CN106299160A - A kind of using plasma technical finesse nano silver wire the method preparing organic optoelectronic device flexible electrode by substrate transfer - Google Patents
A kind of using plasma technical finesse nano silver wire the method preparing organic optoelectronic device flexible electrode by substrate transfer Download PDFInfo
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- CN106299160A CN106299160A CN201611001115.8A CN201611001115A CN106299160A CN 106299160 A CN106299160 A CN 106299160A CN 201611001115 A CN201611001115 A CN 201611001115A CN 106299160 A CN106299160 A CN 106299160A
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- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K71/00—Manufacture or treatment specially adapted for the organic devices covered by this subclass
- H10K71/60—Forming conductive regions or layers, e.g. electrodes
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- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
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Abstract
A kind of using plasma technical finesse nano silver wire also shifts the method preparing OLED flexible electrode by substrate, belongs to organic optoelectronic technical field.First configuration nano silver wire solution, then spin coating nano silver wire on silicon chip, after obtaining nano silver wire thin film, by Cement Composite Treated by Plasma nano silver wire thin film, on the one hand eliminates the PVP of nanowire surface, on the one hand have also been changed the surface topography of nano silver wire；Spin coating photocrosslinkable polymer on silicon chip afterwards so that it is nano silver wire thin film is completely covered, after ultra violet lamp, uses scalpel to be separated with silicon substrate by photocrosslinkable polymer, finally gives the nano silver wire transparency electrode of high conductivity.The method of the invention reduces the surface roughness of nano silver wire thin film, improves the uniformity of nano silver wire film surface, and prepared OLED flexible electrode is better than the electrode that traditional heat treatment method obtains in electric conductivity, and more time-consuming.
Description
Technical field
The invention belongs to organic optoelectronic technical field, be specifically related to a kind of using plasma technical finesse nano silver wire
And the method preparing OLED flexible electrode is shifted by substrate.
Background technology
OLED (Organic Light Emitting Diode) has that luminous efficiency is high, driving voltage is low, fast response time, rich color, right
Ratio Du Gao and the visualization advantages such as angle is big, suffer from splendid application prospect in illumination and plane display field.OLED sends out
Photosphere and carrier blocking layers all use organic material to make, and have good bending property, accordingly, it is capable to no, to prepare performance good
Good flexible electrode just becomes the key of flexible OLED development.At present, the main electrode material that OLED industrialization produces is ITO
(tin-doped indium oxide), this electrode has higher visible light transmittance rate and infrared reflectivity, relatively low resistivity and good
Chemical stability.But after repeatedly bending, the square resistance of ITO electrode can rise rapidly, therefore it is unfavorable for making
Flexible OLED, and the rare of indium resource also makes its manufacturing cost be greatly improved.Therefore, in order to replace ITO electrode, use silver nanoparticle
Flexible electrode prepared by the materials such as line, PEDOT:PSS, Graphene is come out one after another.
Wherein, nano silver wire electrode causes extensively note because it has good electric conductivity and excellent mechanical bend performance
Meaning.Nano silver wire can be prepared by reduction of ethylene glycol silver nitrate, generally also needs to add surfactant polyvinyl pyrrole
Alkanone (poly (vinyl pyrrolidone), PVP) improves silver nanowire growth uniformity.Therefore, the silver nanoparticle prepared
Line surface would generally remain PVP, and this can affect the electric conductivity of nano silver wire.
Nano silver wire thin film is generally prepared by solution methods such as spin coating, rod painting, slot coated.Prepare by this method
Thin film, the distribution of film surface nano silver wire is random, and the contact between nano silver wire and nano silver wire is the most very
Closely.At the node having more nano silver wire to intersect, its apparent height can be higher than other positions, and this can cause nano silver wire thin
The surface roughness of film is too high, and the electric conductivity on surface is uneven.For OLED, due to the thickness that device is overall
The least, the most hundreds of nanometer, if the surface roughness of electrode is excessive, then may to penetrate hole transmission layer the most luminous for electrode layer
Layer, makes device occur bad point in luminescence process.If surface conductivity is uneven, then local current can be caused excessive, heating
Too much, device is burnt out.
In order to solve surface roughness this problem excessive, it has been proposed that a lot of way, such as thermal annealing, applying machinery pressure
Power, substrate transfer etc..Wherein, substrate transfer method will be wrapped in the polymer of liquid by nano silver wire, then makes to use up, heat
Being solidified by polymer etc. method, nano silver wire will be wrapped in the polymer, afterwards can be by it from the substrate of original deposition
On strip down, the surface roughness of nano silver wire the most both can be reduced to the magnitude of a few nanometer, substrate can be realized again
Flexibility.
Plasma is made up of a large amount of free electrons and ion and a small amount of unionized gas molecule and atom, and
It is shown generally as being similar to electroneutral ionized gas.In the plasma, the Coulomb force between charged particle is long range force,
The action effect of Coulomb force collides effect considerably beyond the contingent local short range of charged particle.Band electrochondria in plasma
During son motion, positive charge or negative charge concentration of local can be caused, produce electric field；Electric charge directed movement causes electric current, produces magnetic field.
Electric field and magnetic field to affect the motion of other charged particles, and along with extremely strong heat radiation and conduction of heat.Plasma presses it
Temperature can be divided into high-temperature plasma and low temperature plasma.Wherein the particle temperature in high-temperature plasma be up to up to ten million be
To more than one hundred million degree, it is mainly used in the controllable nuclear fusion of energy field.Particle temperature in low temperature plasma also reach thousands of or even
Tens thousand of degree, can make molecule or atom dissociation, ionization, chemical combination etc., by low temperature plasma can realize etching, removing surface and
Surface modification, material such as prepare at the function.
Summary of the invention
It is an object of the invention to provide the processing method of a kind of nano silver wire electrode, this method by Cement Composite Treated by Plasma and
Substrate transfer method combines.First configuration nano silver wire solution, then spin coating nano silver wire on silicon chip, obtains silver nanoparticle
After line thin film, by Cement Composite Treated by Plasma nano silver wire, on the one hand eliminate the PVP on nano silver wire surface, on the one hand also change
The surface topography of nano silver wire, then transfers to, in flexible substrate, reduce by nano silver wire by substrate transfer method simultaneously
Know clearly the surface roughness of nano silver wire thin film, improve the uniformity of nano silver wire film surface, finally given performance good
Good nano silver wire OLED flexible electrode.
A kind of using plasma technical finesse nano silver wire of the present invention is the most soft by substrate transfer preparation OLED
The method of property electrode, it concretely comprises the following steps:
1) spin coating nano silver wire solution on substrate after the cleaning process, obtains nano silver wire thin film；
2) the nano silver wire thin film that Cement Composite Treated by Plasma is prepared on substrate is used；
3) spin coating photocrosslinkable polymer on nano silver wire thin film after treatment；
4) ultra violet lamp photocrosslinkable polymer is used so that it is solidification；
5) photocrosslinkable polymer after solidification is stripped down from substrate, thus finally given and be polymerized with photo-crosslinking
Thing is the nano silver wire OLED flexible electrode of substrate.
Said method step 1) described in substrate 1 be the rigid substrate such as silicon chip, glass；
Said method step 1) described in a diameter of 20～100 nanometers of nano silver wire, a length of 20～150 microns,
The concentration of nano silver wire solution is 1～10mg/mL, and the solvent of nano silver wire solution is ethanol, isopropanol etc., spin coating nano silver wire
The speed of thin film is 5000～9000 revs/min, and the thickness of nano silver wire thin film is 50～400 nanometers.
Said method step 2) described in the source of the gas of plasma be the noble gas such as argon, nitrogen, so can in case
Only nano silver wire is oxidized.The power of Cement Composite Treated by Plasma is 80～150W, and the process time of plasma is 1～30 minute,
The best power size of Cement Composite Treated by Plasma and process time need to enter respectively according to the length of nano silver wire and the difference of diameter
Row optimizes；
Said method step 3) described in photocrosslinkable polymer be ultra-violet curing optical cement or EVA glue (ethylene-acetate
Vinyl ester copolymers), the thickness of the photocrosslinkable polymer that spin coating obtains is 30～70 microns；
Said method step 4) described in the power of uviol lamp be 100～200W, the time of ultra violet lamp is 3～4
Minute.
Accompanying drawing explanation
The square resistance variation diagram of different disposal time sample in Fig. 1: embodiment 1.Line 1,2,3,4,5,6 represents use respectively
Cement Composite Treated by Plasma 1min, the sample of 5min, 10min, 15min, 20min, 30min, line 7 and line 8 represent the most respectively without
Cement Composite Treated by Plasma and toast the sample of 15min at 150 DEG C.
The optical transmittance schematic diagram of different disposal time sample in Fig. 2: embodiment 1.Curve 1,2,3,4,5,6 generation respectively
Table Cement Composite Treated by Plasma 1min, the sample of 5min, 10min, 15min, 20min, 30min, curve 7 and curve 8 are then distinguished
Represent sample that is the most plasma-treated and that toast 15min at 150 DEG C.
Blue film paste position and nano silver wire OLED flexible electrode shape in Fig. 3: embodiment 2.
Fig. 4: (a) is through plasma treatment with without the OLED brightness-voltage curve of plasma treatment；(b) warp
Cross plasma treatment and the OLED current density voltage curve without plasma treatment.
Detailed description of the invention
Embodiment 1
In order to confirm feasibility and the superiority of this method, we have made silver nanoparticle according to step described in summary of the invention
Line electrode, tests square resistance and the transmitance of electrode.It is embodied as step as follows:
1) prepare the silicon chip of 8 2.5cm × 2.5cm, use the cotton balls wiping silicon chip surface being moistened with acetone, ethanol successively,
Use deionized water rinsing silicon chip afterwards, remove the Cotton Gossypii residual on surface.It is sequentially placed into acetone, ethanol and deionization the most again
Carrying out supersound process in water, the time of supersound process is 5 minutes.After process completes, nitrogen air gun is used to be blown by silicon chip surface
Dry；
2) configuration concentration is the nano silver wire of 5mg/mL, and the solvent of nano silver wire is ethanol, a diameter of the 90 of nano silver wire
Nanometer, a length of 20～60 microns；Rock solution after having configured 5 minutes, make nano silver wire more be evenly dispersed in ethanol
In solvent；
3) in step 1) the silicon chip surface spin-coating step 2 that obtains) the nano silver wire solution that obtains, the rotating speed of spin coating is 8000
Revolutions per second, the spin coating parameters on 8 silicon chips keeps consistent, thus obtains nano silver wire thin film on a silicon substrate, the thickness of thin film
It is 150 nanometers；
4) being respectively adopted the different process time (1min, 5min, 10min, 15min, 20min, 30min) comes silver nanoparticle
Line thin film carries out Cement Composite Treated by Plasma, to probe into the optimal process time.The generator of plasma is HARRICK
The plasma cleaning instrument that PLASMA produces, the power of setting is 100W, and the source of the gas of plasma is argon.Additionally also has one not
The silicon chip and the process that carry out Cement Composite Treated by Plasma heat 150 DEG C of bakings silicon chip of 15 minutes as a control group；
5) after having processed, at nano silver wire surface spin coating photocrosslinkable polymer NOA63, the thickness of spin coating is 40 microns；
Being put into by silicon chip afterwards in darkroom and use ultra violet lamp 4 minutes, uviol lamp power is 150W.After irradiation completes, photo-crosslinking is polymerized
Thing becomes solid completely, is wrapped in wherein by nano silver wire.
6) blade is used to be separated with silicon chip edge by NOA63, then with tweezers, NOA63 is whole together with nano silver wire thin film
Strip down from silicon chip, complete substrate transfer, thus prepare the nano silver wire OLED flexible electrical with low square resistance
Pole.
7) use the optical transmittance of UV3600 spectrophotometer test sample after, use four probe square resistance tests
The square resistance of instrument test sample, and compare the treatment effect of different disposal time.
8) change of the square resistance of different disposal time sample is as shown in Figure 1.Each sample tests 6 at diverse location
The value of square resistance, the point in figure is these 6 worth averages, error bar then represent often in group data and average it
The maximum of difference, if error is bar, (in FIG, error bar is the amplitude that meansigma methods both sides swing) is the biggest, then prove
The nano silver wire on print surface is the most uneven.As can be seen from the figure:
1) when plasma treatment is 15min, effect is best, and square resistance can be reduced to 7.2 Ω/；
2) when the process time is between 5～20min, the uniformity of nano silver wire is improved and square resistance substantially drops
Low, thus during Cement Composite Treated by Plasma 5～20min, all can significantly improve the performance of nano silver wire thin film；
3) treatment effect of plasma 1min is still better than 150 DEG C of bakings 15 minutes, therefore may certify that plasma
Process is the very effective a kind of method improving nano silver wire electric conductivity.
9. the situation of change of the optical transmittance of different disposal time sample is as shown in Figure 2.The length scanning model of transmitance
Enclosing is 400～800 nanometers, and the transmitance typically choosing 550 nanometers is reference value.
As can be seen from the figure:
1) untreated nano silver wire transmitance is the highest, reaches 77.3% in 550 nanometers, after Cement Composite Treated by Plasma thoroughly
Rate of crossing generally decreases, but is above 150 DEG C of bakings nano silver wire of 15 minutes.
2) although the optical transmittance of nano silver wire slightly reduces after plasma treatment, but its amplitude reduced and square
The reduction amplitude of resistance is compared much smaller.
As can be seen here, after Cement Composite Treated by Plasma, the combination property of nano silver wire electrode is strengthened.
Embodiment 2
In order to confirm that nano silver wire electrode after treatment is suitably applied flexible OLED, we use above-mentioned electrode system
Make OLED.Specifically comprise the following steps that
1) use the method mentioned in embodiment 1 to make nano silver wire electrode, owing to needs make OLED, therefore exist
Step 2) need to add a step afterwards, i.e. paste the PVC indigo plant membrane adhesive tape of strip structure near edge in the both sides of substrate top surface,
Carry out spin coating the most again, nano silver wire thin film so can be made only to be spin-coated on the substrate of zone line, thus realize bar shaped
The preparation of electrode, the position of blue film stickup and the shape of electrode are as shown in Figure 3.Once can put during due to preparation OLED
The print entered is limited, therefore the process time of plasma choose that effect in embodiment 1 is best 15 minutes；
2) using evaporation coating mechanism to make OLED, the structure of device is:
NOA63/ nano silver wire/MoO3(2nm)/m-M(30nm)/NPB(20nm)/Alq3(50nm)/Liq(0.5nm)/Al
(100nm)；
We made respectively OLED based on the nano silver wire electrode through 15 minutes plasma treatment and based on
OLED through 150 DEG C of heat treatments nano silver wire electrode of 15 minutes；
3) I-V characteristic of OLED is tested；
Fig. 4 (a) and (b) are luminance-voltage and the current density voltage curve of device respectively, as can be seen from the figure warp
The thread OLED of silver nanoparticle crossing plasma treatment whether still will be better than undressed silver at electric current in brightness
Nano wire.
In sum: after plasma treatment, the square resistance of nano silver wire thin film significantly reduces, and transmitance is almost
Unaffected, compared to heat treatment, the time of plasma treatment is shorter, and effect is more preferable.By the electrode system after plasma treatment
After becoming OLED, the electric current of device and brightness are intended to be substantially better than the device without plasma treatment, it is seen that at plasma
Reason is a kind of efficiency height and effect significant nano silver wire Electrode treatment method.
Claims (6)
1. a using plasma technical finesse nano silver wire prepare organic optoelectronic device flexible electrical by substrate transfer
The method of pole, its step is as follows:
1) spin coating nano silver wire solution on substrate after the cleaning process, obtains nano silver wire thin film；
2) the nano silver wire thin film that Cement Composite Treated by Plasma is prepared on substrate is used；
3) spin coating photocrosslinkable polymer on nano silver wire thin film after treatment；
4) ultra violet lamp photocrosslinkable polymer is used so that it is solidification；
5) photocrosslinkable polymer after solidification is stripped down from substrate, thus finally given and with photocrosslinkable polymer be
The nano silver wire OLED flexible electrode of substrate.
2. using plasma technical finesse nano silver wire as claimed in claim 1 a kind of being shifted by substrate is prepared organic
The method of opto-electronic device flexible electrode, it is characterised in that: said method step 1) described in substrate 1 be silicon chip or glass firm
Property substrate.
3. using plasma technical finesse nano silver wire as claimed in claim 1 a kind of being shifted by substrate is prepared organic
The method of opto-electronic device flexible electrode, it is characterised in that: said method step 1) described in nano silver wire a diameter of 20
～100 nanometers, a length of 20～150 microns, the concentration of nano silver wire solution is 1～10mg/mL, the solvent of nano silver wire solution
For ethanol or isopropanol, the speed of spin coating nano silver wire thin film is 5000～9000 revs/min, and the thickness of nano silver wire thin film is
50～400 nanometers.
4. using plasma technical finesse nano silver wire as claimed in claim 1 a kind of being shifted by substrate is prepared organic
The method of opto-electronic device flexible electrode, it is characterised in that: said method step 2) described in the source of the gas of plasma be argon
Gas or nitrogen, the power of Cement Composite Treated by Plasma is 80～150W, and the process time of plasma is 1～30 minute.
5. using plasma technical finesse nano silver wire as claimed in claim 1 a kind of being shifted by substrate is prepared organic
The method of opto-electronic device flexible electrode, it is characterised in that: said method step 3) described in photocrosslinkable polymer be ultraviolet
Solidification optical cement or EVA glue, the thickness of the photocrosslinkable polymer that spin coating obtains is 30～70 microns.
6. using plasma technical finesse nano silver wire as claimed in claim 1 a kind of being shifted by substrate is prepared organic
The method of opto-electronic device flexible electrode, it is characterised in that: said method step 4) described in the power of uviol lamp be 100～
200W, the time of ultra violet lamp is 3～4 minutes.
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| CN108539058A (en) * | 2018-05-28 | 2018-09-14 | 吉林建筑大学 | A kind of preparation method of nano silver wire grid electrode |
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