CN103050169B - Flexible transparent electrode and preparation method thereof - Google Patents
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Abstract
The invention discloses a flexible transparent electrode comprising a transparent polymer substrate, and a laminating layer of a silver nanowire film and a grapheme film attached to the transparent substrate. According to the flexible transparent electrode, the silver nanowire film and the grapheme film achieve an unexpected synergistic effect through the laminating layer, and the prepared flexible transparent electrode has high light transmittance, small resistance and good flexibility.
Description
Technical field
The present invention relates to a kind of flexible transparent electrode and preparation method thereof.
Background technology
Tin indium oxide (ITO) to be widely used various photoelectric device as transparent conductive film, comprises imageing sensor, solar cell (OPV), liquid crystal display, organic electroluminescent (OLED) and touch panel.Along with the requirement that increase and the product quality of market demand improve, these metal oxides expose series of problems: (1) phosphide element allowable exploitation is limited; (2) they are unstable under acidity and alkali condition; (3) their ion diffuse pollutes polymeric layer; (4) their inflexibility characteristic cannot meet the requirement of flexible device; (5) bad near infrared region properties of transparency.Therefore development of new transparent conductive film has important theoretical and practical significance.
At present, the transparent conductive material being expected to alternative ITO has doping ZnO, conducting polymer (as: poly-3,4-ethene dioxythiophene/polystyrolsulfon acid, poly-3,4-ethylene dioxythiophene/poly styrene sulfonate), carbon nano-tube, Graphene, metal gate and nano silver wire etc.Wherein especially be concerned by people due to advantage in flexible, stability and conductivity etc. of carbon nano-tube, Graphene and nano silver wire.The Graphene utilizing chemical gaseous phase depositing process to prepare obtains application on the touchscreen.But because Graphene is difficult to avoid introducing defect in growth course, its film resistor is mostly at 500 Ω/more than.The transparent conductive film prepared by nano silver wire can obtain the film resistor of about 100 Ω/ when visible light transmittance rate is about 90%.Rice Univ USA researcher is attached on Au, Cu or Al metal gate by the Graphene that CVD is grown, and obtains the composite and flexible transparency electrode of film resistor within the scope of 5 to 30 Ω/ (ACS Nano, 2011,5,6472 – 6479).Due to the complicated process of preparation of metal gate, be faced with the challenge of the aspects such as size scale and price, therefore still there is difficulty in application aspect.The seminar in Texas ,Usa university Jane Austen branch school golden nanometer particle, nano silver wire and graphene oxide with mixed uniformly form compound, obtaining light transmittance is 70%, and resistance is transparent conductive film (ACS Nano, 2012 of about 30 Ω/, 6,5157 – 5163).This seminar is also layered on a small amount of nano silver wire on the graphene film of CVD growth, significantly reduce the interior resistance in graphene film between domain, the resistance of graphene film is made to be down to 30-80 Ω/ (Nano Lett.2012,12,5679-5683) by 1000 Ω/.The composite construction of Graphene and Nano silver grain, nano wire have also been obtained in China to be studied widely, and focusing mostly on is being that predecessor prepares graphene-supported Nano silver grain with graphene oxide.The researcher of University of Electronic Science and Technology proposes the space utilizing Graphene to fill nano silver wire film, forms mixing pilotaxitic texture, and then improves the conductivity of nano silver wire film and the adhesiveness with substrate.In above-mentioned report, nano silver wire and Graphene are the structure between mixed phase, do not form independently membrane structure separately, and its performance boost such as light transmittance and resistance space is very limited.
Summary of the invention
The object of this invention is to provide a kind of flexible transparent electrode and preparation method thereof.
For solving the problems of the technologies described above, technical scheme of the present invention is:
A kind of flexible transparent electrode, comprises the lamination of transparent polymer substrate and the nano silver wire film adhered on a transparent substrate and graphene film.
Existing obvious boundary between above-mentioned nano silver wire film and graphene film, the connection both achieving again on two-dimentional yardstick, and create beyond thought cooperative effect.
In order to meet various demand, the laminated construction of described nano silver wire film and graphene film is
wherein, Ag is expressed as nano silver wire film, and G is expressed as graphene film, and n is expressed as the number of plies, and its value is 1-10.
In order to ensure the light transmittance of flexible transparent electrode, the thickness of described every layer of nano silver wire film is 5-300nm; The thickness of described every layer graphene film is 0.2-20nm.
In order to take into account the good light transmittance of flexible transparent electrode and little resistance simultaneously, the laminated thickness of described nano silver wire film and graphene film is 5-320nm.
Conveniently prepare, ensure properties of product simultaneously, described graphene film is graphene film prepared by chemical vapour deposition (CVD) or the graphene film being reduced preparation by graphene oxide; Described nano silver wire film is by spin coating, spraying, self assembly, inkjet printing or method for printing screen preparation.
Conveniently prepare, ensure properties of product, reduce costs, described transparent polymer substrate is PETG (PET) substrate, polyimides (PI) substrate, dimethyl silicone polymer (PDMS) substrate, polymethyl methacrylate (PMMA) substrate or Merlon (PC) substrate simultaneously.
The preparation method of above-mentioned flexible transparent electrode, being prepared as of described nano silver wire film: nano silver wire is dispersed in ethanol, isopropyl alcohol or nitrogen dimethylformamide solvent, nano silver wire solution, nano silver wire solution taked spray, be coated with, self assembly, inkjet printing or screen printing mode prepare nano silver wire film; Described nano silver wire solution concentration is 0.01-10mg/ml.
The technology that the present invention is not particularly limited is prior art.
Nano silver wire film of the present invention and graphene film reach beyond thought cooperative effect by lamination, prepared flexible transparent electrode, have higher light transmittance, less resistance and good pliability.
Accompanying drawing explanation
Fig. 1 is the present invention
the structural representation of the flexible transparent electrode of shape, wherein n is 1.
Fig. 2 is the present invention
the structural representation of the flexible transparent electrode of shape, wherein n is 1.
Fig. 3 is the present invention
the structural representation of the flexible transparent electrode of shape, wherein n is 1.
Fig. 4 is the present invention
the flexible electrode scanning electron microscope (SEM) photograph of shape.
In figure, 1 is nano silver wire film, and 2 is graphene film, and 3 is flexible substrate.
Embodiment
In order to understand the present invention better, illustrate content of the present invention further below in conjunction with embodiment, but content of the present invention is not only confined to the following examples.
Embodiment 1
1. PETG (PET) transparent flexible substrate outer protective film is removed;
2. be dispersed in alcohol solvent by nano silver wire, obtain the nano silver wire solution that concentration is 6mg/ml, take spraying method to prepare nano silver wire film in the flexible substrate of step 1. gained, the thickness of gained nano silver wire film is 20nm;
3. the graphene film that CVD grows is transferred on nano silver wire film, namely on nano silver wire film, superpose graphene film;
4. placed 50 minutes in the environment of 20 ° of C by superposition film, solvent remaining in removing superimposed layer, is formed
form structure, wherein n=1, obtain described flexible electrode.
5. the flexible electrode thickness obtained is 30nm, and its light transmittance is 85%, corresponding film resistor 10 (± 5) Ω/.
Embodiment 2
1. polyimides (PI) transparent flexible substrate outer protective film is removed, be placed on sol evenning machine;
2. nano silver wire is dispersed in isopropyl alcohol, obtains the nano silver wire solution that concentration is 0.5mg/ml, take the mode that is coated with in the flexible substrate of step 1. gained on prepare nano silver wire film, the thickness of gained nano silver wire film is 50nm;
3. graphene film prepared by chemical oxidization method is transferred on nano silver wire film, nano silver wire film superposes graphene film.
4. placed 10 minutes in the environment of 120 ° of C by superposition film, solvent remaining in removing superimposed layer, is formed
form structure, wherein n=1, obtain described flexible electrode.
5. the flexible electrode thickness obtained is 52nm, and its light transmittance is 86%, corresponding film resistor 9 (± 5) Ω/.
Embodiment 3
1. dimethyl silicone polymer (PDMS) transparent flexible substrate outer protective film is removed;
2. nano silver wire is dispersed in nitrogen dimethylformamide (DMF), obtain the nano silver wire solution that concentration is 2mg/ml, take self assembly mode in the flexible substrate of step 1. gained on prepare nano silver wire film, the thickness of gained nano silver wire film is 30nm;
3. the graphene film that CVD grows is transferred on nano silver wire film, nano silver wire film superposes graphene film.
4. placed 20 minutes in the environment of 30 ° of C by superposition film, solvent remaining in removing superimposed layer, is formed
form structure, wherein n=1, obtain described flexible electrode.
5. the flexible electrode thickness obtained is 40nm, and its light transmittance is 87%, corresponding film resistor 9 (± 5) Ω/.
Embodiment 4
1. polymethyl methacrylate (PMMA) transparent flexible substrate outer protective film is removed;
2. the graphene film that CVD grows is transferred in PET film;
3. nano silver wire is in ethanol dispersed, obtain the nano silver wire solution that concentration is 3mg/ml, graphene film uses the mode of spraying superpose nano silver wire film, the thickness of nano silver wire film is 100nm;
4. superposition film is placed 20 minutes in the environment of room temperature 30 ° of C, solvent remaining in removing superimposed layer.Formed
form structure, wherein n=1, obtain described flexible electrode.
5. the flexible electrode thickness obtained is 115nm, and its light transmittance is 84%, corresponding film resistor 9 (± 5) Ω/.
Embodiment 5
1. Merlon (PC) transparent flexible substrate outer protective film is removed;
2. nano silver wire is in ethanol dispersed, obtain the nano silver wire solution that concentration is 10mg/ml, take spraying method to prepare nano silver wire film in the flexible substrate of step 1. gained, nano silver wire film thickness is at 5nm;
3. the graphene film that CVD grows is transferred on nano silver wire film, nano silver wire film superposes graphene film;
4. again take spraying method on superimposed layer, adhere to nano silver wire film, nano silver wire film thickness is 5nm;
5. placed 10 minutes in the environment of 120 ° of C by superposition film, solvent remaining in removing superimposed layer, is formed
form structure, wherein n=1, obtain described flexible electrode;
6. the flexible electrode thickness obtained is 12nm, and its light transmittance is 83%, corresponding film resistor 8 (± 5) Ω/.
Embodiment 6
1. PETG (PET) transparent flexible substrate outer protective film is removed;
2. the graphene film that CVD grows is transferred on nano silver wire film, graphene film is transferred on clean pet polymer film;
3. nano silver wire is in ethanol dispersed, obtain the nano silver wire solution that concentration is 1mg/ml, graphene film uses the mode of spraying superpose nano silver wire film.The thickness of nano silver wire film is 90nm;
4. again will that CVD grows or prepared by chemical oxidization method graphene film be adopted to transfer on nano silver wire film;
5. placed 12 minutes in the environment of 50 ° by superposition film, solvent remaining in removing superimposed layer, is formed
form structure, wherein n=1, obtain described flexible electrode;
6. the flexible electrode thickness obtained is 95nm, and its light transmittance is 83%, corresponding film resistor 8 (± 5) Ω/.
Embodiment 7
1. PETG (PET) transparent flexible substrate outer protective film is removed;
2. nano silver wire is in ethanol dispersed, obtain the nano silver wire solution that concentration is 5mg/ml, take spraying method to prepare nano silver wire film in the flexible substrate of step 1. gained, nano silver wire film thickness is 50nm;
3. the graphene film that CVD grows is transferred on nano silver wire film, nano silver wire film superposes graphene film;
4. again take spraying method on superimposed layer, adhere to nano silver wire film, nano silver wire film thickness is 50nm;
5. again by adopting that CVD grows or prepared by chemical oxidization method graphene film to transfer on superposition film, again graphene film is superposed;
6. placed 15 minutes in the environment of 50 ° by superposition film, solvent remaining in removing superimposed layer, is formed
form structure, wherein n=8, obtain described flexible electrode;
7. the flexible electrode thickness obtained is 102nm, and its light transmittance is 78%, corresponding film resistor 6 (± 5) Ω/.
Comparative example 1
1. PETG (PET) transparent flexible substrate outer protective film is removed;
2. be transferred on PET by the Graphene that CVD grows, the thickness of graphene film is 10nm, and light transmittance is 90 ~ 96%, and film resistor is at 400 ~ 1200 Ω/.
Comparative example 2
1. PETG (PET) transparent flexible substrate outer protective film is removed;
2. nano silver wire is in ethanol dispersed, obtain the nano silver wire solution that concentration is 6mg/ml, take spraying method to prepare nano silver wire film on the polymeric substrates of cleaning, nano silver wire film thickness is 20nm;
3. the flexible electrical obtained extremely light transmittance is 83%, corresponding film resistor 40 Ω/.
Comparative example 3
According to Nano Lett.2012,12,5679-5683 report, nano silver wire is dispersed on Graphene, its modify after Graphene when 90% light transmittance its film resistor at 24 (± 3.6) Ω/.But its Graphene branch mode used needs high temperature (350 ° of C), cannot be applied on polymer flexibility film.
Comparative example 4
With reference to (number of patent application: 201110096775.X, 201110096846.6,201110096782.X, 201110096791.9) graphite oxide and nano silver wire mixing, then be spin-coated on PE, obtain the light transmittance of film near 75%, film resistor 30 Ω/.
Claims (7)
1. a flexible transparent electrode, is characterized in that: flexible transparent electrode comprises the lamination of transparent polymer substrate and the nano silver wire film adhered on a transparent substrate and graphene film;
The structure of the lamination of described nano silver wire film and graphene film is
or
wherein, Ag is expressed as nano silver wire film, and G is expressed as graphene film, and n is expressed as the number of plies, and its value is 1-10;
Being prepared as of described nano silver wire film: nano silver wire is dispersed in ethanol, isopropyl alcohol or nitrogen dimethylformamide solvent, nano silver wire solution, nano silver wire solution is taked be coated with, self assembly, inkjet printing or screen printing mode prepares nano silver wire film;
Described nano silver wire solution concentration is 0.01-10mg/ml.
2. flexible transparent electrode as claimed in claim 1, is characterized in that: the thickness of described every layer of nano silver wire film is 5-300nm.
3. flexible transparent electrode as claimed in claim 1 or 2, is characterized in that: the thickness of described every layer graphene film is 0.2-20nm.
4. flexible transparent electrode as claimed in claim 1 or 2, is characterized in that: the laminated thickness of described nano silver wire film and graphene film is 5-320nm.
5. flexible transparent electrode as claimed in claim 1 or 2, is characterized in that: described graphene film is prepared by chemical vapour deposition (CVD) or reduced by graphene oxide and prepares.
6. flexible transparent electrode as claimed in claim 1 or 2, is characterized in that: described nano silver wire film is for preparing by spin coating, self assembly, inkjet printing or method for printing screen.
7. flexible transparent electrode as claimed in claim 1 or 2, is characterized in that: transparent polymer substrate is dimethyl silicone polymer substrate, polymethyl methacrylate substrate or polycarbonate substrate.
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