CN102222607A - Transfer method special for graphene thin film prepared by CVD (chemical vapor deposition) method - Google Patents
Transfer method special for graphene thin film prepared by CVD (chemical vapor deposition) method Download PDFInfo
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- CN102222607A CN102222607A CN2011101300368A CN201110130036A CN102222607A CN 102222607 A CN102222607 A CN 102222607A CN 2011101300368 A CN2011101300368 A CN 2011101300368A CN 201110130036 A CN201110130036 A CN 201110130036A CN 102222607 A CN102222607 A CN 102222607A
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Abstract
The invention discloses a transfer method special for a graphene thin film prepared by a CVD (chemical vapor deposition) method, belonging to the technical field of novel materials and semi-conductor process. The method comprises the following steps: spin-coating organic colloid or a high polymer used as a supporting layer on the surface of the graphene thin film; hardening the graphene thin film spin-coated with the organic colloid or high polymer; immersing the hardened graphene thin film and a substrate at the bottom in deionized water to separate a metal layer from a SiO2 layer; putting the separated supporting layer/ graphene thin film/ metal layer in a chemical corrosion liquid to remove the metal layer; transferring the supporting layer/ the graphene thin film to a target substrate, and heating the so that the graphene thin film is closely attached to the target substrate; and removing the supporting layer to finally realize the transfer of the graphene thin film. Compared with the traditional method that the BOE (buffered oxide etch) solution is utilized to corrode the SiO2 layer, the transfer method disclosed by the invention can avoid the corrosion of the BOE solution on the metal layer and also can prevent the pollution to the graphene thin film.
Description
Technical field
The present invention relates to new material and semiconductor process techniques field, particularly a kind of transfer method of the wafer scale graphene film at chemical gas-phase deposition method preparation.
Background technology
Graphene is the monatomic graphite crystal film of the cellular two-dimensional structure of hexagonal lattice that is made of carbon atom, it is except the character with CNT, also have and enrich very much and novel physical, chemical property: its thermal conductivity height, electronics and hole mobility are roughly suitable, and theoretical expectation is up to 2x10
5Cm
2/ V.s is 100 times of the electron mobilities of Si, be 300 times of hole mobility, and electron mobility and hole mobility is temperature independent, and two-dimensional electron gas density reaches 10
13/ cm
2, saturation drift velocity reaches 10
8Cm/s is 6~7 times of Si, and its Fermi's speed is 1/300 of the light velocity.Therefore, Graphene is considered to advance the material and the technology of the tool potentiality of microelectric technique future development.
Summary of the invention
In order to address the above problem, to the present invention proposes a kind of CVD (Chemical Vapor Deposition) method of utilizing and realize the method that the high-quality of wafer scale Graphene from metallic film to any target substrate shifts.
To achieve these goals, the transfer method of the graphene film at CVD method preparation provided by the invention, the graphene film of described CVD method preparation comprises graphene film layer/metal level/SiO
2Layer/Si layer may further comprise the steps:
Be coated with organic colloid or high molecular polymer as supporting layer on described graphene film surface;
The described graphene film that has been coated with organic colloid or high molecular polymer is carried out post bake;
Graphene film after described post bake finished is immersed in the deionized water together with bottom substrate, makes described metal level and described SiO
2Layer separates;
Supporting layer/graphene film after the described separation/metal level is put into chemical corrosion liquid remove metal level;
Described supporting layer/graphene film is transferred on the target substrate, and heating makes described graphene film be close to described target substrate;
Remove described supporting layer, realize the transfer of described graphene film.
As preferably, described high molecular polymer is a kind of among dimethyl silicone polymer, polymethyl methacrylate, the positive glue 9912 of photoetching, the photoresist AZ5206.
As preferably, described post bake process is to carry out under 100 ℃ ~ 185 ℃ temperature range.
As preferably, to described metal level and SiO
2Layer carries out adding ultrasonic in the process.
As preferably, described chemical corrosion liquid is HNO
3, described HNO
3Concentration be 0.1M or 0.25M.
As preferably, described chemical corrosion liquid is FeCl
3Solution or Fe (NO
3)
3Solution, described FeCl
3Solution or Fe (NO
3)
3The concentration of solution is respectively 0.5M or 1M.
As preferably, described target substrate is SiO
2A kind of in substrate, glass substrate, metal substrate and the PDMS substrate.
As preferably, the step of removing described supporting layer may further comprise the steps:
Use the MOS grade acetone earlier, the back uses MOS level ethanol that described graphene film surface colloid is removed;
The described graphene film that is removed surperficial colloid put into volume ratio can be provided is 1: 1 hydrogen and ar gas environment, in 400 ℃ the high temperature cavity, the residual colloid on described graphene film surface is removed in annealing.
The 3rd step of the transfer method of the graphene film at CVD method preparation provided by the invention utilizes the power of mediating of deionized water directly to make metal level and SiO
2Layer separates, with traditional use BOE solution corrosion SiO
2The method of layer is compared, and has avoided the corrosion of BOE solution to metal level, has also avoided the pollution to graphene film simultaneously.
Description of drawings
The employing CVD method preparation that Fig. 1 provides for the embodiment of the invention graphene film meron structure chart;
The process chart that Fig. 2 provides for the embodiment of the invention at the transfer method of the graphene film of CVD method preparation.
Embodiment
In order to understand the present invention in depth, the present invention is described in detail below in conjunction with drawings and the specific embodiments.
Embodiment:
Accompanying drawing 1 is for adopting the graphene film meron structure of CVD method preparation, and the graphene film of the CVD method preparation that present embodiment provides comprises graphene film layer/metal Ni layer/SiO
2Layer/Si layer.
The process chart at the transfer method of the graphene film of CVD method preparation that accompanying drawing 2 provides for the embodiment of the invention, present embodiment is by SiO with the graphene film of preparation on metallic nickel
2/ Si substrate-transfer is on target substrate.
Concrete steps are as follows:
The first step is coated with organic colloid or high molecular polymer as supporting layer on the graphene film surface.Present embodiment is to be coated with the positive glue of photoetching 9912 on the graphene film surface as supporting layer, and the process that is coated with uses sol evenning machine to finish, and is coated with rotating speed: 4 seconds 400rpm of preceding commentaries on classics, and 60 seconds 5500rpm are changeed in the back, and the thickness of the positive glue of photoetching is 1.1 μ m.
In second step, the graphene film that has been coated with organic colloid or high molecular polymer is carried out post bake.Present embodiment is to be placed on 115 ℃ the hot plate post bake 2min with being coated with Graphene substrate as the positive glue 9912 of the photoetching of supporting layer.
The 3rd goes on foot, and the graphene film after post bake is finished is immersed in the deionized water together with bottom substrate, makes metal level and SiO
2Layer separates.Present embodiment is that the Graphene substrate that post bake is mutual is put into the 100mL deionized water, add ultrasonic, to promote metal Ni layer and SiO
2Layer separates, after 15 minutes, and positive glue 9912/ graphene film of photoetching/Ni metal level and SiO
2/ Si layer separates, and positive glue 9912/ graphene film of photoetching/Ni metal level floats on the water surface.
In the 4th step, the supporting layer/graphene film/metal level after separating is put into chemical corrosion liquid remove metal level.Present embodiment is with 8.125g FeCl
3Powder is slowly put into above-mentioned deionized water, makes it be mixed with the FeCl of 0.5M
3Solution in this course, need make positive glue 9912/ graphene film of photoetching/Ni metal level be in the liquid environment always, produces fold to avoid it after running into air, after the Ni metal is corroded fully after 1 minute, with SiO
2/ Si layer shifts out, and only stays the positive glue 9912/ graphene film layer of photoetching at FeCl
3Solution surface is floating.Chemical corrosion liquid can also be mixed with 1MFeCl
3Fe (the NO of solution or 0.5M
3)
3Fe (the NO of solution or 1M
3)
3Solution.In addition, if graphene film is used to study the electromagnetic transmission characteristic, chemical corrosion liquid can also be mixed with the HNO that concentration is 0.1M or 0.25M
3
The 5th step, supporting layer/graphene film to be transferred on the target substrate, heating makes graphene film be close to target substrate.Present embodiment is to dilute above-mentioned FeCl with deionized water
3Solution in this process, need make the positive glue 9912/ graphene film layer of photoetching be in the liquid environment always, produces fold to avoid it after running into air.The target substrate of present embodiment is selected SiO cheaply
2/ Si substrate, wherein, SiO
2Layer thickness is 100nm, SiO
2Adopt thermal oxidation process to be grown in the Si surface, with SiO
2/ Si substrate is put in the deionized water, makes positive glue 9912/ graphene film layer and the SiO of photoetching
2/ Si substrate is attached together the back and breaks away from aqueous environment, with positive glue 9912/ graphene film of photoetching/SiO
2/ Si puts on 100 ℃ of hot plates and dries by the fire 10s, makes graphene film and target substrate SiO
2/ Si is close to.
The 6th step, remove supporting layer, realize the transfer of graphene film.Present embodiment is with positive glue 9912/ graphene film of photoetching/SiO
2/ Si successively puts into MOS grade acetone and ethanol, and the positive glue 9912 of photoetching is removed, but still there is the positive glue 9912 of residual photoetching on the graphene film surface, with graphene film/SiO
2/ Si puts in the high temperature cavity (feed 1900sccm hydrogen and 1700sccm argon gas, cavity temperature is 400 ℃), anneals 1 hour, and the positive glue 9912 of the residual photoetching on graphene film surface is removed, and graphene film is successfully transferred to target substrate SiO
2On/the Si.
When using the transfer method of the graphene film at CVD method preparation provided by the invention since the 3rd step utilize the power of mediating of deionized water directly to make metal level and SiO
2Layer separates, with traditional use BOE solution corrosion SiO
2The method of layer is compared, and has avoided the corrosion of BOE solution to metal level, has also avoided the pollution to graphene film simultaneously.
The transfer method of the graphene film at CVD method preparation provided by the invention also has conveniently, low cost and other advantages, can realize the high-quality transfer of wafer scale size graphene film.
In addition, because the 3rd the basic step going on foot of removing of the transfer method of the graphene film at CVD method preparation provided by the invention belongs to common method, compatible good with conventional method.
Above-described embodiment; purpose of the present invention, technical scheme and beneficial effect are further described; institute is understood that; the above only is the specific embodiment of the present invention; be not limited to the present invention; within the spirit and principles in the present invention all, any modification of being made, be equal to replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (8)
1. transfer method at the graphene film of CVD method preparation, the graphene film of described CVD method preparation comprises graphene film layer/metal level/SiO
2Layer/Si layer is characterized in that: may further comprise the steps:
Be coated with organic colloid or high molecular polymer as supporting layer on described graphene film surface;
The described graphene film that has been coated with organic colloid or high molecular polymer is carried out post bake;
Graphene film after described post bake finished is immersed in the deionized water together with bottom substrate, makes described metal level and described SiO
2Layer separates;
Supporting layer/graphene film after the described separation/metal level is put into chemical corrosion liquid remove metal level;
Described supporting layer/graphene film is transferred on the target substrate, and heating makes described graphene film be close to described target substrate;
Remove described supporting layer, realize the transfer of described graphene film.
2. the transfer method of the graphene film at CVD method preparation according to claim 1 is characterized in that: described high molecular polymer is a kind of among dimethyl silicone polymer, polymethyl methacrylate, the positive glue 9912 of photoetching, the photoresist AZ5206.
3. the transfer method of the graphene film at CVD method preparation according to claim 1, it is characterized in that: described post bake process is to carry out under 100 ℃ ~ 185 ℃ temperature range.
4. the transfer method of the graphene film at CVD method preparation according to claim 1 is characterized in that: to described metal level and SiO
2Layer carries out adding ultrasonic in the process.
5. the transfer method of the graphene film at CVD method preparation according to claim 1, it is characterized in that: described chemical corrosion liquid is HNO
3, described HNO
3Concentration be 0.1M or 0.25M.
6. the transfer method of the graphene film at CVD method preparation according to claim 1, it is characterized in that: described chemical corrosion liquid is FeCl
3Solution or Fe (NO
3)
3Solution, described FeCl
3Solution or Fe (NO
3)
3The concentration of solution is respectively 0.5M or 1M.
7. the transfer method of the graphene film at CVD method preparation according to claim 1, it is characterized in that: described target substrate is SiO
2A kind of in substrate, glass substrate, metal substrate and the PDMS substrate.
8. the transfer method of the graphene film at CVD method preparation according to claim 1, it is characterized in that: the step of removing described supporting layer may further comprise the steps:
Use the MOS grade acetone earlier, the back uses MOS level ethanol that described graphene film surface colloid is removed;
The described graphene film that is removed surperficial colloid put into volume ratio can be provided is 1: 1 hydrogen and ar gas environment, in 400 ℃ the high temperature cavity, the residual colloid on described graphene film surface is removed in annealing.
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Application publication date: 20111019 |