CN110156001A - A method of transfer graphene film - Google Patents
A method of transfer graphene film Download PDFInfo
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- CN110156001A CN110156001A CN201910622974.6A CN201910622974A CN110156001A CN 110156001 A CN110156001 A CN 110156001A CN 201910622974 A CN201910622974 A CN 201910622974A CN 110156001 A CN110156001 A CN 110156001A
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- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
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- C01B32/194—After-treatment
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
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Abstract
The invention discloses a kind of methods for shifting graphene film, belong to graphene film preparation technical field., the following steps are included: PMMA, which is spun to growth, to be had in the metallic substrates of graphene, being formed has PMMA/ graphene/metallic substrates first structure layer, and metal etch is fallen and is cleaned multiple times for it；The second structure sheaf with PMMA/ graphene is covered in the newborn metallic substrates with target graphene, being formed has PMMA/ graphene/target graphene/metallic substrates third structure sheaf, and metal etch is fallen and is cleaned multiple times；It is heated after being placed in target substrate with the 4th structure of PMMA/ graphene/target graphene, the second structure sheaf is uncovered from target graphene, target graphene is transferred in target substrate.The method that the present invention shifts graphene film, easy to operate, it shifts that quality is high, cleanliness is high, integrality is good and without organic substance residues for graphene film after transfer, and PMMA/ graphene can be repeatedly used as supporting layer.
Description
Technical field
The present invention relates to graphene film preparation technical fields, and in particular to a method of transfer graphene film.
Background technique
Graphene is a kind of two-dimensional material with physical and chemical performance, at present the graphene one of growth on the metallic substrate
As cannot be used directly, need to be transferred to and just can be carried out subsequent applications in the target substrate of non metallic substrate.Graphene turns
It can be related to many chemical substances during shifting, they inevitably pollute graphene, significantly affect the performance of graphene.
Therefore, how pollutant is effectively avoided or is removed, be an important topic of graphene film transfer techniques research.
In graphene film transfer techniques, the method for use is stripping method or PMMA transfer method, and wherein stripping method is usual
Certain destruction can be caused to the integrality of graphene film, and PMMA transfer method is the dissolution method using PMMA as intermediary layer
Indirect branch, the graphene film that this method obtains is easily cracked, and PMMA has residual and can not completely remove, and
Metallic solution can also be remained, and cause graphene transfer of low quality.
Summary of the invention
The object of the present invention is to provide a kind of methods for shifting graphene film, to solve to obtain in existing PMMA transfer method
Graphene film easily cracked, organic substance residues and graphene problem of low quality.
The technical scheme to solve the above technical problems is that
A method of transfer graphene film, comprising the following steps:
(1) by PMMA using spin-coating method uniform fold growth have graphene metallic substrates on, at room temperature stand after simultaneously
Heating makes its film-forming, and being formed has PMMA/ graphene/metallic substrates first structure layer；
(2) metal etch in first structure layer is fallen, and is cleaned multiple times, obtain with PMMA/ graphene
Two structure sheafs；
(3) the second structure sheaf is covered in the newborn metallic substrates with target graphene, being formed has PMMA/ graphite
Alkene/target graphene/metallic substrates third structure sheaf；
(4) metal etch in third structure sheaf is fallen, and is cleaned multiple times, obtained with PMMA/ graphene/target
4th structure sheaf of graphene；
(5) it is heated after the 4th structure being placed in target substrate, the second structure sheaf is taken off from target graphene
It rises, target graphene is transferred in target substrate.
PMMA is first spun in the metallic substrates of growth graphene by the present invention, and is heating and curing, and PMMA and stone are conducive to
It is bonded closely between black alkene, prevents graphene cracked and fold.Then it obtains after metallic substrates having been etched with PMMA/
Second structure sheaf of graphene is cleaned as supporting layer, and to it, removes remaining metal particulate on graphene, it is ensured that
The cleaning of second structure sheaf, then while being shifted using the second structure sheaf as supporting layer to target graphene, are conducive to target graphite
The cleaning of alkene improves the transfer quality of target graphene, and graphene transfer quality is higher, shifts relative to it as supporting layer
The quality requirement of target graphene is also higher.It after the metal etch in third structure sheaf, is cleaned again, removes target
Remaining metal particulate on graphene, it is ensured that the cleaning of target graphene, to be conducive to the transfer quality of target graphene.
The 4th structure is placed on target substrate again and is heated, so that target graphene is come into full contact with target substrate, utilizes graphene
Van der Waals force between target graphene is less than the Van der Waals force between graphene and PMMA, can directly will be as supporting layer
Second structure sheaf is uncovered from target graphene, so that target graphene is transferred in target substrate.Transfer stone of the invention
Organic matter is not contacted with target graphene in the method for black alkene film, therefore target graphene does not have organic substance residues, and
And the present invention is less than the Van der Waals force between graphene and PMMA using the Van der Waals force between graphene and target graphene, obtains
The graphene film high to integrity degree effectively avoids and dissolves PMMA using organic solvent, cause the cracked pleat of graphene
The case where wrinkle.
It should be noted that graphene and target graphene are to grow to obtain by chemical vapour deposition technique in the present invention
, the two and indistinction.
Further, in preferred embodiments of the present invention, metallic substrates include copper in above-mentioned steps (1) and step (3)
Foil substrate, nickel foil substrate or lead foil substrate.
Further, in preferred embodiments of the present invention, the growth side of graphene in above-mentioned steps (1) and step (3)
Method is chemical vapour deposition technique.
Further, in preferred embodiments of the present invention, the solidification temperature in above-mentioned steps (1) is 120 DEG C -150 DEG C,
Curing time is 20min-60min.
Further, in preferred embodiments of the present invention, the etching liquid of above-mentioned steps (2) and step (4) etching use
For the ammonium persulfate of 0.5-1.5mol/L or the iron chloride of 0.5-1.5mol/L.
Further, in preferred embodiments of the present invention, above-mentioned steps (2) and step (4) cleaning step include: first to adopt
It is cleaned multiple times with the dilute hydrochloric acid that mass fraction is 5%-10%, then uses mass fraction for dilute hydroxide of 5%-10%
Sodium is cleaned multiple times, and is finally cleaned multiple times using deionized water.
Further, in preferred embodiments of the present invention, target substrate is silica substrate in above-mentioned steps (5).
Further, in preferred embodiments of the present invention, heating temperature is 80 DEG C -120 DEG C in above-mentioned steps (5), is added
The hot time is 2min-5min.
PMMA in the present invention is polymethyl methacrylate, and it is 2%-6% that the PMMA in step (1), which is mass fraction,
PMMA with using toluene as the mixed solution of organic solvent.
The invention has the following advantages:
1, PMMA is spin-coated on graphene as supporting layer come the graphene that diverts the aim, PMMA and target stone by the present invention
Black alkene is separated by graphene, is avoided target graphene and is in contact with PMMA, so as to avoid having on target graphene
Machine object residual.
2, Van der Waals force of the present invention between the graphene and target graphene of transfer is lower than between graphene and PMMA
Van der Waals force, therefore can and be easy the second structure sheaf with PMMA/ graphene is uncovered from target graphene so that
Target graphene can be completely transferred in target substrate, and the second structure sheaf can be repeatedly used as supporting layer.
3, the present invention also carries out cleaning process in metal etch, can remove gold remaining on graphene and target graphene
Metal particles object, it is ensured that the cleaning of graphene and target graphene, so that it is guaranteed that the cleanliness of target graphene and transfer quality.
4, the method for present invention transfer graphene film, it is easy to operate, graphene film after transfer its shift quality
High, cleanliness height, integrality are good and without organic substance residues, and the second structure sheaf with PMMA/ graphene can as supporting layer
It repeatedly uses.
Detailed description of the invention
In order to illustrate the technical solution of the embodiments of the present invention more clearly, below will be to needed in the embodiment attached
Figure is briefly described, it should be understood that the following drawings illustrates only certain embodiments of the present invention, therefore is not construed as pair
The restriction of range for those of ordinary skill in the art without creative efforts, can also be according to this
A little attached drawings obtain other relevant attached drawings.
Fig. 1 is the process schematic of transfer graphene film of the invention；
Fig. 2 is the optical picture for the target graphene film that the embodiment of the present invention 1 obtains；
Fig. 3 is the optical picture for the graphene film that reference examples of the invention obtain；
Wherein, 1-PMMA；2- graphene；3- metallic substrates；4- target graphene；5- target substrate.
Specific embodiment
With reference to embodiments and principles and features of the present invention are described in attached drawing, and example is served only for explaining this
Invention, is not intended to limit the scope of the present invention.The person that is not specified actual conditions in embodiment, according to normal conditions or manufacturer builds
The condition of view carries out.Reagents or instruments used without specified manufacturer is the conventional production that can be obtained by commercially available purchase
Product.It please refers to shown in Fig. 1, the method for transfer graphene film of the invention, comprising the following steps:
(1) PMMA is being grown into the metallic substrates for having graphene by chemical vapour deposition technique using spin-coating method uniform fold
On, after standing at room temperature and heating makes its film-forming, and being formed has PMMA/ graphene/metallic substrates first structure layer (figure
In 1/2/3 structure)；Wherein, metallic substrates include copper foil substrate, nickel foil substrate or lead foil substrate；Solidification temperature be 120 DEG C-
150 DEG C, curing time 20min-60min.
(2) metal etch in first structure layer is fallen, and is cleaned multiple times, obtain with PMMA/ graphene
Two structure sheafs (1/2 structure in Fig. 1)；Wherein, the etching liquid used is etched as the ammonium persulfate of 0.5-1.5mol/L or 0.5-
The iron chloride of 1.5mol/L；Cleaning step includes: that mass fraction is first used to be cleaned multiple times for the dilute hydrochloric acid of 5%-10%, so
It uses mass fraction to be cleaned multiple times for the dilute sodium hydroxide of 5%-10% afterwards, is finally carried out using deionized water repeatedly clear
It washes.
(3) the second structure sheaf is covered on to the metallic substrates by chemical vapour deposition technique new life with target graphene
On, being formed has PMMA/ graphene/target graphene/metallic substrates third structure sheaf (1/2/4/3 structure in Fig. 1)；Its
In, target substrate is silica substrate.
(4) metal etch in third structure sheaf is fallen, and is cleaned multiple times, obtained with PMMA/ graphene/target
The 4th structure sheaf (1/2/4 structure in Fig. 1) of graphene；Wherein, metallic substrates include copper foil substrate, nickel foil substrate or lead foil
Substrate；Wherein, the etching liquid used is etched as the ammonium persulfate of 0.5-1.5mol/L or the iron chloride of 0.5-1.5mol/L；Cleaning
Step includes: that mass fraction is first used to be cleaned multiple times for the dilute hydrochloric acid of 5%-10%, then uses mass fraction for 5%-
10% dilute sodium hydroxide is cleaned multiple times, and is finally cleaned multiple times using deionized water.
(5) (1/2/4/5 structure in Fig. 1) is heated after the 4th structure being placed in target substrate to it, by the second knot
Structure layer is uncovered from target graphene, and target graphene is transferred in target substrate；Wherein, heating temperature is 80 DEG C -120
DEG C, heating time 2min-5min.
PMMA in the present invention is polymethyl methacrylate, and it is 2%-6% that the PMMA in step (1), which is mass fraction,
PMMA with using toluene as the mixed solution of organic solvent.
Embodiment 1:
The method of the transfer graphene film of the present embodiment, comprising the following steps:
(1) PMMA is being grown to obtain the copper foil base of graphene by chemical vapour deposition technique using spin-coating method uniform fold
On bottom, after standing at room temperature and heating makes its film-forming, and being formed has PMMA/ graphene/copper foil substrate first structure layer；
Wherein, PMMA be mass fraction be 2% PMMA with using toluene as the mixed solution of organic solvent, solidification temperature be 120 DEG C, Gu
The change time is 20min.
(2) copper foil in first structure layer is etched away, and is cleaned multiple times, obtain with PMMA/ graphene
Two structure sheafs；(ammonium persulfate is alternatively at the chlorination of same concentration for the ammonium persulfate of 0.5mol/L for the etching liquid wherein used
Iron)；Cleaning step includes: that mass fraction is first used to be cleaned multiple times for 5% dilute hydrochloric acid, then use mass fraction for
5% dilute sodium hydroxide is cleaned multiple times, and is finally cleaned multiple times using deionized water.
(3) the second structure sheaf is covered on to the copper foil substrate by chemical vapour deposition technique new life with target graphene
On, being formed has PMMA/ graphene/target graphene/copper foil substrate third structure sheaf；
(4) copper foil in third structure sheaf is etched away, and is cleaned multiple times, obtained with PMMA/ graphene/target
4th structure sheaf of graphene；Wherein, the etching liquid used is ammonium persulfate (the replaceable Cheng Tongnong of ammonium persulfate of 0.5mol/L
The iron chloride of degree)；Cleaning step includes: that mass fraction is first used to be cleaned multiple times for 5% dilute hydrochloric acid, then uses quality
The dilute sodium hydroxide that score is 5% is cleaned multiple times, and is finally cleaned multiple times using deionized water.
(5) it is heated after the 4th structure being placed in silica substrate, by the second structure sheaf from target graphene
On uncover, target graphene is transferred in silica substrate；Wherein, heating temperature is 80 DEG C, heating time 5min.
Embodiment 2:
The method of the transfer graphene film of the present embodiment, comprising the following steps:
(1) PMMA is being grown to obtain the nickel foil base of graphene by chemical vapour deposition technique using spin-coating method uniform fold
On bottom, after standing at room temperature and heating makes its film-forming, forms the first structure layer with PMMA/ graphene/nickel foil substrate；
Wherein, PMMA be mass fraction be 4% PMMA with using toluene as the mixed solution of organic solvent, solidification temperature be 135 DEG C, Gu
The change time is 40min.
(2) nickel foil in first structure layer is etched away, and is cleaned multiple times, obtain with PMMA/ graphene
Two structure sheafs；The etching liquid wherein used is the ammonium persulfate of 1mol/L (ammonium persulfate is alternatively at the iron chloride of same concentration)；
Cleaning step includes: that mass fraction is first used to be cleaned multiple times for 7% dilute hydrochloric acid, then uses mass fraction for 7%
Dilute sodium hydroxide is cleaned multiple times, and is finally cleaned multiple times using deionized water.
(3) the second structure sheaf is covered on to the nickel foil substrate by chemical vapour deposition technique new life with target graphene
On, being formed has PMMA/ graphene/target graphene/nickel foil substrate third structure sheaf；
(4) nickel foil in third structure sheaf is etched away, and is cleaned multiple times, obtained with PMMA/ graphene/target
4th structure sheaf of graphene；Wherein, (ammonium persulfate is alternatively at same concentration for the ammonium persulfate of 1mol/L for the etching liquid used
Iron chloride)；Cleaning step includes: that mass fraction is first used to be cleaned multiple times for 7% dilute hydrochloric acid, then using quality point
Number is cleaned multiple times for 7% dilute sodium hydroxide, is finally cleaned multiple times using deionized water.
(5) it is heated after the 4th structure being placed in silica substrate, by the second structure sheaf from target graphene
On uncover, target graphene is transferred in silica substrate；Wherein, heating temperature is 100 DEG C, and heating time is
3.5min。
Embodiment 3:
The method of the transfer graphene film of the present embodiment, comprising the following steps:
(1) PMMA is being grown into the copper foil substrate for having graphene by chemical vapour deposition technique using spin-coating method uniform fold
On, after standing at room temperature and heating makes its film-forming, and being formed has PMMA/ graphene/copper foil substrate first structure layer；Its
In, PMMA is the PMMA that mass fraction is 6% and using toluene as the mixed solution of organic solvent, and solidification temperature is 150 DEG C, solidification
Time is 60min.
(2) copper foil in first structure layer is etched away, and is cleaned multiple times, obtain with PMMA/ graphene
Two structure sheafs；(ammonium persulfate is alternatively at the chlorination of same concentration for the ammonium persulfate of 1.5mol/L for the etching liquid wherein used
Iron)；Cleaning step includes: that mass fraction is first used to be cleaned multiple times for 10% dilute hydrochloric acid, then use mass fraction for
10% dilute sodium hydroxide is cleaned multiple times, and is finally cleaned multiple times using deionized water.
(3) the second structure sheaf is covered on to the copper foil substrate by chemical vapour deposition technique new life with target graphene
On, being formed has PMMA/ graphene/target graphene/copper foil substrate third structure sheaf；
(4) copper foil in third structure sheaf is etched away, and is cleaned multiple times, obtained with PMMA/ graphene/target
4th structure sheaf of graphene；Wherein, the etching liquid used is ammonium persulfate (the replaceable Cheng Tongnong of ammonium persulfate of 1.5mol/L
The iron chloride of degree)；Cleaning step includes: that mass fraction is first used to be cleaned multiple times for 10% dilute hydrochloric acid, then uses matter
The dilute sodium hydroxide that amount score is 10% is cleaned multiple times, and is finally cleaned multiple times using deionized water.
(5) it is heated after the 4th structure being placed in silica substrate, by the second structure sheaf from target graphene
On uncover, target graphene is transferred in silica substrate；Wherein, heating temperature is 120 DEG C, heating time 2min.
Reference examples:
The method of the transfer graphene film of this reference examples, comprising the following steps:
(1) PMMA is being grown to obtain the copper foil base of graphene by chemical vapour deposition technique using spin-coating method uniform fold
On bottom, after standing at room temperature and heating makes its film-forming, forms PMMA/ graphene/copper foil substrate；Wherein, PMMA is quality
The PMMA that score is 2% is with using toluene as the mixed solution of organic solvent, and solidification temperature is 120 DEG C, curing time 20min.
(2) copper foil in PMMA/ graphene/copper foil substrate is etched away, and PMMA is dissolved using acetone organic solvent, most
Graphene film is obtained eventually.Wherein, the etching liquid used is the ammonium persulfate of 0.5mol/L.
By the graphene of embodiment 1 and reference examples being prepared into film row optical detection, as shown in Figures 2 and 3.
It can be seen from the figure that graphene film its clean surface, the complete good and quality that the present embodiment 1 shifts are high, and
There are more organic substance residues on its surface of the graphene film that reference examples shift.
The foregoing is merely presently preferred embodiments of the present invention, is not intended to limit the invention, it is all in spirit of the invention and
Within principle, any modification, equivalent replacement, improvement and so on be should all be included in the protection scope of the present invention.
Claims (8)
1. a kind of method for shifting graphene film, which comprises the following steps:
(1) by PMMA using spin-coating method uniform fold growth have graphene metallic substrates on, at room temperature stand after and heat
Make its film-forming, being formed has PMMA/ graphene/metallic substrates first structure layer；
(2) metal etch in the first structure layer is fallen, and is cleaned multiple times, obtain with PMMA/ graphene
Two structure sheafs；
(3) second structure sheaf is covered in the newborn metallic substrates with target graphene, being formed has PMMA/ graphite
Alkene/target graphene/metallic substrates third structure sheaf；
(4) metal etch in the third structure sheaf is fallen, and is cleaned multiple times, obtained with PMMA/ graphene/target
4th structure sheaf of graphene；
(5) it is heated after the 4th structure being placed in target substrate, by second structure sheaf from target graphene
On uncover, target graphene is transferred in target substrate.
2. the method for transfer graphene film according to claim 1, which is characterized in that golden in step (1) and step (3)
Belonging to substrate includes copper foil substrate, nickel foil substrate or lead foil substrate.
3. the method for transfer graphene film according to claim 1, which is characterized in that stone in step (1) and step (3)
The growing method of black alkene is chemical vapour deposition technique.
4. the method for transfer graphene film according to claim 1-3, which is characterized in that in step (1)
Solidification temperature is 120 DEG C -150 DEG C, curing time 20min-60min.
5. the method for transfer graphene film according to claim 4, which is characterized in that step (2) and step (4) etching
The etching liquid used is the ammonium persulfate of 0.5mol/L-1.5mol/L or the iron chloride of 0.5mol/L-1.5mol/L.
6. the method for transfer graphene film according to claim 4, which is characterized in that step (2) and step (4) cleaning
Step includes: that mass fraction is first used to be cleaned multiple times for the dilute hydrochloric acid of 5%-10%, then uses mass fraction for 5%-
10% dilute sodium hydroxide is cleaned multiple times, and is finally cleaned multiple times using deionized water.
7. the method for transfer graphene film according to claim 4, which is characterized in that target substrate is in step (5)
Silica substrate.
8. according to the method for the described in any item transfer graphene films of claim 5-7, which is characterized in that add in step (5)
Hot temperature is 80 DEG C -120 DEG C, heating time 2min-5min.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113184835A (en) * | 2021-05-12 | 2021-07-30 | 电子科技大学 | Method for transferring graphene through pressure-assisted evaporation |
| CN114203326A (en) * | 2021-12-13 | 2022-03-18 | 中国核动力研究设计院 | Graphene-packaged ultrathin nickel-63 radiation source film and preparation method and application thereof |
| CN115611272A (en) * | 2021-07-13 | 2023-01-17 | 北京石墨烯研究院 | Transfer method of graphene film |
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