CN110739097A - Preparation method of silver nanowire composite transparent conductive film with adjustable work function - Google Patents
Preparation method of silver nanowire composite transparent conductive film with adjustable work function Download PDFInfo
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- H01B5/00—Non-insulated conductors or conductive bodies characterised by their form
- H01B5/14—Non-insulated conductors or conductive bodies characterised by their form comprising conductive layers or films on insulating-supports
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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 preparation method of silver nanowire composite transparent conductive films with adjustable work functions, which comprises the following steps of cleaning and hydrophilizing a transparent conductive film substrate, coating silver nanowire dispersion liquid on the hydrophilized substrate, drying to obtain silver nanowire transparent conductive films, coating precursor solution on the silver nanowire transparent conductive films, drying to obtain silver nanowire composite transparent conductive films, and finally carrying out heat treatment to obtain the silver nanowire composite transparent conductive films with adjustable work functions.
Description
Technical Field
The invention relates to a preparation method of transparent conductive films, in particular to a preparation method of silver nanowire composite transparent conductive films with adjustable work functions.
Background
The silver nanowire transparent conductive film has good photoelectric property and excellent flexibility, and is expected to replace ITO glass widely applied to to be applied to the flexible OLED device.
The work function of the ITO glass is about 4.8eV, and can reach 5.5 eV. after plasma treatment, while the work function of the silver nanowire is only about 4.2eV, which is far lower than that of the ITO glass, a larger potential barrier exists between the ITO glass and an upper layer material in a top-emitting OLED device, which is not beneficial to hole injection and finally reduces the performance and stability of the OLED device.
Disclosure of Invention
The invention aims to provide a preparation method of silver nanowire composite transparent conductive films with adjustable work functions.
In order to solve the technical problems, the invention provides a preparation method of silver nanowire composite transparent conductive films with adjustable work functions, which comprises the following steps:
1) and cleaning the transparent conductive film substrate:
cleaning and drying the substrate to obtain a cleaned substrate;
2) hydrophilization treatment of transparent conductive film substrate
Carrying out U treatment on the cleaned substrate obtained in the step 1)V-O3Processing; obtaining a substrate after hydrophilic treatment;
3) and preparing the silver nanowire transparent conductive film:
coating the silver nanowire dispersion liquid with the concentration of 0.5-7 mg/mL on the substrate obtained in the step 2) after hydrophilic treatment, and drying to obtain a silver nanowire transparent conductive film with the thickness of 50-500 nm;
note that the substrate proceeds with the subsequent step 4) along with the silver nanowire transparent conductive film ;
4) and preparing the silver nanowire composite transparent conductive film:
coating a precursor solution (precursor solution with different work functions) for compounding with the silver nanowires on the silver nanowire transparent conductive film obtained in the step 3), and drying to obtain a silver nanowire composite transparent conductive film with the thickness of 60-600 nm;
note that the subsequent step 5) is performed on the substrate together with the silver nanowire composite transparent conductive film );
5) and heat treatment of the silver nanowire composite transparent conductive film:
and (3) treating the substance (the silver nanowire composite transparent conductive film and the substrate) obtained in the step (4) in an oven at the temperature of (100 +/-10) DEG for 15 +/-3 min to obtain the silver nanowire composite transparent conductive film with the adjustable work function.
The improvement of the preparation method of the silver nanowire composite transparent conductive film with adjustable work function of the invention is as follows:
in the step 4), any of chloroauric acid, chloroplatinic acid, ammonium molybdate, sodium molybdate, organic zinc salt, inorganic zinc salt and inorganic tin salt are used as precursors, and the precursors are dissolved in a solvent II to form a precursor solution, wherein the concentration of the precursors in the precursor solution is 20-100 mg/100 ml.
The preparation method of the silver nanowire composite transparent conductive film with adjustable work function is further improved by steps:
the organic zinc salt is zinc acetate, the inorganic zinc salt is zinc chloride, and the inorganic tin salt comprises stannic chloride;
the solvent II is at least of deionized water, ethanol, methanol, isopropanol and acetone.
The preparation method of the silver nanowire composite transparent conductive film with the adjustable work function is further improved by , wherein the silver nanowire dispersion liquid in the step 3) is obtained by dispersing silver nanowires in the solvent I, and the silver nanowires are 20-30 microns in length and 25-30 nm in diameter.
The preparation method of the silver nanowire composite transparent conductive film with the adjustable work function is further improved by , wherein the solvent I is at least of deionized water, ethanol, methanol, isopropanol, acetone, ethylene glycol and polyethylene glycol.
The preparation method of the silver nanowire composite transparent conductive film with the adjustable work function is further improved by , wherein the coating mode in the step 3) is spin coating, spray coating, blade coating or dipping-pulling method.
The preparation method of the silver nanowire composite transparent conductive film with the adjustable work function is further improved by , wherein the substrate is a glass substrate, a PET (polyethylene terephthalate) substrate, cloth, paper, a PVA (polyvinyl acetate) film, a PU (polyurethane) film or a PDMS film.
The thickness of the substrate is 25-500 mu m, and the difference influence on the performance of the final product cannot be generated in the thickness.
The preparation method of the silver nanowire composite transparent conductive film with the adjustable work function is further improved by , and the step 1) is that the substrate is respectively cleaned in deionized water, ethanol and acetone for 10-20 min by ultrasonic waves, and then dried to obtain the cleaned substrate.
The preparation method of the silver nanowire composite transparent conductive film with the adjustable work function is further improved by , wherein in the step 2), the substrate after cleaning treatment obtained in the step 1) is placed in a UV-O3 cleaning machine and treated for 15min under the power of 300W, so that the substrate after hydrophilic treatment is obtained.
The preparation method of the silver nanowire composite transparent conductive film with adjustable work function is further improved by steps:
in the step 3), 3mg/mL of silver nanowire-ethanol dispersion is adopted, and the thickness of the obtained silver nanowire transparent conductive film is (75 +/-5) nm;
in the step 4), 80mg/mL of ammonium molybdate aqueous solution is adopted, and the thickness of the obtained silver nanowire composite transparent conductive film is (90 +/-10) nm;
finally, the silver nanowire-molybdenum oxide transparent conductive film is obtained.
In the present invention:
the chloroauric acid and the chloroplatinic acid are decomposed into metals in the step 5), wherein the metals are gold and platinum;
ammonium molybdate, sodium molybdate, organic zinc salt, inorganic zinc salt and inorganic tin salt are decomposed and reacted in the step 5) to generate oxides; the oxide is molybdenum oxide, tin oxide or zinc oxide.
The invention improves the silver nanowire transparent conductive film, and particularly realizes the adjustment of work function through compounding.
The invention has the following technical advantages:
1. the invention realizes the adjustment of the work function of the silver nanowire transparent conductive film, realizes the increase or decrease of the work function of the silver nanowire transparent conductive film by adjusting different composite materials, can improve the energy level matching between the silver nanowire and each functional layer, is beneficial to reducing potential barrier and improving the performance of an OLED device.
Description of the drawings: the invention takes chloroauric acid, chloroplatinic acid, ammonium molybdate, sodium molybdate, organic zinc salt, inorganic zinc salt and inorganic tin salt as precursors, and takes composite material as metal or oxide generated by decomposing the precursors through heat treatment.
2. The invention adopts the full solution method to prepare the silver nanowire transparent conductive film and realizes the compounding, does not need vacuum equipment, has simple and reliable method and high repeatability, and is suitable for large-size production.
Detailed Description
The invention is further described with reference to specific examples, but the scope of the invention is not limited thereto.
In the following cases:
the silver nanowires are 20-30 mu m in length and 25-30 nm in diameter; the thickness of the substrate is 25 to 500 μm.
Embodiments 1 and methods for preparing a silver nanowire composite transparent conductive film with adjustable work function sequentially include the following steps:
1) and cleaning the transparent conductive film substrate:
respectively ultrasonically cleaning a glass substrate in deionized water, ethanol and acetone (with the power of 500W) for 15min, and drying at 50 ℃ to constant weight;
the size of the glass substrate in this embodiment is 30 × 30 mm.
2) Hydrophilizing the transparent conductive film substrate:
putting the substrate subjected to the cleaning treatment in the step 1) into a UV-O3 cleaning machine, and placing the substrate into a UV-O machine under the power of 300W3And cleaning for 15min to obtain the substrate after hydrophilic treatment.
3) And preparing the silver nanowire transparent conductive film:
taking 3mg of silver nanowire, diluting to 1mL with ethanol, stirring at 100rpm for 10min, and obtaining 3mg/mL of silver nanowire-ethanol dispersion.
And (3) taking 1mL of silver nanowire-ethanol dispersion liquid to spin-coat on the substrate subjected to the hydrophilization treatment obtained in the step 2), wherein the spin-coating speed is 3500r/min, and the spin-coating time is 60 s. Then naturally airing in the air (to constant weight) to obtain the silver nanowire transparent conductive film;
the thickness of the silver nanowire transparent conductive film is about 75 nm.
4) And preparing the silver nanowire composite transparent conductive film:
and (3) spin-coating 2mL of 80mg/mL ammonium molybdate aqueous solution on the silver nanowire transparent conductive film obtained in the step 3), wherein the spin-coating speed is 5000r/min, and the spin-coating time is 60 s. Then naturally airing in the air (to constant weight) to obtain the silver nanowire composite transparent conductive film; the thickness of the silver nanowire composite transparent conductive film is about 90 nm.
5) And heat treatment of the silver nanowire composite transparent conductive film:
and (3) treating the product obtained in the step (4) (the silver nanowire composite transparent conductive film and the substrate) in an oven at 100 ℃ for 15min to finally obtain the silver nanowire-molybdenum oxide transparent conductive film.
The work function was 5.1eV, the sheet resistance was 24. omega./sq, and the transmittance at 550nm was 86%.
Note: the work function is tested by adopting an ultraviolet electron spectrum, the square resistance is tested by adopting an RTS-9 type double-electric-test four-probe tester, and the transmittance is tested by adopting an ultraviolet-visible spectrophotometer.
Embodiment 2, preparation methods of silver nanowire composite transparent conductive film with adjustable work function, sequentially performing the following steps:
1) and cleaning the transparent conductive film substrate:
respectively ultrasonically cleaning the PU substrate in deionized water, ethanol and acetone for 15min, and drying at 40 ℃ to constant weight;
the dimensions of the PU substrate in this example were 10X 50 cm.
2) Hydrophilization treatment of transparent conductive film substrate
Putting the substrate subjected to the cleaning treatment in the step 1) into a UV-O3 cleaning machine, and placing the substrate into a UV-O machine under the power of 300W3Cleaning for 15 min; obtaining the substrate after hydrophilic treatment.
3) And preparing the silver nanowire transparent conductive film:
taking 2mg of silver nanowire, diluting the silver nanowire to 1mL with methanol, and stirring the silver nanowire and the methanol at 100rpm for 10min to obtain 2mg/mL of silver nanowire-methanol dispersion liquid.
And (3) taking 10mL of 2mg/mL silver nanowire-methanol dispersion solution to perform blade coating on the substrate subjected to hydrophilization treatment obtained in the step 2), wherein the blade coating speed is 30mm/s, and the blade coating height is 100 micrometers. Then naturally airing in the air (to constant weight) to obtain the silver nanowire transparent conductive film; the thickness of the silver nanowire transparent conductive film is about 200 nm.
4) And preparing the silver nanowire composite transparent conductive film:
6mL of 60mg/mL chloroauric acid aqueous solution was sprayed on the silver nanowire transparent conductive film obtained in the step 3), the spraying height was 15cm, and the spraying time was 20 s. Then naturally airing in the air (to constant weight) to obtain the silver nanowire composite transparent conductive film; the thickness of the silver nanowire composite transparent conductive film is about 280 nm.
5) And heat treatment of the silver nanowire composite transparent conductive film:
and (3) treating the product obtained in the step (4) (the silver nanowire composite transparent conductive film and the substrate) in an oven at 100 ℃ for 15min to finally obtain the silver nanowire-gold composite transparent conductive film.
The work function was 4.8eV, the sheet resistance was 13. omega./sq, and the transmittance at 550nm was 82%.
Embodiment 3, preparation methods of silver nanowire composite transparent conductive film with adjustable work function, sequentially performing the following steps:
1) and cleaning the transparent conductive film substrate:
respectively ultrasonically cleaning a PET substrate in deionized water, ethanol and acetone for 15min, and drying at 40 ℃ to constant weight;
the dimensions of the PET substrate in this example were 30X 45 cm.
2) Hydrophilization treatment of transparent conductive film substrate
Putting the substrate subjected to the cleaning treatment in the step 1) into a UV-O3 cleaning machine, and placing the substrate into a UV-O machine under the power of 300W3Cleaning for 15 min; obtaining the substrate after hydrophilic treatment.
3) And preparing the silver nanowire transparent conductive film:
taking 0.5mg of silver nanowire, diluting to 1mL with isopropanol, stirring at 100rpm for 10min, and obtaining 0.5mg/mL of silver nanowire-isopropanol dispersion liquid.
Immersing the PET substrate obtained in the step 2) after the hydrophilization treatment into 2000mL of 0.5mg/mL silver nanowire-isopropanol dispersion liquid, and extracting after immersing for 10s, wherein the pulling speed is 20 mm/s. Then naturally airing in the air (to constant weight) to obtain the silver nanowire transparent conductive film;
the thickness of the silver nanowire transparent conductive film is about 450 nm.
4) And preparing the silver nanowire composite transparent conductive film:
dissolving zinc acetate and urea in a mixed solution of deionized water and ethanol in a mass ratio of 1:1, wherein the final concentration of the zinc acetate is 20mg/mL, and the final concentration of the urea is 15mg/mL, and preparing the zinc precursor solution.
5mL of zinc precursor solution is coated on the silver nanowire transparent conductive film obtained in the step 3) in a scraping way, the scraping speed is 50mm/s, the scraping height is 10 micrometers, and then the silver nanowire transparent conductive film is naturally dried in the air (to constant weight) to obtain the silver nanowire composite transparent conductive film, wherein the thickness of the silver nanowire composite transparent conductive film is about 540 nm;
5) and heat treatment of the silver nanowire composite transparent conductive film:
and (3) treating the product obtained in the step (4) (the silver nanowire composite transparent conductive film and the substrate) in an oven at 100 ℃ for 15min to finally obtain the silver nanowire-zinc oxide composite transparent conductive film.
The work function was 3.2eV, the sheet resistance was 6. omega./sq, and the transmittance at 550nm was 77%.
Comparative example 1-1, the volume of the "80 mg/mL ammonium molybdate aqueous solution" in step 4) of example 1 was changed to 2mL instead of deionized water; otherwise, the same procedure as in example 1 was repeated.
The work function of the finally obtained conductive film is 4.2eV, the square resistance is 25 omega/sq, and the transmittance at 550nm is 86%.
In the case, the work function is not changed, and when the top-emitting OLED device is used as a transparent anode, a potential barrier exists between the top-emitting OLED device and a high polymer material, so that the performance of the OLED device is influenced.
Comparative example 1-2, the "80 mg/mL ammonium molybdate aqueous solution" in step 4) of example 1 was changed to "15 mg/mL ammonium molybdate aqueous solution", and the volume amount remained unchanged and was 2 mL; the rest is equivalent to embodiment 1.
The work function of the finally obtained conductive film is 4.2eV, the square resistance is 25 omega/sq, and the transmittance at 550nm is 86%.
In this case, the content of molybdenum oxide was too small to form a uniform silver nanowire-molybdenum oxide composite film, and the work function was not changed.
Comparative examples 1 to 3, the "80 mg/mL ammonium molybdate aqueous solution" in step 4) of example 1 was changed to "160 mg/mL ammonium molybdate aqueous solution", and the volume amount remained unchanged and was 2 mL; the rest was equivalent to example 1.
The work function of the finally obtained film is 5.5eV, the square resistance is more than 1000 omega/sq, and the transmittance at 550nm is 53 percent.
The film obtained in this case had poor photoelectric properties and could not be used for a transparent anode.
Comparative example 2, the final concentration of zinc acetate of step 4) of example 3 was changed to 20mg/mL of sodium acetate, and the volume amount remained unchanged and remained 5 mL; the rest is equivalent to example 3.
The final result is: the uniform silver nanowire composite film cannot be formed, the photoelectric property is too poor, the silver nanowire composite film cannot be used, and the work function cannot be tested.
Finally, it is also noted that the above-mentioned lists merely illustrate a few specific embodiments of the invention. It is obvious that the invention is not limited to the above embodiments, but that many variations are possible. All modifications which can be derived or suggested by a person skilled in the art from the disclosure of the present invention are to be considered within the scope of the invention.
Claims (10)
1. The preparation method of the silver nanowire composite transparent conductive film with adjustable work function is characterized by comprising the following steps:
1) and cleaning the transparent conductive film substrate:
cleaning and drying the substrate to obtain a cleaned substrate;
2) hydrophilization treatment of transparent conductive film substrate
Carrying out UV-O on the substrate subjected to the cleaning treatment obtained in the step 1)3Processing; obtaining a substrate after hydrophilic treatment;
3) and preparing the silver nanowire transparent conductive film:
coating the silver nanowire dispersion liquid with the concentration of 0.5-7 mg/mL on the substrate obtained in the step 2) after hydrophilic treatment, and drying to obtain a silver nanowire transparent conductive film with the thickness of 50-500 nm;
4) and preparing the silver nanowire composite transparent conductive film:
coating the precursor solution for compounding with the silver nanowires on the silver nanowire transparent conductive film obtained in the step 3), and drying to obtain a silver nanowire composite transparent conductive film with the thickness of 60-600 nm;
5) and heat treatment of the silver nanowire composite transparent conductive film:
and (3) treating the substance obtained in the step (4) at the temperature of (100 +/-10) DEG for 15 +/-3) min to obtain the silver nanowire composite transparent conductive film with adjustable work function.
2. The method for preparing the silver nanowire composite transparent conductive film with the adjustable work function, which is characterized by comprising the following steps of:
in the step 4), of chloroauric acid, chloroplatinic acid, ammonium molybdate, sodium molybdate, organic zinc salt, inorganic zinc salt and inorganic tin salt are used as precursors, and the precursors are dissolved in a solvent II to form a precursor solution, wherein the concentration of the precursors in the precursor solution is 20-100 mg/100 ml.
3. The method for preparing the silver nanowire composite transparent conductive film with the adjustable work function, which is characterized by comprising the following steps of:
the organic zinc salt is zinc acetate, the inorganic zinc salt is zinc chloride, and the inorganic tin salt comprises stannic chloride;
the solvent II is at least of deionized water, ethanol, methanol, isopropanol and acetone.
4. The preparation method of the silver nanowire composite transparent conductive film with the adjustable work function as claimed in claims 1-3, which is characterized by comprising the following steps: the silver nanowire dispersion liquid in the step 3) is obtained by dispersing silver nanowires in a solvent I; the silver nanowires have a length of 20-30 μm and a diameter of 25-30 nm.
5. The method for preparing the silver nanowire composite transparent conductive film with the adjustable work function as claimed in claim 4, wherein the solvent I is at least of deionized water, ethanol, methanol, isopropanol, acetone, ethylene glycol and polyethylene glycol.
6. The method for preparing the silver nanowire composite transparent conductive film with the adjustable work function as claimed in claim 4 or 5, which is characterized in that: the coating mode in the step 3) is as follows: spin coating, spray coating, blade coating or dip-draw methods.
7. The method for preparing the silver nanowire composite transparent conductive film with the adjustable work function, which is characterized by comprising the following steps of:
the substrate is a glass substrate, a PET substrate, cloth, paper, a PVA film, a PU film or a PDMS film.
8. The method for preparing the silver nanowire composite transparent conductive film with the adjustable work function, which is characterized by comprising the following steps of: the step 1) is as follows: and respectively ultrasonically cleaning the substrate in deionized water, ethanol and acetone for 10-20 min, and drying to obtain the cleaned substrate.
9. The method for preparing the silver nanowire composite transparent conductive film with the adjustable work function, which is characterized by comprising the following steps of: in the step 2), the substrate after cleaning treatment obtained in the step 1) is placed in a UV-O3 cleaning machine for treatment time of 15min under the power of 300W, so as to obtain the substrate after hydrophilization treatment.
10. The method for preparing the silver nanowire composite transparent conductive film with the adjustable work function, which is characterized by comprising the following steps of:
in the step 3), 3mg/mL of silver nanowire-ethanol dispersion is adopted, and the thickness of the obtained silver nanowire transparent conductive film is (75 +/-5) nm;
in the step 4), 80mg/mL ammonium molybdate aqueous solution is adopted, and the thickness of the obtained silver nanowire composite transparent conductive film is (90 +/-10) nm.
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