WO2013023547A1 - 图案化石墨烯薄膜的制备方法 - Google Patents
图案化石墨烯薄膜的制备方法 Download PDFInfo
- Publication number
- WO2013023547A1 WO2013023547A1 PCT/CN2012/079873 CN2012079873W WO2013023547A1 WO 2013023547 A1 WO2013023547 A1 WO 2013023547A1 CN 2012079873 W CN2012079873 W CN 2012079873W WO 2013023547 A1 WO2013023547 A1 WO 2013023547A1
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- WO
- WIPO (PCT)
- Prior art keywords
- photoresist
- film
- graphene
- substrate
- electron beam
- Prior art date
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Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D5/00—Processes for applying liquids or other fluent materials to surfaces to obtain special surface effects, finishes or structures
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/02—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition
- C23C18/06—Coating on selected surface areas, e.g. using masks
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
-
- 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
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/184—Preparation
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/02—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition
- C23C18/12—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material
- C23C18/1204—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material inorganic material, e.g. non-oxide and non-metallic such as sulfides, nitrides based compounds
- C23C18/1208—Oxides, e.g. ceramics
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/02—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition
- C23C18/12—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material
- C23C18/125—Process of deposition of the inorganic material
- C23C18/1279—Process of deposition of the inorganic material performed under reactive atmosphere, e.g. oxidising or reducing atmospheres
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/02—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition
- C23C18/12—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material
- C23C18/125—Process of deposition of the inorganic material
- C23C18/1295—Process of deposition of the inorganic material with after-treatment of the deposited inorganic material
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- G—PHYSICS
- G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
- G03F—PHOTOMECHANICAL PRODUCTION OF TEXTURED OR PATTERNED SURFACES, e.g. FOR PRINTING, FOR PROCESSING OF SEMICONDUCTOR DEVICES; MATERIALS THEREFOR; ORIGINALS THEREFOR; APPARATUS SPECIALLY ADAPTED THEREFOR
- G03F7/00—Photomechanical, e.g. photolithographic, production of textured or patterned surfaces, e.g. printing surfaces; Materials therefor, e.g. comprising photoresists; Apparatus specially adapted therefor
- G03F7/26—Processing photosensitive materials; Apparatus therefor
- G03F7/40—Treatment after imagewise removal, e.g. baking
-
- G—PHYSICS
- G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
- G03F—PHOTOMECHANICAL PRODUCTION OF TEXTURED OR PATTERNED SURFACES, e.g. FOR PRINTING, FOR PROCESSING OF SEMICONDUCTOR DEVICES; MATERIALS THEREFOR; ORIGINALS THEREFOR; APPARATUS SPECIALLY ADAPTED THEREFOR
- G03F7/00—Photomechanical, e.g. photolithographic, production of textured or patterned surfaces, e.g. printing surfaces; Materials therefor, e.g. comprising photoresists; Apparatus specially adapted therefor
- G03F7/26—Processing photosensitive materials; Apparatus therefor
- G03F7/42—Stripping or agents therefor
- G03F7/422—Stripping or agents therefor using liquids only
Definitions
- Embodiments of the invention relate to a method of making a patterned graphene film. Background technique
- Graphene is a two-dimensional crystal composed of carbon atoms arranged in a honeycomb shape. Due to its quantum transport properties, high conductivity, mobility, and transmittance, graphene and related devices have become a research hotspot in the fields of physics, chemistry, biology, and materials science. To date, a variety of devices have been prepared with graphene as a basic functional unit, including field effect transistors, solar cells, nanogenerators, sensors, and the like.
- graphene can be obtained by various methods such as mechanical stripping, chemical vapor deposition, thermal decomposition of SiC substrates, and chemical methods.
- the mechanical peeling method is a method of repeatedly depositing and peeling an adhesive tape on graphite to prepare graphene. This method is difficult to control the size and number of layers of the graphene sheets obtained, and only a few millimeters of graphene sheets can be obtained.
- the chemical vapor deposition method is a technique in which a carbon source such as decane is heated to about 1000 ° C in a vacuum vessel to be decomposed, and then a graphene film is formed on a metal foil such as Ni or Cu.
- the thermal decomposition method of the SiC substrate is a process in which the SiC substrate is heated to about 1300 ° C to remove Si on the surface, and the remaining C spontaneously recombines to form a graphene sheet.
- the above preparation method is difficult to obtain a large-area graphene film, or the preparation temperature is high and the cost is high, which is disadvantageous for large-scale industrial production of graphene film.
- the chemical method first oxidizes the graphite powder, then dissolves the oxidized graphite powder into the solution, and then coats the substrate with a thin layer of solution and then reduces it.
- the method has the advantages of simple process, low temperature and low cost, and can produce a large-area graphene film, which can realize large-scale industrial production of graphene film.
- Graphene-based electronic devices usually require patterned graphene films.
- graphene film patterning techniques are as follows: 1) Firstly, a patterned catalyst is obtained, thereby growing patterned graphene. Transfer again. This method does not accurately position the patterned graphene onto the device substrate. 2) Transfer a large area of graphene to the device substrate, and then etch the desired patterned graphene by photolithography and etching. This method uses an oxygen plasma etch that inevitably causes radiation damage to graphene and other parts of the device. 3) Using a template, embossing graphene where graphene is needed. This method requires different templates for different graphenes, and the template manufacturing process is complicated and the cost is too high.
- Embodiments of the present invention provide a method for preparing a patterned graphene film by a solution method which is simple in operation, low in cost, and can be used on a large scale.
- One embodiment of the present invention provides a method of preparing a patterned graphene film, comprising the steps of:
- the substrate obtained in the step 2) is subjected to a reduction treatment in a helium vapor, and the graphene oxide in the step 2) is processed into graphene to obtain a graphene film;
- a photoresist (or an electron beam exposure glue) is patterned on a substrate by a micro-machining process such as ultraviolet lithography (or electron beam lithography), wherein a region where a graphene pattern needs to be formed is exposed and developed.
- a micro-machining process such as ultraviolet lithography (or electron beam lithography)
- the graphene oxide solution is applied to the surface of the above substrate by spin coating, spray coating or the like to form a film, and then reduced in a crucible vapor to obtain a graphene film.
- the substrate is immersed in a photoresist stripper or acetone to remove the photoresist on the surface of the substrate and the graphene film on the photoresist to obtain a patterned graphene film.
- a patterned graphene film is prepared by simply forming a patterned photoresist or an electron beam exposure paste on a substrate.
- the method is simple in operation, low in cost, and large in size
- the mold is used, and the substrate is not damaged, and is suitable for various substrates, and the application of the solution method to prepare graphene is expanded.
- FIG. 1 is a schematic view showing formation of a patterned photoresist on a substrate according to an embodiment of the present invention
- FIG. 2 is a schematic view showing film formation of a graphene oxide solution on a substrate according to an embodiment of the present invention
- BRIEF DESCRIPTION OF THE INVENTION A schematic diagram of a patterned graphene film with a substrate prepared in accordance with an embodiment of the invention
- FIG. 4 is a process flow diagram of a method of preparing a patterned graphene film in accordance with an embodiment of the present invention. detailed description
- a method of preparing a patterned graphene film according to an embodiment of the present invention includes the following steps.
- the substrate may be glass, metal, quartz or an organic film, etc.
- the organic film is, for example, a PET film, a PS film, a PE film, a PAN film or the like.
- the thickness of the photoresist or electron beam exposure gel is, for example, 1 to 10 ⁇ m.
- the electron beam exposure gel is, for example, PMMA, COP, GeSe, PBS or the like.
- aqueous solution of hydrazine is heated, for example, to 60 to 90 ° C, and the obtained substrate is placed in a closed container, and the substrate is fumigated with hydrazine vapor, for example, for 24 to 48 hours (h), and subjected to reduction treatment to obtain a graphene film.
- coating methods such as spin coating, blade coating, spray coating, etc. described above can be carried out using process equipment and process conditions well known to those skilled in the art.
- a method of preparing a patterned graphene film includes the following steps:
- PMMA2 was spin-coated on a glass substrate 1, and the thickness of the PMMA was 5 ⁇ m, and ruthenium was patterned by an electron beam etching process, in which the ruthenium in the region where the graphene pattern was to be formed was removed. As shown in Figure 1.
- a method of preparing a patterned graphene film includes the following steps:
- a positive photoresist 2 is spin-coated on a polyethylene terephthalate (PET) film substrate 1, the thickness of the photoresist is ⁇ , and the photoresist is patterned by an ultraviolet lithography process.
- the photoresist in which the region in which the graphene pattern is to be formed is removed by an exposure process. As shown in Figure 1.
- the substrate obtained in the step 4) is immersed in the photoresist stripping solution (SYIC9000, Shanghai Xinyang Semiconductor Materials Co., Ltd.) for 10 minutes to remove the photoresist and the graphene film on the photoresist to obtain patterned graphite. Alkene film. As shown in Figure 3.
- the photoresist stripping solution SYIC9000, Shanghai Xinyang Semiconductor Materials Co., Ltd.
- a method of preparing a patterned graphene film includes the following steps:
- a negative photoresist 2 is spin-coated on the aluminum foil substrate 1, the thickness of the negative photoresist is ⁇ , and the photoresist is patterned by an ultraviolet lithography etching process, wherein a graphene pattern needs to be formed. The photoresist of the region is removed by an exposure process. As shown in Figure 1.
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Physics & Mathematics (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Nanotechnology (AREA)
- Metallurgy (AREA)
- Mechanical Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- General Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Inorganic Chemistry (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- Crystallography & Structural Chemistry (AREA)
- Composite Materials (AREA)
- Manufacturing & Machinery (AREA)
- Ceramic Engineering (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
Description
Claims
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
US13/805,407 US20130149463A1 (en) | 2011-08-12 | 2012-08-09 | Method of manufacturing patterned graphene film |
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201110231196.1 | 2011-08-12 | ||
CN2011102311961A CN102653454A (zh) | 2011-08-12 | 2011-08-12 | 一种图案化石墨烯薄膜的制备方法 |
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Publication Number | Publication Date |
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WO2013023547A1 true WO2013023547A1 (zh) | 2013-02-21 |
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Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
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PCT/CN2012/079873 WO2013023547A1 (zh) | 2011-08-12 | 2012-08-09 | 图案化石墨烯薄膜的制备方法 |
Country Status (3)
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US (1) | US20130149463A1 (zh) |
CN (1) | CN102653454A (zh) |
WO (1) | WO2013023547A1 (zh) |
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US9118078B2 (en) * | 2009-03-20 | 2015-08-25 | Northwestern University | Method of forming a film of graphite oxide single layers, and applications of same |
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US9090805B2 (en) * | 2010-03-29 | 2015-07-28 | Sungyunkwan University Foundation For Corporate Collaboration | Graphene oxide reducing agent comprising a reducing agent containing a halogen element, method for manufacturing a reduced graphene oxide using same, and use of the reduced graphene oxide manufactured by the method |
CN101941694A (zh) * | 2010-09-07 | 2011-01-12 | 湘潭大学 | 一种高分散性石墨烯的制备方法 |
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2011
- 2011-08-12 CN CN2011102311961A patent/CN102653454A/zh active Pending
-
2012
- 2012-08-09 WO PCT/CN2012/079873 patent/WO2013023547A1/zh active Application Filing
- 2012-08-09 US US13/805,407 patent/US20130149463A1/en not_active Abandoned
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US20090146111A1 (en) * | 2007-12-07 | 2009-06-11 | Samsung Electronics Co., Ltd. | Reduced graphene oxide doped with dopant, thin layer and transparent electrode |
WO2010074918A1 (en) * | 2008-12-23 | 2010-07-01 | The Trustees Of The University Of Pennsylvania | High yield preparation of macroscopic graphene oxide membranes |
CN101872120A (zh) * | 2010-07-01 | 2010-10-27 | 北京大学 | 一种图形化石墨烯的制备方法 |
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CN105217605A (zh) * | 2015-07-20 | 2016-01-06 | 合肥国轩高科动力能源有限公司 | 一种图案化石墨烯的制备方法 |
CN107655856A (zh) * | 2017-09-07 | 2018-02-02 | 齐鲁工业大学 | 氧化石墨烯阵列变色薄膜/复合薄膜的制备方法及应用 |
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CN102653454A (zh) | 2012-09-05 |
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