CN110299222A - A kind of visible transparent conductive film and preparation method thereof - Google Patents
A kind of visible transparent conductive film and preparation method thereof Download PDFInfo
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- CN110299222A CN110299222A CN201910686601.5A CN201910686601A CN110299222A CN 110299222 A CN110299222 A CN 110299222A CN 201910686601 A CN201910686601 A CN 201910686601A CN 110299222 A CN110299222 A CN 110299222A
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- H01—ELECTRIC ELEMENTS
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- H01B13/00—Apparatus or processes specially adapted for manufacturing conductors or cables
- H01B13/0026—Apparatus for manufacturing conducting or semi-conducting layers, e.g. deposition of metal
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- H—ELECTRICITY
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- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
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Abstract
The invention discloses a kind of visible transparent conductive films, are prepared in transparent substrates, the conductive layer with silver nanowires preparation in the transparent substrates；The transition zone that there is conductive capability and adhesive force to promote ability for setting between the transparent substrates and conductive layer, for enhancing the adhesive force between conductive layer and transparent substrates and enhancing the electric conductivity of conductive layer；With the protective layer with conductive capability on the conductive layer, avoid silver nanowires by oxidation damage.It is simple, low in cost that preparation condition is included using a kind of visible transparent conductive film and preparation method thereof of the invention, realizes that sample layer is spaced apart with rubbing method and infusion method, mild condition, strong operability；The size that film is made can be by substrate sizes come flexible modulation；Gained visible transparent conductive film transmitance height, good conductivity, can be widely applied in fields such as solar battery, touch screen, light transmission electromagnetic protections.
Description
Technical field
The present invention relates to a kind of visible transparent conductive films and preparation method thereof, belong to optical film technology field.
Background technique
Transparent conductive film is because of its high transparency and good electric conductivity, in touch screen, solar battery, light-emitting diodes
Pipe, optical window electromagnetic protection etc. have very broad application prospect.It is saturating that transparent conductive film is broadly divided into metal oxide
Bright conductive film, transparent graphene conductive film, macromolecule transparent conductive film and metal nanometer line transparent conductive film etc..
Wherein, belong to the indium tin oxide transparent conductive film (ITO) of transparent conductive metal oxide film because of its high transparency, protrusion
Electric conductivity and maturation preparation process the advantages that and become and be most widely used at present and universal a kind of electrically conducting transparent is thin
Film, people have also done numerous studies to it.But there are still the limitations of some disadvantages to apply for its own: (1) having in the raw material of ITO dilute
There is indium metal, belong to non-renewable resources, with the increasingly reduction of yield, price is also more expensive, therefore cost of manufacture improves；
(2) though ITO manufacture craft is mature, complex, costly, yield is relatively very low, and cost performance is low；(3) ITO easily adsorbs air
In carbon dioxide and water, after chemically reacting occur " mildew ", influence using.Therefore, it is necessary to develop a kind of alternative
Transparent conductive film can evade these disadvantages under the premise of guaranteeing light transmittance and electric conductivity.
Silver nanowires is a kind of one-dimensional metal nano material, adjustable with draw ratio, conductivity is high, optical clear etc. is excellent
Point, and may be homogenously dispersed in the volatile solvents such as water, ethyl alcohol, isopropanol.Be cross-linked with each other transparent leading of being formed by silver nanowires
Conductive film can have both high transparency and superior electrical conductivity, and preparation process is simple and quick, be the ideal film for substituting ITO.But silver is received
Rice noodles, which are directly exposed to air, to be easily oxidized, and is influenced property of thin film, is restricted its application range to a certain extent.
Summary of the invention
Goal of the invention of the invention is: in view of the above problems, provide a kind of visible transparent conductive film and
Preparation method, a kind of visible transparent conductive film of the invention is high to visible light transmittance, electric conductivity is strong, film size can
It adjusts, stability height, preparation condition is simple, low in cost.
The technical solution adopted by the invention is as follows:
A kind of visible transparent conductive film, is prepared in transparent substrates, has silver nanowires system in the transparent substrates
Standby conductive layer；There is conductive capability and adhesive force to promote the transition zone of ability for setting between the transparent substrates and conductive layer,
For enhancing the adhesive force between conductive layer and transparent substrates and enhancing the electric conductivity of conductive layer；With tool on the conductive layer
There is the protective layer of conductive capability, avoids silver nanowires by oxidation damage.
Preferably, the transparent substrates are the transparent materials such as glass, PET.
Preferably, the transition zone is made of conductive, transparent high molecular material.
Preferably, the transition zone is made of diallyl dimethyl ammoniumchloride, specifically by immersion polydiene
Diallyidimethylammonium chloride solution is made.
In above scheme, diallyl dimethyl ammoniumchloride itself is conductive, by impregnating polydiene propyl two
Ammonio methacrylate can enhance the binding force between silver nanowires line and line, enhance electric conductivity, can also enhance silver nanowires and base
Adhesive force between bottom.
Preferably, the protective layer is made of conductive, transparent high molecular material.
Preferably, the protective layer is made of diallyl dimethyl ammoniumchloride, specifically by immersion polydiene
Diallyidimethylammonium chloride solution is made.
In above scheme, silver nanowires and air can be effectively isolated by diallyl dimethyl ammoniumchloride, avoid silver
Nano wire is by oxidation damage；Diallyl dimethyl ammoniumchloride itself is conductive simultaneously, by impregnating polydiene third
Base alkyl dimethyl ammonium chloride can enhance the binding force between silver nanowires line and line, enhance electric conductivity.
Preferably, the conductive layer is handled by the mixed solution of sodium borohydride aqueous solution and ethyl alcohol.
In above scheme, conductive layer can be enhanced and lead after the processing of the mixed solution of sodium borohydride aqueous solution and ethyl alcohol
The electric conductivity of electric layer.
The preparation method of above-mentioned visible transparent conductive film, it is characterised in that: the following steps are included:
Step a: being cleaned by ultrasonic substrate ethyl alcohol and deionized water and dry up, be put into plasma cleaner clean the surface,
Obtain the substrate of surface hydrophilic；
Step b: substrate obtained by step a is placed in diallyl dimethyl ammoniumchloride solution, takes out, spends after immersion
Ionized water is uniformly rinsed and is dried up, and is placed in coating cloth deck and is fixed；
Step c: silver nanowires solution is dripped in substrate top, after silver nanowires solution is pulled into film with bar, is placed in true
It is dried in vacuo in empty drying box；
Step d: gained film in step c is placed in the mixed solution of sodium borohydride aqueous solution and ethyl alcohol and is impregnated, after taking-up
It is rinsed and is dried up with ethyl alcohol；
Step e: film obtained by step d being placed in diallyl dimethyl ammoniumchloride solution after impregnating and taken out, deionization
Water is rinsed and is dried up, and obtains visible transparent conductive film.
It is dried with nitrogen preferably, drying up to be all made of in above-mentioned steps.
Preferably, substrate is cleaned 4-8 times with deionized water and EtOH Sonicate in step a.
Preferably, the power of Ion Cleaning machine is 50-150W, and the test process time is set as 1-20min in step a.
Preferably, the concentration of the diallyl dimethyl ammoniumchloride solution is 1-5mg/mL in step b, impregnate
Time is 1-10min.
Preferably, the silver nanowires solution is by silver nanowires Centrifugal dispersion in deionized water and isopropanol in step c
It is made in mixed solution, silver nanowires concentration is 0.1-1mg/mL, and the volume ratio of deionized water and isopropanol is 0.1-1.
Preferably, the drop-down speed of the bar is 1-5cm/s in step c.
Preferably, the vacuum drying time is 1-10min in step c, drying temperature is 30-100 DEG C.
Preferably, the mixed solution concentration of the sodium borohydride aqueous solution and ethyl alcohol is 0.1-1mol/L in step d,
The volume ratio of sodium borohydride aqueous solution and ethyl alcohol is 1:1, soaking time 0.5-5min.
Preferably, the concentration of the diallyl dimethyl ammoniumchloride solution is 0.1-5mg/mL, leaching in step e
The bubble time is 1-10min.
A kind of visible transparent conductive film of the invention and preparation method thereof, silver nanowires is as one-dimensional metal nanometer material
Material has the characteristics that draw ratio is big, good conductivity, may be homogenously dispersed in the easy volatile solvents such as water, ethyl alcohol and isopropanol；It impregnates
The glass surface of diallyl dimethyl ammoniumchloride is crossed in electronegativity, silver nanowires is easily adsorbed to glass surface, enhancing knot
Conjunction property；Diallyl dimethyl ammoniumchloride itself is conductive, by impregnating diallyl dimethyl ammoniumchloride, can increase
Binding force between strong silver nanowires line and line, enhances electric conductivity；Diallyl dimethyl ammoniumchloride can be used as protective layer, will
Silver nanowires is effectively isolated with air, avoids silver nanowires by oxidation damage.
In conclusion by adopting the above-described technical solution, the beneficial effects of the present invention are:
(1) preparation condition is simple, low in cost, realizes that sample layer is spaced apart with rubbing method and infusion method, mild condition,
Strong operability；
(2) size that film is made can be by substrate sizes come flexible modulation；
(3) gained visible transparent conductive film transmitance height, good conductivity, can be in solar battery, touch screen, light transmission
The fields such as electromagnetic protection are widely applied.
Detailed description of the invention
Examples of the present invention will be described by way of reference to the accompanying drawings, in which:
Fig. 1 is visible transparent conductive film preparation step figure；
Fig. 2 is the scanning electron microscope (SEM) photograph of silver nanowires；
Fig. 3 is light transmittance curve of 1 made membrane of embodiment in visible region (400-760nm)；
Fig. 4 is light transmittance curve of 2 made membranes of embodiment in visible region (400-760nm)；
Fig. 5 is light transmittance curve of 3 made membranes of embodiment in visible region (400-760nm).
Specific embodiment
All features disclosed in this specification or disclosed all methods or in the process the step of, in addition to mutually exclusive
Feature and/or step other than, can combine in any way.
Any feature disclosed in this specification unless specifically stated can be equivalent or with similar purpose by other
Alternative features are replaced.That is, unless specifically stated, each feature is an example in a series of equivalent or similar characteristics
?.
As shown in Figure 1, a kind of visible transparent conductive film and preparation method thereof, needs to handle by substrate surface, leaching
Steep diallyl dimethyl ammoniumchloride solution, preparation silver nanowires transparent conductive film, silver nanowires transparent conductive film table
Surface treatment impregnates the key steps such as diallyl dimethyl ammoniumchloride solution.
Fig. 2 is the silver nanowires scanning electron microscope (SEM) photograph used in the present invention, and draw ratio 1000, purity are greater than 90%.
Embodiment 1
Step a: glass ethyl alcohol and deionized water are cleaned by ultrasonic 4 times repeatedly, with being dried with nitrogen, are laid flat clear into plasma
Clean the surface in washing machine, the power of plasma cleaner are 120W, time 5min, and operating process, which should be noted, marks glass to be located
Reason face, to prevent influencing to be film-made effect；
Step b: sheet glass obtained by step a is placed in the diallyl dimethyl ammoniumchloride solution that concentration is 1mg/mL
In, it is taken out after impregnating 5min, is dried with nitrogen after uniformly being rinsed with deionized water, is placed in coating cloth deck and fixes, pay attention to processed glass
Glass is face-up；
Step c: silver nanowires solution is dripped in sheet glass top, with bar by silver nanowires solution with the speed of 3cm/s
Uniformly drop-down film forming is placed in dry 5min in the vacuum oven that temperature is 60 DEG C；Silver nanowires solution is by the 0.2mg/ of 1mL
It is made in the mixed solution that mL silver nanowires Centrifugal dispersion 1mL deionized water and isopropanol volume ratio are 0.2；
Step d: film obtained by step c is placed in the mixed solution of sodium borohydride aqueous solution and ethyl alcohol that concentration is 1mol/L
1min is impregnated, wherein the volume ratio of sodium borohydride aqueous solution and ethyl alcohol is 1:1, is uniformly rinsed after taking-up with ethyl alcohol and is blown with nitrogen
It is dry；
Step e: film obtained by step d is placed in the diallyl dimethyl ammoniumchloride solution of 1mg/mL after impregnating 5min
Take out, deionized water uniformly rinses after with being dried with nitrogen, acquisition visible transparent conductive film.
Fig. 3 is the light transmittance test curve of the transparent conducting thin film for preparing in visible region (400~760nm), wherein
The light transmittance of 550nm green light is up to 97%；The sheet resistance of transparent conducting thin film is 215 Ω/.
Embodiment 2
Step a: glass ethyl alcohol and deionized water are cleaned by ultrasonic 6 times repeatedly, with being dried with nitrogen, are laid flat clear into plasma
Clean the surface in washing machine, the power of plasma cleaner are 80W, time 10min, and operating process, which should be noted, marks glass to be located
Reason face, to prevent influencing to be film-made effect；
Step b: sheet glass obtained by step a is placed in the diallyl dimethyl ammoniumchloride solution that concentration is 1mg/mL
In, it is taken out after impregnating 5min, is dried with nitrogen after uniformly being rinsed with deionized water, is placed in coating cloth deck and fixes, pay attention to processed glass
Glass is face-up；
Step c: silver nanowires solution is dripped in sheet glass top, with bar by silver nanowires solution with the speed of 3cm/s
Uniformly drop-down film forming is placed in dry 5min in the vacuum oven that temperature is 60 DEG C；Silver nanowires solution is by the 0.4mg/ of 1mL
It is made in the mixed solution that mL silver nanowires Centrifugal dispersion 1mL deionized water and isopropanol volume ratio are 0.5；
Step d: film obtained by step c is placed in the mixed solution of sodium borohydride aqueous solution and ethyl alcohol that concentration is 1mol/L
2min is impregnated, wherein the volume ratio of sodium borohydride aqueous solution and ethyl alcohol is 1:1, is uniformly rinsed after taking-up with ethyl alcohol and is blown with nitrogen
It is dry；
Step e: film obtained by step d is placed in the diallyl dimethyl ammoniumchloride solution of 1mg/mL after impregnating 5min
Take out, deionized water uniformly rinses after with being dried with nitrogen, acquisition visible transparent conductive film.
Fig. 4 is the light transmittance test curve of the transparent conducting thin film for preparing in visible region (400~760nm), wherein
The light transmittance of 550nm green light is up to 95%；The sheet resistance of transparent conducting thin film is 55 Ω/.
Embodiment 3
Step a: glass ethyl alcohol and deionized water are cleaned by ultrasonic 4 times repeatedly, with being dried with nitrogen, are laid flat clear into plasma
Clean the surface in washing machine, the power of plasma cleaner are 130W, time 3min, and operating process, which should be noted, marks glass to be located
Reason face, to prevent influencing to be film-made effect；
Step b: sheet glass obtained by step a is placed in the diallyl dimethyl ammoniumchloride solution that concentration is 2mg/mL
In, it is taken out after impregnating 1min, is dried with nitrogen after uniformly being rinsed with deionized water, is placed in coating cloth deck and fixes, pay attention to processed glass
Glass is face-up；
Step c: silver nanowires solution is dripped in sheet glass top, with bar by silver nanowires solution with the speed of 3cm/s
Uniformly drop-down film forming is placed in dry 10min in the vacuum oven that temperature is 50 DEG C；Silver nanowires solution is by 1mL's
It is made in the mixed solution that 0.8mg/mL silver nanowires Centrifugal dispersion 1mL deionized water and isopropanol volume ratio are 0.9；
Step d: film obtained by step c is placed in the mixed solution of sodium borohydride aqueous solution and ethyl alcohol that concentration is 1mol/L
1min is impregnated, wherein the volume ratio of sodium borohydride aqueous solution and ethyl alcohol is 1:1, is uniformly rinsed after taking-up with ethyl alcohol and is blown with nitrogen
It is dry；
Step e: film obtained by step d is placed in the diallyl dimethyl ammoniumchloride solution of 2mg/mL after impregnating 3min
Take out, deionized water uniformly rinses after with being dried with nitrogen, acquisition visible transparent conductive film.
Fig. 3 is the light transmittance test curve of the transparent conducting thin film for preparing in visible region (400~760nm), wherein
The light transmittance of 550nm green light is up to 90%；The sheet resistance of transparent conducting thin film is 26 Ω/.
In addition, also done lack step b comparative test (between glass and silver nanowires impregnate polydiene dimethylamine
Ammonium chloride solution)；The result shows that the sheet resistance for lacking the latter made transparent conductive film of step b is larger, while silver nanowire layer
It is easy to fall off from glass；This illustrates that diallyl dimethyl ammoniumchloride can enhance the electric conductivity of transparent conductive film, together
The adhesive force of Shi Zengjia transparent conductive film.
In addition, also having done the comparative test for lacking step d (using the processing of the mixed solution of sodium borohydride aqueous solution and ethyl alcohol
The step of film)；The result shows that the sheet resistance for lacking the latter made transparent conductive film of step d is big, illustrate to use sodium borohydride water
Its electric conductivity can be enhanced in the mixed solution Processing Ag nano wire film of solution and ethyl alcohol；This is because water-soluble by sodium borohydride
The processing of the mixed solution of liquid and ethyl alcohol, can clear up the impurity on silver nanowires surface, the electric conductivity of enhanced film.
Experiment shows that the lower poorer light transmittance of its electric conductivity of silver nanowires concentration is better, silver nanowires concentration it is higher its
Electric conductivity is better, and light transmittance is poorer；When silver nanowires concentration is 0.1-1mg/mL, visible transparent conductive film obtained
Electric conductivity and light transmittance are all preferable；When silver nanowires concentration is lower than 0.1mg/mL, it is seen that light transparent conductive film electric conductivity
Poor to meet the requirements, when silver nanowires concentration is as low as certain value, light transmittance tends towards stability but poorly conductive；When silver is received
When rice noodles concentration is higher than 1mg/mL, it is seen that light transparent conductive film light transmittance is poor to meet the requirements, when silver nanowires concentration
When height arrives certain value, electric conductivity increases less but light transmittance continues to be deteriorated.
The invention is not limited to specific embodiments above-mentioned.The present invention, which expands to, any in the present specification to be disclosed
New feature or any new combination, and disclose any new method or process the step of or any new combination.
Claims (11)
1. a kind of visible transparent conductive film, is prepared in transparent substrates, it is characterised in that: have silver in the transparent substrates
The conductive layer of nano wire preparation；
There is conductive capability and adhesive force to promote the transition zone of ability for setting between the transparent substrates and conductive layer, for enhancing
Adhesive force between conductive layer and transparent substrates and the electric conductivity for enhancing conductive layer；With with conductive energy on the conductive layer
The protective layer of power, avoids silver nanowires by oxidation damage.
2. visible transparent conductive film as described in claim 1, it is characterised in that: the transition zone is by polydiene propyl two
Ammonio methacrylate is made.
3. visible transparent conductive film as described in claim 1, it is characterised in that: the protective layer is by polydiene propyl two
Ammonio methacrylate is made.
4. visible transparent conductive film as described in claim 1, it is characterised in that: the conductive layer passes through sodium borohydride water
The processing of the mixed solution of solution and ethyl alcohol.
5. the preparation method of visible transparent conductive film according to any one of claims 1-4, it is characterised in that: including with
Lower step:
Step a: substrate ethyl alcohol and deionized water are cleaned by ultrasonic and are dried up, plasma cleaner clean the surface is put into, obtains
The substrate of surface hydrophilic；
Step b: substrate obtained by step a is placed in diallyl dimethyl ammoniumchloride solution, is taken out after immersion, uses deionization
Water is rinsed and is dried up；
Step c: silver nanowires solution is dripped in substrate top, and after silver nanowires solution is pulled into film with bar, it is dry to be placed in vacuum
It is dried in vacuo in dry case；
Step d: gained film in step c is placed in the mixed solution of sodium borohydride aqueous solution and ethyl alcohol and is impregnated, second is used after taking-up
Alcohol is rinsed and is dried up；
Step e: film obtained by step d being placed in diallyl dimethyl ammoniumchloride solution after impregnating and taken out, deionized water punching
It washes and dries up, obtain visible transparent conductive film.
6. visible transparent conductive film as claimed in claim 5 and preparation method thereof, it is characterised in that: described in step b
The concentration of diallyl dimethyl ammoniumchloride solution is 1-5mg/mL, soaking time 1-10min.
7. visible transparent conductive film as claimed in claim 5 and preparation method thereof, it is characterised in that: described in step c
Silver nanowires solution is made in deionized water and isopropyl alcohol mixture by silver nanowires Centrifugal dispersion, and silver nanowires concentration is
The volume ratio of 0.1-1mg/mL, deionized water and isopropanol is 0.1-1.
8. visible transparent conductive film as claimed in claim 5 and preparation method thereof, it is characterised in that: described in step c
The drop-down speed of bar is 1-5cm/s.
9. visible transparent conductive film as claimed in claim 5 and preparation method thereof, it is characterised in that: described in step c
The vacuum drying time is 1-10min, and drying temperature is 30-100 DEG C.
10. visible transparent conductive film as claimed in claim 5 and preparation method thereof, it is characterised in that: in step d, institute
The mixed solution concentration for stating sodium borohydride aqueous solution and ethyl alcohol is 0.1-1mol/L, the volume ratio of sodium borohydride aqueous solution and ethyl alcohol
For 1:1, soaking time 0.5-5min.
11. visible transparent conductive film as claimed in claim 5 and preparation method thereof, it is characterised in that: in step e, institute
The concentration for stating diallyl dimethyl ammoniumchloride solution is 0.1-5mg/mL, soaking time 1-10min.
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| CN112071472A (en) * | 2020-09-15 | 2020-12-11 | 安徽宇航派蒙健康科技股份有限公司 | Graphene silver nanowire composite conductive film and preparation method thereof |
| CN112210991A (en) * | 2020-08-21 | 2021-01-12 | 盐城工学院 | Electrostatic spraying method of silver nanowire anti-electromagnetic fabric |
| CN113205903A (en) * | 2021-04-23 | 2021-08-03 | 广东省科学院新材料研究所 | Transparent conductive film and preparation method thereof |
| CN113223752A (en) * | 2021-04-15 | 2021-08-06 | 华南理工大学 | Flexible stretchable transparent conductive film and preparation method and application thereof |
| CN114420344A (en) * | 2022-02-14 | 2022-04-29 | 苏州诺菲纳米科技有限公司 | Processing method for reducing sheet resistance of silver nanowire conductive film |
| CN114613546A (en) * | 2022-02-28 | 2022-06-10 | 浙江大华技术股份有限公司 | Special-shaped base transparent conductive film and preparation method and application thereof |
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