CN108075041A - A kind of flexible compound electrode, its preparation method and application - Google Patents
A kind of flexible compound electrode, its preparation method and application Download PDFInfo
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- CN108075041A CN108075041A CN201611025181.9A CN201611025181A CN108075041A CN 108075041 A CN108075041 A CN 108075041A CN 201611025181 A CN201611025181 A CN 201611025181A CN 108075041 A CN108075041 A CN 108075041A
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Abstract
The present invention provides a kind of flexible compound electrode, its preparation method and application, the flexible compound electrode preparation method comprise the following steps：Pyridine, trivalent iron salt catalyst and alcohols solvent are uniformly mixed, obtain performed polymer mixed liquor, and it is coated uniformly on substrate, the heat drying under no water oxygen environment, it puts it into again and has been added dropwise 3, in the reaction kettle of 4 ethene dioxythiophene monomers, gas phase polymerization is carried out by the way that gas is heated, be passed through to reaction kettle, obtains flexible compound electrode.The smaller graphene film of size can be together in series by adopting this method, and realized that solwution method prepares large area flexible combination electrode, had a wide range of applications in organic electroluminescence device and solar cell.
Description
Technical field
The present invention relates to the preparing technical fields of flexible compound electrode, and in particular to a kind of graphene flexible compound electrode with
And it is provided with the organic electroluminescence device of the flexible compound electrode and flexible compound electrode.
Background technology
Organic electroluminescence device (English full name is Organic Light Emitting Device, referred to as OLED)
As next generation's illumination and display technology, have that colour gamut is wide, response is fast, wide viewing angle, pollution-free, high contrast, planarization etc. are excellent
Point.
Typical organic electroluminescence device generally comprises transparent substrate, first transparency electrode, second electrode and sets
In two interelectrode organic light-emitting units.The transparent electrode used now is generally ITO, because ITO mechanical properties are poor, generally
Think that ITO is not suitable for use in flexible transparent electrode.Industry thinks that metal nanometer line, graphene etc. are to make flexible electrode at present
Ideal material.But how large area prepare and transfer graphene, how using existing smaller scale graphene, how to utilize
The problems such as with expansion grapheme material two dimension electric conductivity, it is still necessary to solve.
CN105118681A discloses a kind of method for manufacturing graphene-based tri compound flexible electrode, including：By first
Conducting polymer, which is dissolved in organic solvent, obtains the first conductive polymer solution；First conductive polymer solution is spun on flexibility
It is in substrate and dry, form the first conductive polymer coating；Using the first conductive polymer coating as working electrode, with graphene oxide point
Dispersion liquid is electrolyte, and graphene layer is formed with cyclic voltammetry；The gas blowout oxygen on the first conducting polymer/graphene composite film
Agent is simultaneously vapor-deposited in the second conducting polymer monomer atmosphere, forms the first conducting polymer/graphene/the second and leads
Electric polymer laminated film.The conducting polymer that the method obtains is unstable, typically contains acidic materials, such as p-methyl benzenesulfonic acid
PSS；In addition cyclic voltammetry film forming homogeneity is poor, and technological process is complicated, is unfavorable for large-scale industrial production.
A kind of preparation method of graphene/silicons of CN105552333A/conducting polymer composite negative pole material, belongs to electrochemistry
With new energy materials field.The method comprises the steps of firstly, preparing graphene oxide composite material is gone out, by graphene oxide and silica flour, polymer monomer
Mixing, polymerize polymer monomer, then convection drying obtains graphene oxide/silicon/conducting polymer under certain conditions
Then film composite material prepares graphene/silicon/conductive polymer foams composite material using hydrazine hydrate steam reduction method.
This method film forming roughness is very big, it is impossible to applied to display field；And largely chemically reacted in preparation process, by-product and
Particle is not easy management and control.
The content of the invention
For this purpose, the technical problems to be solved by the invention in existing graphene combination electrode material in preparation process nothing
The problem of prepared by method large area, and then a kind of flexible compound electrode preparation method is provided, it can be by the smaller graphene film of size
It is together in series, realizes that solwution method prepares large area flexible combination electrode.
For achieving the above object, the present invention adopts the following technical scheme that：
A kind of preparation method of flexible compound electrode, comprises the following steps：
S1, pyridine, trivalent iron salt catalyst and alcohols solvent are uniformly mixed, obtain performed polymer mixed liquor；
S2, graphene is added in the performed polymer mixed liquor of step S1 preparations, and be coated uniformly on substrate, in nothing
Heat drying under water oxygen environment, obtain containing graphene, pyridine, trivalent iron salt catalyst dry substrate；
S3, the dry substrate for preparing step S2, are put into and have been added dropwise in the reaction kettle of 3,4-rthylene dioxythiophene monomer,
Gas phase polymerization is carried out by the way that gas is heated, be passed through to reaction kettle, obtains flexible compound electrode；The gas is N2With/
Or inert gas.
Pyridine in the performed polymer mixed liquor：Trivalent iron salt catalyst：Alcohols solvent molar ratio is (0.95-1.05):
(9.5-10.5):(95-105)。
The trivalent iron salt catalyst is p-methyl benzenesulfonic acid iron or ferric trichloride, and the alcohols solvent is n-butanol.
Gas flow rate is 0-1m in the step S33/ h is preferably 0.1-1m3//h, heating temperature are 40-90 DEG C, preferably
For 50-60 DEG C.
Above-mentioned reaction process is：
By being simultaneously passed through gas simultaneously to reaction kettle heating, 3,4-rthylene dioxythiophene monomer EDOT gasifies, and with gas
Form is contacted with the catalyst on substrate, under the catalytic action of catalyst, polymerisation occurs, is become by EDOT monomers
PEDOT (polyethylene dioxythiophene) polymer.During polymerisation occurs, graphene does not participate in reaction, but in the process,
Polymer can join together in growth course by the graphene of fragmentation as seam fragment cloth.
The preparation method of the flexible compound electrode, further includes following step：
S4, the flexible compound electrode that step S3 is obtained is cleaned using water or alcohols solvent, removes its surface
Trivalent iron salt catalyst.
A kind of flexible compound electrode is prepared using the method.
A kind of organic electroluminescence device including substrate and sequentially forms first electrode layer on the substrate, hair
Light unit and the second electrode lay, the first electrode and/or second electrode are the flexible compound electrode, described flexible multiple
The thickness of composite electrode is 50nm-1000nm.
Organic electroluminescence device is top light-emitting organic electroluminescent device, and first electrode is the flexible compound electricity
Pole.
A kind of solar battery sheet, including the anode, photoelectric conversion unit and transparent cathode being sequentially overlapped, the light transmission
Cathode is the flexible compound electrode described in claim 7.
The above technical solution of the present invention has the following advantages over the prior art：
1st, the present invention provides a kind of flexible compound electrode preparation method, comprise the following steps：Pyridine, trivalent iron salt catalysis
Agent and alcohols solvent are uniformly mixed, and obtain performed polymer mixed liquor；Graphene is added in performed polymer mixed liquor, is gathered using gas phase
Flexible compound electrode is obtained by the reaction in conjunction, then washes away the catalyst of electrode surface.Adopting this method can be smaller by size
Graphene film be together in series, realize solwution method prepare large area flexible combination electrode.
Above-mentioned reaction process by reaction kettle heating and being passed through gas, 3,4-rthylene dioxythiophene monomer EDOT gas simultaneously
Change, and contacted in gaseous form with the catalyst on substrate, under the catalytic action of catalyst, polymerisation occurs, by EDOT
Monomer becomes PEDOT (polyethylene dioxythiophene) polymer.During polymerisation occurs, graphene does not participate in reaction, but
During being, polymer can join together in growth course by the graphene of fragmentation as seam fragment cloth.
2nd, in reactant of the invention for graphene without particular/special requirement, be as long as no block or large area aggregation shape
Can, additive amount can be added arbitrarily according to conductive with light transmission rate needs, therefore possess wide industrial prospect.
3rd, present invention employs gas phase polymerization mode, inventor has made intensive studies discovery to the flow velocity of gas,
The flow velocity of gas is bigger, and the speed of polymerisation film forming is faster, but electric conductivity is bad；The flow velocity of gas is smaller, during reaction
Between it is longer, the film thickness of polymerisation is thicker, and electric conductivity is better, but light transmission rate decline.The present inventor is by anti-
Retrial is tested, and most gas flow rate is determined as 0-1m at last3/ h is preferably 0.1-1m3/h。
4th, inventor also has made intensive studies the temperature of phase polymerization reaction, it turns out that the higher film forming speed of temperature is more
Soon, but electric conductivity is variant, and by studying and testing repeatedly, most reaction temperature is determined as 40-90 DEG C at last, is preferably
50-60℃。
5th, there is excellent mechanics to bend for the OLED device of flexible compound electrode using the present invention and solar cell, can
To carry out bending, curling as needed.
Description of the drawings
Fig. 1 is flexible compound electrode production process schematic diagram；
Fig. 2 is the structure diagram of top light-emitting organic electroluminescent device；
Fig. 3 is the structure diagram of solar battery sheet.
Specific embodiment
In order to make the object, technical solutions and advantages of the present invention clearer, embodiments of the present invention will be made below
Further it is described in detail.The present invention can be embodied in many different forms, and should not be construed as limited to illustrate herein
Embodiment.On the contrary, provide these embodiments so that the disclosure will be thorough and complete, and will be the design of the present invention
Those skilled in the art are fully conveyed to, the present invention will only be defined by the appended claims.
The present invention can be embodied in many different forms, and should not be construed as limited to embodiment set forth herein.
On the contrary, provide these embodiments so that the disclosure will be thorough and complete, and the design of the present invention will be fully conveyed to
Those skilled in the art, the present invention will only be defined by the appended claims.In the accompanying drawings, for clarity, Ceng He areas can be exaggerated
The size and relative size in domain.It should be appreciated that when element such as layer, region or substrate are referred to as " being formed in " or " set
" another element " on " when, which can be arranged directly on another element or there may also be intermediary elements.
On the contrary, when element is referred to as on " being formed directly into " or " being set directly at " another element, there is no intermediary elements.
A kind of preparation method of flexible compound electrode, comprises the following steps：
S1, pyridine, trivalent iron salt catalyst and alcohols solvent are uniformly mixed, obtain performed polymer mixed liquor.
Pyridine in the performed polymer mixed liquor：Trivalent iron salt catalyst：Alcohols solvent molar ratio is (0.95-1.05):
(9.5-10.5):(95-105).The trivalent iron salt catalyst can be p-methyl benzenesulfonic acid iron or ferric trichloride, the alcohol
Class solvent can be n-butanol.S2, graphene is added in the performed polymer mixed liquor of step S1 preparations, and is coated uniformly on base
On plate, the heat drying under no water oxygen environment, obtain containing graphene, pyridine, trivalent iron salt catalyst dry substrate；Its
The temperature of middle heat drying is not strict with, as long as alcohols solvent can be promoted to evaporate.
S3, the dry substrate for preparing step S2, are put into and have been added dropwise in the reaction kettle of 3,4-rthylene dioxythiophene monomer,
Gas phase polymerization is carried out by the way that gas is heated, be passed through to reaction kettle, obtains flexible compound electrode；The gas is N2With/
Or inert gas, gas flow rate 0-1m3/ h is preferably 0.1-1m3Heating temperature is 40-90 DEG C in/h, the step S3, excellent
Elect 50-60 DEG C as.
S4, the flexible compound electrode that step S3 is obtained is cleaned using water or alcohols solvent, removes its surface
Trivalent iron salt catalyst.
Above-mentioned reaction process is：By to reaction kettle heating and being passed through gas, 3,4-rthylene dioxythiophene monomer simultaneously
EDOT gasifies, and is contacted in gaseous form with the catalyst on substrate, and under the catalytic action of catalyst, polymerisation occurs,
PEDOT (polyethylene dioxythiophene) polymer is become by EDOT monomers.During polymerisation occurs, graphene is not participated in instead
Should, but in the process, polymer can join together in growth course by the graphene of fragmentation as seam fragment cloth.
A kind of flexible compound electrode is prepared by the above method.
A kind of organic electroluminescence device including substrate and sequentially forms first electrode layer on the substrate, hair
Light unit and the second electrode lay, which is characterized in that the first electrode and/or second electrode are electric for the flexible compound
Pole, the thickness of the flexible compound electrode is 50nm-1000nm.
Organic electroluminescence device is top light-emitting organic electroluminescent device, and first electrode is the flexible compound electricity
Pole.
A kind of solar battery sheet, including the anode, photoelectric conversion unit and transparent cathode being sequentially overlapped, feature exists
In the transparent cathode is the flexible compound electrode.
Embodiment 1
As shown in Figure 1, the preparation method of the flexible compound electrode of the present embodiment, comprises the following steps：
S1, pyridine, trivalent iron salt catalyst and alcohols solvent are uniformly mixed, obtain 100g performed polymer mixed liquors；Wherein
Pyridine：Trivalent iron salt catalyst (p-methyl benzenesulfonic acid iron)：Alcohols solvent (n-butanol) molar ratio is 1:10:100.
S2,50g graphenes are added in the performed polymer mixed liquor of step S1 preparations, and are coated uniformly on substrate,
The heat drying under no water oxygen environment, obtain containing graphene, pyridine, trivalent iron salt catalyst dry substrate；
S3, the dry substrate for preparing step S2, are put into and have been added dropwise in the reaction kettle of 3,4-rthylene dioxythiophene monomer,
By being heated to 50-60 DEG C to reaction kettle, being passed through flow velocity as 0.5-1m3The N of/h2Gas carries out gas phase polymerization, obtains flexibility
Combination electrode；
S4, the flexible compound electrode that step S3 is obtained is cleaned using distilled water, removes the trivalent iron salt on its surface
Catalyst is to get flexible compound electrode.
Embodiment 2
The preparation method of the flexible compound electrode of the present embodiment, comprises the following steps：
S1, pyridine, trivalent iron salt catalyst and alcohols solvent are uniformly mixed, obtain 100g performed polymer mixed liquors；Wherein
Pyridine：Trivalent iron salt catalyst (ferric trichloride)：Alcohols solvent (n-butanol) molar ratio is 0.95:10.5:95.
S2,60g graphenes are added in the performed polymer mixed liquor of step S1 preparations, and are coated uniformly on substrate,
The heat drying under no water oxygen environment, obtain containing graphene, pyridine, trivalent iron salt catalyst dry substrate；
S3, the dry substrate for preparing step S2, are put into and have been added dropwise in the reaction kettle of 3,4-rthylene dioxythiophene monomer,
By being heated to 40-50 DEG C to reaction kettle, being passed through flow velocity as 0-0.5m3The inert gas of/h carries out gas phase polymerization, obtains
Flexible compound electrode；
S4, the flexible compound electrode that step S3 is obtained is cleaned using ethanol solution, removes the ferric iron on its surface
Salt catalyst is to get flexible compound electrode.
Embodiment 3
The preparation method of the flexible compound electrode of the present embodiment, comprises the following steps：
S1, pyridine, trivalent iron salt catalyst and alcohols solvent are uniformly mixed, obtain 100g performed polymer mixed liquors；Wherein
Pyridine：Trivalent iron salt catalyst (p-methyl benzenesulfonic acid iron)：Alcohols solvent (n-butanol) molar ratio is 1.05:9.5:105.
S2,20g graphenes are added in the performed polymer mixed liquor of step S1 preparations, and are coated uniformly on substrate,
The heat drying under no water oxygen environment, obtain containing graphene, pyridine, trivalent iron salt catalyst dry substrate；
S3, the dry substrate for preparing step S2, are put into and have been added dropwise in the reaction kettle of 3,4-rthylene dioxythiophene monomer,
By being heated to 60-90 DEG C to reaction kettle, being passed through flow velocity as 0.1-0.5m3The N of/h2Gas carries out gas phase polymerization, obtains soft
Property combination electrode；
S4, the flexible compound electrode that step S3 is obtained is cleaned using distilled water, removes the trivalent iron salt on its surface
Catalyst is to get flexible compound electrode.
It should be noted that the flexible compound electrode of the present invention for graphene without particular/special requirement, as long as no block or
Person's large area assembles shape, and additive amount can be added arbitrarily according to conductive with light transmission rate needs, need not stick to reality
Apply the dosage of example 1 to 3.
Embodiment 4
As shown in Fig. 2, a kind of top light-emitting organic electroluminescent device, including substrate 1 and is sequentially formed at the substrate
On first electrode layer 2, luminescence unit 3 and the second electrode lay 4, the first electrode layer 2 is prepared for embodiment 1-3
Flexible compound electrode Hybrid-electrode, the thickness of the flexible compound electrode is 50nm-1000nm.The luminous list
Member 3 is conventional luminescent layer, generally includes hole injection layer, hole transmission layer, luminescent layer, electron transfer layer, electron injecting layer etc..
Flexible compound electrode provided by the invention has versatility, to luminescence unit without particular/special requirement.
Embodiment 5
As shown in figure 3, a kind of solar battery sheet, including the substrate 5, anode 6,7 and of photoelectric conversion unit being sequentially overlapped
Transparent cathode 8, the transparent cathode 8 are the flexible compound electrode that embodiment 1-3 is prepared.The photoelectric conversion unit
7 be conventional structure, and flexible compound electrode provided by the invention has versatility, to photoelectric conversion unit without particular/special requirement.In view of
The not this Applicant's Abstract graph inventive point of photoelectric conversion unit, therefore this is repeated no more.
Obviously, the above embodiments are merely examples for clarifying the description, and is not intended to limit the embodiments.It is right
For those of ordinary skill in the art, can also make on the basis of the above description it is other it is various forms of variation or
It changes.There is no necessity and possibility to exhaust all the enbodiments.And the obvious variation thus extended out or
Among changing still in the protection domain of the invention.
Claims (10)
1. a kind of preparation method of flexible compound electrode, which is characterized in that comprise the following steps：
S1, pyridine, trivalent iron salt catalyst and alcohols solvent are uniformly mixed, obtain performed polymer mixed liquor；
S2, graphene is added in the performed polymer mixed liquor of step S1 preparations, and be coated uniformly on substrate, in no water oxygen
Heat drying under environment, obtain containing graphene, pyridine, trivalent iron salt catalyst dry substrate；
S3, the dry substrate for preparing step S2, are put into and have been added dropwise in the reaction kettle of 3,4-rthylene dioxythiophene monomer, pass through
To reaction kettle heating, gas progress gas phase polymerization is passed through, obtains flexible compound electrode；The gas is N2It is and/or lazy
Property gas.
2. the preparation method of flexible compound electrode according to claim 1, which is characterized in that the performed polymer mixed liquor
Middle pyridine：Trivalent iron salt catalyst：Alcohols solvent molar ratio is (0.95-1.05):(9.5-10.5):(95-105).
3. the preparation method of flexible compound electrode according to claim 1 or 2, which is characterized in that
The trivalent iron salt catalyst is p-methyl benzenesulfonic acid iron or ferric trichloride, and the alcohols solvent is n-butanol.
4. the preparation method of flexible compound electrode according to claim 1, which is characterized in that gas stream in the step S3
Speed is 0-1m3Heating temperature is 40-90 DEG C in/h, the step S3.
5. the preparation method of flexible compound electrode according to claim 4, which is characterized in that temperature is heated in the step S3
It spends for 50-60 DEG C.
6. the preparation method of flexible compound electrode according to claim 1, which is characterized in that further include following step：
S4, the flexible compound electrode that step S3 is obtained is cleaned using water or alcohols solvent, removes the trivalent on its surface
Iron salt catalyst.
7. a kind of flexible compound electrode, which is characterized in that be prepared using claim 1-6 any one of them methods.
8. a kind of organic electroluminescence device, including substrate and sequentially form first electrode layer on the substrate, shine
Unit and the second electrode lay, which is characterized in that the first electrode and/or second electrode are the flexibility described in claim 7
Combination electrode, the thickness of the flexible compound electrode is 50nm-1000nm.
9. organic electroluminescence device according to claim 8, which is characterized in that organic electroluminescence device shines for top
Organic electroluminescence device, first electrode are the flexible compound electrode described in claim 7.
10. a kind of solar battery sheet, including the anode, photoelectric conversion unit and transparent cathode being sequentially overlapped, which is characterized in that
The transparent cathode is the flexible compound electrode described in claim 7.
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| CN109870174A (en) * | 2019-03-08 | 2019-06-11 | 华南协同创新研究院 | A kind of flexible electrode and preparation method thereof |
| CN114864301A (en) * | 2022-04-12 | 2022-08-05 | 武汉工程大学 | Poly (3, 4-ethylenedioxythiophene)/graphene oxide composite electrode material and preparation method thereof |
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