CN107068291A - A kind of nano silver wire transparent conductive film that shifts is to the method for flexible substrate - Google Patents
A kind of nano silver wire transparent conductive film that shifts is to the method for flexible substrate Download PDFInfo
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Abstract
The present invention provides a kind of transfer nano silver wire transparent conductive film to the method for flexible substrate, comprises the following steps：(1) the spin coating nano silver wire dispersion liquid on cleaning substrate, obtains nano silver wire film, is positioned over after being dried in 120 DEG C of heating plates, 30min is heat-treated in 220 DEG C of baking ovens；(2) the spin-on silicon dioxide aeroge dispersion liquid on nano silver wire film, is made nano silver wire/aerosil composite conductive thin film, is dried in 120 DEG C of heating plates；(3) it is heating and curing after well mixed PDMS being applied into the surface of composite conductive thin film, AgNWs aerosil PDMS composite and flexible transparency electrodes is made；(4) PDMS after solidification is directly peeled off from glass substrate, completes the transfer of nano silver wire transparent conductive film.The present invention realizes the complete transfer of nano silver wire transparency electrode, effectively the joint resistance between reduction nano wire, reduces the surface roughness of network, the nano silver wire flexible transparent conductive film of function admirable is prepared, with actual application value.
Description
Technical field
The present invention provides a kind of nano silver wire transparent conductive film that shifts to the method for flexible substrate.
Background technology
In recent years, with the integrated development with softly changing of photoelectric device, wearable, foldable, portable soft elastic
Device is increasingly paid close attention to by domestic and foreign scholars.Wherein flexibility stress sensor has soft elastic characteristic because of it, can attach
In irregular or rigid objects surface, it can also be fitted with human body skin, in intelligent display, medical treatment ＆ health monitoring device and electricity
There is potential application prospect in the fields such as sub- skin.But it is many at present dependent on silicon substrate etching, flexible substrate in sensor production
The manufacturing process of the high energy consumptions such as surface plasma processing, metal deposit.Therefore how to prepare low cost and it is highly sensitive soft
Property strain gauge turn into one challenge.
Flexible substrates and electrode material are the important components of flexible sensor.Most popular soft elastic is served as a contrast at present
Bottom material is dimethyl silicone polymer (PDMS), and most popular electrode material is that nano silver wire (AgNWs) electrically conducting transparent is thin
Film.Nano silver wire is because with excellent photoelectric properties, preparation technology uses the liquid phase method of fast and low-cost, and room temperature film-forming condition
There is good compatibility with low melting point flexible substrate, excellent mechanical resistant stretching and flexural property are most possible replacement tradition
The material of ito transparent electrode, realized in recent years flexible LED show and the electronic equipment such as touch-screen application.PDMS is one
The macromolecule organic silicon compound is planted, with optical transparence, biocompatibility, manufacturing process is quickly easy.The PDMS of sheet
With good soft elastic, extensibility can be the preferred substrate material for developing soft elastic electronic equipment all the time more than 100%
Material.The method used at present be mainly directly by PDMS be coated on nano silver wire transparent conductive film be made AgNWs-PDMS answer
Composite electrode is peeled off again, but the electrode sheet resistance is big, and electric conductivity is low, directly influences the sensitivity of sensor, therefore can not meet reality
The need for border is applied.The reason for there are these, one is that caking property on transparent conductive film between nano silver wire is weaker, two
Be PDMS because the physics and chemical interaction that are formed between methyl blocking, with nano silver wire are all very weak, conduction can only be realized
The part transfer of network.So find it is a kind of by the nano silver wire film effectively complete method being transferred on PDMS substrates, it is right
Improving the performance of flexible nano photoelectric device has important application value.
The content of the invention
The technical problems to be solved by the invention are：A kind of transfer nano silver wire transparent conductive film is provided to flexible substrate
Method, realize the complete transfer of nano silver wire transparency electrode, the electric conductivity of nano silver wire network can be greatly enhanced and uniform
Property, effectively reduce the joint resistance between nano wire, the excellent nano silver wire flexible transparent conductive film of processability, with reality
Border application value.
The present invention solves its technical problem and uses following technical scheme：
The transfer nano silver wire transparent conductive film that the present invention is provided comprises the following steps to the method for flexible substrate：
(1) nano silver wire transparent conductive film is prepared：
The spin coating nano silver wire alcohol dispersion liquid on cleaning substrate, obtains nano silver wire transparent conductive film, is positioned over 120
After being dried in DEG C heating plate, 30min is heat-treated in an oven；
(2) aerosil/AgNWs composite conductive thin films are prepared：
The spin-on silicon dioxide aeroge dispersion liquid on nano silver wire transparent conductive film, obtained aerosil/
AgNWs composite conductive thin films, and it is positioned over drying in 120 DEG C of heating plates；
(3) flexible nano silver wire transparent conductive film is prepared：
Well mixed PDMS is applied to behind the surface of aerosil/AgNWs composite conductive thin films and heated admittedly
Change；PDMS after solidification is directly peeled off from glass substrate, the transfer of nano silver wire transparent conductive film is realized, obtains flexibility
Nano silver wire transparent conductive film.
In above-mentioned steps (1), the cleaning substrate is glass substrate.
In above-mentioned steps (1), a diameter of 100~300nm of the nano silver wire, length is 100~150 μm.
In above-mentioned steps (1), use sol evenning machine using rotating speed as 1000~1600 revs/min of progress spin coatings, deposit 1~4 layer
The nano silver wire film of different arranging densities is formed, heat treatment temperature is 200 DEG C~250 DEG C.
In above-mentioned steps (2), the aerosil dispersion liquid is to divide gas phase nano silica with 4 ω t%
Dissipate what is formed in absolute ethyl alcohol.
In above-mentioned steps (2), sol evenning machine is used using rotating speed as 500~1000 revs/min of progress spin coatings.
In above-mentioned steps (3), PDMS be use the silicon rubber of Dow corning 184 with prepolymer and curing agent in mass ratio
10：1 is well mixed.
In above-mentioned steps (3), the coating method is any one in spin-coating method, Meyer rod method and drop-coating.
In above-mentioned steps (3), the technique that is heating and curing is：Temperature 60 C~120 DEG C, time 30min~6h.
Flexible nano silver wire transparent conductive film prepared by the above method, it is used as the material for preparing flexible photoelectric device.
The present invention has the advantages that following main compared with prior art：
1. in the transfer method provided, be heat-treated to nano silver wire film, effectively improve between nano silver wire
Caking property, reduce joint resistance, reduce network surface roughness, be greatly enhanced nano silver wire network electric conductivity and
Even property.
2. in the transfer method provided, introducing aerosil, nano silver wire and PDMS phases after transfer are solved
Interaction is weak, the problem of significantly losing conductance, and AgNWs- aerosil-PDMS combination electrodes are made, silver is realized
The complete transfer of nano wire transparency electrode, has potential application value to the performance for improving flexible nano photoelectric device.
3. the transfer method provided is simple to operation, cost is low, with actual application value.
Brief description of the drawings
Fig. 1 is the complete process flow figure of transfer method.
Fig. 2 is the SEM of obtained flexible nano silver wire transparent conductive film in embodiments of the invention 1
In photo, the nano silver wire network structure formed, a diameter of 100~300nm of nano silver wire.
Fig. 3 is the sheet resistance variation tendency of the nano silver wire transparent conductive film before and after embodiments of the invention 1~3 are shifted
Figure.
Fig. 4 is the transmittance curve figure of the nano silver wire transparent conductive film before and after embodiments of the invention 1~3 are shifted.
Embodiment
With reference to specific embodiments and the drawings, the invention will be further described, but does not limit the present invention.
Embodiment 1：
Referring to accompanying drawing 1, the present invention comprises the following steps：
(1) nano silver wire transparent conductive film is prepared：
Nano silver wire absolute ethyl alcohol dispersant liquid drop is added in the substrate of glass of cleaning, revolved with 1200 revs/min of rotating speed
Apply, 1 layer of deposition has the nano silver wire network substrate of certain arranging density, then will scribble nano silver wire transparent conductive film
Substrate of glass is positioned in 120 DEG C of heating plate 10 minutes, that is, obtains nano silver wire transparent conductive film, uses UV, visible light light splitting
Photometer measures now that transmitance is 81.7% at 550nm wavelength, and sheet resistance is measured with four probes for 11.35 Ω sq-1。
(2) aerosil/AgNWs composite conductive thin films are prepared：
Gas phase nano silica is scattered in 12ml ethanol solutions with 4 ω t% mass fraction, to step
(1) in obtain nano silver wire transparent conductive film on the dispersion liquid is added dropwise to whole substrate is completely covered, then with 600 turns/
The rotating speed spin coating of minute obtains aerosil/AgNWs composite conductive thin films, and is positioned over 10 in 120 DEG C of heating plate
Minute.
(3) flexible nano silver wire transparent conductive film is prepared：
Using the silicon rubber of Dow corning 184, with prepolymer and curing agent in mass ratio 10：1 it is well mixed obtain PDMS,
PDMS is added dropwise to whole film is completely covered in the surface of the composite conductive thin film obtained into step (2), then with 600 revs/min
The rotating speed spin coating of clock obtains the structure of PDMS/ aerosils/AgNWs/ glass, after 80 DEG C solidify 3h, by PDMS/ bis-
Silica aerogel/AgNWs directly from substrate of glass peel off, that is, obtain flexible nano silver wire transparent conductive film, with it is ultraviolet can
See spectrophotometer measure now at 550nm wavelength transmitance be 87.1%, using the present invention transfer method add it is thin
The transmitance of film, sheet resistance is measured with four probes for 13.34 Ω sq-1, realize the complete transfer of nano silver wire transparency electrode, pole
The earth improves the electric conductivity and uniformity of nano silver wire network, the effectively joint resistance between reduction nano wire, reduction network
Surface roughness, the excellent nano silver wire flexible transparent conductive film of processability.
Embodiment 2：Referring to accompanying drawing 1, the present invention comprises the following steps：
(1) nano silver wire absolute ethyl alcohol dispersant liquid drop is added in the substrate of glass of cleaning, with 1200 revs/min of rotating speed
Spin coating, 2 layers of deposition has the nano silver wire network substrate of certain arranging density, then will scribble nano silver wire transparent conductive film
Substrate of glass be positioned in 120 DEG C of heating plate 10 minutes, that is, nano silver wire transparent conductive film is obtained, with UV, visible light point
Light photometer measures now that transmitance is 74.38% at 550nm wavelength, and sheet resistance is measured with four probes for 5.67 Ω sq-1, because
The increase of nanowire deposition number of times, nano silver wire network increases, therefore transmitance decreases compared with embodiment 1, and conductance then increases.
(2) gas phase nano silica is scattered in 12ml ethanol solutions with 4 ω t% mass fraction, Xiang Bu
Suddenly the dispersion liquid is added dropwise to whole substrate is completely covered in the nano silver wire transparency electrode obtained in (1), then with 600 revs/min
The rotating speed spin coating of clock obtains aerosil/AgNWs composite conductive thin films and is positioned in 120 DEG C of heating plate 10 points
Clock.
(3) silicon rubber of Dow corning 184 is used, with prepolymer and curing agent in mass ratio 10：1 well mixed obtains
PDMS, is added dropwise PDMS to whole film is completely covered to the surface of laminated film, is then obtained with 600 revs/min of rotating speed spin coating
To the structure of PDMS/ aerosils/AgNWs/ glass, after 80 DEG C solidify 3h, by PDMS/ aerosils/
AgNWs is directly peeled off from substrate of glass, that is, is obtained flexible nano silver wire transparent conductive film, surveyed with ultraviolet-uisible spectrophotometer
Now transmitance is 77.8% at 550nm wavelength, the transmitance of film is added using the transfer method of the present invention, with four
Probe measures sheet resistance for 6.67 Ω sq-1, the complete transfer of nano silver wire transparency electrode is realized, nano silver wire is greatly enhanced
Joint resistance between the electric conductivity and uniformity of network, effectively reduction nano wire, reduces the surface roughness of network, preparative
The excellent nano silver wire flexible transparent conductive film of energy.
Embodiment 3：Referring to accompanying drawing 1, the present invention comprises the following steps：
(1) nano silver wire absolute ethyl alcohol dispersant liquid drop is added in the substrate of glass of cleaning, with 1200 revs/min of rotating speed
Spin coating, 3 layers of deposition has the nano silver wire network substrate of certain arranging density, then will scribble nano silver wire transparent conductive film
Substrate of glass be positioned in 120 DEG C of heating plate 10 minutes, that is, nano silver wire transparent conductive film is obtained, with UV, visible light point
Light photometer measures now that transmitance is 64.96% at 550nm wavelength, and sheet resistance is measured with four probes for 2.44 Ω sq-1, because
The increase of nanowire deposition number of times, nano silver wire network increases, therefore transmitance decreases compared with embodiment 2, and conductance then increases.
(2) gas phase nano silica is scattered in 12ml ethanol solutions with 4 ω t% mass fraction, Xiang Bu
Suddenly the dispersion liquid is added dropwise to whole substrate is completely covered in the nano silver wire transparency electrode obtained in (1), then with 600 revs/min
The rotating speed spin coating of clock obtains aerosil/AgNWs composite conductive thin films and is positioned in 120 DEG C of heating plate 10 points
Clock.
(3) silicon rubber of Dow corning 184 is used, with prepolymer and curing agent in mass ratio 10：1 well mixed obtains
PDMS, is added dropwise PDMS to whole film is completely covered to the surface of laminated film, is then obtained with 600 revs/min of rotating speed spin coating
To the structure of PDMS/ aerosils/AgNWs/ glass, after 80 DEG C solidify 3h, by PDMS/ aerosils/
AgNWs is directly peeled off from substrate of glass, that is, is obtained flexible nano silver wire transparent conductive film, surveyed with ultraviolet-uisible spectrophotometer
Now transmitance is 66.22% at 550nm wavelength, the transmitance of film is added using the transfer method of the present invention, used
Four probes measure sheet resistance for 3.31 Ω sq-1, the complete transfer of nano silver wire transparency electrode is realized, silver nanoparticle is greatly enhanced
Joint resistance between the electric conductivity and uniformity of gauze network, effectively reduction nano wire, reduces the surface roughness of network, prepares
The nano silver wire flexible transparent conductive film of function admirable.
Embodiment 4：Referring to accompanying drawing 1, the present invention comprises the following steps：
(1) nano silver wire absolute ethyl alcohol dispersant liquid drop is added in the substrate of glass of cleaning, with 1200 revs/min of rotating speed
Spin coating, 4 layers of deposition has the nano silver wire network substrate of certain arranging density, then will scribble nano silver wire transparent conductive film
Substrate of glass be positioned in 120 DEG C of heating plate 10 minutes, that is, nano silver wire transparent conductive film is obtained, with UV, visible light point
Light photometer measures now that transmitance is 60.6% at 550nm wavelength, and sheet resistance is measured with four probes for 0.78 Ω sq-1, because
The increase of nanowire deposition number of times, nano silver wire network increases, therefore transmitance decreases compared with embodiment 3, and conductance then increases.
(2) gas phase nano silica is scattered in 12ml ethanol solutions with 4 ω t% mass fraction, Xiang Bu
Suddenly the dispersion liquid is added dropwise to whole substrate is completely covered in the nano silver wire transparency electrode obtained in (1), then with 600 revs/min
The rotating speed spin coating of clock obtains aerosil/AgNWs composite conductive thin films and is positioned in 120 DEG C of heating plate 10 points
Clock.
(3) silicon rubber of Dow corning 184 is used, with prepolymer and curing agent in mass ratio 10：1 well mixed obtains
PDMS, is added dropwise PDMS to whole film is completely covered to the surface of laminated film, is then obtained with 600 revs/min of rotating speed spin coating
To the structure of PDMS/ aerosils/AgNWs/ glass, after 80 DEG C solidify 3h, by PDMS/ aerosils/
AgNWs is directly peeled off from substrate of glass, that is, is obtained flexible nano silver wire transparent conductive film, surveyed with ultraviolet-uisible spectrophotometer
Now transmitance is 62.37% at 550nm wavelength, the transmitance of film is added using the transfer method of the present invention, used
Four probes measure sheet resistance for 1.59 Ω sq-1, the complete transfer of nano silver wire transparency electrode is realized, silver nanoparticle is greatly enhanced
Joint resistance between the electric conductivity and uniformity of gauze network, effectively reduction nano wire, reduces the surface roughness of network, prepares
The nano silver wire flexible transparent conductive film of function admirable.
The method that above-described embodiment is provided, is overcome in current transfer method, and PDMS is directly coated on silver by use more
Obtained AgNWs-PDMS combination electrodes, the problem of conductance loss is serious are peeled off on nano wire film, after solidification again.Remember according to document
Carry, the nano silver wire transparent conductive film sheet resistance prepared in substrate of glass is 1.77 Ω sq-1, after transfer, sheet resistance is increased to
21.6Ω·sq-1.The inventive method is heat-treated after obtained nano silver wire film, silver wire in increase conductive network
With the caking property of silver wire.Aerosil is introduced, is spun on nano silver wire conductive film, is coated PDMS, is solidified
Afterwards, AgNWs- aerosil-PDMS combination electrodes are obtained, in the case where transmitance is more than 80%, before and after transfer
Sheet resistance is respectively 11.35 Ω sq-1With 13.34 Ω sq-1, sheet resistance increase degree it is small, good conduction is still kept after transfer
Rate.
Above example is only to technical solution of the present invention for example, being not construed as protecting the claims in the present invention
The limitation of scope, other any Spirit Essences without departing from the present invention and the modification made under principle, modification, replacement, combine,
Simplify, should be equivalent substitute mode, be included within protection scope of the present invention.
Claims (10)
1. a kind of nano silver wire transparent conductive film that shifts is to the method for flexible substrate, it is characterized in that comprising the following steps：
(1) nano silver wire transparent conductive film is prepared：
The spin coating nano silver wire alcohol dispersion liquid on cleaning substrate, obtains nano silver wire transparent conductive film, is positioned over 120 DEG C and adds
After being dried on hot plate, 30min is heat-treated in an oven；
(2) aerosil/AgNWs composite conductive thin films are prepared：
The spin-on silicon dioxide aeroge dispersion liquid on nano silver wire transparent conductive film, is made aerosil/AgNWs
Composite conductive thin film, and it is positioned over drying in 120 DEG C of heating plates；
(3) flexible nano silver wire transparent conductive film is prepared：
It is heating and curing after well mixed PDMS is applied into the surface of aerosil/AgNWs composite conductive thin films；Will
PDMS after solidification is directly peeled off from glass substrate, is realized the transfer of nano silver wire transparent conductive film, is obtained flexible silver and receive
Rice noodles transparent conductive film.
2. the nano silver wire transparent conductive film according to claim 1 that shifts is to the method for flexible substrate, it is characterised in that
It is glass substrate that substrate is cleaned described in step (1).
3. the nano silver wire transparent conductive film according to claim 1 that shifts is to the method for flexible substrate, it is characterised in that
A diameter of 100~300nm of nano silver wire described in step (1), length is 100~150 μm.
4. the nano silver wire transparent conductive film according to claim 1 that shifts is to the method for flexible substrate, it is characterised in that
In step (1), use sol evenning machine using rotating speed as 1000~1600 revs/min of progress spin coatings, deposit 1~4 layer and form different arrangements
The nano silver wire film of density, heat treatment temperature is 200 DEG C~250 DEG C.
5. the nano silver wire transparent conductive film according to claim 1 that shifts is to the method for flexible substrate, it is characterised in that
In step (2), the aerosil dispersion liquid is that with 4 ω t% gas phase nano silica is scattered in into absolute ethyl alcohol
Middle formation.
6. the nano silver wire transparent conductive film according to claim 1 that shifts is to the method for flexible substrate, it is characterised in that
In step (2), sol evenning machine is used using rotating speed as 500~1000 revs/min of progress spin coatings.
7. the nano silver wire transparent conductive film according to claim 1 that shifts is to the method for flexible substrate, it is characterised in that
In step (3), PDMS is to use the silicon rubber of Dow corning 184 with prepolymer and curing agent in mass ratio 10：1 is well mixed.
8. the nano silver wire transparent conductive film according to claim 1 that shifts is to the method for flexible substrate, it is characterised in that
In step (3), the coating method is any one in spin-coating method, Meyer rod method and drop-coating.
9. the nano silver wire transparent conductive film according to claim 1 that shifts is to the method for flexible substrate, it is characterised in that
In step (3), the technique that is heating and curing is：Temperature 60 C~120 DEG C, time 30min~6h.
10. the flexible nano silver wire transparent conductive film that in claim 1 to 9 prepared by any methods described is used as preparing flexible light
The material of electrical part.
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