CN110310763A - A kind of preparation method of the flexible transparent electrode based on PEDOT:PSS and silver nanowires - Google Patents
A kind of preparation method of the flexible transparent electrode based on PEDOT:PSS and silver nanowires Download PDFInfo
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Abstract
The flexible transparent electrode and preparation method thereof based on PEDOT:PSS and silver nanowires that the present invention provides a kind of, belong to technical field of semiconductors, the following steps are included: silver nanowires is put into solvent by (1), by the way that dispersing agent is added, evenly dispersed silver nanowires aqueous solution is obtained；(2) silver nanowires aqueous solution is added in modified PEDOT:PSS aqueous solution and obtains blend solution, PEDOT:PSS and the mass ratio of silver nanowires are 1:0.5-2 in blend solution；(3) blend solution is coated on substrate, obtains flexible transparent electrode after 80-230 DEG C of heat treatment.The present invention coats after PEDOT:PSS is blended with silver nanowires; the film of formation can wrap up silver nanowires; protect silver nanowires; prevent it from aoxidizing and increasing resistance; it is not in the phenomenon that resistance increases sharply that electrode that single layer structure is prepared experience, which repeatedly folds, stable mechanical performance, in addition; PEDOT:PSS has preferable film forming, thermal stability and translucency, is more satisfactory material of main part.
Description
Technical field
The invention belongs to technical field of semiconductors, and in particular to a kind of flexibility based on PEDOT:PSS and silver nanowires is saturating
The preparation method of prescribed electrode.
Background technique
Following photoelectric device will integrate the characteristics such as light, durable, reliable and stable, wearable, wherein most prominent spy
The direction that point is just towards flexible large area electron is developed, therefore it is to work as that preparation, which meets the flexible transparent electrode of future usage requirement,
Previous important research direction.Currently, tin indium oxide (ITO) is in photoelectric device such as touch screen, display and solar energy
Battery etc. is a kind of electrode material being most widely used, and is formed a film on flexible substrates by magnetron sputtering technique, also base
Originally it can satisfy the not high occasion of some flexibility requirements, this is because ITO has very excellent electrical conductivity and light transmittance, still
There is also some fatal disadvantages for it, for example matter is crisp, preparation process is complicated, at high cost, expensive.Therefore, it finds a kind of soft
It is good toughness, simple process, low in cost, and the ITO alternative materials with preferable electric conductivity and light transmittance become key.
Silver nanowires have excellent electric conductivity, bent, scalable, light transmittance is high and moderate, it is considered to be
A kind of most promising material of flexible transparent electrode is prepared, but, connecing silver nanowires between longitudinal relative to silver nanowires
Electric shock resistance is higher, poor for the adhesive force of substrate and environmentally sensitive, is easy to aoxidize in air, these problems limitation
The application development of silver nanowires in the opto-electronic device.
PEDOT is the polymer of EDOT (3,4-rthylene dioxythiophene monomer), with molecular structure is simple, energy gap is small, electric
The features such as conductance is high, be widely used as organic thin film solar cell, organic electroluminescent LED, electrochromic device, thoroughly
The research in the fields such as prescribed electrode, but the processability of PEDOT is bad.Polyelectrolyte polystyrolsulfon acid (PSS) is adulterated
Into PEDOT, can solve the processing problems of PEDOT, the PEDOT:PSS film of acquisition have high conductivity, high mechanical strength,
High transparency.PEDOT:PSS has many advantages, such as that good thermal stability and translucency and preparation process are simple, is flexible and transparent
Ideal one of the material of electrode.Nevertheless, the electric conductivity of PEDOT:PSS is not still able to satisfy the requirement as electrode,
Main problem is the PSS ingredient wherein to insulate, although the introducing of PSS improves the dissolubility and film forming of system,
So that the electric conductivity of polymer is declined, to also limit its scope of application to a certain extent.
In the prior art in order to which the electric conductivity for enhancing PEDOT can introduce conductive layer in PEDOT interlayer, silver nanowires is such as set
Layer, the structure that PEDOT layers of formation, silver nanowire layer are mingled with, since every layer in multilayered structure of bending stress is different, for a long time
Bending or repeatedly bending in the case of, the overall performance of film can be deteriorated, make sheet resistance with the increase of number of bends and
Become larger, mechanical stability is poor.
Summary of the invention
In view of this, the present invention provides a kind of preparation side of flexible transparent electrode based on PEDOT:PSS and silver nanowires
Method can prepare the high transparent electrode of thermal stability height, stable mechanical performance, good conductivity, transparency.
The present invention is a kind of preparation method of flexible transparent electrode based on PEDOT:PSS and silver nanowires, including following
Step:
(1) silver nanowires is put into solvent, dispersing agent is added, obtains silver nanowires aqueous solution, dispersing agent can be polyethylene
One of pyrrolidones, sodium carboxymethylcellulose, calgon, sodium tripolyphosphate are a variety of, and the diameter of silver nanowires is
25-30 nm, length are 20-25 μm, and the mass concentration of silver nanowires aqueous solution is 0.5-10 mg/ml.Silver nanowires exists
The uniformity of dispersion in PEDOT:PSS solution directly influences the electric conductivity of film.Silver nanowires itself may be enclosed with table
Face activating agent, but these surfactants may not be able to cross silver nanowires particle in guarantee silver nanoparticle aqueous solution (suspension)
It can be uniformly dispersed, so needing to add suitable dispersing agent silver nanowires can be uniformly dispersed in suspension, solvent
It can be deionized water.
(2) silver nanowires aqueous solution is added in modified PEDOT:PSS aqueous solution and obtains blend solution, silver nanowires
It is dispersed in the aqueous solution of PEDOT:PSS and forms homogeneous system, the solid concentration of PEDOT:PSS aqueous solution is 1.0-1.3%, institute
Stating PEDOT:PSS and the mass ratio of silver nanowires in blend solution is 1:0.5-2, since silver is received under the conditions of long-time is placed
Rice noodles are easy to reunite, therefore blend solution needs to stir using magnetic before the use, guarantees that silver nanowires is dispersed in
In PEDOT:PSS aqueous solution, whether distribution of the silver nanowires in surface layer film uniformly directly affects its electrode after coating
Electric conductivity, so the uniformity of blend solution directly affects the electric conductivity of finished product.
The work function of the PEDOT:PSS is more than or equal to 5.0 eV or is less than or equal to 3 eV.Meanwhile PEDOT:PSS changes
Property uses one of polyethyleneimine, polyethoxy aziridine, ZnO nanoparticle or a variety of.
The work function of PEDOT:PSS has wider adjustability, PEDOT:PSS work function (5.0 usually with higher
EV or more), using the transparent electrode of the PEDOT:PSS preparation more than or equal to 5.0 eV of work function can be to be used for as anode
In organic electro-optic device；But the work function of PEDOT:PSS can be by compound with ZnO nanoparticle, or uses polyethylene
Imines (PEI) and its derivative polyethoxy aziridine (PEIE) etc. handle PEDOT layers of PEDOT solution or modification, reduce
The work function of PEDOT:PSS makes work function be less than or equal to 3.0 eV, and the electrode prepared, can be by right as cathode
The adjusting of PEDOT:PSS work function realizes the whole soln device preparation technology based on PEDOT:PSS unitary system, simplifies device
Part preparation process reduces production cost.
(3) blend solution is coated on substrate, flexible and transparent electricity is obtained after 80-230 DEG C of heat treatment 5-20min
Pole.
Soda-lime glass substrate can be used in substrate, and cleaning treatment is needed before use, and the process of processing includes using dedicated
Glass cleaner, acetone, isopropanol and deionized water etc. successively carry out each ultrasonic cleaning in 10 minutes, and with being dried with nitrogen, so
It is handled 10 minutes using UV ozone afterwards；It is also possible to PET flexible substrate, scale removal process is acetone, isopropanol and deionized water
Deng successively carrying out each ultrasonic cleaning in 10 minutes, and with being dried with nitrogen, then handled 5 minutes using UV ozone.Blend solution
Coating method can be used spin-coating method, spin speed is 1000-4000 revs/min, spin-coating time 1-2 minutes.
PEDOT:PSS has preferable thermal stability, and heat treatment temperature can achieve 200 DEG C or more, with silver nanowires
Optimal heat treatment temperature can have relatively good matching.Heat treatment is the processing that silver nanowires random grid conductive film layer is formed
Method, PEDOT:PSS can also fill the node of silver nanowires, improve the electric conductivity of system.
The effect that heat treatment improves film layer conductive capability is obvious, square resistance (hereinafter referred to as sheet resistance) main source of film layer
Contact resistance between silver nanowires.Before not heat-treated, the contact in film layer between silver nanowires be may be considered
Stacked overlap joint under gravity, and since silver nanowires is liquid phase method preparation, on silver nanowires surface, remaining has protective agent
Or surfactant PVP, so the sheet resistance of the silver nanowires film without Overheating Treatment is relatively higher, there are also the skies promoted
Between.For example 200 DEG C of heat treatment can exclude the remaining PVP of silver nanowires lap-joint and contact it directly, while can be with
Make the overlapped points between silver nanowires that melting welding occur, realize the metallurgical bonding of contact point, so that contact resistance reduces.Another party
Face, heat treatment can make PEDOT:PSS film have the more regular appearance structure for more having orientation, so that PEDOT:PSS's leads
Electrically enhancing.
The grid of different-diameter silver nanowires composition, nanometer size effect is strong and weak different, the temperature and time of heat treatment
It is not quite similar, generally between 120 ~ 220 DEG C.Usual silver nanowires is thicker, and temperature capacity is stronger, the heat treatment temperature of film layer
Higher, the time is also longer.The preferable thermal stability of PEDOT:PSS enough adapts to the preparation processing of various sizes of silver nanowires.
PEDOT:PSS is as cementing medium, the work using the mobility and gelatification of Polymer Solution, on macromolecular chain
Property the formation of functional group and substrate surface be bonded, while macromolecular chain is filled in the gap of silver nanowires conductive grid, PEDOT:
PSS itself is conductive, and filling grid-gap can increase the electric conductivity of electrode, film forming.In addition the two is blended and can protect
The transparency for demonstrate,proving the transparent electrode of support avoids the defect of the reduction of translucency caused by multiple-layer stacked, the structure energy of single layer
Enough make electrode that there is good mechanical stability.
Further, since the work function of PEDOT:PSS have wider adjustability, can by select Different treatments,
Prepare anode or cathode based on PEDOT:PSS.
Present invention is mainly applied to luminescent device and solar cell device, these devices have translucency requirement to electrode,
So the translucency of product is an important parameter, the quality of luminescent device and solar cell device is directly affected.
Both PEDOT:PSS and silver nanowires are combined by the present invention, are learnt from other's strong points to offset one's weaknesses, and the advantage of the two is given full play to,
Not only there is good electric conductivity, film forming and light transmittance, but also there is preferable flexibility and stability, in addition, using whole soln
Processing technology can be adapted for the printing preparation of device, realize flexible broad area device application.In addition of the invention by PEDOT:
PSS is coated after being blended with silver nanowires, and the film of formation can wrap up silver nanowires, protection silver nanowires prevent its aoxidize and
Increase resistance, even if it is not in what resistance increased sharply that the electrode that the structure of single layer is prepared repeatedly folds when installation
In addition phenomenon, stable mechanical performance use PEDOT:PSS rather than individual PEDOT, production process is simple, do not have to be added
Special solvent, and the thermal stability of product and translucency are fine.
Detailed description of the invention
Fig. 1 is a kind of flexible and transparent based on PEDOT:PSS and silver nanowires provided in the specific embodiment of the invention
The light transmittance figure of the transparent electrode of the preparation method preparation of electrode；
Fig. 2 is a kind of flexible transparent electrode based on PEDOT:PSS and silver nanowires provided in the specific embodiment of the invention
The figure compared with the resistance meanders performance of the commercial flexible ITO electrode based on PET.
Specific embodiment
The present invention will be described in detail With reference to embodiment.
Embodiment 1
A kind of preparation method of the flexible transparent electrode based on PEDOT:PSS and silver nanowires, comprising the following steps:
(1) silver nanowires is put into solvent, polyethylene of dispersing agent pyrrolidones is added, obtains silver nanowires aqueous solution, Yin Na
The diameter of rice noodles is 25 nm, and length is 20 μm, and the mass concentration of silver nanowires aqueous solution is 0.5mg/ml；
(2) silver nanowires aqueous solution is added in modified PEDOT:PSS aqueous solution and obtains blend solution, silver nanowires dispersion
Homogeneous system is formed in the aqueous solution of PEDOT:PSS, the solid concentration of PEDOT:PSS aqueous solution is 1.0%, and the blending is molten
PEDOT:PSS and the mass ratio of silver nanowires are 1:0.5 in liquid, and the work function of the PEDOT:PSS is equal to 5.0 eV；
(3) it by 1000 revs/min of the blend solution, is spun on soda-lime glass substrate within spin-coating time 1 minute, 100 DEG C of heat treatments
Flexible and transparent anode electrode is obtained after 5min.
The square resistance of gained flexible transparent electrode is 43.68 Ω/, and the light transmittance at 550nm is 88%.
Embodiment 2
A kind of preparation method of the flexible transparent electrode based on PEDOT:PSS and silver nanowires, comprising the following steps:
(1) silver nanowires is put into solvent, sodium hexametaphosphate dispersant is added, obtains silver nanowires aqueous solution, silver nanowires
Diameter be 30 nm, length is 25 μm, and the mass concentration of silver nanowires aqueous solution is 10 mg/ml；
(2) silver nanowires aqueous solution is added in modified PEDOT:PSS aqueous solution and obtains blend solution, silver nanowires dispersion
Homogeneous system is formed in the aqueous solution of PEDOT:PSS, the solid concentration of PEDOT:PSS aqueous solution is 1.3%, and the blending is molten
PEDOT:PSS and the mass ratio of silver nanowires are 1:2 in liquid, and the work function of the PEDOT:PSS is equal to 3 eV.Meanwhile
PEDOT:PSS modification uses polyethyleneimine；
(3) it by 4000 revs/min of the blend solution, is spun on soda-lime glass substrate within spin-coating time 2 minutes, 150 DEG C of heat treatments
Flexible transparent electrode (cathode) is obtained after 20min.
The square resistance of gained flexible transparent electrode is 34.82 Ω/, and the work function of film surface is 4.84eV,
Light transmittance at 550nm is 89%.
Polyethyleneimine is changed into the performance and this implementation of the electrode of polyethoxy aziridine or ZnO nanoparticle preparation
Example is close.
Embodiment 3
A kind of preparation method of the flexible transparent electrode based on PEDOT:PSS and silver nanowires, comprising the following steps:
(1) silver nanowires is put into solvent, pentasodium triphosphate of dispersing agent is added, obtains silver nanowires aqueous solution, silver nanowires
Diameter be 26 nm, length is 22 μm, and the mass concentration of silver nanowires aqueous solution is 5 mg/ml；
(2) silver nanowires aqueous solution is added in modified PEDOT:PSS aqueous solution and obtains blend solution, silver nanowires dispersion
Homogeneous system is formed in the aqueous solution of PEDOT:PSS, the solid concentration of PEDOT:PSS aqueous solution is 1.1%, and the blending is molten
PEDOT:PSS and the mass ratio of silver nanowires are 1:1 in liquid, and the work function of the PEDOT:PSS is 5.5 eV；
(3) it by 2000 revs/min of the blend solution, is spun on soda-lime glass substrate within spin-coating time 1.5 minutes, at 200 DEG C of heat
Flexible transparent electrode is obtained after reason 10min.
The square resistance of gained flexible transparent electrode is 38.86 Ω/, and the light transmittance at 550nm is 88%.
Embodiment 4
A kind of preparation method of the flexible transparent electrode based on PEDOT:PSS and silver nanowires, comprising the following steps:
(1) silver nanowires is put into solvent, pentasodium triphosphate of dispersing agent is added, obtains silver nanowires aqueous solution, silver nanowires
Diameter be 26 nm, length is 22 μm, and the mass concentration of silver nanowires aqueous solution is 5 mg/ml；
(2) silver nanowires aqueous solution is added in modified PEDOT:PSS aqueous solution and obtains blend solution, silver nanowires dispersion
Homogeneous system is formed in the aqueous solution of PEDOT:PSS, the solid concentration of PEDOT:PSS aqueous solution is 1.1%, and the blending is molten
PEDOT:PSS and the mass ratio of silver nanowires are 1:1 in liquid, and the work function of the PEDOT:PSS is 5.5 eV；
(3) it by 2000 revs/min of the blend solution, is spun on soda-lime glass substrate within spin-coating time 1 minute, 230 DEG C of heat treatments
Flexible transparent electrode is obtained after 10min.
The square resistance of gained flexible transparent electrode is 43.76 Ω/, and the light transmittance at 550nm is 88%.
Embodiment 5
A kind of preparation method of the flexible transparent electrode based on PEDOT:PSS and silver nanowires, comprising the following steps:
(1) silver nanowires is put into solvent, dispersing agent sodium carboxymethylcellulose is added, obtains silver nanowires aqueous solution, Yin Na
The diameter of rice noodles is 30 nm, and length is 22 μm, and the mass concentration of silver nanowires aqueous solution is 5 mg/ml；
(2) silver nanowires aqueous solution is added in modified PEDOT:PSS aqueous solution and obtains blend solution, silver nanowires dispersion
Homogeneous system is formed in the aqueous solution of PEDOT:PSS, the solid concentration of PEDOT:PSS aqueous solution is 1.1%, and the blending is molten
PEDOT:PSS and the mass ratio of silver nanowires are 1:1 in liquid, and the work function of the PEDOT:PSS is 5.5 eV；
(3) it by 3000 revs/min of the blend solution, is spun on PET substrate within spin-coating time 1 minute, after 80 DEG C of heat treatment 10min
Obtain flexible transparent electrode.
The square resistance of gained flexible transparent electrode is 51.21 Ω/, and the light transmittance at 550nm is greater than 92%.
Embodiment 6
A kind of preparation method of the flexible transparent electrode based on PEDOT:PSS and silver nanowires, comprising the following steps:
(1) silver nanowires is put into solvent, pentasodium triphosphate of dispersing agent is added, obtains silver nanowires aqueous solution, silver nanowires
Diameter be 25 nm, length is 22 μm, and the mass concentration of silver nanowires aqueous solution is 5 mg/ml；
(2) silver nanowires aqueous solution is added in modified PEDOT:PSS aqueous solution and obtains blend solution, silver nanowires dispersion
Homogeneous system is formed in the aqueous solution of PEDOT:PSS, the solid concentration of PEDOT:PSS aqueous solution is 1.1%, and the blending is molten
PEDOT:PSS and the mass ratio of silver nanowires are 1:1 in liquid, and the work function of the PEDOT:PSS is 5.5 eV；
(3) it by 2000 revs/min of the blend solution, is spun on PET substrate within spin-coating time 1 minute, 100 DEG C of heat treatment 10min
After obtain flexible transparent electrode.
The square resistance of gained flexible transparent electrode is 38.71 Ω/, and the work function of film surface is 4.86eV,
Light transmittance at 550nm is greater than 91%, as shown in Figure 1.In addition, as shown in Fig. 2, being carried out under conditions of bending radius is 5 millimeters
The crooked experiment of membrane electrode (the Ag- PET in figure), in experiment bending range, square resistance is almost unchanged, passes through
Nearly 300 bendings, resistance change rate is less than 2%, and the ITO-PET in the commercial flexible ITO(figure based on PET) electrode
Resistance change rate by 30 times after being bent just more than 300%.Transparent flexible electrode in the present invention shows excellent machinery
Stability.
Embodiment 7
A kind of preparation method of the flexible transparent electrode based on PEDOT:PSS and silver nanowires, comprising the following steps:
(1) silver nanowires is put into solvent, polyethylene of dispersing agent pyrrolidones, calgon, sodium tripolyphosphate is added, obtains
To silver nanowires aqueous solution, the diameter of silver nanowires is 25-30 nm, and length is 20-25 μm, the quality of silver nanowires aqueous solution
Concentration is 0.5-10 mg/ml.
(2) silver nanowires aqueous solution is added in modified PEDOT:PSS aqueous solution and obtains blend solution, silver nanowires
It is dispersed in the aqueous solution of PEDOT:PSS and forms homogeneous system, the solid concentration of PEDOT:PSS aqueous solution is 1.0-1.3%, institute
Stating PEDOT:PSS and the mass ratio of silver nanowires in blend solution is 1:0.5-2, and the work function of the PEDOT:PSS is greater than
Equal to 5.0 eV or it is less than or equal to 3 eV.Meanwhile PEDOT:PSS modification uses polyethyleneimine, polyethoxy ethylene
One of imines, ZnO nanoparticle are a variety of.
(3) by 1000-4000 revs/min of the blend solution, soda-lime glass substrate, PET are spun within spin-coating time 1-2 minutes
In flexible substrate, flexible transparent electrode is obtained after 80-160 DEG C of heat treatment 5-20min.
Both PEDOT:PSS and silver nanowires are combined by the present invention, are learnt from other's strong points to offset one's weaknesses, and the advantage of the two is given full play to,
Not only there is good electric conductivity, film forming and light transmittance, but also there is preferable flexibility and stability, in addition, using whole soln
Processing technology can be adapted for the printing preparation of device, realize flexible broad area device application.In addition of the invention by PEDOT:
PSS is coated after being blended with silver nanowires, and the film of formation can wrap up silver nanowires, prevents it from aoxidizing and increasing resistance, single
Even if it is not in the phenomenon that resistance increases sharply, mechanicalness that the electrode that the structure of layer is prepared repeatedly folds when installation
It can stablize, in addition use PEDOT:PSS rather than individual PEDOT, production process is simple, without special solvent is added,
And the thermal stability and translucency of product are fine.
The present invention is not limited to above-mentioned specific embodiment, and the invention may be variously modified and varied.All foundations
Technical spirit of the invention should be included in the present invention to embodiment of above any modification, equivalent replacement, improvement and so on
Protection scope.
Claims (8)
1. a kind of preparation method of the flexible transparent electrode based on PEDOT:PSS and silver nanowires, which is characterized in that including following
Step:
(1) silver nanowires is put into solvent, by the way that dispersing agent is added, obtains evenly dispersed silver nanowires aqueous solution；
(2) silver nanowires aqueous solution is added in modified PEDOT:PSS aqueous solution and obtains blend solution, the blend solution
Middle PEDOT:PSS and the mass ratio of silver nanowires are 1:0.5-2；
(3) blend solution is coated on substrate, obtains flexible transparent electrode after 80-230 DEG C of heat treatment.
2. a kind of preparation method of flexible transparent electrode based on PEDOT:PSS and silver nanowires according to claim 1,
It is characterized in that, the work function of the PEDOT:PSS is more than or equal to 5.0 eV.
3. a kind of preparation method of flexible transparent electrode based on PEDOT:PSS and silver nanowires according to claim 1,
It is characterized in that, the work function of the PEDOT:PSS is less than or equal to 3 eV.
4. a kind of preparation method of flexible transparent electrode based on PEDOT:PSS and silver nanowires according to claim 3,
It is characterized in that, the PEDOT:PSS is modified to use polyethyleneimine, polyethoxy aziridine, in ZnO nanoparticle
It is one or more.
5. a kind of preparation method of flexible transparent electrode based on PEDOT:PSS and silver nanowires according to claim 1,
It is characterized in that, the diameter of the silver nanowires is 25-30 nm, length is 20-25 μm.
6. a kind of preparation method of flexible transparent electrode based on PEDOT:PSS and silver nanowires according to claim 5,
It is characterized in that, the mass concentration of silver nanowires aqueous solution is 0.5-10 mg/ml.
7. a kind of preparation method of flexible transparent electrode based on PEDOT:PSS and silver nanowires according to claim 1,
It is characterized in that, the solid concentration of the PEDOT:PSS aqueous solution is 1.0-1.3%.
8. a kind of preparation method of flexible transparent electrode based on PEDOT:PSS and silver nanowires according to claim 1,
It is characterized in that, the dispersing agent is polyvinylpyrrolidone, in sodium carboxymethylcellulose, calgon, sodium tripolyphosphate
It is one or more.
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