CN108766628B - Preparation method of silver nanowire-oxide sol composite transparent electrode - Google Patents
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Abstract
The invention discloses a preparation method of a silver nanowire-oxide sol composite transparent electrode, which comprises the following steps: respectively carrying out ultrasonic treatment on the substrate in deionized water, ethanol and acetone for 10-20 min, and drying to obtain a treated substrate; the mixed solution consists of silver nanowires, oxide sol, a stabilizer, a surfactant, a film forming aid and a solvent, and is stirred at a speed of 400-600 r/min for 30-90 min to obtain silver nanowire-oxide sol composite conductive ink; and uniformly coating the silver nanowire-oxide sol composite conductive ink on the treated substrate, and evaporating the solvent to obtain the silver nanowire-oxide sol composite transparent electrode. The method of the invention can improve the conductivity of the transparent electrode, has low production cost and is suitable for large-scale production.
Description
Technical Field
The invention relates to a preparation method of a silver nanowire transparent electrode, in particular to a preparation method of a silver nanowire-oxide sol composite transparent electrode.
Background
The transparent electrode has excellent visible light transmittance and conductivity, and is widely applied to a plurality of photoelectric conversion devices, such as OLED (organic light emitting diode) equipment, touch screens, thin-film solar cells, transparent heating equipment and the like. Currently, tin-doped indium oxide (ITO) conductive glass electrodes are most widely used in industry. However, ITO transparent electrodes also face a number of challenges. First, the In element reserves are small, resulting In limited sources of ITO. Meanwhile, the ITO electrode is manufactured by generally adopting modes such as sputtering and the like, vacuum equipment is needed, and higher requirements are provided for the thermal stability of the substrate. In addition, ITO is an oxide, which is brittle and cannot be bent, and these characteristics do not meet the flexibility requirements of next-generation wearable devices.
Compared with other materials such as graphene, conductive polymers, gold nanowires and the like, the silver nanowire transparent electrode has better conductivity and stability, is expected to replace a tin-doped indium oxide (ITO) conductive glass electrode which is widely applied at present, and is widely applied to the fields of OLED, wearable equipment, solar cells and the like. At present, in the silver nanowire transparent electrode prepared in the prior art, the silver nanowires are simply stacked, and the contact resistance between the silver nanowires is large, so that the conductivity of the film is greatly influenced. In order to improve the conductivity of the silver nanowire transparent electrode, methods such as covering the surface of the silver nanowire with graphene (CN104934109A, CN104492677A) and adding a cellulose layer (CN104867621A) on the substrate can be adopted, but the methods have the disadvantages of high material cost, difficulty in preparation and the like, and are not suitable for large-scale application.
The oxide sol has the advantages of wide source, low cost and the like, and can effectively improve various performances of the transparent conductive film after being compounded with the silver nanowire transparent conductive film (CN 104162681A). At present, silver nanowires and different oxides are compounded to prepare a film, and the sol-compounded silver nanowire transparent conductive film mainly adopts sol distribution spin coating and other modes, is complex to operate, has great influence on the transmittance of the film and is not suitable for continuous production; or the silver nanowires are modified by adopting oxides and then the conductive film is prepared, and the modified silver nanowires need to be separated, so that the production cost is increased. The metal oxide composite silver nanowire transparent conductive film (CN106782891A) was first coated with silver nanowires, and then with an oxide sol. The silver nanowire film prepared by the method is fragile and easy to oxidize, vulcanize or be damaged by external force while the process is complicated. Therefore, the coating of the oxide sol must be performed by spray coating or spin coating, which increases the preparation cost and is not suitable for mass production.
In view of the above, there is a need for improvements in the prior art.
Disclosure of Invention
The invention aims to provide a preparation method of a silver nanowire-oxide sol composite transparent electrode, which improves the conductivity of the transparent electrode, has low production cost and is suitable for large-scale production.
In order to solve the technical problems, the invention provides a preparation method of a silver nanowire-oxide sol composite transparent electrode, which comprises the following steps:
1) and processing the transparent electrode substrate:
respectively carrying out ultrasonic treatment on the substrate in deionized water, ethanol and acetone for 10-20 min, and drying to obtain a treated substrate;
2) and preparing the silver nanowire-oxide sol composite conductive ink:
the mixed solution consists of silver nanowires, oxide sol, a stabilizer, a surfactant, a film-forming aid and a solvent (namely, the silver nanowires, the oxide sol, the stabilizer, the surfactant and the film-forming aid are added into the solvent to form mixed solution);
in the mixed solution, the content of the silver nanowires is 0.5-5 mg/mL, the content of solids in the oxide sol is 5-150 ppm (mass/volume), the volume concentration of the stabilizer is 0.01-5%, the content of the surfactant is 0.01-5 mg/mL, the content of the film-forming additive is 0.01-20 mg/mL, and the balance is the solvent;
stirring the mixed solution at a speed of 400-600 r/min for 30-90 min to obtain silver nanowire-oxide sol composite conductive ink;
3) and preparing the silver nanowire-oxide sol composite transparent electrode:
uniformly coating the silver nanowire-oxide sol composite conductive ink obtained in the step 2) on the treated substrate obtained in the step 1), and evaporating the solvent to obtain the silver nanowire-oxide sol composite transparent electrode.
The improvement of the preparation method of the silver nanowire-oxide sol composite transparent electrode of the invention is as follows:
the oxide sol is SiO2Sol, Al2O3Sol, TiO2Sol, ZrO2At least one of sol, ITO sol and AZO sol;
the stabilizer is at least one of ammonia water, AMP-95, monomethylamine, formamide and propylamine;
the surfactant is at least one of triton (X100, X114 or X45), Zonyl FSN, Zonyl FSO, Zonyl FSH or Dynol (604 or 607);
the film forming auxiliary agent is at least one of hydroxymethyl propyl cellulose (HPMC), methyl cellulose (CMC), xanthan gum, Polyurethane (PU), polyvinyl alcohol (PVA) and tripropylene glycol (TPG).
The preparation method of the silver nanowire-oxide sol composite transparent electrode is further improved as follows: the particle size range of the oxide sol is 5 nm-150 nm.
The preparation method of the silver nanowire-oxide sol composite transparent electrode is further improved as follows: the solvent is at least one of deionized water, ethanol, acetone, ethylene glycol and polyethylene glycol.
The preparation method of the silver nanowire-oxide sol composite transparent electrode is further improved as follows: the substrate is at least one of a glass substrate, a PET substrate, cloth, paper, a PVA film and a PDMS film.
The preparation method of the silver nanowire-oxide sol composite transparent electrode is further improved as follows: and 2) stirring the mixed solution for 60min at a speed of 500r/min to obtain the silver nanowire-oxide sol composite conductive ink.
Compared with the prior art, the invention has the technical advantages that:
1. the preparation of the silver nanowire-oxide sol composite transparent conductive film is realized by configuring the silver nanowire-oxide sol composite conductive ink and then directly coating the film by using the composite conductive ink with better stability, the process is simple, the method is suitable for large-scale production, and the prepared conductive ink is stable within 3 months.
2. When the silver nanowire-oxide sol composite conductive ink is used for directly coating the film, the film can be formed by any coating process in one step, and the prepared film has better mechanical and chemical stability and is more suitable for large-scale production.
3. The silver nanowire-oxide sol composite transparent electrode disclosed by the invention has the advantages that the silver nanowires are mutually and tightly connected through the capillary force formed by the agglomeration of the oxide sol during drying, the contact resistance among the silver nanowires is reduced, and the conductivity of the electrode is improved. The preparation process is simple and suitable for large-scale production.
4. The preparation method is simple and reliable and has high repeatability. The oxide sol is adopted, so that the price is low, and the production cost is favorably reduced.
Drawings
The following describes embodiments of the present invention in further detail with reference to the accompanying drawings.
FIG. 1 is a microscopic morphology view of a silver nanowire transparent electrode without composite oxide sol of comparative example 1-1;
fig. 2 is a microscopic topography of the oxide sol composite silver nanowire transparent electrode of example 1.
Detailed Description
The invention will be further described with reference to specific examples, but the scope of the invention is not limited thereto.
In the following case, the diameter of the silver nanowire is 40-60 nanometers, and the length is 45-65 μm; in the aluminum-doped zinc oxide sol (AZO), the doping amount of aluminum is 12 percent of the weight of a solid phase; in the tin-doped indium oxide sol (ITO), the doping amount of tin is 8% of the solid phase weight.
Example 1, a method for preparing a silver nanowire-oxide sol composite transparent electrode, sequentially comprises the following steps:
1) and processing the transparent electrode substrate: respectively performing ultrasonic treatment on the substrate in deionized water, ethanol and acetone for 15min, and drying (blowing dry with nitrogen), wherein the size of the substrate is 30cm multiplied by 100 cm.
The substrate can be at least one of glass, a PET substrate, cloth, paper, a PVA film, a PDMS film and other materials, and the substrate adopted in the embodiment is a glass substrate.
2) And preparing the silver nanowire-oxide sol composite conductive ink (hereinafter referred to as conductive ink) by the following steps:
adding silver nanowires, oxide sol, a stabilizer, a surfactant and a film-forming aid into a solvent to obtain a mixed solution;
stirring the mixed solution at a speed of 400-600 r/min for 30-90 min to obtain silver nanowire-oxide sol composite conductive ink;
the oxide sol can be SiO2Sol (silica sol), Al2O3Sol (alumina sol), TiO2Sol (titanium dioxide sol), ZrO2At least one of oxide sols such as sol (zirconia sol), ITO sol (tin-doped indium oxide sol) or AZO sol (aluminum-doped zinc oxide sol), and the like, and the particle size range of the oxide sols is 5nm to 150 nm.
The stabilizer can be at least one of ammonia water, AMP-95, monomethylamine, formamide or propylamine.
The surfactant can be at least one of triton (X100, X114 or X45), Zonyl FSN, Zonyl FSO, Zonyl FSH or Dynol (604 or 607).
The film forming auxiliary agent can adopt at least one of hydroxymethyl propyl cellulose (HPMC), methyl cellulose (CMC), xanthan gum, Polyurethane (PU), polyvinyl alcohol (PVA) or tripropylene glycol (TPG).
The solvent can be at least one of deionized water, ethanol, acetone, isopropanol, ethylene glycol or polyethylene glycol.
In this example, silver nanowires, SiO2Adding sol (particle size of 100nm), ammonia water, triton X100 and HPMC (hydroxypropyl methyl cellulose) into a proper amount of isopropanol solvent to obtain a mixed solution;
the content of silver nanowires in the mixed solution is 1.2mg/mL and SiO is2The sol concentration is 75ppm, the HPMC concentration is 2mg/mL, the Triton X100 concentration is 0.01mg/mL, the ammonia water volume concentration is 2%, and the balance is isopropanol. And stirring the mixed solution for 1h at 500r/min to obtain the conductive ink, namely the silver nanowire-silicon dioxide sol composite conductive ink.
3) And preparing the silver nanowire-oxide sol composite transparent electrode:
dropping 9mL of the conductive ink obtained in the step 2) on the substrate treated in the step 1), carrying out blade coating by using a 20-micrometer wire rod at a speed of 10mm/s and a blade coating distance of 100cm, and evaporating a solvent (isopropanol) to obtain the silver nanowire-oxide sol composite transparent electrode, namely the silver nanowire-silica sol composite transparent electrode, wherein a micro-topography of the electrode is shown in FIG. 2.
Note: the substrate size multiplied by the bar height gives the total volume of the wet film, which again increases the required conductive ink by 50%. The total volume of the wet film in this example was 30 × 100 × 20/10000-6 cc, i.e. 6 × 1.5-9 mL of conductive ink was required.
The sheet resistance of the transparent electrode is 27 omega/sq, the 550nm transmittance is 87 percent, and the quality factor phi isTC＝9.20×10-3Ω-1。
Quality factor formula:
where T represents the transmittance and Rs represents the resistance per square in Ω.
Note: the larger the quality factor value, the better the conductivity of the transparent electrode.
Embodiment 2, a method for preparing a silver nanowire-zirconia sol composite transparent electrode, sequentially comprises the following steps:
1) and processing the transparent electrode substrate:
respectively carrying out ultrasonic treatment on a glass substrate in deionized water, ethanol and acetone for 15min, and drying the glass substrate by using nitrogen, wherein the size of the substrate is 30cm multiplied by 100 cm;
2) and preparing the silver nanowire-zirconia sol composite conductive ink:
silver nanowires, ZrO2 sol (particle size 16nm), AMP-95, Zonyl FSO-100 and CMC were added to an appropriate amount of ethanol solvent to obtain a mixed solution.
The content of silver nanowires in the mixed solution is 0.6mg/mL, the concentration of ZrO2 sol is 100ppm, the concentration of CMC is 4mg/mL, the concentration of Zonyl FSO-100 is 0.6mg/mL, the volume concentration of AMP-95 is 2 percent, and the balance is ethanol.
And stirring the mixed solution for 1h at 500r/min to obtain the conductive ink, namely the silver nanowire-zirconia sol composite conductive ink.
3) And preparing the silver nanowire-zirconia sol composite transparent electrode:
dripping 13.5mL of the conductive ink obtained in the step 2) on the substrate treated in the step 1), carrying out blade coating by using a 30-micrometer wire rod at the speed of 8mm/s and the blade coating distance of 100cm, and evaporating a solvent (ethanol) to obtain the silver nanowire-zirconia sol composite transparent electrode;
the sheet resistance of the transparent electrode is 9 omega/sq, 550nmTransmittance of 75%, quality factor phiTC＝6.25×10-3Ω-1。
Embodiment 3, a method for preparing a silver nanowire-alumina sol composite transparent electrode, comprising the following steps:
1) and processing the transparent electrode substrate:
and respectively carrying out ultrasonic treatment on the glass substrate in deionized water, ethanol and acetone for 15min, and blow-drying by nitrogen, wherein the size of the substrate is 30cm multiplied by 100 cm.
2) And preparing the silver nanowire-alumina sol composite conductive ink:
silver nanowires, Al2O3Adding the sol (with the particle size of 40nm), formamide, Zonyl FSH and xanthan gum into a proper amount of deionized water solvent to obtain a mixed solution.
The content of silver nanowires in the mixed solution is 4mg/mL, and Al is2O3The sol concentration is 40ppm, the xanthan gum concentration is 4mg/mL, the Zonyl FSH concentration is 2.6mg/mL, the formamide volume concentration is 3.4%, and the balance is deionized water. And stirring the mixed solution for 1h at 500r/min to obtain the conductive ink, namely the silver nanowire-alumina sol composite conductive ink.
3) And preparing the silver nanowire-oxide sol composite transparent electrode:
dripping about 6.8mL of the conductive ink obtained in the step 2) on the substrate treated in the step 1), carrying out blade coating by using a 15-micrometer wire rod at the speed of 4mm/s and the blade coating distance of 100cm, and evaporating a solvent (deionized water) to obtain the silver nanowire-alumina sol composite transparent electrode;
the sheet resistance of the transparent electrode is 56 omega/sq, the 550nm transmittance is 89%, and the quality factor phi isTC＝5.57×10-3Ω-1。
Embodiment 4, a method for preparing a silver nanowire-aluminum doped zinc oxide sol composite transparent electrode, comprising the following steps:
1) and processing the transparent electrode substrate:
respectively carrying out ultrasonic treatment on the PET substrate in deionized water, ethanol and acetone for 15min, and drying by using nitrogen. The substrate size was 30cm x100 cm.
2) And preparing the silver nanowire-aluminum doped zinc oxide sol composite conductive ink:
adding silver nanowires, AZO sol, propylamine, triton X114 and PVA into a proper amount of acetone solvent to obtain a mixed solution.
The content of silver nanowires in the mixed solution is 1mg/mL, the concentration of AZO sol is 55ppm, the concentration of PVA is 2.8mg/mL, the concentration of Triton X114 is 1.3mg/mL, the volume concentration of propylamine is 2.2 percent, and the balance is acetone, and after the mixed solution is stirred for 1h at 500r/min, the conductive ink, namely the silver nanowire-aluminum doped zinc oxide sol composite conductive ink, is obtained.
3) And preparing the silver nanowire-aluminum doped zinc oxide sol composite transparent electrode:
dripping about 11.3mL of the conductive ink obtained in the step 2) on the substrate treated in the step 1), carrying out blade coating by using a 25-micrometer scraper at the speed of 5mm/s and the blade coating distance of 100cm, and evaporating a solvent to obtain the silver nanowire-aluminum-doped zinc oxide sol composite transparent electrode;
the sheet resistance of the transparent electrode is 31 omega/sq, the 550nm transmittance is 86 percent, and the quality factor phi isTC＝7.14×10-3Ω-1。
Embodiment 5, a method for preparing a silver nanowire-tin-doped indium oxide sol composite transparent electrode, comprising the following steps:
1) and processing the transparent electrode substrate:
respectively performing ultrasonic treatment on the PVA film in deionized water, ethanol and acetone for 15min, and blow-drying with nitrogen, wherein the substrate size is 30cm multiplied by 100 cm.
2) And preparing the silver nanowire-tin-doped indium oxide sol composite conductive ink:
adding silver nanowires, ITO sol, methylamine, Dynol604 and xanthan gum into a proper amount of ethanol and ethylene glycol mixed solvent (ethanol: ethylene glycol ═ 4:1) to obtain a mixed solution.
The content of silver nanowires in the mixed solution is 3mg/mL, the concentration of ITO sol is 130ppm, the concentration of xanthan gum is 3.5mg/mL, the concentration of Zonyl FSO-100 is 4mg/mL, the volume concentration of propylamine is 2 percent, and the balance is a mixed solvent of ethanol and ethylene glycol. And stirring the mixed solution for 1h at 500r/min to obtain the conductive ink, namely the silver nanowire-tin-doped indium oxide sol composite conductive ink.
3) And preparing the silver nanowire-tin-doped indium oxide sol composite transparent electrode:
dripping 9mL of the conductive ink obtained in the step 2) on the substrate treated in the step 1), carrying out blade coating by using a 20-micrometer wire rod at the speed of 6mm/s and the blade coating distance of 100cm, and evaporating a solvent to obtain the silver nanowire-tin-doped indium oxide sol composite transparent electrode;
the sheet resistance of the transparent electrode is 21 omega/sq, the 550nm transmittance is 81 percent, and the quality factor phi isTC＝5.79×10-3Ω-1。
Comparative example 1-1, the use of SiO2 sol in step 2) of example 1 was eliminated, i.e., the mixture did not contain SiO2 sol, and the rest was identical to example 1.
The microscopic topography of the transparent electrode is shown in FIG. 1, the sheet resistance is 86 Ω/sq, and the 550nm transmittance is 87%. Quality factor phiTC＝2.89×10-3Ω-1。
As can be seen from comparative example 1-1, when the use of the oxide sol (SiO2 sol) was eliminated, the silver nanowires were stacked only under the gravity, and the resistance at the contact of the silver nanowires was high, resulting in poor conductivity of the obtained transparent electrode.
Comparative example 1-2, the concentration of SiO2 sol in step 2) of example 1 was increased from "75 ppm" to "160 ppm", and the remainder was identical to example 1.
The sheet resistance of the transparent electrode was >1 k.OMEGA./sq, and the 550nm transmittance was 87%.
As can be seen from comparative examples 1-2, the transparent electrode had conductivity not comparable to that of the oxide Sol (SiO) used2Sol) is proportional. When SiO is used2When the concentration of the sol exceeds 150ppm, a large amount of SiO is agglomerated among the silver nano-wires2The sol particles hinder the electron transport and even make the transparent electrode non-conductive.
Comparative examples 1 to 3, the use of aqueous ammonia in step 2) of example 1 was eliminated, and the remainder was the same as in example 1.
Silver nanowire and SiO2The sol particles are agglomerated and cannot form a film.
Comparative examples 1 to 4, the use of triton X-100 in step 2) of example 1 was eliminated, and the remainder was identical to example 1.
The wettability of the silver nanowire composite ink to a substrate is poor, the final transparent electrode is not uniform, and the deviation of the sheet resistance and the transmittance of different points is more than 30%.
Comparative examples 1-5, the use of HPMC in step 2) of example 1 was eliminated and the remainder was identical to example 1.
The film can not be formed, and the solute is obviously agglomerated.
Comparative examples 1-6, the HPMC concentration in step 2) of example 1 was increased to 21mg/mL, the rest being equivalent to example 1.
The ink viscosity was too high to form a film.
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 (5)
1. The preparation method of the silver nanowire-oxide sol composite transparent electrode is characterized by comprising the following steps of:
1) and processing the transparent electrode substrate:
respectively carrying out ultrasonic treatment on the substrate in deionized water, ethanol and acetone for 10-20 min, and drying to obtain a treated substrate;
2) and preparing the silver nanowire-oxide sol composite conductive ink:
the mixed solution consists of silver nanowires, oxide sol, a stabilizer, a surfactant, a film-forming assistant and a solvent;
in the mixed solution, the content of silver nanowires is 0.6-4 mg/mL, the content of solid matters in oxide sol is 40-130 ppm, the volume concentration of a stabilizer is 2-3.4%, the content of a surfactant is 0.01-2.6 mg/mL, the content of a film-forming aid is 2-4 mg/mL, and the balance is a solvent;
stirring the mixed solution at a speed of 400-600 r/min for 30-90 min to obtain silver nanowire-oxide sol composite conductive ink;
the oxide sol is SiO2Sol, Al2O3Sol, TiO2Sol, ZrO2At least one of sol, ITO sol and AZO sol;
the stabilizer is at least one of ammonia water, AMP-95, monomethylamine, formamide and propylamine;
the surfactant is at least one of Triton X-100, Triton X-114, Triton X-45, Zonyl FSN, Zonyl FSO, Zonyl FSH, Dynol604, and Dyno 607;
the film-forming auxiliary agent is at least one of hydroxymethyl propyl cellulose (HPMC), methyl cellulose (CMC), xanthan gum, Polyurethane (PU), polyvinyl alcohol (PVA) and tripropylene glycol (TPG);
the particle size range of the oxide sol is 5 nm-150 nm;
3) and preparing the silver nanowire-oxide sol composite transparent electrode:
uniformly coating the silver nanowire-oxide sol composite conductive ink obtained in the step 2) on the treated substrate obtained in the step 1), and evaporating the solvent to obtain the silver nanowire-oxide sol composite transparent electrode.
2. The method for preparing a silver nanowire-oxide sol composite transparent electrode according to claim 1, wherein:
the solvent is at least one of deionized water, ethanol, acetone, ethylene glycol and polyethylene glycol.
3. The method for preparing a silver nanowire-oxide sol composite transparent electrode according to claim 2, wherein:
the substrate is at least one of a glass substrate, a PET substrate, cloth, paper, a PVA film and a PDMS film.
4. The method for preparing a silver nanowire-oxide sol composite transparent electrode according to claim 3, wherein:
and 2) stirring the mixed solution for 60min at a speed of 500r/min to obtain the silver nanowire-oxide sol composite conductive ink.
5. The method for preparing a silver nanowire-oxide sol composite transparent electrode according to claim 1, wherein:
in the step 2), the content of the silver nanowires in the mixed solution is 1.2mg/mL and SiO is2The sol concentration is 75ppm, the hydroxymethyl propyl cellulose concentration is 2mg/mL, the triton X100 concentration is 0.01mg/mL, the ammonia water volume concentration is 2%, and the balance is isopropanol.
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| CN107346672A (en) * | 2016-05-05 | 2017-11-14 | 深圳市润麒麟科技发展有限公司 | A kind of transparent conductive film containing nano-silver thread and preparation method thereof |
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