CN108231245A - A kind of transparent conductive film and preparation method thereof - Google Patents
A kind of transparent conductive film and preparation method thereof Download PDFInfo
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Abstract
The present invention relates to a kind of transparent conductive films and preparation method thereof, belong to conductive film preparing technical field.The present invention is using copper chloride as copper source, oleic acid and oleyl amine are as derivant, glucose is reducing agent, polyvinylpyrrolidone is stabilizer, prepared uniform high length-diameter ratio, diameter, good dispersion, regular appearance copper nano-wire, pass through formation with smaller line density network, so as to provide longer permeation pathway and reduce internal copper knot point, resistivity is reduced, realizes low haze, the high grade of transparency, high conductivity and the transparent metal film layer of excellent mechanical flexibility and intensity, is recycled poly-（3,4 Ethylenedioxy Thiophenes）﹣ polystyrolsulfon acid aqueous solutions, cover copper nano-wire, composite membrane is prepared to improve the inoxidizability of copper nano-wire, enhance the ability that metallic diaphragm absorbs energy in folding deformation, reduce the sliding degree of conducting particles, so as to reduce the resistance change rate of film layer, the flexibility and electrical stability of product are further improved.
Description
Technical field
The present invention relates to a kind of transparent conductive films and preparation method thereof, belong to conductive film preparing technical field.
Background technology
In nature, conductor is often opaque and flexible poor, such as metal material, graphite；And transparent material
It is often non-conductive, such as glass, crystal.The traditional concept of people has been broken in the appearance of transparent conductive film, it is that one kind both had
Translucency and conductive function film.
For transparent conductive film as a kind of important photoelectric material, in visible light region, iuuminting rate is high, anti-in infrared band
It is very high to penetrate rate.Due to the photoelectric characteristic for having these excellent, transparent conductive film is in light emitting diode, lighting transistor, solar energy
The fields such as battery, touch screen are widely used.
It is transparent that transparent conductive film, which can be divided into oxide system transparent conductive film, macromolecular transparent conductive film and nano material,
Conductive film.Oxide system transparent conductive film is most widely used in optoelectronic areas.Conducting polymer is with conjugatedπbond
Insulator macromolecule be changed into a kind of conjugated polymer of conductor after being aoxidized or being restored doping.Therefore it is conductive high poly-
Object not only has high molecular structure feature, you can plasticity, corrosion resistance, MOLECULE DESIGN structure diversification, electromagnetic shielding etc., also
With metal high conductivity and the characteristic of semiconductor.Large specific surface area, the size of nano material are small, surface can and surface
Power is high, has the special performances such as small-size effect, skin effect, quantum size effect, quantum tunneling effect.These are special
Property causes nano material to be widely used in electronic device, optical device, space flight and aviation etc..
The quality of transparent conductive film is mainly reflected on light transmittance, resistivity, structure and the surface topography of visible region.It is soft
The electrical and optical performance of property substrate is strongly dependent on the microstructure of matrix, the stoichiometric ratio of various composition, impurity
Type and concentration etc., therefore, the matrix preparation process of flexible substrates have the performance of transparent conductive film particularly important influence.
The performance of transparent conductive film is also influenced other than being influenced by flexible substrates performance by preparation method.At present, it is transparent
The common preparation method of conductive film has：Spin-coating method, Meyer rod coating method, vacuum filtration method, spray coating method etc..
With science and technology be constantly progressive and the rapid development of electronic device, people are for the demand of mobile electronic device
Increasingly improve.The appearance of flexible transparent conducting film just meets the needs of people.The photoelectric properties of flexible transparent conducting film can
To compare favourably with traditional hard transparent conductive oxide film.Flexible transparent conducting film can be applied to thin-film solar cells,
The fields such as touch screen, wearable device, electronic skin.Although China has begun to grind the performance of flexible transparent conducting film
Study carefully, but develop very slow.How to obtain high transparency, low resistance, bending resistance are strong, mist degree is low flexible transparent conducting film according to
It is so problem to be solved.Therefore, the excellent flexible transparent conducting film of photoelectric properties, mechanical performance is developed with important
Meaning.
Invention content
The technical problems to be solved by the invention：Have for most widely used transparent conductive film currently on the market crisp
Property, it is impossible to need to fold, stretch, distort or the place of serious bending uses the problem of, provide a kind of electrically conducting transparent
Film and preparation method thereof.
In order to solve the above technical problems, the technical solution adopted by the present invention is：
The transparent conductive film includes basement membrane layer, metallic diaphragm, conducting polymer film layer.
The basement membrane layer is polyimides（PI）, polyethylene terephthalate（PET）, poly- naphthalenedicarboxylic acid ethylene glycol
Ester（PEN）, polyether sulfone（PES）, nylon（Nylon）, polytetrafluoroethylene (PTFE)（PTFE）, polyether-ether-ketone（PEEK）, makrolon（PC）、
Polyarylate（PAR）Or any one in glass.
The metallic diaphragm is copper nano-wire film layer, a concentration of 0.01 is configured to by the copper nano-wire of high length-diameter ratio~
The alcoholic solution of 1.0g/L is formed for 1~3 layer with 1000~1200r/min in the spin coating of basement membrane layer surface.
The copper nano-wire of the high length-diameter ratio be with copper chloride, oleic acid, oleyl amine, glucose, polyvinylpyrrolidone,
1~3h is reacted at 120~150 DEG C to be made.
The parts by weight of each material be 12~24 parts of copper chlorides, 8.75~17.50 parts of polyvinylpyrrolidones, 15~30
Part oleic acid, 1.5~3.0 parts of oleyl amines,
15~30 parts of glucose.
The conducting polymer film layer is poly-（3,4- Ethylenedioxy Thiophenes）﹣ polystyrolsulfon acid film layers, by gathering（3,
4- Ethylenedioxy Thiophenes）﹣ polystyrolsulfon acids aqueous solution is with 800~1000r/min in 1~2 layer of basement membrane layer surface spin coating
It forms.
It is described poly-（3,4- Ethylenedioxy Thiophenes）﹣ polystyrolsulfon acids aqueous solution is sub- for kayexalate and 3,4-
Ethylenedioxy thiophene in mass ratio 2.5：1 mixing, through sodium peroxydisulfate, Ferric Sulfate Hydrafe react 15~20h after with amberlite
Fat reacts, and filters to obtain ion exchange liquid, is diluted with water and is made.
The specific steps are：
（1）Take kayexalate, add in deionized water and dissolve, add 3,4- Ethylenedioxy Thiophenes, sodium peroxydisulfate,
Ferric sulfate is stirred to react after 15~20h and reacts 2~4h with ion exchange resin, filters to obtain ion exchange liquid；
（2）It is 1.0~1.2% that ion exchange liquid is diluted with water to solid content, is obtained poly-（3,4- Ethylenedioxy Thiophenes）﹣ polyphenyl
Vinyl sulfonic acid aqueous solution；
（3）By copper chloride, polyvinylpyrrolidone dissolving in deionized water, oleic acid, oleyl amine ultrasonic disperse are added, is heated to
Glucose is added in after 50~60 DEG C, 8~10h is stirred to react, then 1~3h is reacted at 120~150 DEG C, is washed after centrifugation
Obtain copper nano-wire；
（4）Copper nano-wire is taken to add in ultrasonic disperse in absolute ethyl alcohol, obtains copper nano-wire alcoholic solution；
（5）Basilar memebrane after cleaning is fitted into spin coater, using copper nano-wire alcoholic solution as coating liquid, and with 1000~1200r/
Min is in 1~3 layer of basement membrane surface spin coating, natural air drying after the completion of coating, then using solid content as 1.0~1.2% it is poly-（3,4- is sub-
Ethylenedioxy thiophene）﹣ polystyrolsulfon acids aqueous solution is coating liquid, with 800~1000r/min in basement membrane surface spin coating 1~2
Layer, natural air drying after the completion of coating obtain transparent conductive film.
Compared with other methods, advantageous effects are the present invention：
（1）The present invention is copper source, oleic acid and oleyl amine as derivant using copper chloride, and glucose is reducing agent, polyvinylpyrrolidine
Ketone is stabilizer, prepared uniform high length-diameter ratio, diameter, good dispersion, regular appearance copper nano-wire, by formed have
The network of smaller line density so as to provide longer permeation pathway and reduce internal copper knot point, reduces resistivity, realizes
The transparent metal film layer of low haze, the high grade of transparency, high conductivity and excellent mechanical flexibility and intensity recycles poly-（3,4- is sub-
Ethylenedioxy thiophene）﹣ polystyrolsulfon acid aqueous solutions cover copper nano-wire, prepare composite membrane to improve the antioxygen of copper nano-wire
The property changed, while the ability that metallic diaphragm absorbs energy in folding deformation is enhanced, the sliding degree of conducting particles is reduced, from
And the resistance change rate of film layer is reduced, further improve the flexibility and electrical stability of product；
（2）The present invention substitutes hard substrate with flexible substrates, and it is saturating that substitution transparent conductive oxide film prepares metal/conducting polymer
Bright conductive film, process is simple, easily operated, cost is relatively low and has higher efficiency, and transparent conductive film obtained has preferable
Electric conductivity and good conductibility, and transmissivity is excellent.
Specific embodiment
25~50g kayexalates are taken, are added in 200~300mL deionized waters, are stirred with 300~400r/min
20~30min, adds 10~20g3,4- Ethylenedioxy Thiophenes, 0.1~0.2g sodium peroxydisulfates, 0.1~0.2g ferric sulfate,
Continue to be stirred to react 15~20h, add in anion exchange resin after reaction and react 1~2h, filter to get filtrate, into filtrate
It adds in cation exchange resin and reacts 1~2h, filter to obtain ion exchange liquid, ion exchange liquid is diluted with water to solid content is
1.0~1.2%, it obtains poly-（3,4- Ethylenedioxy Thiophenes）﹣ polystyrolsulfon acid aqueous solutions, take 12~24g copper chlorides, 8.75~
17.50g polyvinylpyrrolidones add in 1.5~3.0L deionized waters, 10~15min are stirred with 300~400r/min
15~30g oleic acid is added in afterwards, and 1.5~3.0g oleyl amines disperse 15~20min with 200~300W ultrasonic echographies, are again heated to 50
~60 DEG C, 15~30g glucose is added in, 8~10h is stirred to react, then be transferred in hydrothermal reaction kettle, is reacted at 120~150 DEG C
1~3h, is fitted into 10~15min of centrifugation in centrifuge, must precipitate after being cooled to room temperature, precipitation 3~5 is washed with absolute ethyl alcohol
It is washed with deionized again after secondary 3~5 times, obtains copper nano-wire, take 0.1~1.0g copper nano-wires, add in 1~10L absolute ethyl alcohols
In, 30~40min is disperseed with 180~240W ultrasonic echographies, obtains copper nano-wire alcoholic solution, the PET film after cleaning is packed into rotation
In painting machine, using copper nano-wire alcoholic solution as coating liquid, and with 1000~1200r/min in 1~3 layer of PET film surface spin coating, coating
Natural air drying after the completion, then using solid content as 1.0~1.2% it is poly-（3,4- Ethylenedioxy Thiophenes）﹣ polystyrolsulfon acids are water-soluble
Liquid is coating liquid, and with 800~1000r/min in 1~2 layer of PET film surface spin coating, natural air drying after the completion of coating obtains transparent lead
Electrolemma.
Example 1
25g kayexalates are taken, are added in 200mL deionized waters, 20min is stirred with 300r/min, adds 10g3,4-
Ethylenedioxy Thiophene, 0.1g sodium peroxydisulfates, 0.1g ferric sulfate continue to be stirred to react 15h, add in anion after reaction and hand over
Resin reaction 1h is changed, is filtered to get filtrate, cation exchange resin reaction 1h is added in into filtrate, filters to obtain ion exchange liquid, it will
It is 1.0% that ion exchange liquid, which is diluted with water to solid content, is obtained poly-（3,4- Ethylenedioxy Thiophenes）﹣ polystyrolsulfon acid aqueous solutions,
12g copper chlorides are taken, 8.75g polyvinylpyrrolidones are added in 1.5L deionized waters, after being stirred 10min with 300r/min
15g oleic acid is added in, 1.5g oleyl amines disperse 15min with 200W ultrasonic echographies, are again heated to 50 DEG C, add in 15g glucose, stir
Reaction 8h is mixed, then is transferred in hydrothermal reaction kettle, 1h is reacted at 120 DEG C, is fitted into centrifuge and centrifuges after being cooled to room temperature
10min must be precipitated, and washed with absolute ethyl alcohol and be washed with deionized again 3 times after precipitating 3 times, obtained copper nano-wire, 0.1g copper is taken to receive
Rice noodles are added in 1L absolute ethyl alcohols, are disperseed 30min with 180W ultrasonic echographies, are obtained copper nano-wire alcoholic solution, after cleaning
PET film is fitted into spin coater, using copper nano-wire alcoholic solution as coating liquid, and with 1000r/min in 1 layer of PET film surface spin coating, painting
Natural air drying after the completion of covering, then using solid content as 1.0% it is poly-（3,4- Ethylenedioxy Thiophenes）﹣ polystyrolsulfon acid aqueous solutions
For coating liquid, with 800r/min in 1 layer of PET film surface spin coating, natural air drying after the completion of coating obtains transparent conductive film.
Example 2
28g kayexalates are taken, are added in 250mL deionized waters, 25min is stirred with 350r/min, adds 15g3,4-
Ethylenedioxy Thiophene, 0.1g sodium peroxydisulfates, 0.1g ferric sulfate continue to be stirred to react 18h, add in anion after reaction and hand over
Resin reaction 1h is changed, is filtered to get filtrate, cation exchange resin reaction 1h is added in into filtrate, filters to obtain ion exchange liquid, it will
It is 1.1% that ion exchange liquid, which is diluted with water to solid content, is obtained poly-（3,4- Ethylenedioxy Thiophenes）﹣ polystyrolsulfon acid aqueous solutions,
18g copper chlorides are taken, 12.75g polyvinylpyrrolidones are added in 2.3L deionized waters, after being stirred 12min with 350r/min
18g oleic acid is added in, 1.8g oleyl amines disperse 18min with 250W ultrasonic echographies, are again heated to 55 DEG C, add in 20g glucose, stir
Reaction 9h is mixed, then is transferred in hydrothermal reaction kettle, 2h is reacted at 130 DEG C, is fitted into centrifuge and centrifuges after being cooled to room temperature
12min must be precipitated, and washed with absolute ethyl alcohol and be washed with deionized again 4 times after precipitating 4 times, obtained copper nano-wire, 0.5g copper is taken to receive
Rice noodles are added in 5L absolute ethyl alcohols, are disperseed 35min with 210W ultrasonic echographies, are obtained copper nano-wire alcoholic solution, after cleaning
PET film is fitted into spin coater, using copper nano-wire alcoholic solution as coating liquid, and with 1100r/min in 2 layers of PET film surface spin coating, painting
Natural air drying after the completion of covering, then using solid content as 1.1% it is poly-（3,4- Ethylenedioxy Thiophenes）﹣ polystyrolsulfon acid aqueous solutions
For coating liquid, with 900r/min in 1 layer of PET film surface spin coating, natural air drying after the completion of coating obtains transparent conductive film.
Example 3
50g kayexalates are taken, are added in 300mL deionized waters, 30min is stirred with 400r/min, adds 20g3,4-
Ethylenedioxy Thiophene, 0.2g sodium peroxydisulfates, 0.2g ferric sulfate continue to be stirred to react 20h, add in anion after reaction and hand over
Resin reaction 2h is changed, is filtered to get filtrate, cation exchange resin reaction 2h is added in into filtrate, filters to obtain ion exchange liquid, it will
It is 1.2% that ion exchange liquid, which is diluted with water to solid content, is obtained poly-（3,4- Ethylenedioxy Thiophenes）﹣ polystyrolsulfon acid aqueous solutions,
24g copper chlorides are taken, 17.50g polyvinylpyrrolidones are added in 3.0L deionized waters, after being stirred 15min with 400r/min
30g oleic acid is added in, 3.0g oleyl amines disperse 20min with 300W ultrasonic echographies, are again heated to 60 DEG C, add in 30g glucose, stir
Reaction 10h is mixed, then is transferred in hydrothermal reaction kettle, 3h is reacted at 150 DEG C, is fitted into centrifuge and centrifuges after being cooled to room temperature
15min must be precipitated, and washed with absolute ethyl alcohol and be washed with deionized again 5 times after precipitating 5 times, obtained copper nano-wire, 1.0g copper is taken to receive
Rice noodles are added in 10L absolute ethyl alcohols, are disperseed 40min with 240W ultrasonic echographies, are obtained copper nano-wire alcoholic solution, after cleaning
PET film is fitted into spin coater, using copper nano-wire alcoholic solution as coating liquid, and with 1200r/min in 3 layers of PET film surface spin coating, painting
Natural air drying after the completion of covering, then using solid content as 1.2% it is poly-（3,4- Ethylenedioxy Thiophenes）﹣ polystyrolsulfon acid aqueous solutions
For coating liquid, with 1000r/min in 2 layers of PET film surface spin coating, natural air drying after the completion of coating obtains transparent conductive film.
Reference examples：The transparent conductive film of Hangzhou company production.
The transparent conductive film of example and reference examples is detected, specific detection is as follows：
The test of electric property：Use what is produced by Suzhou Jingge Electronic Co., Ltd., model ST2258C numbers four are visited
Needle tester measures the square resistance of transparent conductive film (thin slice square resistance rate).When measuring, it is only necessary to which probe is gently pressed
On the surface of transparent conductive film, square resistance is just shown on display.
The test of optical property：It is produced using Beijing Pu Xi all purpose instruments Co., Ltd, the purple of model TU-1900
Outside-visible spectrophotometer measures the translucency of conductive film.In testing, conductive film and clean PET are cut into 3cm*3cm sizes
Square (PET is object of reference), be fixed on absorption cell, measured with double faced adhesive tape.Test parameter is：Test speed is
2nm/s, wavelength scanning range 300nm-900nm.
The test of bending resistance：One end of transparent conductive film is fixed on the cantilever of plated film pulling machine, the one of pulling machine
On in cycle once, bent repeatedly, finally measure the square resistance after bending, assessed with the change rate of square resistance
The bending resistance of conductive film.
The test of mist degree：Use the light of model WGW produced by Shanghai Instrument Physical Optics Instrument Co., Ltd.
Electric mist degree instrument measures the mist degree of conductive film.Test method：The handle of photoelectricity mist degree instrument is placed on pushed-open position, in sample room not
Sample is put into, rotation button makes the registration on display be " 0 ".Handle is in position of furthering, and conductive film sample is put into sample room
Product, rotation button make registration be " 100 ".Aforesaid operations repeatedly make stable reading.Conductive membrane sample is put into sample room, it will
Handle is placed in pushed-open position, and the number on display screen is exactly the haze value (%) of the sample.
Specific testing result such as table 1.
1 performance characterization contrast table of table
| Detection project | Example 1 | Example 2 | Example 3 | Reference examples |
| Square resistance/sq | 84.6 | 80.3 | 82.2 | 70 |
| Light transmittance % | 92.1 | 88.9 | 89.6 | 80.5 |
| Square resistance growth rate % | 25 | 17 | 16 | 10 |
| Haze value % | 4 | 5.5 | 4.3 | 6.8 |
As shown in Table 1, the transparent conductive film that prepared by the present invention has excellent photoelectric properties, bending resistance and good stabilization
Property.
Claims (8)
1. a kind of transparent conductive film, which is characterized in that the transparent conductive film includes basement membrane layer, metallic diaphragm, conductive polymer
Sub- film layer.
2. a kind of transparent conductive film as described in claim 1, which is characterized in that the basement membrane layer is polyimides（PI）、
Polyethylene terephthalate（PET）, polyethylene naphthalate（PEN）, polyether sulfone（PES）, nylon（Nylon）, it is poly-
Tetrafluoroethene（PTFE）, polyether-ether-ketone（PEEK）, makrolon（PC）, polyarylate（PAR）Or any one in glass.
3. a kind of transparent conductive film as described in claim 1, which is characterized in that the metallic diaphragm is copper nano-wire film
Layer is configured to the alcoholic solution of a concentration of 0.01~1.0g/L by the copper nano-wire of high length-diameter ratio, with 1000~1200r/min in base
1~3 layer of counterdie layer surface spin coating forms.
4. a kind of transparent conductive film as claimed in claim 3, which is characterized in that the copper nano-wire of the high length-diameter ratio is with chlorine
Change copper, oleic acid, oleyl amine, glucose, polyvinylpyrrolidone, 1~3h is reacted at 120~150 DEG C and is made.
5. a kind of transparent conductive film as claimed in claim 4, which is characterized in that the parts by weight of each material are 12~24 parts
Copper chloride, 8.75~17.50 parts of polyvinylpyrrolidones, 15~30 parts of oleic acid, 1.5~3.0 parts of oleyl amines,
15~30 parts of glucose.
6. a kind of transparent conductive film as described in claim 1, which is characterized in that the conducting polymer film layer is poly-（3,4-
Ethylenedioxy Thiophene）﹣ polystyrolsulfon acid film layers, by gathering（3,4- Ethylenedioxy Thiophenes）﹣ polystyrolsulfon acids are water-soluble
Liquid is formed for 1~2 layer with 800~1000r/min in the spin coating of basement membrane layer surface.
7. a kind of transparent conductive film as claimed in claim 6, which is characterized in that described poly-（3,4- Ethylenedioxy Thiophenes）﹣
Polystyrolsulfon acid aqueous solution is kayexalate and 3,4- Ethylenedioxy Thiophene in mass ratio 2.5：1 mixing, passes through
Sodium sulphate, Ferric Sulfate Hydrafe are reacted after reacting 15~20h with ion exchange resin, are filtered to obtain ion exchange liquid, are diluted with water system
Into.
A kind of 8. preparation method of transparent conductive film as described in claim 1~7 any one, which is characterized in that specific step
Suddenly it is：
（1）Take kayexalate, add in deionized water and dissolve, add 3,4- Ethylenedioxy Thiophenes, sodium peroxydisulfate,
Ferric sulfate is stirred to react after 15~20h and reacts 2~4h with ion exchange resin, filters to obtain ion exchange liquid；
（2）It is 1.0~1.2% that ion exchange liquid is diluted with water to solid content, is obtained poly-（3,4- Ethylenedioxy Thiophenes）﹣ polyphenyl
Vinyl sulfonic acid aqueous solution；
（3）By copper chloride, polyvinylpyrrolidone dissolving in deionized water, oleic acid, oleyl amine ultrasonic disperse are added, is heated to
Glucose is added in after 50~60 DEG C, 8~10h is stirred to react, then 1~3h is reacted at 120~150 DEG C, is washed after centrifugation
Obtain copper nano-wire；
（4）Copper nano-wire is taken to add in ultrasonic disperse in absolute ethyl alcohol, obtains copper nano-wire alcoholic solution；
（5）Basilar memebrane after cleaning is fitted into spin coater, using copper nano-wire alcoholic solution as coating liquid, and with 1000~1200r/
Min is in 1~3 layer of basement membrane surface spin coating, natural air drying after the completion of coating, then using solid content as 1.0~1.2% it is poly-（3,4- is sub-
Ethylenedioxy thiophene）﹣ polystyrolsulfon acids aqueous solution is coating liquid, with 800~1000r/min in basement membrane surface spin coating 1~2
Layer, natural air drying after the completion of coating obtain transparent conductive film.
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