed every time to remove etching liquid, then
3h is dried in 45 DEG C of vacuum drying oven.0.75h is kept under condition of negative pressure, special-shaped structural part B is had into graphene film
Side fits in the corresponding sides of special-shaped structural part A, to discharge the air between graphene film and special-shaped structural part A, so
Afterwards the special-shaped structural part A and special-shaped structural part B after laminating is placed in into UV radiation dose 550mJ/cm2In environment, until ultraviolet
Glue loses viscosity, comes off from graphene film surface completely, and removes together with layer of silica gel, and so, graphene film is then shifted
To special-shaped structural part A.
Embodiment 6
1) growth of graphene film
Prepared and special-shaped structural part A shape identical metallic matrix C using metallic copper, metallic matrix C is placed in into chemical gas
In phase cvd furnace, 1050 DEG C are warming up to, negative pressure pressure is 50Pa, and hydrogen flowing quantity is 20sccm, and methane flow is 30sccm, reaction
Time is 40min, and the superficial growth of metallic matrix C goes out a layer graphene thin film.
2) graphene film is transferred to on-plane surface special-shaped structural part
There is the ultraviolet glue that the side coating thickness of graphene film is 100 μm in metallic matrix C, in 90 DEG C of bakings
15min solidifies.By 100 parts of vinyl silicone oil, 10 parts of containing hydrogen silicone oil, 0.5 part of methylpentynol and 0.2
Double (alkynyl) (cyclic diolefine alkynyl) platinum complexes of part mix 5min under rotating speed 2000r/min and obtain by planetary stirring machine
Silica gel presoma, silica gel presoma is coated in ultraviolet glue, and in 60 DEG C of bakings until being fully cured to form layer of silica gel.Will tool
The metallic matrix C for having layer of silica gel is immersed in the iron chloride that concentration is 1mol/L, until copper metal basal board C completes etching and obtains
Special-shaped structural part B, then special-shaped structural part B is immersed in into rinsing three times in deionized water, 60min is rinsed every time to remove etching
Liquid, then dries 4h in 50 DEG C of vacuum drying oven.1h is kept under condition of negative pressure, has Graphene thin special-shaped structural part B
The side of film fits in the corresponding sides of special-shaped structural part A, to discharge the sky between graphene film and special-shaped structural part A
Gas, is then placed in UV radiation dose 800mJ/cm by the special-shaped structural part A and special-shaped structural part B after laminating2In environment, until
Ultraviolet glue loses viscosity, comes off from graphene film surface completely, and removes together with layer of silica gel, and so, graphene film is then
It is transferred on special-shaped structural part A.
Embodiment 7
1) growth of graphene film
Prepared and special-shaped structural part A shape identical metallic matrix C using metallic nickel, metallic matrix C is placed in into chemical gas
In phase cvd furnace, 1000 DEG C are warming up to, negative pressure pressure is 1Pa, and hydrogen flowing quantity is 5sccm, and methane flow is 10sccm, during reaction
Between be 10min, the superficial growth of metallic matrix C goes out a layer graphene thin film.
2) graphene film is transferred to on-plane surface special-shaped structural part
There is the foamed glue that the side coating thickness of graphene film is 100 μm in metallic matrix C, at 80 DEG C 5min is toasted
Solidification.By 100 parts of vinyl silicone oil, 1 part of containing hydrogen silicone oil, 0.1 part of 3-Phenyl-1-butyn-3-ol and 0.1 part it is double
(alkynyl) (cyclic diolefine alkynyl) platinum complex is mixed before 1min obtains silica gel by planetary stirring machine under rotating speed 1500r/min
Body is driven, silica gel presoma is coated on foamed glue, and in 40 DEG C of bakings until being fully cured to form layer of silica gel.Will be with silica gel
The metallic matrix C of layer is immersed in the Ammonium persulfate. that concentration is 0.1mol/L, until nickel metal basal board C completes etching obtains different
Shape structural member B, then special-shaped structural part B is immersed in into rinsing three times in deionized water, 30min is rinsed every time to remove etching liquid,
Then 2h is dried in 50 DEG C of vacuum drying oven.Under condition of negative pressure, special-shaped structural part B had into the side patch of graphene film
Together in the corresponding sides of special-shaped structural part A, to discharge the air between graphene film and special-shaped structural part A, then will patch
Special-shaped structural part A and special-shaped structural part B after conjunction is placed in 120 DEG C of environment, until foamed glue loses viscosity, completely from Graphene
Film surface comes off, and removes together with layer of silica gel, and so, graphene film is then transferred on special-shaped structural part A.
Embodiment 8
1) growth of graphene film
Prepared and special-shaped structural part A shape identical metallic matrix C using metallic nickel, metallic matrix C is placed in into chemical gas
In phase cvd furnace, 1025 DEG C are warming up to, negative pressure pressure is 25Pa, and hydrogen flowing quantity is 10sccm, and methane flow is 20sccm, reaction
Time is 25min, and the superficial growth of metallic matrix C goes out a layer graphene thin film.
2) graphene film is transferred to on-plane surface special-shaped structural part
There is the foamed glue that the side coating thickness of graphene film is 60 μm in metallic matrix C, at 85 DEG C 10min is toasted
Solidification.By 100 parts of vinyl silicone oil, 8 parts of containing hydrogen silicone oil, 0.3 part of 3-Phenyl-1-butyn-3-ol and 0.15 part
Double (alkynyls) (cyclic diolefine alkynyl) platinum complex mixes 3min under rotating speed 1800r/min and obtains silica gel by planetary stirring machine
Presoma, silica gel presoma is coated on foamed glue, and in 50 DEG C of bakings until being fully cured to form layer of silica gel.Will be with silicon
The metallic matrix C of glue-line is immersed in the nitric acid that concentration is 0.5mol/L, until nickel metal basal board C completes etching and obtains abnormity
Structural member B, then special-shaped structural part B is immersed in into rinsing three times in deionized water, 45min is rinsed every time to remove etching liquid, so
Dry 3h in 45 DEG C of vacuum drying oven afterwards.0.75h is kept under condition of negative pressure, special-shaped structural part B is had into graphene film
Side fit in the corresponding sides of special-shaped structural part A, to discharge the air between graphene film and special-shaped structural part A,
Then the special-shaped structural part A and special-shaped structural part B after laminating is placed in 135 DEG C of environment, until foamed glue loses viscosity, completely
Come off from graphene film surface, and remove together with layer of silica gel, so, graphene film is then transferred on special-shaped structural part A.
Embodiment 9
1) growth of graphene film
Prepared and special-shaped structural part A shape identical metallic matrix C using metallic nickel, metallic matrix C is placed in into chemical gas
In phase cvd furnace, 1050 DEG C are warming up to, negative pressure pressure is 50Pa, and hydrogen flowing quantity is 20sccm, and methane flow is 30sccm, reaction
Time is 40min, and the superficial growth of metallic matrix C goes out a layer graphene thin film.
2) graphene film is transferred to on-plane surface special-shaped structural part
There is the foamed glue that the side coating thickness of graphene film is 100 μm in metallic matrix C, in 90 DEG C of bakings
15min solidifies.By 100 parts of vinyl silicone oil, 10 parts of containing hydrogen silicone oil, 0.5 part of 3-Phenyl-1-butyn-3-ol and 0.2
Double (alkynyl) (cyclic diolefine alkynyl) platinum complexes of part mix 5min under rotating speed 2000r/min and obtain by planetary stirring machine
Silica gel presoma, silica gel presoma is coated on foamed glue, and in 60 DEG C of bakings until being fully cured to form layer of silica gel.Will tool
The metallic matrix C for having layer of silica gel is immersed in the ammonium nitrate that concentration is 1mol/L, until nickel metal basal board C completes etching and obtains
Special-shaped structural part B, then special-shaped structural part B is immersed in into rinsing three times in deionized water, 60min is rinsed every time to remove etching
Liquid, then dries 4h in 50 DEG C of vacuum drying oven.1h is kept under condition of negative pressure, has Graphene thin special-shaped structural part B
The side of film fits in the corresponding sides of special-shaped structural part A, to discharge the sky between graphene film and special-shaped structural part A
Gas, is then placed in the special-shaped structural part A and special-shaped structural part B after laminating in 150 DEG C of environment, until foamed glue loses viscosity,
Completely come off from graphene film surface, and remove together with layer of silica gel, so, graphene film is then transferred to special-shaped structural part
On A.
Embodiment 10
1) growth of graphene film
Prepared and special-shaped structural part A shape identical metallic matrix C using metallic nickel, metallic matrix C is placed in into chemical gas
In phase cvd furnace, 1000 DEG C are warming up to, negative pressure pressure is 1Pa, and hydrogen flowing quantity is 5sccm, and methane flow is 10sccm, during reaction
Between be 10min, the superficial growth of metallic matrix C goes out a layer graphene thin film.
2) graphene film is transferred to on-plane surface special-shaped structural part
There is the ultraviolet glue that the side coating thickness of graphene film is 100 μm in metallic matrix C, at 80 DEG C 5min is toasted
Solidification.By 100 parts of vinyl silicone oil, 1 part of containing hydrogen silicone oil, 0.1 part of methyl ethylene cyclotetrasiloxane and 0.1 part
Double (alkynyls) (cyclic diolefine alkynyl) platinum complex mixes 1min under rotating speed 1500r/min and obtains silica gel by planetary stirring machine
Presoma, silica gel presoma is coated in ultraviolet glue, and in 40 DEG C of bakings until being fully cured to form layer of silica gel.Will be with silicon
The metallic matrix C of glue-line is immersed in the nitric acid that concentration is 0.1mol/L, until nickel metal basal board C completes etching and obtains abnormity
Structural member B, then special-shaped structural part B is immersed in into rinsing three times in deionized water, 30min is rinsed every time to remove etching liquid, so
Dry 2h in 40 DEG C of vacuum drying oven afterwards.0.5h is kept under condition of negative pressure, special-shaped structural part B is had into graphene film
Side fits in the corresponding sides of special-shaped structural part A, to discharge the air between graphene film and special-shaped structural part A, so
Afterwards the special-shaped structural part A and special-shaped structural part B after laminating is placed in into UV radiation dose 300mJ/cm2In environment, until ultraviolet
Glue loses viscosity, comes off from graphene film surface completely, and removes together with layer of silica gel, and so, graphene film is then shifted
To special-shaped structural part A.
Embodiment 11
1) growth of graphene film
Prepared and special-shaped structural part A shape identical metallic matrix C using metallic nickel, metallic matrix C is placed in into chemical gas
In phase cvd furnace, 1025 DEG C are warming up to, negative pressure pressure is 25Pa, and hydrogen flowing quantity is 10sccm, and methane flow is 20sccm, reaction
Time is 25min, and the superficial growth of metallic matrix C goes out a layer graphene thin film.
2) graphene film is transferred to on-plane surface special-shaped structural part
There is the ultraviolet glue that the side coating thickness of graphene film is 60 μm in metallic matrix C, at 85 DEG C 10min is toasted
Solidification.By 100 parts of vinyl silicone oil, 8 parts of containing hydrogen silicone oil, 0.3 part of methyl ethylene cyclotetrasiloxane and 0.15 part
Double (alkynyl) (cyclic diolefine alkynyl) platinum complexes 3min mixed under rotating speed 1800r/min by planetary stirring machine obtain silicon
Glue presoma, silica gel presoma is coated in ultraviolet glue, and in 50 DEG C of bakings until being fully cured to form layer of silica gel.To have
The metallic matrix C of layer of silica gel is immersed in the nitric acid that concentration is 0.5mol/L, until nickel metal basal board C completes etching obtains different
Shape structural member B, then special-shaped structural part B is immersed in into rinsing three times in deionized water, 45min is rinsed every time to remove etching liquid,
Then 3h is dried in 45 DEG C of vacuum drying oven.0.75h is kept under condition of negative pressure, has Graphene thin special-shaped structural part B
The side of film fits in the corresponding sides of special-shaped structural part A, to discharge the sky between graphene film and special-shaped structural part A
Gas, is then placed in UV radiation dose 550mJ/cm by the special-shaped structural part A and special-shaped structural part B after laminating2In environment, until
Ultraviolet glue loses viscosity, comes off from graphene film surface completely, and removes together with layer of silica gel, and so, graphene film is then
It is transferred on special-shaped structural part A.
Embodiment 12
1) growth of graphene film
Prepared and special-shaped structural part A shape identical metallic matrix C using metallic nickel, metallic matrix C is placed in into chemical gas
In phase cvd furnace, 1050 DEG C are warming up to, negative pressure pressure is 50Pa, and hydrogen flowing quantity is 20sccm, and methane flow is 30sccm, reaction
Time is 40min, and the superficial growth of metallic matrix C goes out a layer graphene thin film.
2) graphene film is transferred to on-plane surface special-shaped structural part
There is the ultraviolet glue that the side coating thickness of graphene film is 100 μm in metallic matrix C, in 90 DEG C of bakings
15min solidifies.By 100 parts of vinyl silicone oil, 10 parts of containing hydrogen silicone oil, 0.5 part of methyl ethylene cyclotetrasiloxane and
0.2 part double (alkynyl) (cyclic diolefine alkynyl) platinum complexes mix 5min by planetary stirring machine under rotating speed 2000r/min
Silica gel presoma is obtained, silica gel presoma is coated in ultraviolet glue, and in 60 DEG C of bakings until being fully cured to form layer of silica gel.
Metallic matrix C with layer of silica gel is immersed in the nitric acid that concentration is 1mol/L, until copper metal basal board C completes to etch
To special-shaped structural part B, then special-shaped structural part B is immersed in into rinsing three times in deionized water, 60min is rinsed every time to remove etching
Liquid, then dries 4h in 50 DEG C of vacuum drying oven.1h is kept under condition of negative pressure, has Graphene thin special-shaped structural part B
The side of film fits in the corresponding sides of special-shaped structural part A, to discharge the sky between graphene film and special-shaped structural part A
Gas, is then placed in UV radiation dose 800mJ/cm by the special-shaped structural part A and special-shaped structural part B after laminating2In environment, until
Ultraviolet glue loses viscosity, comes off from graphene film surface completely, and removes together with layer of silica gel, and so, graphene film is then
It is transferred on special-shaped structural part A.
Presently preferred embodiments of the present invention is the foregoing is only, not to limit the present invention, all essences in the present invention
Any modification, equivalent and improvement made within god and principle etc., should be included within the scope of the present invention.
Claims (10)
1. the transfer method of on-plane surface polymorphic structure graphene film, it is characterised in that it comprises the steps：
Step one, prepares the anisotropic approach part A shape identical metallic matrix C with graphene film to be transferred；
Step 2, by chemical vapour deposition technique the metallic matrix C surface deposited graphite alkene thin film；
Step 3, in the metallic matrix C there is the side of graphene film to coat one layer of stripping glue, and dry solidification；
Step 4, in the metallic matrix C there is the side of the stripping glue to deposit by silica gel presoma drying cured
The layer of silica gel for being formed afterwards；
Step 5, the metallic matrix C in step 4 is placed in etching liquid, to be removed and obtain abnormity after the metallic matrix C
Structural member B；
Step 6, under negative pressure of vacuum environment, the special-shaped structural part B is had the side of graphene film according to ratcheting shape
Fit on the special-shaped structural part A, under separation condition, graphene film is separated with the stripping glue, and removes the stripping
From glue and the layer of silica gel so that be covered with graphene film on special-shaped structural part A.
2. the transfer method of on-plane surface polymorphic structure graphene film as claimed in claim 1, it is characterised in that the metal
The material of matrix C is copper or nickel.
3. the transfer method of on-plane surface polymorphic structure graphene film as claimed in claim 1, it is characterised in that in step 2
In, the method for the chemical vapor deposition is：It is 1000~1050 in reaction temperature using methane and hydrogen as working gas
DEG C, negative pressure pressure be 1~50Pa under conditions of, react 10~40min.
4. the transfer method of the on-plane surface polymorphic structure graphene film as described in claims 1 to 3 is arbitrary, it is characterised in that
In step 3, the coating thickness for peeling off glue is 10~100 μm.
5. the transfer method of on-plane surface polymorphic structure graphene film as claimed in claim 4, it is characterised in that the stripping
Glue is foamed glue or ultraviolet glue.
6. the transfer method of on-plane surface polymorphic structure graphene film as claimed in claim 1, it is characterised in that in step 4
In, the silica gel presoma includes the following component of following parts by weight：
7. the transfer method of on-plane surface polymorphic structure graphene film as claimed in claim 6, it is characterised in that the suppression
Agent is 1- acetenyl -1- Hexalin, methylpentynol, 3-Phenyl-1-butyn-3-ol and ethylene methacrylic basic ring four
Any one or a few in siloxanes.
8. the transfer method of on-plane surface polymorphic structure graphene film as claimed in claim 6, it is characterised in that the catalysis
Agent is platinum-vinyl siloxane coordination compound, double (alkynyls) (cyclic diolefine alkynyl) platinum complex and double (alkynyls) double (triphenyls
Phosphine) any one or a few in platinum complex.
9. the transfer method of on-plane surface polymorphic structure graphene film as claimed in claim 5, it is characterised in that in step 6
In, when the stripping glue is foamed glue, the separation condition is to be heated in the case where temperature range is for 120~150 DEG C.
10. the transfer method of on-plane surface polymorphic structure graphene film as claimed in claim 5, it is characterised in that in step
In six, when it is described stripping glue be ultraviolet glue when, the separation condition be ultraviolet amount of radiation be 300~800mJ/cm2Under
Radiated.
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| CN102901763A (en) * | 2012-09-25 | 2013-01-30 | 清华大学 | Deoxyribonucleic acid (DNA) sequencing device based on graphene nanopore-microcavity-solid-state nanopore and manufacturing method |
| CN105315958A (en) * | 2015-10-28 | 2016-02-10 | 苏州天脉导热科技有限公司 | Addition heat-conducting self-adhesive silicone rubber and preparation method thereof |
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| CN102901763A (en) * | 2012-09-25 | 2013-01-30 | 清华大学 | Deoxyribonucleic acid (DNA) sequencing device based on graphene nanopore-microcavity-solid-state nanopore and manufacturing method |
| CN105315958A (en) * | 2015-10-28 | 2016-02-10 | 苏州天脉导热科技有限公司 | Addition heat-conducting self-adhesive silicone rubber and preparation method thereof |
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