CN109573995A - A kind of method that basic anhydride are grapheme modified - Google Patents
A kind of method that basic anhydride are grapheme modified Download PDFInfo
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- CN109573995A CN109573995A CN201811358231.4A CN201811358231A CN109573995A CN 109573995 A CN109573995 A CN 109573995A CN 201811358231 A CN201811358231 A CN 201811358231A CN 109573995 A CN109573995 A CN 109573995A
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- basic anhydride
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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
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/194—After-treatment
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- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K30/00—Organic devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation
- H10K30/80—Constructional details
- H10K30/81—Electrodes
- H10K30/82—Transparent electrodes, e.g. indium tin oxide [ITO] electrodes
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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
- C01B2204/00—Structure or properties of graphene
- C01B2204/20—Graphene characterized by its properties
- C01B2204/22—Electronic properties
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E10/00—Energy generation through renewable energy sources
- Y02E10/50—Photovoltaic [PV] energy
- Y02E10/549—Organic PV cells
Abstract
Present invention discloses a kind of methods that basic anhydride are grapheme modified, the described method comprises the following steps: S1: one layer of methyl phenyl ethers anisole of copper foil surface spin coating with graphene be poly- or then PMMA polymethyl methacrylate as graphene supporting layer etches copper foil；S2: obtained graphene film is transferred in target substrate after being standardized cleaning and is dried；S3: one layer of basic anhydride film is prepared in graphene substrate surface；Graphene substrate after cleaning, drying is transferred to one layer of copper film of vapor deposition in vacuum chamber, and is placed in 5 ~ 10 min of irradiation under ultraviolet lamp, obtains the graphene anode of performance improvement.This method propose basic anhydride film layer is formed on graphene interface, device photoelectric performance can be had an impact, provide effective technological means for photoelectricity, electronic component performance boost.
Description
Technical field
The present invention relates to a kind of method that basic anhydride are grapheme modified, it can be used for electronic component, photoelectric device
Electrode belongs to field of semiconductor devices.
Background technique
Organic semiconducting materials have many advantages, such as that light weight, flexibility are good, at low cost, in solar battery, light-emitting diodes
The fields such as pipe, laser are widely used.Current is limited in conventional oxidation indium tin (ITO) electrode used in above-mentioned semiconductor device
Shortage of resources, expensive and frangible, acid labile, so that being not easy the stable device of processability.In recent years, scholars
Making great efforts to seek that a kind of transmitance is high, flexibility is good, is capable of the material of large area preparation to substitute existing ITO electrode material
Material.
Graphene is the sp of single layer2Hydbridized carbon atoms are with the combined film of hexagon " honeycomb " shape lattice.It
Transmitance height, good mechanical property, work function are adjustable, therefore have just obtained the extensive concerns of scientists since self-discovery and grind
Study carefully.But graphene is widely used in the fields such as solar battery, light emitting diode, laser also certain difficulty.
First it sheet resistance it is big, work function and adjacent materials transport layer energy level mismatch；Secondly, graphene is a kind of hydrophobic material,
In spin coating adjacent materials transport layer, water system material is difficult to form uniform film layer on the surface of graphene, this all can be to charge in device
Transmission inside part has an adverse effect, to keep electric current relatively low, device performance is deteriorated.The emphasis studied at present is exactly to graphite
Alkene is doped the work function for adjusting graphene to reduce the sheet resistance of graphene and promotes graphene hydrophily.
Summary of the invention
The object of the invention is to propose that a kind of basic anhydride are repaired to solve the above-mentioned problems in the prior art
The method for adoring graphene.
A kind of the purpose of the invention will be achieved through the following technical solutions: side that basic anhydride are grapheme modified
Method the described method comprises the following steps:
S1: one layer of methyl phenyl ethers anisole of copper foil surface spin coating with graphene be poly- or PMMA polymethyl methacrylate, as graphite
Alkene supporting layer, then etches copper foil；
S2: obtained graphene film is transferred in target substrate and is standardized cleaning (60 DEG C of hot acetones cleans three repeatedly
Time, it is every all over 10 minutes) it dries afterwards；
S3: one layer of basic anhydride film is prepared in graphene substrate surface；Graphene substrate after cleaning, drying is transferred to vacuum
One layer of copper film of indoor vapor deposition, and 5 ~ 10 min of irradiation under ultraviolet lamp are placed in, obtain the graphene anode of performance improvement.
Preferably, the graphene is the graphene of mechanical stripping, is prepared by epitaxial growth method or vapour deposition process
To single-layer or multi-layer graphene, the graphite-based lamella is prepared by oxidation-reduction method.
It preferably, is 300-1000 nm in the film thickness of the PMMA of copper foil surface spin coating in the S1 step, PMMA's
Spincoating conditions are 10-4000 rpm.
Preferably, in the S1 step, the etching liquid of the copper foil is ammonium persulfate or iron chloride.
Preferably, in the S2 step, target substrate be glass, silicon wafer, metal foil, polyethylene terephthalate PET,
The rigidity such as polyimides PI or tunica fibrosa or flexible substrates.
Preferably, in the S3 step, basic anhydride film with a thickness of 0.1~100 nm, basic anhydride are metal
Oxide, the oxide are molybdenum oxide, cobalt oxide, tungsten oxide, copper oxide or nickel oxide.
Preferably, the preparation method of the metal oxide is solution spin-coating method, electron beam deposition or magnetron sputtering.
Preferably, the metal oxide can be oxidized to metal oxide by metal.
Preferably, metal oxide film, valence band or highest occupied molecular orbital are between graphene work function and neighboring transmission
Between the valence band or highest occupied molecular orbital of material, and in incremental or decline trend, it is used as anode modification layer.
Preferably, metal oxide film, conduction band or lowest unoccupied molecular orbital are between graphene work function and adjacent biography
Between the conduction band or lowest unoccupied molecular orbital of defeated material, and in incremental or decline trend, it is used as cathodic modification layer.
The invention adopts the above technical scheme compared with prior art, has following technical effect that this method can be substantially
Degree promotes the photoelectricity or electronic component performance that graphene makees electrode.It can be used as photoelectricity/electronics device with the graphene after its modification
Part electrode, method of modifying has many advantages, such as simple process, significant effect, low in cost, especially flexible in photoelectricity/electronic device
Devices field possesses broad application prospect.
The present invention provides a kind of methods that basic anhydride are grapheme modified, propose and form alkali on graphene interface
Property oxide film layer, can have an impact device photoelectric performance, provide effectively for photoelectricity, electronic component performance boost
Technological means.
This method can regulate and control graphene work function and improve the hydrophily of graphene, have simple process, operability
By force, the advantages that significant effect.This method is particularly suitable for using graphene as the flexible optoelectronic of electrode or electronic component.
The present invention dexterously uses basic anhydride as interface-modifying layer to adjust the work function of Graphene electrodes and change
Kind graphene hydrophily, the electrode prepared shows fabulous stability, and device performance is significantly improved, and can replace
The business polarizing electrodes such as ITO electrode, carbon nanotube, the metal nanometer line that generation is widely used at present, have greatly pushed photoelectricity, electronics
Technical field, especially flexible optoelectronic/electronic component field development process.
Present invention uses a kind of common metal oxide, i.e. copper oxide (CuOx), come it is grapheme modified, and by its
Applied to organic solar batteries field, to highlight modifying interface to the castering action of device performance.CuO used in the present inventionxOne
Aspect has adjusted the work function of graphene, reduces the carrier transport potential barrier between electrode and transport layer；On the other hand it is promoted
The hydrophily of graphene, improves the film forming of water-based material on the surface of graphene, reduces series resistance in device, thus
Greatly increase the performance of device.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of organic solar batteries device of the invention.
Fig. 2 is the work function of the graphene of the invention through copper oxide before and after treatment.
Fig. 3 is the contact angle of the graphene of the invention through copper oxide before and after treatment.
Fig. 4 is the contact angle of the graphene of the invention through copper oxide before and after treatment.
Fig. 5 is C-V characteristic of the graphene of copper oxide of the invention before and after the processing as the organic solar batteries of electrode
Curve.
Wherein, appended drawing reference are as follows:
1, target substrate；2, anode graphite alkene；3, interface-modifying layer；4, hole transmission layer；5, organic solar batteries active layer；
6, electron transfer layer；7, metal electrode layer.
Specific embodiment
The purpose of the present invention, advantage and feature, by by the non-limitative illustration of preferred embodiment below carry out diagram and
It explains.These embodiments are only the prominent examples using technical solution of the present invention, it is all take equivalent replacement or equivalent transformation and
The technical solution of formation, all falls within the scope of protection of present invention.
Present invention discloses a kind of methods that basic anhydride are grapheme modified, the described method comprises the following steps:
S1: one layer of methyl phenyl ethers anisole of copper foil surface spin coating with graphene be poly- or PMMA polymethyl methacrylate, as graphite
Alkene supporting layer, then etches copper foil；
S2: obtained graphene film is transferred in target substrate after being standardized cleaning and is dried；
S3: one layer of basic anhydride film is prepared in graphene substrate surface；Graphene substrate after cleaning, drying is transferred to vacuum
One layer of copper film of indoor vapor deposition, and 5 ~ 10 min of irradiation under ultraviolet lamp are placed in, obtain the graphene anode of performance improvement.
The graphene be mechanical stripping graphene, by epitaxial growth method or vapour deposition process be prepared single layer or
Multi-layer graphene, the graphite-based lamella are prepared by oxidation-reduction method.
It is 300-1000nm, the spincoating conditions of PMMA in the film thickness of the PMMA of copper foil surface spin coating in the S1 step
For 10-4000 rpm.In the S1 step, the etching liquid of the copper foil is ammonium persulfate or iron chloride.
In the S2 step, target substrate is glass, silicon wafer, metal foil, polyethylene terephthalate PET, polyamides Asia
The rigidity such as amine PI or tunica fibrosa or flexible substrates.
In the S3 step, basic anhydride film with a thickness of 0.1~100 nm, basic anhydride are metal oxide,
The oxide is molybdenum oxide, cobalt oxide, tungsten oxide, copper oxide or nickel oxide.The preparation method of the metal oxide is molten
Liquid spin-coating method, electron beam deposition or magnetron sputtering.The metal oxide can be oxidized to metal oxide by metal.
The valence of metal oxide film, valence band or highest occupied molecular orbital between graphene work function and neighboring transmission material
Between band or highest occupied molecular orbital, and in incremental or decline trend, it is used as anode modification layer.Metal oxide film, conduction band
Or lowest unoccupied molecular orbital is between the conduction band or lowest unoccupied molecular orbital of graphene work function and neighboring transmission material
Between, and in incremental or decline trend, it is used as cathodic modification layer.
Below with CuOxFor application of the film layer in organic solar batteries, modifying interface is described to organic solar
The castering action of battery performance, specific embodiment are as follows:
A, the preparation and processing of Graphene electrodes
In one layer of PMMA of copper foil surface spin coating with graphene as graphene supporting layer, then etched with ammonium persulfate solution
Copper foil；In turn, obtained graphene film is transferred in substrate of glass after being standardized cleaning and is dried；Then, by graphite
Alkenyl piece, which is transferred in vacuum chamber, is deposited one layer of copper film, and 7 min are irradiated under ultraviolet lamp, obtains the graphene sun of performance improvement
Pole.
B, prepared by hole transmission layer
PEDOT:PSS is filtered twice with the water system filtering head that filter mesh gap diameter is 0.45 mm, it will after sonicated
PEDOT:PSS is spin-coated on graphene/copper oxide film substrate, and spincoating conditions are 2000 rpm, and spin-coating time is 1 min, then
120 DEG C of 20 min of annealing obtain hole transmission layer.PEDOT:PSS film with a thickness of 40 nm.
C, prepared by active layer
PCE-10 and PC71BM is configured in solvent chlorobenzene according to the concentration of 10 mg:15 mg/mL, obtains active layer solution.
In glove box, in the graphene/copper oxide/surface PEDOT:PSS spin coating active layer solution PCE-10:PC71BM, rotation
Painting condition is 1000 rpm, and spin-coating time is 1 min, 30 min of room temperature annealing.Piece made is placed in vacuum chamber, is taken out true
Sky is to 1.9*10-3 Pa。
D, electron transfer layer and cathode layer preparation
The successively vacuum evaporation LiF and Al on above-mentioned active layer forms electron transfer layer and cathode layer to get organic solar
Battery.Wherein the evaporation rate of LiF and Al is respectively 0.25 Hz/s and 15 Hz/s, and 34 Hz and 2000 Hz are deposited respectively.LiF
Thickness with Al is respectively 0.5 nm and 90 nm.
Such as Fig. 1, the present embodiment organic solar batteries share 7 film layer structures, and the 1st layer is glass, as organic sun
The substrate of energy battery；2nd layer is graphene, is the anode of organic solar batteries；3rd layer is then copper oxide, and effect is to repair
Decorations graphene is to improve the work function of graphene and reduce graphene surface contact angle；Layer 4-7 is that the hole of battery passes respectively
Defeated layer, active layer, electron transfer layer and cathode layer.
As shown in Fig. 2, one layer of copper film is deposited on the surface of graphene, copper is converted into copper oxide under ultraviolet processing.Through peroxide
After changing Copper treatment, the work function of graphene surface is increased, and is more matched with the energy level of hole transmission layer, is reduced hole and transmitting
Potential barrier in the process is conducive to the raising of device performance.The ordinate of Fig. 2 is intensity, and abscissa is in conjunction with energy.
As shown in Figure 3 and Figure 4, after copper dioxide is handled, the contact angle of graphene surface is reduced, and hydrophily improves, and is made
The film layer coverage rate for obtaining hole transmission layer is higher, and film layer more evenly, facilitates charge transmission, so that device performance is improved, so that
It has huge potential using value in photoelectronics.
Fig. 5 be use it is bent as the C-V characteristic of the organic solar batteries of anode through copper oxide graphene before and after the processing
Line.Fig. 5 abscissa is open-circuit voltage, and ordinate is short-circuit current density, after aoxidizing Copper treatment graphene, the volt-ampere of device
Characteristic is more obvious, and device performance is also improved.
By forming one or more layers basic anhydride film on the surface of graphene, it can achieve following effect: (1) improving stone
The work function of black alkene, so that the level-density parameter degree of it and device film layer improves；(2) graphene surface contact angle is reduced, so that water
Property film material wellability on the surface of graphene be improved, film layer coverage rate improves.Graphene after modification can be used for light
Electricity/electronic device electrode achievees the effect that promote device performance.The photoelectricity prepared in this way/electronic device process letter
List, significant effect, low in cost, in photoelectricity/electronic device, especially flexible device field possesses broad application prospect.
The present invention dexterously uses basic anhydride as interface-modifying layer to adjust the work function of Graphene electrodes and change
Kind graphene hydrophily, the electrode prepared shows admirably stability, and device performance is significantly improved, can be with
The business polarizing electrodes such as ITO electrode, carbon nanotube, the metal nanometer line being widely used at present are substituted, photoelectricity, electricity have greatly been pushed
Sub- technical field, especially flexible optoelectronic/electronic component field development process.
The present invention uses a kind of common metal oxide, i.e. copper oxide (CuOx), come it is grapheme modified, and by its
Applied to organic solar batteries field, to highlight modifying interface to the castering action of device performance.CuO used in the present inventionx
On the one hand the work function for having adjusted graphene, reduces the carrier transport potential barrier between electrode and transport layer；On the other hand it mentions
The hydrophily for having risen graphene improves the film forming of water-based material on the surface of graphene, reduces series resistance in device, from
And substantially increase the performance of device.
Still there are many embodiment, all technical sides formed using equivalents or equivalent transformation by the present invention
Case is within the scope of the present invention.
Claims (10)
1. a kind of method that basic anhydride are grapheme modified, it is characterised in that: the described method comprises the following steps:
S1: one layer of methyl phenyl ethers anisole of copper foil surface spin coating with graphene be poly- or PMMA polymethyl methacrylate, as graphite
Alkene supporting layer, then etches copper foil；
S2: obtained graphene film is transferred in target substrate after being standardized cleaning and is dried；
S3: one layer of basic anhydride film is prepared in graphene substrate surface；Graphene substrate after cleaning, drying is transferred to vacuum
One layer of copper film of indoor vapor deposition, and 5 ~ 10 min of irradiation under ultraviolet lamp are placed in, obtain the graphene anode of performance improvement.
2. a kind of grapheme modified method of basic anhydride according to claim 1, it is characterised in that: the graphene
For the graphene of mechanical stripping, single-layer or multi-layer graphene, the stone are prepared by epitaxial growth method or vapour deposition process
Black substrate layer is prepared by oxidation-reduction method.
3. a kind of grapheme modified method of basic anhydride according to claim 1, it is characterised in that:
It is 300-1000nm in the film thickness of the PMMA of copper foil surface spin coating, the spincoating conditions of PMMA are 10- in the S1 step
4000 rpm。
4. a kind of grapheme modified method of basic anhydride according to claim 1, it is characterised in that: the S1 step
In, the etching liquid of the copper foil is ammonium persulfate or iron chloride.
5. a kind of grapheme modified method of basic anhydride according to claim 1, it is characterised in that: the S2 step
In, target substrate is the rigidity such as glass, silicon wafer, metal foil, polyethylene terephthalate PET, polyimides PI or tunica fibrosa
Or flexible substrates.
6. a kind of grapheme modified method of basic anhydride according to claim 1, it is characterised in that: the S3 step
In, basic anhydride film with a thickness of 0.1~100 nm, basic anhydride are metal oxide, the oxide be molybdenum oxide,
Cobalt oxide, tungsten oxide, copper oxide or nickel oxide.
7. a kind of grapheme modified method of basic anhydride according to claim 6, it is characterised in that: the metal oxygen
The preparation method of compound is solution spin-coating method, electron beam deposition or magnetron sputtering.
8. a kind of grapheme modified method of basic anhydride according to claim 6, it is characterised in that: the metal oxygen
Compound can be oxidized to metal oxide by metal.
9. a kind of grapheme modified method of basic anhydride according to claim 6, it is characterised in that: metal oxide
The valence band or highest occupied molecular rail of film, valence band or highest occupied molecular orbital between graphene work function and neighboring transmission material
Between road, and in incremental or decline trend, it is used as anode modification layer.
10. a kind of grapheme modified method of basic anhydride according to claim 6, it is characterised in that: metal oxidation
Object film, conduction band or lowest unoccupied molecular orbital between graphene work function and neighboring transmission material conduction band or minimum do not occupy
Between molecular orbit, and in incremental or decline trend, it is used as cathodic modification layer.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110376163A (en) * | 2019-07-04 | 2019-10-25 | 浙江大学 | Humidity sensor and preparation method based on graphene and the more single fibers of side throwing list |
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Application publication date: 20190405 |