CN109384218A - A kind of preparation method of graphene grid film - Google Patents
A kind of preparation method of graphene grid film Download PDFInfo
- Publication number
- CN109384218A CN109384218A CN201811518846.9A CN201811518846A CN109384218A CN 109384218 A CN109384218 A CN 109384218A CN 201811518846 A CN201811518846 A CN 201811518846A CN 109384218 A CN109384218 A CN 109384218A
- Authority
- CN
- China
- Prior art keywords
- graphene
- film
- plate
- grid
- copper foil
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Classifications
-
- 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
- C01B32/186—Preparation by chemical vapour deposition [CVD]
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B13/00—Apparatus or processes specially adapted for manufacturing conductors or cables
- H01B13/0026—Apparatus for manufacturing conducting or semi-conducting layers, e.g. deposition of metal
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B5/00—Non-insulated conductors or conductive bodies characterised by their form
- H01B5/12—Braided wires or the like
-
- 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
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Nanotechnology (AREA)
- Inorganic Chemistry (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
The present invention relates to a kind of preparation methods of graphene grid film; the main thought of this method is in graphene film preparation process; the graphene film that spin coating has PMMA protective layer is adsorbed on the quartz plate with photoetching agent pattern, photoetching agent pattern is removed later and its graphene film on surface obtains graphene grid film.Single-layer graphene structure subject to the graphene grid film of this method preparation, uniformly unify in grid woven areas thickness, attribute identical with the graphene film not prepared graphically is maintained, while solving the problems, such as that graphene conductive film is not easy to be prepared into matrix structure, it is simple and easy.
Description
Technical field
The present invention relates to technical field of graphene.More particularly to a kind of preparation method of graphene grid film.
Background technique
Graphene has high conductivity (> 6 × 106S/m), the high current density (10 carried8A/cm2, than
High 2 ~ 3 orders of magnitude of copper).Theoretically the thickness of single-layer graphene only has 0.345nm, thus it is with excellent optical property.
2.3% visible light not only can be absorbed in single-layer graphene, therefore light transmittance is 97.7%.
Its excellent optically and electrically performance, so that it has huge application potential in transparent conductive film.And stone
There is good light transmittance to guarantee working efficiency for black alkene grid film, and can further improve its optical property, to meet high-performance saturating
The demand of bright conductive film.
Summary of the invention
The present invention provides a kind of preparation method of graphene grid film, further increases graphene film light transmittance, together
When solve the problems, such as that graphene conductive film is not easy to be prepared into matrix structure.
A kind of preparation method of graphene grid film, comprising the following steps:
Step 1: growing graphene film in copper foil surface by chemical vapour deposition technique, graphene/copper foil is placed in later even
In glue machine, with rate 50 ~ 100s of spin coating of 1500-3200 r/min, PMMA acetone soln is spin-coated on table on graphene/copper foil
Face；It places it on warm table, be heated to 60 ~ 100 °C and keep the temperature 20 ~ 40min；
Step 2: copper foil is floated on the ferric chloride solution of 0.8 ~ 1.2mol/L, copper foil lower surface is contacted with ferric chloride solution
Corroded, 6 ~ 12h of etching time；The upper graphene film for floating on ferric chloride solution is picked up and is placed in deionization Overwater-floating
It washes, repeats three times；
Step 3: quartzy plate is placed in deionized water, it is cleaned by ultrasonic 5min；It places it in sol evenning machine later, with 2000 ~
Photoresist is spin-coated on quartzy plate upper surface by rate 10 ~ 30s of spin coating of 4000r/min；By the quartzy plate of spin coating photoresist
It is placed on warm table, is heated to 60 ~ 90 °C and keeps the temperature 8 ~ 15min；
Step 4: being exposed using photoresist of the grid mask plate to quartzy plate upper surface, 10 ~ 40s of time for exposure；Later
Develop to photoresist, developing time is 30 ~ 60s；Quartzy plate after development is placed in deionized water, is cleaned by ultrasonic
7min is repeated three times；
Step 5: the graphene film floated in deionized water in step 1 is picked up with the upper surface of quartz plate, make its suction
It invests on photoengraving pattern, quartz plate setting is drained into 20 ~ 40min；The quartz plate for being adsorbed with graphene film is placed in warm table,
It is heated to 90 ~ 130 °C and keeps the temperature 15 ~ 30min.
Step 6: quartz plate is placed in acetone, heating water bath is to 35 ~ 55 °C and keeps the temperature 20 ~ 40min, removes photoresist
Pattern and its graphene film on surface；Quartz plate is pulled out from acetone soln, is placed in deionized water and rinses, repeats three
Time, it is dried with nitrogen.
Further, in step 4 kind, mesh grid mask plate select rectangle grid mask plate, round grid mask plate or
Positive five sides grid mask plate.
Compared with prior art, beneficial effects of the present invention are as follows:
1. the present invention prepares graphene grid film using the method for graphene film absorption photoetching agent pattern, this process flow is easy
Operation, can prepare different graphene mesh grid structures.Single-layer graphene structure subject to the graphene grid film of preparation, grid line width
And the period can any combination；The graphene grid film thickness of preparation is uniform, and there is no grid woven areas thickness is skimble-scamble
Problem；Graphene grid film transmission rate is high simultaneously.
2. a kind of preparation method of graphene grid film of the present invention is compared with existing copper mesh prepares graphene grid film,
The grid film of preparation belongs to uniform quasi- single thin film, maintains attribute identical with the graphene film not prepared graphically,
Its translucency, uniformity and electric conductivity are high；Solve the problems, such as that graphene conductive film is not easy to be prepared into matrix structure, this method letter
It is single easy.
Detailed description of the invention
Fig. 1 is line width 100um prepared by the present invention, the optical microscopy map of the graphene grid film of period 500um；Its
In, Fig. 1 (a) is under 50 power microscopes, and Fig. 1 (b) is under 20 power microscopes；
Fig. 2 is line width 200um prepared by the present invention, the optical microscopy map of the graphene grid film of period 500um；Wherein, Fig. 2
It (a) is under 50 power microscopes, Fig. 2 (b) is under 20 power microscopes；
Fig. 3 is the line width 100um of experiment preparation, the Raman light of the grid woven areas of the graphene grid film of period 500um
Spectrogram.
Specific embodiment
Below by specific embodiment combination attached drawing, invention is further described in detail.Wherein different embodiments
Middle similar component uses associated similar element numbers.In the following embodiments, many datail descriptions be in order to
The application is better understood.However, those skilled in the art can recognize without lifting an eyebrow, part of feature
It is dispensed, or can be substituted by other elements, material, method in varied situations.In some cases, this Shen
Please it is relevant it is some operation there is no in the description show or describe, this is the core in order to avoid the application by mistake
More descriptions are flooded, and to those skilled in the art, these relevant operations, which are described in detail, not to be necessary, they
Relevant operation can be completely understood according to the general technology knowledge of description and this field in specification.
The main thought of the method for the present invention is that spin coating is had to the graphite of PMMA protective layer in graphene film preparation process
Alkene film is adsorbed on the quartz plate with photoetching agent pattern, removes photoetching agent pattern later and its graphene film on surface obtains
To graphene grid film.
Embodiment 1:
A kind of preparation method of very thin copper mesh, sequentially includes the following steps:
Step 1: growing graphene film in copper foil surface by chemical vapour deposition technique, graphene/copper foil is placed in later even
In glue machine, with the rate spin coating 70s of 2500 r/min, PMMA acetone soln is spin-coated on graphene/copper foil upper surface；It is set
In on warm table, being heated to 80 °C and keep the temperature 30min；
Step 2: copper foil is floated on the ferric chloride solution of 0.9mol/L, copper foil lower surface contacts progress with ferric chloride solution
Corrosion, etching time 8h；The upper graphene film for floating on ferric chloride solution is picked up to be placed in deionized water and is rinsed, is repeated
Three times；
Step 3: quartzy plate is placed in deionized water, it is cleaned by ultrasonic 5min.It places it in sol evenning machine later, with
Photoresist is spin-coated on quartzy plate upper surface by the rate spin coating 15s of 3200r/min；The quartzy plate of spin coating photoresist is set
In on warm table, being heated to 75 °C and keep the temperature 12min；
Step 4: being exposed using photoresist of the rectangle grid mask plate to quartzy plate upper surface, time for exposure 20s；It
Develop afterwards to photoresist, developing time 45s；Quartzy plate after development is placed in deionized water, is cleaned by ultrasonic
7min is repeated three times；
Step 5: the graphene film floated in deionized water in step 1 is picked up with the upper surface of quartz plate, make its suction
It invests on photoengraving pattern, quartz plate setting is drained into 30min；The quartz plate for being adsorbed with graphene film is placed in warm table, is added
Heat is to 110 °C and keeps the temperature 20min；
Step 6: quartz plate is placed in acetone, heating water bath is to 45 °C and keeps the temperature 35min, removes photoetching agent pattern and its table
The graphene film in face；Quartz plate is pulled out from acetone soln, is placed in deionized water and rinses, repeats three times, is dried with nitrogen.
Referring to Figure 1, Fig. 1 is the line width 100um of method preparation through this embodiment, the graphene grid of period 500um
The optical microscopy map of film can find out that graphene grid membrane structure prepared by the present invention is uniform, and line width is from figure
100um, period 500um.
Fig. 2 is referred to, Fig. 2 is the line width 200um of method preparation through this embodiment, the graphene grid of period 500um
The optical microscopy map of film can find out that graphene grid membrane structure prepared by the present invention is uniform, and line width is from figure
200um, period 500um.
Fig. 3 is referred to, Fig. 3 is the line width 100um prepared for method through this embodiment, the graphene mesh of period 500um
The Raman spectrogram of the grid woven areas of grid film can find out, graphene grid film is in grid woven areas from figure
Raman spectrum is single layer feature, shows single-layer graphene knot subject to it, is maintained and the graphene film phase that does not prepare graphically
Same attribute.
Embodiment 2:
The present embodiment is not both with embodiment 1: using round grid mask plate to the light of quartzy plate upper surface in step 4
Photoresist is exposed, time for exposure 15s；Develop later to photoresist, developing time 30s；Quartz after development is put down
Plate is placed in deionized water, is cleaned by ultrasonic 7min, is repeated three times；Other steps and parameter are same as the specific embodiment one.
Embodiment 3:
The present embodiment is not both with embodiment 1: using positive five sides grid mask plate to quartzy plate upper surface in step 4
Photoresist is exposed, time for exposure 30s.Develop later to photoresist, developing time 60s；By the quartz after development
Plate is placed in deionized water, is cleaned by ultrasonic 7min, is repeated three times；Other steps and parameter are same as the specific embodiment one.
Use above specific case is illustrated the present invention, is merely used to help understand the present invention, not to limit
The system present invention.For those skilled in the art, according to the thought of the present invention, can also make several simple
It deduces, deform or replaces.
Claims (2)
1. a kind of preparation method of graphene grid film, it is characterised in that:
The following steps are included:
Step 1: growing graphene film in copper foil surface by chemical vapour deposition technique, graphene/copper foil is placed in later even
In glue machine, with rate 50 ~ 100s of spin coating of 1500-3200 r/min, PMMA acetone soln is spin-coated on table on graphene/copper foil
Face；It places it on warm table, be heated to 60 ~ 100 °C and keep the temperature 20 ~ 40min；
Step 2: copper foil is floated on the ferric chloride solution of 0.8 ~ 1.2mol/L, copper foil lower surface is contacted with ferric chloride solution
Corroded, 6 ~ 12h of etching time；The upper graphene film for floating on ferric chloride solution is picked up and is placed in deionization Overwater-floating
It washes, repeats three times；
Step 3: quartzy plate is placed in deionized water, it is cleaned by ultrasonic 5min；It places it in sol evenning machine later, with 2000 ~
Photoresist is spin-coated on quartzy plate upper surface by rate 10 ~ 30s of spin coating of 4000r/min；By the quartzy plate of spin coating photoresist
It is placed on warm table, is heated to 60 ~ 90 °C and keeps the temperature 8 ~ 15min；
Step 4: being exposed using photoresist of the grid mask plate to quartzy plate upper surface, 10 ~ 40s of time for exposure；Later
Develop to photoresist, developing time is 30 ~ 60s；Quartzy plate after development is placed in deionized water, is cleaned by ultrasonic
7min is repeated three times；
Step 5: the graphene film floated in deionized water in step 1 is picked up with the upper surface of quartz plate, make its suction
It invests on photoengraving pattern, quartz plate setting is drained into 20 ~ 40min；The quartz plate for being adsorbed with graphene film is placed in warm table,
It is heated to 90 ~ 130 °C and keeps the temperature 15 ~ 30min；
Step 6: quartz plate is placed in acetone, heating water bath is to 35 ~ 55 °C and keeps the temperature 20 ~ 40min, removes photoetching agent pattern
And its graphene film on surface；Quartz plate is pulled out from acetone soln, is placed in deionized water and rinses, is repeated three times, nitrogen
Air-blowing is dry.
2. the preparation method of very thin copper mesh according to claim 1, it is characterised in that:
In step 4 kind, mesh grid mask plate selects rectangle grid mask plate, round grid mask plate or positive five side grid to cover
Film version.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811518846.9A CN109384218B (en) | 2018-12-12 | 2018-12-12 | Preparation method of graphene grid film |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811518846.9A CN109384218B (en) | 2018-12-12 | 2018-12-12 | Preparation method of graphene grid film |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN109384218A true CN109384218A (en) | 2019-02-26 |
| CN109384218B CN109384218B (en) | 2020-11-10 |
Family
ID=65429138
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201811518846.9A Active CN109384218B (en) | 2018-12-12 | 2018-12-12 | Preparation method of graphene grid film |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN109384218B (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113504588A (en) * | 2021-07-06 | 2021-10-15 | 西安工业大学 | Preparation method of electromagnetic shielding compatible infrared anti-reflection film device |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101872120A (en) * | 2010-07-01 | 2010-10-27 | 北京大学 | Method for preparing patterned graphene |
| CN103000535A (en) * | 2012-12-31 | 2013-03-27 | 西安电子科技大学 | Preparation method for side gating graphene field effect transistor |
| CN103199020A (en) * | 2013-03-05 | 2013-07-10 | 中国科学院上海微系统与信息技术研究所 | Preparing method and detecting method of liquid grid type grapheme field-effect tube based on polyimide (PI) |
| US20170032962A1 (en) * | 2015-07-27 | 2017-02-02 | Graphenea, S.A. | Equipment and method to automatically transfer a graphene monolayer to a substrate |
| CN108428794A (en) * | 2018-01-26 | 2018-08-21 | 吉林大学 | Utilize the lossless transfer of photoresist supporting layer and method and the application of patterned Graphene |
-
2018
- 2018-12-12 CN CN201811518846.9A patent/CN109384218B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101872120A (en) * | 2010-07-01 | 2010-10-27 | 北京大学 | Method for preparing patterned graphene |
| CN103000535A (en) * | 2012-12-31 | 2013-03-27 | 西安电子科技大学 | Preparation method for side gating graphene field effect transistor |
| CN103199020A (en) * | 2013-03-05 | 2013-07-10 | 中国科学院上海微系统与信息技术研究所 | Preparing method and detecting method of liquid grid type grapheme field-effect tube based on polyimide (PI) |
| US20170032962A1 (en) * | 2015-07-27 | 2017-02-02 | Graphenea, S.A. | Equipment and method to automatically transfer a graphene monolayer to a substrate |
| CN108428794A (en) * | 2018-01-26 | 2018-08-21 | 吉林大学 | Utilize the lossless transfer of photoresist supporting layer and method and the application of patterned Graphene |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113504588A (en) * | 2021-07-06 | 2021-10-15 | 西安工业大学 | Preparation method of electromagnetic shielding compatible infrared anti-reflection film device |
Also Published As
| Publication number | Publication date |
|---|---|
| CN109384218B (en) | 2020-11-10 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| JP5833747B2 (en) | Double-sided patterned transparent conductive film and method for producing the same | |
| CN102979516B (en) | Workmanship of indoor microscopic oil displacement model | |
| CN104134749B (en) | Layer flexible plane embeds laminate patch electrode and preparation method thereof and the application in organic field single-crystal field effect transistor | |
| CN107424682B (en) | A kind of preparation method of the porous metal film transparent conductive electrode with fractal structure | |
| CN106449565B (en) | Manufacturing method based on graphene bigger serface flexible heat sink device | |
| CN103151245B (en) | Film patterning method | |
| CN103205701A (en) | A vapor deposition mask plate and a production method thereof | |
| CN102556950A (en) | Tunable artificial electromagnetic material based on three-layer structure and preparation method thereof | |
| CN106336521B (en) | A kind of resin compound, transparent conductive film and its graphical preparation method | |
| CN107765511A (en) | The graphic method of graphene and nano silver wire compound transparent electricity conductive film | |
| CN109972087B (en) | Preparation method of microelectrode deposition mask | |
| CN105655242B (en) | The preparation method of doped graphene and graphene PN junction device | |
| CN109384218A (en) | A kind of preparation method of graphene grid film | |
| CN105093823B (en) | A kind of manufacturing method of gap electrode, gap electrode and display panel | |
| CN103840243B (en) | A kind of manufacture method of flexible co-planar waveguide | |
| CN202530150U (en) | Evaporation mask plate | |
| CN105006482B (en) | A kind of preparation method of graphene field effect transistor | |
| KR20190099903A (en) | Method of patterning a hybrid transparent electrode | |
| CN102810464B (en) | Photoetching method | |
| CN104393027B (en) | A kind of full carbon graphite alkene device and preparation method thereof | |
| CN109440029A (en) | A kind of preparation method of very thin copper mesh | |
| CN108449927B (en) | Metal film and manufacturing method thereof | |
| CN109713159A (en) | A kind of top electrode is patterned with the preparation method of organic electroluminescence devices | |
| KR20110073786A (en) | Method for forming a transparent conductive film for a flexible substrate using low-temperature and selective atomic layer forming process | |
| CN107221497B (en) | Manufacturing method of lead and display panel |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |