CN104150476B - The not damaged transfer method of process for preparing graphenes by chemical vapour deposition - Google Patents
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Abstract
The invention discloses the not damaged transfer method of a kind of process for preparing graphenes by chemical vapour deposition, including: step 1, spin coating organic solvent coating on graphene film；Step 2, metal etch solution dissolve metallic substrates；Step 3, transfer graphene in target substrate；Step 4, drip a small amount of described PMMA solution to form new PMMA film；Step 5, processing graphene film with acetone steam successively, acetone soln soaks graphene film, more described graphene film does annealing 3～5h to remove organic solvent clad.The method that the present invention provides is simple, efficient, economical, it is possible to being cleaned, large-area transfer on target base by graphene film, the graphene film shifted can keep complete architectural feature.
Description
Technical field
The invention belongs to materials science field, use chemical vapour deposition technique to prepare particularly to one
The not damaged transfer method of Graphene.
Background technology
Graphene (Graphene) be a kind of be the cancellated carbonaceous of hexagon by monolayer carbon atomic arrangement
Novel film material.In single-layer graphene, electronics and hole (Hole) carrier mobility are expected in room temperature
It is up to down 100 times i.e. 200,000 cm of silicon (Si)2/ Vs, can tolerate 100,000,000～200,000,000 A/cm2Electric current
Density, this is about 100 times of copper dosis tolerata.The Graphene of monolayer has the light of up to 97.7% simultaneously
Transmitance, this is not only for visible ray, also includes major part infrared ray.Therefore, for being desirable with
For the solaode that infrared ray generates electricity, Graphene is expected to become epoch-making nesa coating.With
The ITO being unsuitable for bending compares, and is also equipped with flexible higher advantage.Graphene is as commonly using at present
ITO substitution material, for touch panel, flexible liquid crystal panel, solaode and organic EL shine
The expectation enjoying people such as bright.It addition, utilize the high carrier mobility of Graphene and the high migration velocity can
To make the transistor of THz frequency, utilize the saturated absorption character of Graphene can make femto-second laser.
Graphene due to its excellence electric conductivity, light transmission, conductivity of heat and mechanical property and at electronics, optics etc.
Many fields illustrate huge potential using value.Can prepare large area, low cost Graphene thin
Film is the precondition realizing the potential application of Graphene.Chemical gaseous phase deposition (CVD) method due to composition and
The controllability of environment has become to be prepared high-quality big size graphene and realizes the most effective of its commercial application
Method, the method is divided into preparation and two processes of transfer of Graphene, and the former has tended to ripe, and CVD
Graphene film prepared by method generally selects metallic substrates, but Graphene is fabricated to various device and then needs
Want the Graphene of different base.Prior art generally uses substrate etching method, in substrate etching process,
Need to drip PMMA solution on graphene film, and PMMA solution to affect follow-up Graphene thin
The performance of the device of film production, therefore, removes the PMMA solution on graphene film also the most up hill and dale
The complete structure of graphene film will not be destroyed, be the key factor realizing not damaged transfer graphene film.
In prior art, approach in following 3 is generally had to remove PMMA: the approach of graphenic surface residual
One, graphene film is soaked in acetone soln 24h；Approach two, first process graphite with acetone steam
Alkene thin film, the more described graphene film processed is immersed acetone soln 24h；Approach three, by described
The graphene film that step 4 obtains does annealing 3～5h.
Therefore, how the Graphene especially large scale Graphene not damaged grown on the metallic substrate is turned
Move on in target substrate, be still a huge challenge, be the key that can realize Graphene commercial application.
Summary of the invention
Based on the problems referred to above, the invention provides the not damaged of a kind of process for preparing graphenes by chemical vapour deposition
Transfer method, the method is molten by spin coating organic solvent coating on graphene film, metal etch solution
Solve metallic substrates, transfer graphene in target substrate, remove organic solvent clad again, accurately control
Make the technological parameter of each process, it is achieved the not damaged transfer of Graphene, wherein remove organic solvent clad
It is the key obtaining high purity graphite alkene thin film, this case processes graphene film with acetone steam successively,
Acetone soln soaks graphene film, then makes annealing treatment described graphene film, obtained graphite
Alkene film surface is totally more a lot of than the graphene film without annealing, and also reduces Graphene
Thin film crack and the density of crackle.And the method is simple, efficient, economical, it is possible to by graphene film
Cleaning, large-area transferring on target base, the graphene film shifted can keep complete knot
Structure feature.
For achieving the above object, the present invention is achieved through the following technical solutions:
A kind of not damaged transfer method of process for preparing graphenes by chemical vapour deposition, wherein, including:
Step 1, growth has the metallic substrates of graphene film be placed on sol evenning machine, have graphite in growth
The Copper Foil upper surface drop coating polymetylmethacrylate organic solvent coating of alkene, starts sol evenning machine,
Make PMMA uniform coated graphite alkene thin film, then metallic substrates is placed on warm table, dry PMMA
Solvent；
Step 2, the metallic substrates scribbling PMMA solvent described step 1 obtained put into metal etch
In solution, remove metallic substrates；
Step 3, by using target substrate that graphene film is transferred to the beaker equipped with deionized water,
Rinsing 10～15min at normal temperatures, then with target substrate, graphene film is picked up, it is placed on warm table baking
Dry, remove the moisture between graphene film and graphene film and target substrate；
Step 4, drip a small amount of described PMMA solution on graphene film surface that described step 3 obtains,
The PMMA film being gathered in before being allowed on described graphene film is dissolved, and forms new PMMA film；
Step 5, process graphene film with acetone steam, the described graphene film that then will process
Immerse the acetone soln 0.5～1h PMMA solution with removal graphene film surface, then to described graphite
Alkene thin film does annealing 3～5h.
Preferably, the not damaged transfer method of described process for preparing graphenes by chemical vapour deposition, wherein,
Described metallic substrates is can be with the metal of chemical gaseous phase depositing process catalytic growth graphene film.
Preferably, the not damaged transfer method of described process for preparing graphenes by chemical vapour deposition, wherein,
Described metallic substrates is Copper Foil, nickel foil, copper film, nickel film or corronil.
Preferably, the not damaged transfer method of described process for preparing graphenes by chemical vapour deposition, wherein,
Described metal etch solution is FeCl3Solution, Fe (NO3)3Solution, Fe2(SO4)3Solution, solution concentration
Scope is 0.5～2mol/L.
Preferably, the not damaged transfer method of described process for preparing graphenes by chemical vapour deposition, wherein,
In described step 2, metallic substrates soaks 15～20min in metal etch solution.
Preferably, the not damaged transfer method of described process for preparing graphenes by chemical vapour deposition, wherein,
In described step 5, the time of acetone steam process graphene film is 10～20min.
Preferably, the not damaged transfer method of described process for preparing graphenes by chemical vapour deposition, wherein,
Described target substrate is the one in semiconductor base, Organic substance substrate.
The not damaged transfer method of a kind of process for preparing graphenes by chemical vapour deposition that the present invention provides, it has
Benefit effect includes: dissolve gold by spin coating organic solvent coating on graphene film, metal etch solution
Belong to substrate, transfer graphene in target substrate, remove organic solvent clad again, accurately control each
The technological parameter of process, it is achieved the not damaged transfer of Graphene.And the method is simple, efficient, economical,
Graphene film can be cleaned, large-area transfer on target base, the graphene film shifted
Can keep complete architectural feature, and obtained graphene film surface is very clean, Graphene is thin
The density of film surface crack and crackle is low.
Detailed description of the invention
Below in conjunction with detailed description of the invention, the present invention is described in further detail, to make art technology
Personnel can implement according to this with reference to description word.
A kind of not damaged transfer method of process for preparing graphenes by chemical vapour deposition, wherein, including:
Step 1, growth has the metallic substrates of graphene film be placed on sol evenning machine, have graphite in growth
The Copper Foil upper surface drop coating polymetylmethacrylate organic solvent coating of alkene, starts sol evenning machine,
Make PMMA uniform coated graphite alkene thin film, then metallic substrates is placed on warm table, dry PMMA
Solvent, described metallic substrates selects Copper Foil, nickel foil, copper film, nickel film or corronil；
Step 2, the metallic substrates scribbling PMMA solvent described step 1 obtained put into metal etch
In solution, soaking 15～20min, remove metallic substrates, described metal etch solution is FeCl3Solution,
Fe(NO3)3Solution, Fe2(SO4)3Solution, solution concentration scope is 0.5～2mol/L；
Step 3, by using target substrate that graphene film is transferred to the beaker equipped with deionized water,
Rinsing 10～15min at normal temperatures, then with target substrate, graphene film is picked up, it is placed on warm table baking
Dry, remove the moisture between graphene film and graphene film and target substrate；
Step 4, drip a small amount of described PMMA solution on graphene film surface that described step 3 obtains,
The PMMA film being gathered in before being allowed on described graphene film is dissolved, and forms new PMMA film；
Step 5, processing graphene film with acetone steam, the process time is 10～20min, then will at
The described graphene film managed immerses acetone soln 0.5～1h to remove graphene film surface
PMMA solution, more described graphene film is done annealing 3～5h, wherein, target substrate in this case
Use the one in semiconductor base, Organic substance substrate.
Although by the method forming PMMA film on graphene film surface in this case, reducing Graphene
Thin film crack and the density of crackle, but PMMA adhesion is relatively strong, so removing with acetone
Before PMMA, then PMMA film is made to dissolve at the graphene film surface a small amount of PMMA solution of dropping,
Form new PMMA film, optimize the mechanical stress on graphene film surface, then by thin for described Graphene
Film immerses acetone soln 0.5～1h to remove the PMMA solution on graphene film surface.But, even if
By destroying the technical improvement method of the PMMA film on graphene film, the surface of graphene film still has
Certain PMMA thin film exists, and the performance that the device of follow-up preparation obtains also can be affected.For research
The most preferably remove the PMMA of residual, the described graphene film after acetone soln soaks is moved back
Fire processes, and the graphenic surface obtained is more a lot of with the graphenic surface of acetone solution than only.
Embodiment
The not damaged transfer method of a kind of process for preparing graphenes by chemical vapour deposition, it is by following technique stream
Cheng Shixian, including:
Step 1, growth has the Copper Foil substrate of graphene film be placed on sol evenning machine, have graphite in growth
The Copper Foil upper surface drop coating polymetylmethacrylate organic solvent coating of alkene, starts sol evenning machine,
Make PMMA uniform coated graphite alkene thin film, then Copper Foil substrate is placed on warm table, dry PMMA
Solvent；
FeCl is put in step 2, the Copper Foil substrate scribbling PMMA solvent described step 1 obtained3Molten
In liquid, soaking 20min, remove Copper Foil substrate, solution concentration scope is 1.5mol/L；
Step 3, by using organosilicon substrate that graphene film is transferred to the beaker equipped with deionized water,
Rinse 15min at normal temperatures, then with organosilicon substrate, graphene film is picked up, be placed on warm table baking
Dry, remove the moisture between graphene film and graphene film and organosilicon substrate；
Step 4, drip a small amount of described PMMA solution on graphene film surface that described step 3 obtains,
The PMMA film being gathered in before being allowed on described graphene film is dissolved, and forms new PMMA film；
Step 5, processing graphene film with acetone steam, the process time is 20min, then will process
Described graphene film immerse acetone soln 1h with remove graphene film surface PMMA solution,
Described graphene film is annealing 3h again.
The present embodiment and tri-kinds of approach phases of PMMA of process graphene film remained on surface in prior art
Ratio, the graphene film surface that the present embodiment obtains is the cleanest, uses the graphite that the present embodiment obtains
The device performance that alkene thin film makes is the most optimum.
Although embodiment of the present invention are disclosed as above, but it is not restricted to description and embodiment party
Listed utilization in formula, it can be applied to various applicable the field of the invention completely, for being familiar with ability
For the personnel in territory, be easily achieved other amendment, therefore without departing substantially from claim and etc. homotype
Enclosing under limited general concept, the present invention is not limited to specific details and shown here as the reality with description
Execute example.
Claims (5)
1. the not damaged transfer method of a process for preparing graphenes by chemical vapour deposition, it is characterised in that bag
Include:
Step 1, growth has the Copper Foil of graphene film be placed on sol evenning machine, have Graphene in growth
Copper Foil upper surface drop coating polymetylmethacrylate organic solvent coating, starts sol evenning machine, makes
PMMA uniform coated graphite alkene thin film, then Copper Foil is placed on warm table, dry PMMA solvent；
Metal etch solution put into by step 2, the Copper Foil scribbling PMMA solvent described step 1 obtained
In, remove Copper Foil；
Step 3, by using target substrate that graphene film is transferred to the beaker equipped with deionized water,
Rinsing 10～15min at normal temperatures, then by target substrate, graphene film is picked up, it is placed on warm table baking
Dry, remove the moisture between graphene film and graphene film and target substrate；
Step 4, drip a small amount of described PMMA on graphene film surface that described step 3 obtains organic
Solvent, the PMMA film being gathered in before being allowed on described graphene film is dissolved, is formed new PMMA
Film；
Step 5, with acetone steam process graphene film 10～20min, the described stone that then will process
Ink alkene thin film immerses the acetone soln 0.5～1h PMMA organic solvent with removal graphene film surface,
Described graphene film is done annealing 3～5h again.
2. the not damaged transfer method of process for preparing graphenes by chemical vapour deposition as claimed in claim 1,
It is characterized in that, described Copper Foil is can be with the Copper Foil of chemical gaseous phase depositing process catalytic growth graphene film.
3. the not damaged transfer method of process for preparing graphenes by chemical vapour deposition as claimed in claim 1,
It is characterized in that, described metal etch solution is FeCl3Solution, Fe (NO3)3Solution, Fe2(SO4)3Solution,
Solution concentration scope is 0.5～2mol/L.
4. the not damaged transfer method of process for preparing graphenes by chemical vapour deposition as claimed in claim 1,
It is characterized in that, in described step 2, Copper Foil soaks 15～20min in metal etch solution.
5. the not damaged transfer method of process for preparing graphenes by chemical vapour deposition as claimed in claim 1,
It is characterized in that, described target substrate is Organic substance substrate.
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