WO2020233315A1 - 超低雾度银纳米线薄膜的导电墨水及其制备方法和应用 - Google Patents
超低雾度银纳米线薄膜的导电墨水及其制备方法和应用 Download PDFInfo
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- WO2020233315A1 WO2020233315A1 PCT/CN2020/085833 CN2020085833W WO2020233315A1 WO 2020233315 A1 WO2020233315 A1 WO 2020233315A1 CN 2020085833 W CN2020085833 W CN 2020085833W WO 2020233315 A1 WO2020233315 A1 WO 2020233315A1
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D11/00—Inks
- C09D11/02—Printing inks
- C09D11/03—Printing inks characterised by features other than the chemical nature of the binder
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D11/00—Inks
- C09D11/52—Electrically conductive inks
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- the invention belongs to the technical field of conductive inks for metal nanowires, and particularly relates to a conductive ink for ultra-low haze silver nanowire films, and a preparation method and application thereof.
- ITO indium tin oxide
- the two major performance indicators of transparent conductive films that are the most concerned for high-definition screens are transmittance and haze, which are closely related to the size of the silver nanowires used in the film. Therefore, ultra-fine, ultra-high aspect ratio silver nanometers are prepared
- the line is the key. With excellent silver nanowires, it is necessary to ensure that they are randomly and uniformly distributed in the film to reduce light scattering and obtain satisfactory optical indicators, which is directly related to the performance of the ink used for film formation. Therefore, the conductive ink with stable preparation performance and one-time film formation meeting the requirements is the key to the success or failure of high-definition screen applications.
- the present invention provides a conductive ink with ultra-low haze silver nanowire film and a preparation method and application thereof.
- the conductive ink is prepared by a low-cost, simple and effective method, and is prepared by ultra-fine,
- the synthesis of ultra-large aspect ratio silver nanowires and the adjustment of the ink film-forming characteristics can achieve one-time film formation to meet various optical, electrical, mechanical and stability indicators required for high-definition screen films.
- each 100ml conductive ink contains the following components:
- Silver nanowire 50-1000mg
- Silver nanowire solvent 90-99ml
- Viscosity modifier 0.1-2g
- Dispersant solvent 0.1-1ml
- 50-1000 mg of silver nanowires are prepared from the following components:
- Silver nitrate 0.5-10g
- Halogen ion reagent 0.04-0.8g
- the molecular mass of the PVP is greater than 300,000.
- the halogen ion reagent includes one or more of NaCl, NaBr, FeCl 3 , tetrapropylammonium chloride, and tetrapropylammonium bromide.
- the silver nanowire solvent, silica sol solvent, dispersant solvent and leveling agent solvent are all deionized water or alcohol solvent; when the silver nanowire solvent is deionized water, the silica sol solvent and dispersant solvent
- the leveling agent solvent is also deionized water; when the silver nanowire solvent is an alcohol solvent, the silica sol solvent, dispersant solvent and leveling agent solvent are also alcoholic solvents.
- the alcohol solvent is any one or a mixture of ethanol, propanol, ethylene glycol, and glycerol.
- the viscosity modifier includes one or more of cellulose ether and its derivatives, and cellulose ether and its derivatives include hydroxyethyl cellulose, methyl hydroxyethyl cellulose, and hydroxypropyl cellulose.
- cellulose ether and its derivatives include hydroxyethyl cellulose, methyl hydroxyethyl cellulose, and hydroxypropyl cellulose.
- the dispersant includes triethylhexyl phosphoric acid, sodium lauryl sulfate, methylpentanol, cellulose derivatives, polyacrylamide, polyacrylate polymers, Guer gum, fatty acid polyethylene glycol One or more of esters.
- the leveling agent includes one or more of acrylic resin, urea-formaldehyde resin, melamine-formaldehyde resin, saturated resin, polyacrylic acid, and carboxymethyl cellulose.
- the diameter of the silica nanoparticles is 5-20 nm.
- a method for preparing conductive ink of ultra-low haze silver nanowire film includes the following steps:
- Step A1 Weigh 0.4-20g of PVP into ethylene glycol, heat it at 130°C for 2 hours until the PVP is completely dissolved, and then cool naturally to obtain a PVP ethylene glycol solution;
- Step A2 Weigh 0.5-10g AgNO 3 and add it to ethylene glycol, and in a water bath at 4-8°C, sonicate at 100 Hz for 7-9 minutes until AgNO 3 is completely dissolved to obtain an AgNO 3 ethylene glycol solution;
- Step A3 Weigh 0.04-0.8g of halide ion reagent and dissolve it in ethylene glycol to obtain a halide ion glycol solution;
- Step A4 Place the ethylene glycol in a flask, and immerse the flask in an oil bath at room temperature, and sequentially add the halide ion ethylene glycol solution obtained in Step A3 and the AgNO 3 ethylene glycol solution obtained in Step A2. , The PVP glycol solution obtained in step A1 is injected into the flask, and mechanically stirred for 10-30 minutes;
- the total amount of ethylene glycol is 132-1500ml, preferably, the amount of ethylene glycol in step A1 is 15-17ml, the amount of ethylene glycol in step A2 is 15ml, and the amount of ethylene glycol in step A3
- the amount of alcohol is 2-4ml;
- Step A5. Blow in nitrogen gas, and turn on the oil bath to heat up. After 15-20 minutes, it will reach 180°C. After reaching the temperature, stop the nitrogen flow and set the temperature to 170°C. With the aid of mechanical stirring, it will decrease to 170°C after 3-8 minutes. °C, continue to stir for 2 minutes and then stop the mechanical stirring. After the reaction is kept at 170°C for 1-1.2h, take it out and place it in cold water at 5-15°C to quench to room temperature to obtain a solution containing silver nanowires;
- Step B preparation of silver nanowire ink
- Step B1 After filtering and cleaning the solution containing silver nanowires obtained in step A5 under a positive pressure of 0.1-0.3kPa, take the filter cake and disperse it in a 5% PVP aqueous solution, shake it at room temperature for 10 minutes, and let it stand for 9 After -15h, take the supernatant, filter and clean with 0.1-0.3kPa positive pressure for 3-5 times, filter and clean 3-5 times, take the filter cake on the filter membrane and disperse it in the 5% PVP aqueous solution for use.
- the filter cake is silver nanowires;
- Step B2 Disperse 0.1-2g of viscosity modifier in 90-99ml of silver nanowire solvent, shake for 10-20h at room temperature until completely dissolved and uniformly dispersed to obtain a solution,
- Step B3 adding 50-1000 mg of the silver nanowire obtained in step B1 to the solution obtained in step B2 to obtain a silver nanowire dispersion;
- Step B4 Take 3-70mg of dispersant and place it in 0.1-1ml of dispersant solvent to obtain a dispersant solution, then add the dispersant solution to the silver nanowire dispersion obtained in step B3, and shake for 1-2h at room temperature until mixed Evenly,
- Step B5 Take 4-85mg of leveling agent and place it in 0.1-1ml of leveling agent solvent to obtain the leveling agent solution, then add the leveling agent solution to the solution obtained in step B4, and shake for 1-2h at room temperature until mixed Evenly
- Step B6 Take 0.2-8.5g of silica nanoparticles with a diameter of 5-20nm and place them in 1-8ml of silica sol solvent to obtain a silica sol solution with a concentration of 0.2-1.0625g/ml, and combine the silica sol solution with that obtained in step B5 The solution is mixed and shaken at room temperature for 2-5 hours until the mixture is uniform, and the conductive ink is obtained after uniform mixing.
- the conductive ink of the above-mentioned ultra-low haze silver nanowire film or the ultra-low haze silver nanowire film prepared by the above preparation method is applied to a high-definition screen.
- the present invention has the following beneficial effects:
- the silver nanowires needed for the ink are synthesized by the low-temperature liquid phase method, through the use of organic surfactants and inorganic selective adsorption ions, and changing the experimental temperature of different reaction stages to control the nucleation and growth process of the silver nanowires. Prepare silver nanowires that meet the size required to greatly reduce light scattering.
- silica sol a reagent to improve film stability, is specially added to the conductive ink. Because silica sol has good water solubility, it does not affect the film formation of the ink, and at the same time, it relies on the crosslinking effect of the silica sol to increase the film when the film is dried. The bonding force with the substrate and the formation of a protective layer on the surface of the film can slow down the oxidation and vulcanization of the film in use.
- Figure 1 is a distribution diagram of the diameter of silver nanowires in the conductive ink of the present invention
- FIG. 2 is a distribution diagram of the length of silver nanowires in the conductive ink of the present invention.
- Figure 3(a) is a scanning electron microscope image of the conductive ink without silica sol
- Figure 3(b) is a scanning electron microscope image of the conductive ink with silica sol added in Example 1;
- FIG. 4 is a diagram of optical index of film transmittance formed by conductive ink in the present invention.
- Fig. 5 is a diagram showing the optical index of haze of the conductive ink film in the present invention.
- Figure 6(a) is a scanning electron microscope image of the conductive ink without adding silica sol 3M tape after sticking
- Figure 6(b) is a scanning electron microscope image of the conductive ink in Example 1 after adding silica sol and sticking with 3M tape;
- Figure 7(a) is a scanning electron microscope image of the conductive ink without silica sol after being tested with a 3H pencil
- Figure 7(b) is a scanning electron microscope image of the conductive ink in Example 1 after silica sol being tested with a 3H pencil .
- Polyvinylpyrrolidone is referred to as PVP.
- a method for preparing conductive ink of ultra-low haze silver nanowire film includes the following steps:
- Step A1 Weigh 0.84g PVP (molecular mass 500,000) into a 250ml Erlenmeyer flask, put 15ml ethylene glycol solution into it, and place it on the heating plate at 130°C for 2h until the PVP is completely dissolved and then cooled naturally to obtain PVP Ethylene glycol solution
- Step A2 Weigh 0.6g AgNO 3 and add it to 15 mL of ethylene glycol. In a 4°C water bath, perform ultrasound at 100 Hz for 7 minutes until AgNO 3 is completely dissolved to obtain an AgNO 3 ethylene glycol solution;
- Step A3 Weigh 0.02g NaCl and 0.02g NaBr respectively and dissolve them in 1ml ethylene glycol to obtain two halogen ion ethylene glycol solutions;
- Step A4 Weigh 100 mL of ethylene glycol and place it in a flask, and immerse the flask in an oil bath at room temperature, and sequentially add the halide ion ethylene glycol solution obtained in Step A3 and the AgNO 3 ethylene glycol obtained in Step A2. The solution and the PVP ethylene glycol solution obtained in step A1 are injected into the flask and mechanically stirred for 10 minutes;
- Step A5. Blow in nitrogen and turn on the oil bath to heat. After 15 minutes, it will reach 180°C. After reaching the temperature, stop the nitrogen flow and set the temperature to 170°C. With the aid of mechanical stirring, it will drop to 170°C after 3 minutes, and continue to stir. Stop the mechanical stirring after 2 minutes. After the reaction is kept at 170°C for 1 hour, it is taken out and placed in cold water at 5°C to be quenched to room temperature to obtain a solution containing silver nanowires;
- Step B Preparation of silver nanowire ink
- Step B1 After filtering and cleaning the solution containing silver nanowires obtained in step A under a positive pressure of 0.1kPa, take the filter cake and disperse it in a 5% PVP aqueous solution, shake at room temperature for 10 minutes, and then stand still. 9h, take the supernatant, and then use 0.1kPa positive pressure to filter and clean 3 times, filter and clean 3 times, take the filter cake on the filter membrane and disperse it in the 5% mass fraction PVP aqueous solution for later use, the filter cake is silver nanowire;
- Step B2 Disperse 200 mg of viscosity modifier hydroxypropyl methylcellulose in 96.7 ml of silver nanowire solvent, and shake for 10 hours at room temperature until completely dissolved and uniformly dispersed to obtain a solution;
- Step B3 adding 50 mg of the silver nanowires obtained in step B1 to the solution obtained in step B2 to obtain a silver nanowire dispersion;
- Step B4 Take 6 mg of dispersant sodium lauryl sulfate and place it in 0.15 ml of dispersant solvent to obtain a dispersant solution, then add the dispersant solution to the silver nanowire dispersion obtained in step B3, and shake for 1.5 hours at room temperature To mix well;
- Step B5 Take 7.5 mg of the leveling agent urea-formaldehyde resin and place it in 0.15 ml of the leveling agent solvent to obtain the leveling agent solution, then add the leveling agent solution to the solution obtained in step B4, and shake for 1.5 hours at room temperature until the mixture is uniform ;
- Step B6 Take 0.75g of silica nanoparticles with a diameter of 5nm in 3ml of silica sol solvent to obtain a silica sol solution with a concentration of 0.25g/ml, mix the silica sol solution with the solution obtained in step B5, and shake at room temperature 3h until the mixture is uniform, and the conductive ink is obtained after uniform mixing.
- the silver nanowire solvent, silica sol solvent, dispersant solvent and leveling agent solvent are all deionized water.
- a method for preparing conductive ink of ultra-low haze silver nanowire film includes the following steps:
- Step A1 Weigh 0.4g of PVP (molecular weight 360,000) into 15ml of ethylene glycol solution, and place it on a heating plate at 130°C for 2 hours until the PVP is completely dissolved and then naturally cooled to obtain a PVP glycol solution;
- Step A2 Weigh 0.5g of AgNO 3 and add it to 15 mL of ethylene glycol, and in a 6°C water bath, ultrasound at 100 Hz for 8 minutes until the AgNO 3 is completely dissolved to obtain an AgNO 3 ethylene glycol solution;
- Step A3 Weigh 0.1g of NaCl and dissolve it in 4ml of ethylene glycol to obtain a NaCl ethylene glycol solution;
- Step A4 Weigh 100 mL of ethylene glycol and place it in a flask, and immerse the flask in an oil bath at room temperature, and sequentially combine the NaCl ethylene glycol solution obtained in Step A3 and the AgNO 3 ethylene glycol solution obtained in Step A2 , The PVP ethylene glycol solution obtained in step A1 is injected into the flask and mechanically stirred for 20 minutes;
- Step A5. Blow in nitrogen gas and turn on the oil bath to heat up. After 18 minutes, it will reach 180°C. When the temperature is reached, stop the nitrogen flow and set the temperature to 170°C. With the aid of mechanical stirring, it will drop to 170°C after 5 minutes, and continue to stir. Stop the mechanical stirring after 2 minutes, keep the reaction at 170°C for 1.1 hours, take it out and place it in cold water at 10°C to quench to room temperature to obtain a solution containing silver nanowires;
- Step B Preparation of silver nanowire ink
- Step B1 After filtering and cleaning the solution containing silver nanowires obtained in step A under a positive pressure of 0.1kPa, take the filter cake and disperse it in a 5% PVP aqueous solution. After shaking at room temperature for 10 minutes, let it stand for 12 hours. Take the supernatant, then filter and clean with 0.1kPa positive pressure for 4 times, filter and clean the filter cake on the filter membrane for 4 times and disperse it into a 5% PVP aqueous solution for use.
- the filter cake is silver nanowires;
- Step B2 Disperse 1 g of viscosity modifier hydroxyethyl cellulose in 98.8 ml of silver nanowire solvent, and shake for 15 hours at room temperature until completely dissolved and uniformly dispersed to obtain a solution;
- Step B3 adding 80 mg of the silver nanowire obtained in step B1 to the solution obtained in step B2 to obtain a silver nanowire dispersion;
- Step B4 Take 3 mg of dispersant triethylhexyl phosphoric acid and place it in 0.1 ml of dispersant solvent to obtain a dispersant solution, then add the dispersant solution to the silver nanowire dispersion obtained in step B3, and shake for 1 hour at room temperature until mixed Evenly
- Step B5 Take 4 mg of the leveling agent acrylic resin and place it in 0.1 ml of the leveling agent solvent to obtain the leveling agent solution, then add the leveling agent solution to the solution obtained in step B4, and shake at room temperature for 1 hour until the mixture is uniform;
- Step B6 Take 0.2g of silica nanoparticles with a diameter of 15nm and place them in 1ml of silica sol solvent to obtain a silica sol solution with a concentration of 0.2g/ml, mix the silica sol solution with the solution obtained in step B5, and shake at room temperature 2h until the mixture is uniform, and the conductive ink is obtained after uniform mixing.
- the silver nanowire solvent, silica sol solvent, dispersant solvent and leveling agent solvent are all ethanol.
- a method for preparing conductive ink of ultra-low haze silver nanowire film includes the following steps:
- Step A1 Weigh 20g of PVP (molecular mass 1.3 million) into 170ml of ethylene glycol solution, and place it on a heating plate at 130°C for 2 hours until the PVP is completely dissolved and then naturally cooled to obtain a PVP glycol solution;
- Step A2 Weigh 10g of AgNO 3 and add it to 150 mL of ethylene glycol. In a water bath at 8° C., ultrasonic wave at 100 Hz for 9 min until AgNO 3 is completely dissolved to obtain an AgNO 3 ethylene glycol solution;
- Step A3 Weigh 0.8g FeCl 3 and dissolve it in 40ml ethylene glycol to obtain FeCl 3 ethylene glycol solution;
- Step A4 Weigh 1140 mL of ethylene glycol and place it in a flask, and immerse the flask in an oil bath at room temperature.
- the FeCl 3 ethylene glycol solution obtained in Step A3 and the AgNO 3 ethylene glycol solution obtained in Step A2 are sequentially added.
- the solution and the PVP ethylene glycol solution obtained in step A1 are injected into the flask and mechanically stirred for 30 minutes;
- Step A5. Blow in nitrogen gas and turn on the oil bath to heat up. After 20 minutes, it will reach 180°C. After reaching the temperature, stop the nitrogen flow and set the temperature to 170°C. With the aid of mechanical stirring, it will drop to 170°C after 8 minutes, and continue to stir. Stop the mechanical stirring after 2 minutes. After the reaction is kept at 170°C for 1.2 hours, it is taken out and placed in cold water at 15°C to be quenched to room temperature to obtain a solution containing silver nanowires;
- Step B Preparation of silver nanowire ink
- Step B1 After filtering and cleaning the silver nanowire-containing solution obtained in step A under a positive pressure of 0.3kPa, the filter cake is dispersed in a 5% PVP aqueous solution, shaken at room temperature for 10 minutes, and then left for 15 hours. Take the supernatant, filter and wash with a positive pressure of 0.3kPa for 5 times, and disperse the filter cake on the filter membrane into a 5% PVP aqueous solution for use.
- the filter cake is silver nanowires;
- Step B2 Disperse 2 g of the viscosity modifier methyl hydroxyethyl cellulose in 94.8 ml of silver nanowire solvent, and shake for 20 hours at room temperature until completely dissolved and uniformly dispersed to obtain a solution;
- Step B3 adding 1 g of the silver nanowire obtained in step B1 to the solution obtained in step B2 to obtain a silver nanowire dispersion;
- Step B4 Take 70 mg of dispersant methyl pentanol and place it in 0.2 ml of dispersant solvent to obtain a dispersant solution, then add the dispersant solution to the silver nanowire dispersion obtained in step B3, and shake for 1-2 hours at room temperature to well mixed;
- Step B5 Take 85 mg of the leveling agent melamine formaldehyde resin and place it in 1 ml of the leveling agent solvent to obtain the leveling agent solution, then add the leveling agent solution to the solution obtained in step B4, and shake at room temperature for 2 hours until the mixture is uniform;
- Step B6 Take 8.4g of silica nanoparticles with a diameter of 20nm and place them in 4ml of silica sol solvent to obtain a silica sol solution with a concentration of 2.1g/ml, mix the silica sol solution with the solution obtained in step B5, and shake at room temperature 5h until the mixture is uniform, and the conductive ink is obtained after uniform mixing.
- the silver nanowire solvent, silica sol solvent, dispersant solvent and leveling agent solvent are all propanol.
- a method for preparing conductive ink of ultra-low haze silver nanowire film includes the following steps:
- Step A1 Weigh 0.5g of PVP (molecular mass 600,000) into 17ml of ethylene glycol solution, and place it on a heating plate at 130°C for 2h until the PVP is completely dissolved and then cooled naturally to obtain a PVP ethylene glycol solution;
- Step A2 Weigh 0.5g of AgNO 3 and add it to 15 mL of ethylene glycol. In a water bath at 5° C., ultrasonic wave at 100 Hz for 8 minutes until AgNO 3 is completely dissolved to obtain an AgNO 3 ethylene glycol solution;
- Step A3 Weigh 0.04 g of halide ion reagent tetrapropylammonium chloride and dissolve it in 4 ml of ethylene glycol to obtain a halide ion glycol solution;
- Step A4 Weigh 110 mL of ethylene glycol and place it in a flask, and immerse the flask in an oil bath at room temperature, and sequentially combine the halide ion ethylene glycol solution obtained in Step A3 and the AgNO 3 ethylene glycol obtained in Step A2. The solution and the PVP ethylene glycol solution obtained in step A1 are injected into the flask and mechanically stirred for 20 minutes;
- Step A5. Blow in nitrogen gas and turn on the oil bath to heat up. After 20 minutes, it will reach 180°C. After reaching the temperature, stop the nitrogen flow and set the temperature to 170°C. With the aid of mechanical stirring, it will drop to 170°C after 3 minutes and continue to stir. Stop the mechanical stirring after 2 minutes. After the heat preservation reaction is at 170°C for 1 hour, take it out and place it in cold water at 10°C to quench to room temperature to obtain silver nanowires;
- Step B Preparation of silver nanowire ink
- Step B1 After filtering and cleaning the silver nanowires obtained in step A under a positive pressure of 0.1kPa, disperse the filter cake into a 5% PVP aqueous solution, shake it at room temperature for 10 minutes, and let it stand for 9 hours, then take the supernatant Then use 0.1kPa positive pressure filtration and cleaning for 5 times, and after filtration and cleaning for 5 times, take the filter cake on the filter membrane and disperse it into a 5% PVP aqueous solution for use.
- the filter cake is silver nanowires;
- Step B2 Disperse 2 g of viscosity modifier ethyl hydroxyethyl cellulose in 90 ml of silver nanowire solvent, and shake for 10 hours at room temperature until completely dissolved and uniformly dispersed to obtain a solution;
- Step B3 adding 80 mg of the silver nanowires obtained in step B1 to the solution obtained in step B2 to obtain a silver nanowire dispersion;
- Step B4 Take 70 mg of dispersant polyacrylamide and place it in 1 ml of dispersant solvent to obtain a dispersant solution, and then add the dispersant solution to the silver nanowire dispersion obtained in step B3, and shake at room temperature for 1 hour until the mixture is uniform;
- Step B5 Take 85 mg of the leveling agent polyacrylic acid and place it in 1 ml of the leveling agent solvent to obtain the leveling agent solution, then add the leveling agent solution to the solution obtained in step B4, and shake at room temperature for 1 hour until the mixture is uniform;
- Step B6 Take 8.5 g of silica nanoparticles with a diameter of 10 nm and place them in 8 ml of silica sol solvent to obtain a silica sol solution with a concentration of 1.0625 g/ml, mix the silica sol solution with the solution obtained in step B5, and shake at room temperature 2h until the mixture is uniform, and the conductive ink is obtained after uniform mixing.
- the silver nanowire solvent, silica sol solvent, dispersant solvent and leveling agent solvent are all ethylene glycol.
- a method for preparing conductive ink of ultra-low haze silver nanowire film includes the following steps:
- Step A1 Weigh 20g of PVP (molecular mass 1.3 million) into 16ml of ethylene glycol solution, and place it on a heating plate at 130°C for 2 hours until the PVP is completely thermally dissolved and then naturally cooled to obtain a PVP glycol solution;
- Step A2 Weigh 10g of AgNO 3 and add it to 15 mL of ethylene glycol. In a water bath at 8° C., sonicate at 100 Hz for 7 minutes until AgNO 3 is completely dissolved to obtain an AgNO 3 ethylene glycol solution;
- Step A3 Weigh 0.8g of halide ion reagent tetrapropylammonium bromide and dissolve it in 4ml of ethylene glycol to obtain a halide ion glycol solution;
- Step A4 Weigh 1200 mL of ethylene glycol and place it in a flask, and immerse the flask in an oil bath at room temperature, and sequentially combine the halide ion ethylene glycol solution obtained in Step A3 and the AgNO 3 ethylene glycol obtained in Step A2. The solution and the PVP ethylene glycol solution obtained in step A1 are injected into the flask and mechanically stirred for 30 minutes;
- Step A5. Blow in nitrogen gas and turn on the oil bath to heat up. After 20 minutes, it will reach 180°C. After reaching the temperature, stop the nitrogen flow and set the temperature to 170°C. With the aid of mechanical stirring, it will drop to 170°C after 8 minutes, and continue to stir. Stop the mechanical stirring after 2 minutes, keep the reaction at 170°C for 1 hour, take it out and place it in cold water at 15°C to quench to room temperature to obtain silver nanowires;
- Step B Preparation of silver nanowire ink
- Step B1 After filtering and cleaning the silver nanowires obtained in step A once under a positive pressure of 0.2kPa, take the filter cake and disperse it in a 5% PVP aqueous solution. After shaking for 10 minutes at room temperature, let it stand for 15 hours and take the supernatant. Then use 0.2kPa positive pressure to filter and clean 3 times, filter and clean 3 times, take the filter cake on the filter membrane and disperse it into a 5% PVP aqueous solution for use.
- the filter cake is silver nanowires;
- Step B2 Disperse 2 g of the viscosity modifier methyl hydroxypropyl cellulose in 95.6 ml of silver nanowire solvent, and shake for 20 hours at room temperature until completely dissolved and uniformly dispersed to obtain a solution;
- Step B3 adding 1 g of the silver nanowire obtained in step B1 to the solution obtained in step B2 to obtain a silver nanowire dispersion;
- Step B4 Take 70 mg of dispersant Guer gum and place it in 0.2 ml of dispersant solvent to obtain a dispersant solution, then add the dispersant solution to the silver nanowire dispersion obtained in step B3, and shake for 2 hours at room temperature until the mixture is uniform;
- Step B5 Take 85 mg of the leveling agent carboxymethyl cellulose and place it in 0.2 ml of the leveling agent solvent to obtain the leveling agent solution, and then add the leveling agent solution to the solution obtained in step B4, and shake for 2 hours at room temperature until mixed Evenly
- Step B6 Take 8.4g of silica nanoparticles with a diameter of 15nm and place them in 4ml of silica sol solvent to obtain a silica sol solution with a concentration of 2.1g/ml, mix the silica sol solution with the solution obtained in step B5, and shake at room temperature 5h until the mixture is uniform, and the conductive ink is obtained after uniform mixing.
- the silver nanowire solvent, silica sol solvent, dispersant solvent and leveling agent solvent are all glycerol.
- a method for preparing conductive ink of ultra-low haze silver nanowire film includes the following steps:
- Step A1 Weigh 0.84g of PVP (molecular weight 500,000) into 15ml of ethylene glycol solution, and place it on a heating plate at 130°C for 2h until the PVP is completely dissolved and then naturally cooled to obtain a PVP ethylene glycol solution;
- Step A2 Weigh 0.6g of AgNO 3 and add it to 15 mL of ethylene glycol. In a water bath at 5° C., ultrasonic wave at 100 Hz for 8 minutes until AgNO 3 is completely dissolved to obtain an AgNO 3 ethylene glycol solution;
- Step A3 Weigh 0.05g NaCl and 0.05g NaBr and dissolve them in 2ml ethylene glycol respectively to obtain two halide ion ethylene glycol solutions;
- Step A4 Weigh 110 mL of ethylene glycol and place it in a flask, and immerse the flask in an oil bath at room temperature, and sequentially combine the halide ion ethylene glycol solution obtained in Step A3 and the AgNO 3 ethylene glycol obtained in Step A2. The solution and the PVP ethylene glycol solution obtained in step A1 are injected into the flask and mechanically stirred for 20 minutes;
- Step A5. Blow in nitrogen gas and turn on the oil bath to heat up. After 18 minutes, it will reach 180°C. When the temperature is reached, stop the nitrogen flow and set the temperature to 170°C. With the aid of mechanical stirring, it will drop to 170°C after 5 minutes, and continue to stir. Stop the mechanical stirring after 2 minutes, keep the reaction at 170°C for 1.1h, take it out and place it in cold water at 10°C to quench to room temperature to obtain silver nanowires;
- Step B Preparation of silver nanowire ink
- Step B1 After filtering and cleaning the silver nanowires obtained in step A once under a positive pressure of 0.2kPa, take the filter cake and disperse it in a 5% PVP aqueous solution, shake at room temperature for 10 minutes, and then stand for 12 hours. The supernatant was filtered and cleaned with a positive pressure of 0.2kPa for 4 times. The filter cake on the filter membrane was dispersed in a 5% PVP aqueous solution for use. The filter cake was silver nanowires;
- Step B2 Disperse 0.2 g of the viscosity modifier cellulose hydroxyalkyl ether in 96.7 ml of silver nanowire solvent, and shake for 20 hours at room temperature until it is completely dissolved and uniformly dispersed to obtain a solution;
- Step B3 adding 80 mg of the silver nanowire obtained in step B1 to the solution obtained in step B2 to obtain a silver nanowire dispersion;
- Step B4 Take 6 mg of dispersant fatty acid polyethylene glycol ester and place it in 0.15 ml of dispersant solvent to obtain a dispersant solution, and then add the dispersant solution to the silver nanowire dispersion obtained in step B3, and shake for 1.5 hours at room temperature To mix well;
- Step B5 Take 7.5 mg of the leveling agent saturated resin and place it in 0.15 ml of the leveling agent solvent to obtain the leveling agent solution, then add the leveling agent solution to the solution obtained in step B4, and shake for 1.5 hours at room temperature until the mixture is uniform ;
- Step B6 Take 0.75g of silica nanoparticles with a diameter of 5nm in 3ml of silica sol solvent to obtain a silica sol solution with a concentration of 0.25g/ml, mix the silica sol solution with the solution obtained in step B5, and shake at room temperature 3h until the mixture is uniform, and the conductive ink is obtained after uniform mixing.
- the silver nanowire solvent, silica sol solvent, dispersant solvent and leveling agent solvent are all a mixture of ethanol, propanol, ethylene glycol, and glycerol with a volume ratio of 1:1:1:1.
- a method for preparing conductive ink of ultra-low haze silver nanowire film includes the following steps:
- Step A1 Weigh 8.4g of PVP (molecular mass 360,000) into 160ml of ethylene glycol solution, and place it on a heating plate at 130°C for 2 hours until the PVP is completely dissolved and then naturally cooled to obtain a PVP glycol solution;
- Step A2 Weigh 6g of AgNO 3 and add it to 150 mL of ethylene glycol. In a 7°C water bath, ultrasonic wave at 100 Hz for 8 minutes until the AgNO 3 is completely dissolved to obtain an AgNO 3 ethylene glycol solution;
- Step A3 Weigh 0.8g of NaCl and dissolve it in 40ml of ethylene glycol to obtain a NaCl ethylene glycol solution;
- Step A4 Weigh 1100 mL of ethylene glycol and place it in a flask, and immerse the flask in an oil bath at room temperature, and sequentially add the NaCl ethylene glycol solution obtained in step A3 and the AgNO 3 ethylene glycol solution obtained in step A2 , The PVP ethylene glycol solution obtained in step A1 is injected into the flask and mechanically stirred for 20 minutes;
- Step A5. Blow in nitrogen gas and turn on the oil bath to heat up. After 18 minutes, it will reach 180°C. When the temperature is reached, stop the nitrogen flow and set the temperature to 170°C. With the aid of mechanical stirring, it will drop to 170°C after 5 minutes, and continue to stir. Stop the mechanical stirring after 2 minutes. After the reaction is kept at 170°C for 1 hour, it is taken out and quenched to room temperature in cold water at 10°C to obtain silver nanowires;
- Step B Preparation of silver nanowire ink
- Step B1 After filtering and cleaning the silver nanowires obtained in step A once under a positive pressure of 0.2kPa, take the filter cake and disperse it in a 5% mass fraction PVP aqueous solution, shake it at room temperature for 10 minutes, then let it stand for 12 hours, and take the supernatant Then use 0.2kPa positive pressure to filter and clean for 5 times. Take the filter cake on the filter membrane and disperse it into a 5% PVP aqueous solution for use.
- the filter cake is silver nanowires;
- Step B2 Disperse 2g of viscosity modifier (1g hydroxyethyl cellulose, 0.5g methyl hydroxyethyl cellulose and 0.5g hydroxypropyl methyl cellulose) in 96.7ml silver nanowire solvent and shake for 15h at room temperature , To completely dissolve and disperse uniformly to obtain a solution;
- Step B3 adding 1 g of the silver nanowire obtained in step B1 to the solution obtained in step B2 to obtain a silver nanowire dispersion;
- Step B4 Take 70mg of dispersant (35mg of cellulose derivative and 35mg of polyacrylate polymer) into 0.2ml of dispersant solvent to obtain a dispersant solution, and then add the dispersant solution to the silver nanowire dispersion obtained in step B3 In the solution, shake at room temperature for 1 hour to mix well;
- Step B5 Take 85 mg of leveling agent (35 mg of acrylic resin and 50 mg of saturated resin) and place it in 0.1 ml of leveling agent solvent to obtain a leveling agent solution, and then add the leveling agent solution to the solution obtained in step B4, at room temperature Shake for 1 hour to mix well;
- Step B6 Take 8.4g of silica nanoparticles with a diameter of 15nm and place them in 3ml of silica sol solvent to obtain a silica sol solution with a concentration of 2.8g/ml, mix the silica sol solution with the solution obtained in step B5, and shake at room temperature 3h until the mixture is uniform, and the conductive ink is obtained after uniform mixing.
- the silver nanowire solvent, silica sol solvent, dispersant solvent and leveling agent solvent are all a mixture of ethanol and propanol with a volume ratio of 1:1.
- a method for preparing conductive ink of ultra-low haze silver nanowire film includes the following steps:
- Step A1 Weigh 0.4g of PVP (molecular mass 360,000) into 16ml of ethylene glycol solution, and place it on a heating plate at 130°C for 2 hours until the PVP is completely dissolved and then cooled naturally to obtain a PVP glycol solution;
- Step A2 Weigh 0.5g of AgNO 3 and add it to 15 mL of ethylene glycol, and in a 6°C water bath, ultrasound at 100 Hz for 8 minutes until the AgNO 3 is completely dissolved to obtain an AgNO 3 ethylene glycol solution;
- Step A3 Weigh 0.1g NaCl and 0.3g NaBr and dissolve them in 2ml ethylene glycol, respectively, to obtain two halide ion ethylene glycol solutions;
- Step A4 Weigh 100 mL of ethylene glycol and place it in a flask, and immerse the flask in an oil bath at room temperature, and sequentially add the halide ion ethylene glycol solution obtained in Step A3 and the AgNO 3 ethylene glycol obtained in Step A2. The solution and the PVP ethylene glycol solution obtained in step A1 are injected into the flask and mechanically stirred for 10 minutes;
- Step A5. Blow in nitrogen and turn on the oil bath to heat. After 15 minutes, it will reach 180°C. After reaching the temperature, stop the nitrogen flow and set the temperature to 170°C. With the aid of mechanical stirring, it will drop to 170°C after 3 minutes, and continue to stir. Stop the mechanical stirring after 2 minutes. After the reaction is kept at 170°C for 1 hour, it is taken out and quenched to room temperature in cold water at 5°C to obtain silver nanowires;
- Step B Preparation of silver nanowire ink
- Step B1 After filtering and cleaning the silver nanowires obtained in step A once under a positive pressure of 0.1kPa, take the filter cake and disperse it in a 5% PVP aqueous solution, shake at room temperature for 10 minutes, and then stand for 9 hours. The supernatant is filtered and cleaned with a positive pressure of 0.1kPa for 3 times, and the filter cake on the filter membrane is dispersed into a 5% PVP aqueous solution for use.
- the filter cake is silver nanowires;
- Step B2 Disperse 0.3g of viscosity modifier (0.2g hydroxyethyl cellulose, 0.05g methyl hydroxyethyl cellulose, 0.05g hydroxypropyl methyl cellulose) in 95.6ml silver nanowire solvent at room temperature Shake for 15 hours until it is completely dissolved and evenly dispersed to obtain a solution;
- Step B3 adding 80 mg of the silver nanowire obtained in step B1 to the solution obtained in step B2 to obtain a silver nanowire dispersion;
- Step B4 Take 10mg of dispersant (3mg of triethylhexyl phosphoric acid, 3mg of sodium lauryl sulfate, 2mg of methylpentanol, 2mg of polyacrylamide) in 0.2ml of dispersant solvent to obtain a dispersant solution, and then disperse Add the reagent solution to the silver nanowire dispersion obtained in step B3, and shake for 2 hours at room temperature until the mixture is uniform;
- dispersant 3mg of triethylhexyl phosphoric acid, 3mg of sodium lauryl sulfate, 2mg of methylpentanol, 2mg of polyacrylamide
- Step B5. Take 12mg of leveling agent (3mg acrylic resin, 3mg urea-formaldehyde resin, 2mg melamine formaldehyde resin, 2mg polyacrylic acid, 2mg carboxymethyl cellulose) into 0.2ml leveling agent solvent to obtain leveling agent solution, and then The leveling agent solution is added to the solution obtained in step B4;
- leveling agent 3mg acrylic resin, 3mg urea-formaldehyde resin, 2mg melamine formaldehyde resin, 2mg polyacrylic acid, 2mg carboxymethyl cellulose
- Step B6 Take 1.2g of silica nanoparticles with a diameter of 20nm and place them in 4ml of silica sol solvent to obtain a silica sol solution with a concentration of 0.3g/ml, mix the silica sol solution with the solution obtained in step B5, and shake at room temperature 5h until the mixture is uniform, and the conductive ink is obtained after uniform mixing.
- the silver nanowire solvent, silica sol solvent, dispersant solvent and leveling agent solvent are all deionized water.
- Examples 1-8 are all examples of 100ml conductive ink.
- the amount of each component can be expanded or reduced in proportion to specific needs.
- the dispersant solvent and leveling When the dosage of the solvent is small, the dosage is not included in the total solvent, and the silver nanowire solvent is taken as an integer value for easy production.
- the conductive ink of the ultra-low haze silver nanowire film prepared by the preparation method in Examples 1-8 has the following properties:
- the average diameter of the silver nanowires synthesized in step A of Examples 1-8 is about 20 nanometers, and the aspect ratio is about 1000; this ensures that the films manufactured in Examples 1-8 have an average optical transmission
- the rate is higher than 95% and the haze is lower than 0.5% (as shown in Figures 4 and 5), which meets the optical requirements of high-definition screens.
- the silica sol specially added to the conductive ink tightly fixes the silver nanowires on the substrate, and at the same time forms an aging protection layer on the surface, as shown in the scanning electron microscope (Figure 3(b)).
- the anti-3M tape sticking test shown in Figure 6(b) confirmed the strong bond between the silver nanowires and the substrate.
- the use of silica sol significantly increased the surface hardness of the film to 3H (as shown in Figure 7(b)).
- the conductive ink of the ultra-low haze silver nanowire film prepared by the preparation method in Examples 1-8 is applied to a high-definition screen.
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Abstract
Description
Claims (10)
- 一种超低雾度银纳米线薄膜的导电墨水,其特征在于,每100ml导电墨水中包含以下组分:银纳米线:50-1000mg,银纳米线溶剂:90-99ml,粘度调节剂:0.1-2g,分散剂:3-70mg,分散剂溶剂:0.1-1ml,流平剂:4-85mg,流平剂溶剂:0.1-1ml,二氧化硅纳米颗粒:0.2-8.5g,硅溶胶溶剂:1-8ml;其中:50-1000mg的银纳米线由以下组分制得:PVP:0.4-20g,硝酸银:0.5-10g,卤素离子试剂:0.04-0.8g,乙二醇:132-1500ml。
- 根据权利要求1所述的超低雾度银纳米线薄膜的导电墨水,其特征在于,所述PVP的分子质量大于30万。
- 根据权利要求1所述的超低雾度银纳米线薄膜的导电墨水,其特征在于,所述卤素离子试剂包括NaCl、NaBr、FeCl 3、四丙基氯化铵、四丙基溴化铵中的一种或多种。
- 根据权利要求1所述的超低雾度银纳米线薄膜的导电墨水,其特征在于,所述银纳米线溶剂、硅溶胶溶剂、分散剂溶剂和流平剂溶剂均为去离子水或醇系溶剂;当银纳米线溶剂为去离子水时,硅溶胶溶剂、分散剂溶剂和流平剂溶剂也为去离子水;当银纳米线溶剂为醇系溶剂时,硅溶胶溶剂、分散剂溶剂和流平剂溶剂也为醇系溶剂。
- 根据权利要求4所述的超低雾度银纳米线薄膜的导电墨水,其特征在于,所述醇系溶剂是乙醇、丙醇、乙二醇、丙三醇中的任一种或几种混合。
- 根据权利要求1所述的超低雾度银纳米线薄膜的导电墨水,其特征在于,所述粘度调节 剂包括纤维素醚及其衍生物类中的一种或几种,纤维素醚及其衍生物类包括羟乙基纤维素、甲基羟乙基纤维素、羟丙基甲基纤维素、乙基羟乙基纤维素、甲基羟丙基纤维素、纤维素烷基醚、纤维素羟烷基醚;
- 根据权利要求1所述的超低雾度银纳米线薄膜的导电墨水,其特征在于,所述分散剂包括三乙基己基磷酸、十二烷基硫酸钠、甲基戊醇、纤维素衍生物、聚丙烯酰胺、聚丙烯酸酯聚合物、古尔胶、脂肪酸聚乙二醇酯中的一种或多种;所述流平剂包括丙烯酸树脂、脲醛树脂、三聚氰胺甲醛树脂、饱和树脂、聚丙烯酸、羧甲基纤维素中的一种或多种。
- 根据权利要求1所述的超低雾度银纳米线薄膜的导电墨水,其特征在于,所述二氧化硅纳米颗粒的直径为5~20nm。
- 根据权利要求1-7任一所述的超低雾度银纳米线薄膜的导电墨水的制备方法,其特征在于,包括以下步骤:步骤A、银纳米线的合成,步骤A1、取PVP放入乙二醇中,加热至PVP完全溶解后自然冷却,得到PVP乙二醇溶液;步骤A2、取AgNO 3加入乙二醇中,至AgNO 3完全溶解,得到AgNO 3乙二醇溶液;步骤A3、取卤素离子试剂溶解于乙二醇中,得到卤素离子乙二醇溶液;步骤A4、取乙二醇置于容器中,并将容器浸没在室温的油浴锅中,依次将步骤A3中得到的卤素离子乙二醇溶液、步骤A2中得到的AgNO 3乙二醇溶液、步骤A1中得到的PVP乙二醇溶液注入容器中,机械搅拌;步骤A5、通入氮气,且将油浴锅开启加热至180℃,达温后停止通氮气,并将温度设为170℃,在机械搅拌辅助下3-8min后降为170℃,继续搅拌2min后停止机械搅拌,在170℃保温反应1-1.2h后,取出并放于5-15℃的冷水中淬冷至室温,得到含有银纳米线的溶液;步骤B、银纳米线墨水的配制,步骤B1、将步骤A5中得到的含有银纳米线的溶液过滤清洗一次后,取滤饼分散到PVP水溶液中,静置后取上清液,再过滤清洗3-5次,过滤清洗3-5次均取滤膜上的滤饼分散到PVP水溶液中备用,滤饼为银纳米线;步骤B2、将粘度调节剂分散在银纳米线溶剂中,室温中摇晃,至完全溶解且分散均匀,得到溶液;步骤B3、将步骤B1中得到的银纳米线加入到步骤B2中得到的溶液中,得到银纳米线分散液;步骤B4、取分散剂置于分散剂溶剂中得到分散剂溶液,再将分散剂溶液加入到步骤B3中得到的银纳米线分散液中,室温中摇晃至混合均匀;步骤B5、取流平剂置于流平剂溶剂中得到流平剂溶液,再将流平剂溶液加入到步骤B4中得到的溶液中,室温中摇晃至混合均匀;步骤B6、取二氧化硅纳米颗粒置于硅溶胶溶剂中得到浓度为0.2-1.0625g/ml的硅溶胶溶液,将硅溶胶溶液与步骤B5中得到的溶液混合,室温中摇晃至混合均匀,混合均匀后得到导电墨水。
- 一种根据权利要求1-8任一所述的制备方法制得的超低雾度银纳米线薄膜的导电墨水应用于高清屏。
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