CN107068291B - A method of transfer silver nanowires transparent conductive film to flexible substrate - Google Patents
A method of transfer silver nanowires transparent conductive film to flexible substrate Download PDFInfo
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- CN107068291B CN107068291B CN201710229464.3A CN201710229464A CN107068291B CN 107068291 B CN107068291 B CN 107068291B CN 201710229464 A CN201710229464 A CN 201710229464A CN 107068291 B CN107068291 B CN 107068291B
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Abstract
The present invention provide it is a kind of transfer silver nanowires transparent conductive film to flexible substrate method, the following steps are included: (1) spin coating silver nanowires dispersion liquid on cleaning substrate, silver nanowires film is obtained, is placed in after being dried in 120 DEG C of heating plates, is heat-treated 30min in 220 DEG C of baking ovens;(2) the spin-on silicon dioxide aeroge dispersion liquid on silver nanowires film is made silver nanowires/aerosil composite conductive thin film, dries in 120 DEG C of heating plates;(3) it is heating and curing after uniformly mixed PDMS being applied to the surface of composite conductive thin film, AgNWs- aerosil-PDMS composite and flexible transparent electrode is made;(4) PDMS after solidification is directly removed from glass substrate, completes the transfer of silver nanowires transparent conductive film.The present invention realizes the complete transfer of silver nanowires transparent electrode, and the joint resistance between nano wire is effectively reduced, and reduces the surface roughness of network, prepares the silver nanowires flexible transparent conductive film of function admirable, has practical application value.
Description
Technical field
The present invention provide it is a kind of transfer silver nanowires transparent conductive film to flexible substrate method.
Background technique
In recent years, wearable, foldable, portable flexible with the development that photoelectric device is integrated and softly changes
Device is increasingly by the concern of domestic and foreign scholars.Wherein flexibility stress sensor can be attached because it is with flexible characteristic
It in irregular or rigid objects surface, can be also bonded with human skin, in intelligent display, medical treatment & health monitoring device and electricity
There is potential application prospect in the fields such as sub- skin.But in sensor production, at present mostly dependent on silicon substrate etching, flexible substrate
The manufacturing process of the high energy consumptions such as surface plasma processing, metal deposit.Therefore how to prepare inexpensive and high sensitivity soft
Property strain gauge become one challenge.
Flexible substrates and electrode material are the important components of flexible sensor.Current most popular flexible lining
Bottom material is dimethyl silicone polymer (PDMS), and most popular electrode material is that silver nanowires (AgNWs) electrically conducting transparent is thin
Film.For silver nanowires because having excellent photoelectric properties, preparation process 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 stretches and flexural property is most possible substitution tradition
The material of ito transparent electrode had been realized shown and the application of the electronic equipments such as touch screen in flexible LED in recent years.PDMS is one
Kind the macromolecule organic silicon compound, with optical transparence, biocompatibility, manufacturing process is quickly easy.The PDMS of sheet
With good flexible, extensibility can be more than 100%, be the preferred substrate material for developing flexible electronic equipment all the time
Material.PDMS is mainly directly coated on obtained AgNWs-PDMS on silver nanowires transparent conductive film and answered by currently used method
Composite electrode is removed again, but the electrode sheet resistance is big, and electric conductivity is low, directly influences the sensitivity of sensor, therefore be unable to satisfy reality
The needs of border application.The reason of there are these problems, first is that the caking property on transparent conductive film between silver nanowires is weaker, two
It is PDMS since the physics and chemical interaction that are formed between methyl blocking, with silver nanowires are all very weak, can only realizes conduction
It shifts the part of network.So a kind of method for being effectively completely transferred to silver nanowires film on PDMS substrate is found, it is right
The performance for improving flexible nano photoelectric device has important application value.
Summary of the invention
The technical problems to be solved by the present invention are: providing a kind of transfer silver nanowires transparent conductive film to flexible substrate
Method, realize silver nanowires transparent electrode complete transfer, can greatly improve silver nanowires network electric conductivity and uniformly
Property, the joint resistance between nano wire is effectively reduced, the excellent silver nanowires flexible transparent conductive film of processability has real
Border application value.
The present invention solves its technical problem, and the following technical solution is employed:
Method of the transfer silver nanowires transparent conductive film provided by the invention to flexible substrate, comprising the following steps:
(1) silver nanowires transparent conductive film is prepared:
The spin coating silver nanowires alcohol dispersion liquid on cleaning substrate, obtains silver nanowires transparent conductive film, is placed in 120
After drying in DEG C heating plate, it is heat-treated 30min in an oven;
(2) aerosil/AgNWs composite conductive thin film is prepared:
The spin-on silicon dioxide aeroge dispersion liquid on silver nanowires transparent conductive film, obtained aerosil/
AgNWs composite conductive thin film, and be placed in 120 DEG C of heating plates and dry;
(3) flexible silver nanowires transparent conductive film is prepared:
It is heated admittedly after uniformly mixed PDMS is applied to aerosil/AgNWs composite conductive thin film surface
Change;PDMS after solidification is directly removed from glass substrate, the transfer of silver nanowires transparent conductive film is realized, obtains flexibility
Silver nanowires transparent conductive film.
In above-mentioned steps (1), the cleaning substrate is glass substrate.
In above-mentioned steps (1), the diameter of the silver nanowires is 100~300nm, and length is 100~150 μm.
In above-mentioned steps (1), uses sol evenning machine with revolving speed for 1000~1600 revs/min of progress spin coatings, deposit 1~4 layer
The silver nanowires 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 by gas phase nano silica with 4 ω t% points
It dissipates and is formed in dehydrated alcohol.
In above-mentioned steps (2), use sol evenning machine with revolving speed for 500~1000 revs/min of progress spin coatings.
In above-mentioned steps (3), PDMS be use 184 silicon rubber of Dow corning with prepolymer and curing agent in mass ratio
10:1 is uniformly mixed.
In above-mentioned steps (3), the coating method is any one in spin-coating method, Meyer stick method and drop-coating.
In above-mentioned steps (3), the technique that is heating and curing are as follows: temperature 60 C~120 DEG C, time 30min~6h.
The flexible silver nanowires transparent conductive film of above method preparation, is used as the material for preparing flexible photoelectric device.
The present invention has the advantages that below main compared with prior art:
In transfer method provided by 1., silver nanowires film is heat-treated, is effectively improved between silver nanowires
Caking property, reduce joint resistance, reduce the surface roughness of network, greatly improve silver nanowires network electric conductivity and
Even property.
2. in transfer method provided by, aerosil is introduced, solves silver nanowires and PDMS phase after transfer
The problem of interaction is weak, substantially loses conductivity, is made AgNWs- aerosil-PDMS combination electrode, realizes silver
The complete transfer of nano wire transparent electrode has potential application the performance for improving flexible nano photoelectric device.
3. transfer method provided by is simple to operation, at low cost, has practical application value.
Detailed description of the invention
Fig. 1 is the complete process flow figure of transfer method.
Fig. 2 is the scanning electron microscope of flexible silver nanowires transparent conductive film obtained in the embodiment of the present invention 1
Photo is formed by silver nanowires network structure, and silver nanowires diameter is 100~300nm.
Fig. 3 is the sheet resistance variation tendency of the silver nanowires transparent conductive film of the transfer of the embodiment of the present invention 1~3 front and back
Figure.
Fig. 4 is the transmittance curve figure of the silver nanowires transparent conductive film of the transfer of the embodiment of the present invention 1~3 front and back.
Specific embodiment
The invention will be further described with attached drawing combined with specific embodiments below, but does not limit the present invention.
Embodiment 1:
Referring to attached drawing 1, the present invention the following steps are included:
(1) silver nanowires transparent conductive film is prepared:
Silver nanowires dehydrated alcohol dispersant liquid drop is added in clean substrate of glass, is revolved with 1200 revs/min of revolving speed
It applies, then 1 layer of silver nanowires network substrate with certain arranging density of deposition will be coated with silver nanowires transparent conductive film
Substrate of glass is placed in 120 DEG C of heating plate 10 minutes to get to silver nanowires transparent conductive film, is divided with UV, visible light
Photometer measure at this time at 550nm wavelength transmitance be 81.7%, with four probes measure sheet resistance be 11.35 Ω sq-1。
(2) aerosil/AgNWs composite conductive thin film is prepared:
It disperses gas phase nano silica in 12ml ethanol solution with the mass fraction of 4 ω t%, to step
(1) dispersion liquid is added dropwise to entire substrate is completely covered on the silver nanowires transparent conductive film obtained in, then with 600 turns/
The revolving speed spin coating of minute obtains aerosil/AgNWs composite conductive thin film, and is placed in 10 in 120 DEG C of heating plate
Minute.
(3) flexible silver nanowires transparent conductive film is prepared:
Using 184 silicon rubber of Dow corning, it is uniformly mixed with prepolymer and curing agent 10:1 in mass ratio and obtains PDMS,
PDMS is added dropwise to entire film is completely covered, then with 600 revs/min to the surface of the composite conductive thin film obtained in step (2)
The revolving speed spin coating of clock obtains PDMS/ aerosil/AgNWs/ glass structure, after 80 DEG C of solidification 3h, by PDMS/ bis-
Silica aerogel/AgNWs is directly removed from substrate of glass to get to flexible silver nanowires transparent conductive film, with it is ultraviolet can
See spectrophotometer measure at this time at 550nm wavelength transmitance be 87.1%, increased using transfer method of the invention thin
The transmitance of film, measuring sheet resistance with four probes is 13.34 Ω sq-1, realize the complete transfer of silver nanowires transparent electrode, pole
The earth improves the electric conductivity and uniformity of silver nanowires network, and the joint resistance between nano wire is effectively reduced, reduces network
Surface roughness, the excellent silver nanowires flexible transparent conductive film of processability.
Embodiment 2: referring to attached drawing 1, the present invention the following steps are included:
(1) silver nanowires dehydrated alcohol dispersant liquid drop is added in clean substrate of glass, with 1200 revs/min of revolving speed
Spin coating, 2 layers of silver nanowires network substrate with certain arranging density of deposition, then will be coated with silver nanowires transparent conductive film
Substrate of glass be placed in 120 DEG C of heating plate 10 minutes to get to silver nanowires transparent conductive film, with UV, visible light point
Light photometer measure at this time at 550nm wavelength transmitance be 74.38%, with four probes measure sheet resistance be 5.67 Ω sq-1, because
Nanowire deposition number increases, and silver nanowires network increases, therefore transmitance decreases compared with embodiment 1, and conductivity then increases.
(2) it disperses gas phase nano silica in 12ml ethanol solution with the mass fraction of 4 ω t%, Xiang Bu
Suddenly the dispersion liquid is added dropwise to entire substrate is completely covered, then with 600 revs/min in the silver nanowires transparent electrode obtained in (1)
The revolving speed spin coating of clock obtains aerosil/AgNWs composite conductive thin film and is placed in 120 DEG C of heating plate 10 points
Clock.
(3) 184 silicon rubber of Dow corning is used, is uniformly mixed and is obtained with prepolymer and curing agent 10:1 in mass ratio
PDMS is added dropwise PDMS to entire film is completely covered to the surface of laminated film, is then obtained with 600 revs/min of revolving speed spin coating
To PDMS/ aerosil/AgNWs/ glass structure, after 80 DEG C of solidification 3h, by PDMS/ aerosil/
AgNWs is directly removed from substrate of glass to get to flexible silver nanowires transparent conductive film, is surveyed with ultraviolet-uisible spectrophotometer
At this time at 550nm wavelength transmitance be 77.8%, the transmitance of film is increased using transfer method of the invention, with four
It is 6.67 Ω sq that probe, which measures sheet resistance,-1, the complete transfer of silver nanowires transparent electrode is realized, silver nanowires is greatlyd improve
The electric conductivity and uniformity of network, are effectively reduced the joint resistance between nano wire, reduce the surface roughness of network, preparative
The excellent silver nanowires flexible transparent conductive film of energy.
Embodiment 3: referring to attached drawing 1, the present invention the following steps are included:
(1) silver nanowires dehydrated alcohol dispersant liquid drop is added in clean substrate of glass, with 1200 revs/min of revolving speed
Spin coating, 3 layers of silver nanowires network substrate with certain arranging density of deposition, then will be coated with silver nanowires transparent conductive film
Substrate of glass be placed in 120 DEG C of heating plate 10 minutes to get to silver nanowires transparent conductive film, with UV, visible light point
Light photometer measure at this time at 550nm wavelength transmitance be 64.96%, with four probes measure sheet resistance be 2.44 Ω sq-1, because
Nanowire deposition number increases, and silver nanowires network increases, therefore transmitance decreases compared with embodiment 2, and conductivity then increases.
(2) it disperses gas phase nano silica in 12ml ethanol solution with the mass fraction of 4 ω t%, Xiang Bu
Suddenly the dispersion liquid is added dropwise to entire substrate is completely covered, then with 600 revs/min in the silver nanowires transparent electrode obtained in (1)
The revolving speed spin coating of clock obtains aerosil/AgNWs composite conductive thin film and is placed in 120 DEG C of heating plate 10 points
Clock.
(3) 184 silicon rubber of Dow corning is used, is uniformly mixed and is obtained with prepolymer and curing agent 10:1 in mass ratio
PDMS is added dropwise PDMS to entire film is completely covered to the surface of laminated film, is then obtained with 600 revs/min of revolving speed spin coating
To PDMS/ aerosil/AgNWs/ glass structure, after 80 DEG C of solidification 3h, by PDMS/ aerosil/
AgNWs is directly removed from substrate of glass to get to flexible silver nanowires transparent conductive film, is surveyed with ultraviolet-uisible spectrophotometer
At this time at 550nm wavelength transmitance be 66.22%, the transmitance of film is increased using transfer method of the invention, use
It is 3.31 Ω sq that four probes, which measure sheet resistance,-1, the complete transfer of silver nanowires transparent electrode is realized, silver nanoparticle is greatlyd improve
The electric conductivity and uniformity of gauze network, are effectively reduced the joint resistance between nano wire, reduce the surface roughness of network, preparation
The silver nanowires flexible transparent conductive film of function admirable.
Embodiment 4: referring to attached drawing 1, the present invention the following steps are included:
(1) silver nanowires dehydrated alcohol dispersant liquid drop is added in clean substrate of glass, with 1200 revs/min of revolving speed
Spin coating, 4 layers of silver nanowires network substrate with certain arranging density of deposition, then will be coated with silver nanowires transparent conductive film
Substrate of glass be placed in 120 DEG C of heating plate 10 minutes to get to silver nanowires transparent conductive film, with UV, visible light point
Light photometer measure at this time at 550nm wavelength transmitance be 60.6%, with four probes measure sheet resistance be 0.78 Ω sq-1, because
Nanowire deposition number increases, and silver nanowires network increases, therefore transmitance decreases compared with embodiment 3, and conductivity then increases.
(2) it disperses gas phase nano silica in 12ml ethanol solution with the mass fraction of 4 ω t%, Xiang Bu
Suddenly the dispersion liquid is added dropwise to entire substrate is completely covered, then with 600 revs/min in the silver nanowires transparent electrode obtained in (1)
The revolving speed spin coating of clock obtains aerosil/AgNWs composite conductive thin film and is placed in 120 DEG C of heating plate 10 points
Clock.
(3) 184 silicon rubber of Dow corning is used, is uniformly mixed and is obtained with prepolymer and curing agent 10:1 in mass ratio
PDMS is added dropwise PDMS to entire film is completely covered to the surface of laminated film, is then obtained with 600 revs/min of revolving speed spin coating
To PDMS/ aerosil/AgNWs/ glass structure, after 80 DEG C of solidification 3h, by PDMS/ aerosil/
AgNWs is directly removed from substrate of glass to get to flexible silver nanowires transparent conductive film, is surveyed with ultraviolet-uisible spectrophotometer
At this time at 550nm wavelength transmitance be 62.37%, the transmitance of film is increased using transfer method of the invention, use
It is 1.59 Ω sq that four probes, which measure sheet resistance,-1, the complete transfer of silver nanowires transparent electrode is realized, silver nanoparticle is greatlyd improve
The electric conductivity and uniformity of gauze network, are effectively reduced the joint resistance between nano wire, reduce the surface roughness of network, preparation
The silver nanowires flexible transparent conductive film of function admirable.
Method provided by the above embodiment overcomes in current transfer method, mostly uses and PDMS is directly coated on silver
Obtained AgNWs-PDMS combination electrode is removed on nano wire film, after solidification again, conductivity loses serious problem.Remember according to document
It carries, is 1.77 Ω sq in the silver nanowires transparent conductive film sheet resistance of substrate of glass preparation-1, after transfer, sheet resistance is increased to
21.6Ω·sq-1.The method of the present invention is heat-treated after obtained silver nanowires film, increases silver wire in conductive network
With the caking property of silver wire.Aerosil is introduced, is spun on silver nanowires conductive film, is coated PDMS, is solidified
Afterwards, AgNWs- aerosil-PDMS combination electrode is obtained, in the case where transmitance is greater than 80%, shifts front and back
Sheet resistance is respectively 11.35 Ω sq-1With 13.34 Ω sq-1, sheet resistance increase degree is small, and good conduction is still kept after transfer
Rate.
Above embodiments are only to technical solution of the present invention for example, being not construed as protecting the claims in the present invention
The limitation of range, it is other it is any without departing from the spirit and principles of the present invention made by modification, modification, substitution, combination,
Simplify, should be equivalent substitute mode, be included within the scope of the present invention.
Claims (10)
1. it is a kind of transfer silver nanowires transparent conductive film to flexible substrate method, it is characterized in that the following steps are included:
(1) silver nanowires transparent conductive film is prepared:
The spin coating silver nanowires alcohol dispersion liquid on cleaning substrate, obtains silver nanowires transparent conductive film, is placed in 120 DEG C and adds
After drying on hot plate, it is heat-treated 30min in an oven, increases the caking property of silver wire and silver wire in conductive network;
(2) aerosil/AgNWs composite conductive thin film is prepared:
Aerosil/AgNWs is made in the spin-on silicon dioxide aeroge dispersion liquid on silver nanowires transparent conductive film
Composite conductive thin film, and be placed in 120 DEG C of heating plates and dry;
(3) flexible silver nanowires transparent conductive film is prepared:
It is heating and curing after uniformly mixed PDMS is applied to aerosil/AgNWs composite conductive thin film surface, Gu
After change, AgNWs- aerosil-PDMS combination electrode is obtained, in the case where transmitance is greater than 80%, transfer front and back
Sheet resistance be respectively 11.35 Ω sq-1With 13.34 Ω sq-1, sheet resistance increase degree is small, and good conduction is still kept after transfer
Rate;PDMS after solidification is directly removed from glass substrate, the transfer of silver nanowires transparent conductive film is realized, obtains flexibility
Silver nanowires transparent conductive film.
2. it is according to claim 1 transfer silver nanowires transparent conductive film to flexible substrate method, it is characterised in that
Cleaning substrate described in step (1) is glass substrate.
3. it is according to claim 1 transfer silver nanowires transparent conductive film to flexible substrate method, it is characterised in that
The diameter of silver nanowires described in step (1) is 100~300nm, and length is 100~150 μm.
4. it is according to claim 1 transfer silver nanowires transparent conductive film to flexible substrate method, it is characterised in that
It in step (1), uses sol evenning machine with revolving speed for 1000~1600 revs/min of progress spin coatings, deposits 1~4 layer and form different arrangements
The silver nanowires film of density, heat treatment temperature are 200 DEG C~250 DEG C.
5. it is according to claim 1 transfer silver nanowires transparent conductive film to flexible substrate method, it is characterised in that
In step (2), the aerosil dispersion liquid is to disperse dehydrated alcohol for gas phase nano silica with 4 ω t%
Middle formation.
6. it is according to claim 1 transfer silver nanowires transparent conductive film to flexible substrate method, it is characterised in that
In step (2), use sol evenning machine with revolving speed for 500~1000 revs/min of progress spin coatings.
7. it is according to claim 1 transfer silver nanowires transparent conductive film to flexible substrate method, it is characterised in that
In step (3), PDMS is that 184 silicon rubber of Dow corning is used to be uniformly mixed with prepolymer and curing agent 10:1 in mass ratio.
8. it is according to claim 1 transfer silver nanowires transparent conductive film to flexible substrate method, it is characterised in that
In step (3), the coating method is any one in spin-coating method, Meyer stick method and drop-coating.
9. it is according to claim 1 transfer silver nanowires transparent conductive film to flexible substrate method, it is characterised in that
In step (3), the technique that is heating and curing are as follows: temperature 60 C~120 DEG C, time 30min~6h.
10. the flexible silver nanowires transparent conductive film of any the method preparation, which is used as, in claim 1 to 9 prepares flexible light
The material of electrical part.
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CN106252518A (en) * | 2016-10-25 | 2016-12-21 | 天津市职业大学 | One is low blocks large area perovskite solar cell and preparation method thereof |
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