CN108649104A - A kind of preparation method of flexible transparent electrode - Google Patents
A kind of preparation method of flexible transparent electrode Download PDFInfo
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- CN108649104A CN108649104A CN201810472539.5A CN201810472539A CN108649104A CN 108649104 A CN108649104 A CN 108649104A CN 201810472539 A CN201810472539 A CN 201810472539A CN 108649104 A CN108649104 A CN 108649104A
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- 238000002360 preparation method Methods 0.000 title claims abstract description 34
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 36
- 239000002041 carbon nanotube Substances 0.000 claims abstract description 36
- 229910021393 carbon nanotube Inorganic materials 0.000 claims abstract description 36
- 229920002120 photoresistant polymer Polymers 0.000 claims abstract description 22
- 239000002238 carbon nanotube film Substances 0.000 claims abstract description 12
- 238000004026 adhesive bonding Methods 0.000 claims abstract description 9
- 239000000758 substrate Substances 0.000 claims description 45
- 239000010408 film Substances 0.000 claims description 40
- 239000010409 thin film Substances 0.000 claims description 26
- 238000004544 sputter deposition Methods 0.000 claims description 23
- 239000000725 suspension Substances 0.000 claims description 23
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 16
- 238000005507 spraying Methods 0.000 claims description 13
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 12
- 239000008367 deionised water Substances 0.000 claims description 12
- 229910021641 deionized water Inorganic materials 0.000 claims description 12
- 239000003292 glue Substances 0.000 claims description 12
- 238000000034 method Methods 0.000 claims description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 12
- 239000007789 gas Substances 0.000 claims description 10
- 239000007788 liquid Substances 0.000 claims description 10
- 229910052786 argon Inorganic materials 0.000 claims description 8
- 238000001755 magnetron sputter deposition Methods 0.000 claims description 8
- 238000004528 spin coating Methods 0.000 claims description 8
- 239000007921 spray Substances 0.000 claims description 8
- 238000002604 ultrasonography Methods 0.000 claims description 8
- 229910052793 cadmium Inorganic materials 0.000 claims description 7
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 claims description 7
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 6
- 238000005530 etching Methods 0.000 claims description 6
- 239000000919 ceramic Substances 0.000 claims description 5
- 241000196171 Hydrodictyon reticulatum Species 0.000 claims description 4
- 230000001133 acceleration Effects 0.000 claims description 4
- 235000011054 acetic acid Nutrition 0.000 claims description 4
- 150000001243 acetic acids Chemical class 0.000 claims description 4
- 239000011248 coating agent Substances 0.000 claims description 4
- 238000000576 coating method Methods 0.000 claims description 4
- 239000012528 membrane Substances 0.000 claims description 4
- 229910052751 metal Inorganic materials 0.000 claims description 4
- 239000002184 metal Substances 0.000 claims description 4
- 239000000843 powder Substances 0.000 claims description 4
- 239000002994 raw material Substances 0.000 claims description 4
- 239000002904 solvent Substances 0.000 claims description 4
- 239000004094 surface-active agent Substances 0.000 claims description 4
- 238000001771 vacuum deposition Methods 0.000 claims description 4
- 238000009504 vacuum film coating Methods 0.000 claims description 4
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims description 3
- 229910002651 NO3 Inorganic materials 0.000 claims description 3
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims description 3
- 229960000583 acetic acid Drugs 0.000 claims description 3
- 239000012362 glacial acetic acid Substances 0.000 claims description 3
- 230000003287 optical effect Effects 0.000 claims description 3
- 238000004062 sedimentation Methods 0.000 claims description 3
- 150000002823 nitrates Chemical class 0.000 claims description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims 1
- 229910052593 corundum Inorganic materials 0.000 claims 1
- 229910001845 yogo sapphire Inorganic materials 0.000 claims 1
- 238000005452 bending Methods 0.000 abstract description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 150000001875 compounds Chemical class 0.000 abstract description 2
- 238000003912 environmental pollution Methods 0.000 abstract description 2
- 229910052782 aluminium Inorganic materials 0.000 description 3
- HSJPMRKMPBAUAU-UHFFFAOYSA-N cerium(3+);trinitrate Chemical compound [Ce+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O HSJPMRKMPBAUAU-UHFFFAOYSA-N 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000013467 fragmentation Methods 0.000 description 1
- 238000006062 fragmentation reaction Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 229910052738 indium Inorganic materials 0.000 description 1
- MRNHPUHPBOKKQT-UHFFFAOYSA-N indium;tin;hydrate Chemical compound O.[In].[Sn] MRNHPUHPBOKKQT-UHFFFAOYSA-N 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 239000002574 poison Substances 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- 229910052718 tin Inorganic materials 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
Classifications
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L31/00—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L31/18—Processes or apparatus specially adapted for the manufacture or treatment of these devices or of parts thereof
- H01L31/1884—Manufacture of transparent electrodes, e.g. TCO, ITO
-
- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K30/00—Organic devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation
- H10K30/80—Constructional details
- H10K30/81—Electrodes
- H10K30/82—Transparent electrodes, e.g. indium tin oxide [ITO] electrodes
-
- 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
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E10/00—Energy generation through renewable energy sources
- Y02E10/50—Photovoltaic [PV] energy
- Y02E10/549—Organic PV cells
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
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- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Physics & Mathematics (AREA)
- Electromagnetism (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Computer Hardware Design (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Power Engineering (AREA)
- Carbon And Carbon Compounds (AREA)
- Non-Insulated Conductors (AREA)
Abstract
A kind of preparation method of flexible transparent electrode, step are：(1) preparation of carbon nano-tube film, (2) preparation of Ag/AZO films, (3) Ag/AZO films gluing, (4) uv-exposure, (5) removal photoresist develops, (6) grid is etched, (7) remove the photoresist on grid.Compound Ag/AZO films in the carbon nanotube of the present invention, reduce the sheet resistance of film, have good photoelectric properties, improve the resist bending ability of film, flexible performance is good, moreover it is possible to reduce environmental pollution, reduce cost of manufacture.
Description
Technical field
The present invention relates to transparent electrode technical field more particularly to a kind of preparation methods of flexible transparent electrode.
Background technology
Current transparent electrode is prepared on mostly in the hard substrates such as glass, ceramics, but these hard substrates do not have
It is flexible, frangible not readily transportable, do not adapt to the hair of flexibility, environmental protection, Portable small of the following photoelectric device etc. especially
Exhibition trend, the flexible transparent electrode prepared on flexible substrates do not have good photoelectric properties not only, and flexibility makes it in future
Photoelectric device has more advantage, and flexible transparent electrode can be widely applied to touch screen, portable type solar energy battery, polymer hair
In the flexible photoelectric devices such as optical diode and wearable electronic, the market demand is huge, currently, tin indium oxide ITO occupy it is transparent
Most of share in electrode market, but raw material used when ito thin film when preparation is toxic, all causes damages to human and environment,
And it is expensive, manufacturing cost is improved, In and Sn are thick atom secondary element, readily permeable to enter substrate interior, to
Poison substrate, meanwhile, ito thin film is easily reduced in hydrogen plasma environment, the easy fragmentation of when bending, therefore, is lacked based on above-mentioned
Point, people seek can to substitute the material of ITO, carbon nanotube CNT transparent conductive films because its excellent translucency, electric conductivity and
The characteristic of pliability etc. is concerned, and the translucency of carbon nanotube carbon nanotube thin film is higher, and electric conductivity is poorer, and electric conductivity is got over
Good, translucency is lower, and since carbon nanotube CNT transparent conductive film electric conductivities prepared at present are poor, surface is thicker
It is rough, and by limitation application range.
Invention content
The present invention provides a kind of preparation method of electric conductivity good flexibility transparent electrode in order to solve the above problem.
The technical solution used in the present invention：
A kind of preparation method of flexible transparent electrode, step are：
(1) preparation of carbon nano-tube film：Single armed carbon nanotube is prepared using FCCVD methods, single armed carbon nanotube is handled
After be configured to suspension, carbon nano-tube film is made on PET substrate by spray coating method；
(2) preparation of Ag/AZO films：Using direct current magnetron sputtering process and radio-frequency magnetron sputter method in carbon nanotube thin film obtained
It is coated with Ag films and AZO films successively above；
(3) Ag/AZO films gluing：The thin glue of equal glue machine spin coating AZ310 is used on the substrate PET for be coated with CNT/Ag/AZO,
Rotating speed 3000rad/s, acceleration 3000rad/s, spin-coating time 30s；
(4) uv-exposure：After gluing on hot plate 90 DEG C baking 15min, remove glue-line in solvent after carry out uv-exposure,
Uv power density is 3mw/cm2, time for exposure 34s；
(5) removal photoresist develops：The use of thin glue developing solution AZ300 removals is the photoresist of exposure, by mask plate
On metal grill pattern be transferred on photoresist coating, developing time be 28~32s；
(6) grid is etched：It dries 30min after development at 90 DEG C in baking oven, carries out the adherency that post bake increases glued membrane and substrate
Then power is configured to cadmium liquid, removal etches unwanted Ag/AZO films between grid, and etch period is 23~27s；
(7) photoresist on grid is removed：Sample after etching grid is put into the NaOH solution configured and removes grid
Then the photoresist of upper covering is washed with deionized water net sample and obtains flexible transparent electrode.
The carbon nano-tube film preparation process is：
A., the surfactant that single armed carbon nanotube powder 1g is mixed to the neopelex of 1L a concentration of 1% is molten
CNT suspension is made in liquid；
B. CNT suspension is put into ultrasound 1h in the ultrasonic machine that power is 40W；
C. the good CNT suspension of ultrasound is put into the centrifuge 20min that rotating speed is 1400rpm；
D. it takes the suspension on upper layer and puts into spray gun, by suspension spray on PET substrate, equally distributed CNT is made
Film；
E. substrate is cleaned with deionized water, to wash off neopelex；
F. step d and step e 4~5 times is repeated, certain thickness carbon nanotube thin film is formed.
The PET substrate is previously heated to 100 DEG C before spraying by constent temperature heater, and constant temperature remains to spraying knot
Beam.
The preparation process of the Ag/AZO films is：
(1) substrate frame being attached to the carbon nanotube thin film prepared with high temperature gummed tape in the vacuum coating room of magnetron sputtering apparatus
On, it is 2%Al by Ag targets and doping mass ratio2O3ZnO ceramic targets place target position on, with mechanical pump to vacuum film coating chamber take out
High vacuum is taken, vacuum degree is made to reach 1.5 × 10-3When Pa, it is passed through argon gas；
(2) DC power supply is opened, butterfly blocks the carbon nanotube thin film in substrate frame and carries out pre-sputtering, pre-sputtering 10min
Afterwards, rotary substrate frame, starts sputtering sedimentation Ag films, and rotary speed is 10 turns/min；
(3) after the completion of Ag thin film sputterings, vacuum is extracted again and reaches 1.5 × 10-3Pa, butterfly are passed through argon gas, make gas
When pressure reaches 2Pa, after opening radio-frequency power supply pre-sputtering 10min, sputtering pressure is adjusted to 0.052Pa, after power is adjusted to 1000W,
Rotary substrate frame starts to deposit AZO films.
The preparation raw material of cadmium liquid of going is ammonium ceric nitrate, glacial acetic acid and deionized water, per 1kg cerous nitrate proportionings
180ml glacial acetic acids.
Beneficial effects of the present invention：Compound Ag/AZO films in the carbon nanotube of the present invention, reduce the sheet resistance of film, have
Good photoelectric properties, improve the resist bending ability of film, and flexible performance is good, moreover it is possible to reduce environmental pollution, reduce cost of manufacture.
Specific implementation mode
A kind of preparation method of flexible transparent electrode, step are：
(1) preparation of carbon nano-tube film：Single armed carbon nanotube is prepared using FCCVD methods, single armed carbon nanotube is handled
After be configured to suspension, carbon nano-tube film is made on PET substrate by spray coating method；
(2) preparation of Ag/AZO films：Using direct current magnetron sputtering process and radio-frequency magnetron sputter method in carbon nanotube thin film obtained
It is coated with Ag films and AZO films successively above；
(3) Ag/AZO films gluing：The thin glue of equal glue machine spin coating AZ310 is used on the substrate PET for be coated with CNT/Ag/AZO,
Rotating speed 3000rad/s, acceleration 3000rad/s, spin-coating time 30s；
(4) uv-exposure：After gluing on hot plate 90 DEG C baking 15min, remove glue-line in solvent after carry out uv-exposure,
Uv power density is 3mw/cm2, time for exposure 34s；
(5) removal photoresist develops：The use of thin glue developing solution AZ300 removals is the photoresist of exposure, by mask plate
On metal grill pattern be transferred on photoresist coating, developing time be 28~32s；
(6) grid is etched：It dries 30min after development at 90 DEG C in baking oven, carries out the adherency that post bake increases glued membrane and substrate
Then power is configured to cadmium liquid, removal etches unwanted Ag/AZO films between grid, and etch period is 23~27s；
(7) photoresist on grid is removed：Sample after etching grid is put into the NaOH solution configured and removes grid
Then the photoresist of upper covering is washed with deionized water net sample and obtains flexible transparent electrode.
The carbon nano-tube film preparation process is：
A., the surfactant that single armed carbon nanotube powder 1g is mixed to the neopelex of 1L a concentration of 1% is molten
CNT suspension is made in liquid；
B. CNT suspension is put into ultrasound 1h in the ultrasonic machine that power is 40W；
C. the good CNT suspension of ultrasound is put into the centrifuge 20min that rotating speed is 1400rpm；
D. it takes the suspension on upper layer and puts into spray gun, by suspension spray on PET substrate, equally distributed CNT is made
Film；
E. substrate is cleaned with deionized water, to wash off neopelex；
F. step d and step e 4~5 times is repeated, certain thickness carbon nanotube thin film is formed.
The PET substrate is previously heated to 100 DEG C before spraying by constent temperature heater, and constant temperature remains to spraying knot
Beam.
The preparation process of the Ag/AZO films is：
(1) substrate frame being attached to the carbon nanotube thin film prepared with high temperature gummed tape in the vacuum coating room of magnetron sputtering apparatus
On, it is 2%Al by Ag targets and doping mass ratio2O3ZnO ceramic targets place target position on, with mechanical pump to vacuum film coating chamber take out
High vacuum is taken, vacuum degree is made to reach 1.5 × 10-3When Pa, it is passed through argon gas；
(2) DC power supply is opened, butterfly blocks the carbon nanotube thin film in substrate frame and carries out pre-sputtering, pre-sputtering 10min
Afterwards, rotary substrate frame, starts sputtering sedimentation Ag films, and rotary speed is 10 turns/min；
(3) after the completion of Ag thin film sputterings, vacuum is extracted again and reaches 1.5 × 10-3Pa, butterfly are passed through argon gas, make gas
When pressure reaches 2Pa, after opening radio-frequency power supply pre-sputtering 10min, sputtering pressure is adjusted to 0.052Pa, after power is adjusted to 1000W,
Rotary substrate frame starts to deposit AZO films.
The preparation raw material of cadmium liquid of going is ammonium ceric nitrate, glacial acetic acid and deionized water, per 1kg cerous nitrate proportionings
180ml glacial acetic acids.
Embodiment 1
A kind of preparation method of flexible transparent electrode, step are：
(1) preparation of carbon nano-tube film：Single armed carbon nanotube is prepared using FCCVD methods, single armed carbon nanotube is handled
After be configured to suspension, carbon nano-tube film is made on PET substrate by spray coating method, specially：By single armed carbon nanotube powders
Last 1g mixes is made CNT suspension in the surfactant solution of the neopelex of 1L a concentration of 1%；CNT is hanged
Supernatant liquid is put into ultrasound 1h in the ultrasonic machine that power is 40W；The good CNT suspension of ultrasound is put into the centrifugation that rotating speed is 1400rpm
Machine centrifuges 20min；It takes the suspension on upper layer and puts into spray gun, by suspension spray on PET substrate, be made equally distributed
Carbon nanotube thin film；Substrate is cleaned with deionized water, to wash off neopelex；Repeat step spraying, cleaning step 4~5
It is secondary, certain thickness carbon nanotube thin film is formed, PET substrate is previously heated to 100 DEG C, and constant temperature before spraying by constent temperature heater
Spraying is remained to terminate；
(2) preparation of Ag/AZO films：Using direct current magnetron sputtering process and radio-frequency magnetron sputter method in carbon nanotube thin film obtained
It is coated with Ag films and AZO films successively above, specially：The carbon nanotube thin film prepared is attached to magnetron sputtering with high temperature gummed tape to set
It is 2%Al by Ag targets and doping mass ratio in substrate frame in standby vacuum coating room2O3ZnO ceramic targets place target position
On, high vacuum is extracted to vacuum film coating chamber with mechanical pump, vacuum degree is made to reach 1.5 × 10-3When Pa, it is passed through argon gas；Open direct current
Power supply, butterfly blocks the carbon nanotube thin film in substrate frame and carries out pre-sputtering, and after pre-sputtering 10min, rotary substrate frame starts to splash
Deposition Ag films are penetrated, rotary speed is 10 turns/min；After the completion of Ag thin film sputterings, vacuum is extracted again and reaches 1.5 × 10-3Pa,
Butterfly is passed through argon gas, and when air pressure being made to reach 2Pa, after opening radio-frequency power supply pre-sputtering 10min, sputtering pressure is adjusted to
0.052Pa, after power is adjusted to 1000W, rotary substrate frame starts to deposit AZO films.
(3) Ag/AZO films gluing：The thin glue of equal glue machine spin coating AZ310 is used on the substrate PET for be coated with CNT/Ag/AZO,
Rotating speed 3000rad/s, acceleration 3000rad/s, spin-coating time 30s；
(4) uv-exposure：After gluing on hot plate 90 DEG C baking 15min, remove glue-line in solvent after carry out uv-exposure,
Uv power density is 3mw/cm2, time for exposure 34s；
(5) removal photoresist develops：The use of thin glue developing solution AZ300 removals is the photoresist of exposure, by mask plate
On metal grill pattern be transferred on photoresist coating, developing time be 28~32s；
(6) grid is etched：It dries 30min after development at 90 DEG C in baking oven, promotes film firm, increase glued membrane and substrate
Then adhesion strength is configured to cadmium liquid with the deionized water of 2kg cerous nitrates, 360ml glacial acetic acids and 7L, is not required between removal etching grid
The Ag/AZO films wanted, etch period are 23~27s；
(7) photoresist on grid is removed：Sample after etching grid is put into the NaOH solution configured and removes grid
Then the photoresist of upper covering is washed with deionized water net sample and obtains flexible transparent electrode.
Using ultraviolet specrophotometer to the optical performance test of CNT/Ag/AZO transparent electrode thin films, in visible light
Transmitance is 95.5%, is tested the sheet resistance of CNT/Ag/AZO films, and square resistance is 3.8 Ω/sq, which has
Good flexibility, when being bent 500 times, square resistance is 4.18 Ω/sq.
One embodiment of the present invention has been described in detail above, but the content be only the present invention preferable implementation
Example should not be construed as limiting the practical range of the present invention.It is all according to all the changes and improvements made by the present patent application range
Deng should all still fall within the scope of the patent of the present invention.
Claims (5)
1. a kind of preparation method of flexible transparent electrode, which is characterized in that preparation process is：
(1) preparation of carbon nano-tube film：Single armed carbon nanotube is prepared using FCCVD methods, will be matched after the processing of single armed carbon nanotube
It is set to suspension, carbon nano-tube film is made on PET substrate by spray coating method；
(2) preparation of Ag/AZO films：Using direct current magnetron sputtering process and radio-frequency magnetron sputter method on carbon nanotube thin film obtained
It is coated with Ag films and AZO films successively；
(3) Ag/AZO films gluing：The thin glue of equal glue machine spin coating AZ310, rotating speed are used on the substrate PET for be coated with CNT/Ag/AZO
3000rad/s, acceleration 3000rad/s, spin-coating time 30s；
(4) uv-exposure：After gluing on hot plate 90 DEG C baking 15min, remove glue-line in solvent after carry out uv-exposure, it is ultraviolet
Optical power density is 3mw/cm2, time for exposure 34s；
(5) removal photoresist develops：The use of thin glue developing solution AZ300 removals is the photoresist of exposure, it will be on mask plate
Metal grill pattern is transferred on photoresist coating, and developing time is 28~32s；
(6) grid is etched：It dries 30min after development at 90 DEG C in baking oven, carries out the adhesion strength that post bake increases glued membrane and substrate, so
After be configured to cadmium liquid, unwanted Ag/AZO films between removal etching grid, etch period is 23~27s；
(7) photoresist on grid is removed：Sample after etching grid is put into removal grid overlying in the NaOH solution configured
Then the photoresist of lid is washed with deionized water net sample and obtains flexible transparent electrode.
2. the preparation method of flexible transparent electrode according to claim 1, which is characterized in that the carbon nano-tube film
Preparation process is：
A., in the surfactant solution of neopelex that single armed carbon nanotube powder 1g is mixed to 1L a concentration of 1%
CNT suspension is made；
B. CNT suspension is put into ultrasound 1h in the ultrasonic machine that power is 40W；
C. the good CNT suspension of ultrasound is put into the centrifuge 20min that rotating speed is 1400rpm；
D. it takes the suspension on upper layer and puts into spray gun, by suspension spray on PET substrate, equally distributed carbon nanotube thin film is made；
E. substrate is cleaned with deionized water, to wash off neopelex；
F. step d and step e 4~5 times is repeated, certain thickness carbon nanotube thin film is formed.
3. the preparation method of flexible transparent electrode according to claim 2, which is characterized in that the PET substrate is spraying
100 DEG C are previously heated to by constent temperature heater before applying, and constant temperature remains to spraying and terminates.
4. the preparation method of flexible transparent electrode according to claim 1, which is characterized in that the Ag/AZO films
Preparation process is：
(1) carbon nanotube thin film prepared is attached to high temperature gummed tape in the substrate frame in the vacuum coating room of magnetron sputtering apparatus, it will
Ag targets and doping mass ratio are 2%Al2O3ZnO ceramic targets place target position on, with mechanical pump to vacuum film coating chamber extract Gao Zhen
Sky makes vacuum degree reach 1.5 × 10-3When Pa, it is passed through argon gas；
(2) DC power supply is opened, butterfly blocks the carbon nanotube thin film in substrate frame and carries out pre-sputtering, after pre-sputtering 10min, rotation
Turn substrate frame, start sputtering sedimentation Ag films, rotary speed is 10 turns/min；
(3) after the completion of Ag thin film sputterings, vacuum is extracted again and reaches 1.5 × 10-3Pa, butterfly are passed through argon gas, and air pressure is made to reach
When to 2Pa, after opening radio-frequency power supply pre-sputtering 10min, sputtering pressure is adjusted to 0.052Pa, after power is adjusted to 1000W, rotation
Substrate frame starts to deposit AZO films.
5. the preparation method of flexible transparent electrode according to claim 1, which is characterized in that the preparation for removing cadmium liquid
Raw material is ammonium ceric nitrate, glacial acetic acid and deionized water, and 180ml glacial acetic acids are matched per 1kg cerous nitrates.
Priority Applications (1)
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| CN201810472539.5A CN108649104A (en) | 2018-05-17 | 2018-05-17 | A kind of preparation method of flexible transparent electrode |
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| CN201810472539.5A CN108649104A (en) | 2018-05-17 | 2018-05-17 | A kind of preparation method of flexible transparent electrode |
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| CN108649104A true CN108649104A (en) | 2018-10-12 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110092369A (en) * | 2019-03-25 | 2019-08-06 | 昆明理工大学 | A kind of method and application of nano silver modification carbon nano tube surface |
| US20240103357A1 (en) * | 2021-08-26 | 2024-03-28 | Mitsui Chemicals, Inc. | Pellicle film, pellicle, exposure original plate, exposure device, and method for manufacturing pellicle film |
-
2018
- 2018-05-17 CN CN201810472539.5A patent/CN108649104A/en not_active Withdrawn
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110092369A (en) * | 2019-03-25 | 2019-08-06 | 昆明理工大学 | A kind of method and application of nano silver modification carbon nano tube surface |
| US20240103357A1 (en) * | 2021-08-26 | 2024-03-28 | Mitsui Chemicals, Inc. | Pellicle film, pellicle, exposure original plate, exposure device, and method for manufacturing pellicle film |
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