CN110580973A - Preparation method of silver nanowire film - Google Patents
Preparation method of silver nanowire film Download PDFInfo
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- CN110580973A CN110580973A CN201910744365.8A CN201910744365A CN110580973A CN 110580973 A CN110580973 A CN 110580973A CN 201910744365 A CN201910744365 A CN 201910744365A CN 110580973 A CN110580973 A CN 110580973A
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- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/20—Conductive material dispersed in non-conductive organic material
- H01B1/22—Conductive material dispersed in non-conductive organic material the conductive material comprising metals or alloys
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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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- H—ELECTRICITY
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- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- 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
Abstract
The invention belongs to the technical field of nano materials, and particularly relates to a preparation method of a silver nanowire film. The preparation method of the silver nanowire film comprises the following steps: providing an initial silver nanowire solution; introducing gas with oxidability into the initial silver nanowire solution, and carrying out oxidation reaction on the surface of the silver nanowire to obtain an oxidized silver nanowire solution; and coating the oxidized silver nanowire solution on a substrate for drying treatment to obtain the silver nanowire film. The surface of the silver nanowire is oxidized to form silver metal compounds on the surface, the silver metal compounds can inhibit the generation of plasma resonance on the surface of the silver nanowire, so that the proportion of scattered light is reduced, and further the haze is reduced, and the silver metal compounds generally do not have metal luster, so that the reflection can be reduced, and the haze is further reduced; therefore, the haze of the finally prepared silver nanowire film is remarkably reduced.
Description
Technical Field
The invention belongs to the technical field of nano materials, and particularly relates to a preparation method of a silver nanowire film.
Background
Silver Nanowires (AgNWs) refer to one-dimensional Silver metal materials with the length of micrometer scale and the diameter of nanometer scale, and the length-diameter ratio of the Silver Nanowires can reach more than 1000. Generally, the longer the length and the smaller the diameter of the silver nanowire, the higher the transmittance and the lower the resistance thereof.
The silver nanowire transparent conductive film is a conductive film prepared by combining countless silver nanowires and a proper organic cross-linked body on a flexible substrate. Compared with the traditional Indium Tin Oxide (ITO) transparent conductive film, the silver nanowire transparent conductive film has better light transmittance, conductivity and bending performance and lower production cost.
The silver nanowire is used as a conductor and exists in a metal form, and the Surface of the silver nanowire has a strong Surface Plasmon Resonance (SPR) effect, so that strong scattering is caused when light irradiates the Surface of the silver nanowire, and the haze of the silver nanowire film is greatly improved. Therefore, it is important to achieve better suppression of the SPR effect while maintaining high levels of electrical conductivity and optical performance.
Disclosure of Invention
The invention aims to provide a preparation method of a silver nanowire film, and aims to solve the technical problem of high haze of the existing silver nanowire film.
in order to achieve the purpose, the invention adopts the following technical scheme:
the invention provides a preparation method of a silver nanowire film, which comprises the following steps:
Providing an initial silver nanowire solution;
Introducing gas with oxidability into the initial silver nanowire solution, and carrying out oxidation reaction on the surface of the silver nanowire to obtain an oxidized silver nanowire solution;
And coating the oxidized silver nanowire solution on a substrate for drying treatment to obtain the silver nanowire film.
In one embodiment, the carrier gas of the oxidizing gas is nitrogen, and the flow rate is 50-500 ml/min.
In one embodiment, the oxidizing gas contains 10 to 100mmol/L of oxygen.
In one embodiment, the oxidizing gas contains 0.1 to 5mmol/L hydrogen sulfide.
In an embodiment, in the oxidized silver nanowire solution, the thickness of the oxide layer on the surface of the silver nanowire is 1-20 nm.
In one embodiment, the initial silver nanowire solution has a mass fraction of silver nanowires of 0.01% to 0.2%.
In one embodiment, the temperature for performing the oxidation reaction on the surface of the silver nanowire is 60-160 ℃; and/or the presence of a gas in the gas,
The time for carrying out the oxidation reaction on the surface of the silver nanowire is 10-60 min.
In one embodiment, the temperature of the drying treatment is 60-130 ℃; and/or the presence of a gas in the gas,
The drying time is 25-35 min.
in one embodiment, the silver nanowire film is a transparent conductive film.
In one embodiment, the substrate is selected from any one of a PET film, a TAC film, a PEN film, a CPI film, a COP film, a PDMS film, and a glass film.
The preparation method of the silver nanowire film provided by the invention comprises the steps of firstly introducing gas with oxidability into an initial silver nanowire solution to carry out oxidation reaction on the surface of a silver nanowire, and then coating and drying to obtain the silver nanowire film; the surface of the silver nanowire is oxidized to form silver metal compounds on the surface, the silver metal compounds can inhibit the generation of plasma resonance on the surface of the silver nanowire, so that the proportion of scattered light is reduced, and further the haze is reduced, and the silver metal compounds do not have metal luster, so that the reflection can be reduced, and the haze is further reduced; in conclusion, the haze of the finally prepared silver nanowire film is remarkably reduced through the oxidation of the surface of the silver nanowire.
drawings
Fig. 1 is a schematic flow chart of a method for preparing a silver nanowire film according to an embodiment of the present invention.
Detailed Description
In order to make the technical problems, technical solutions and advantageous effects to be solved by the present invention more clearly apparent, the present invention is further described in detail below with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
The embodiment of the invention provides a preparation method of a silver nanowire film, which comprises the following steps as shown in figure 1:
S01, providing an initial silver nanowire solution;
s02, introducing gas with oxidizability into the initial silver nanowire solution, and carrying out oxidation reaction on the surface of the silver nanowire to obtain an oxidized silver nanowire solution;
And S03, coating the oxidized silver nanowire solution on a substrate for drying treatment to obtain the silver nanowire film.
The preparation method of the silver nanowire film provided by the embodiment of the invention comprises the steps of firstly introducing gas with oxidability into an initial silver nanowire solution to enable the surface of a silver nanowire to carry out oxidation reaction, and then coating and drying to obtain the silver nanowire film; the surface of the silver nanowire is oxidized to form silver metal compounds on the surface, the silver metal compounds can inhibit the generation of plasma resonance on the surface of the silver nanowire, so that the proportion of scattered light is reduced, and further the haze is reduced, and the silver metal compounds do not have metal luster, so that the reflection can be reduced, and the haze is further reduced; in conclusion, the haze of the finally prepared silver nanowire film is remarkably reduced through the oxidation of the surface of the silver nanowire.
Haze (haze) is the percentage of the total transmitted light intensity that is transmitted above an angle of 2.5 ° from the incident light. After the silver metal compound formed by oxidizing the surface of the silver nanowire inhibits the generation of surface plasmon resonance, the proportion of scattered light is reduced, thereby reducing haze. In the embodiment of the invention, the initial silver nanowire solution is obtained after the preparation of the silver nanowires is finished, and a proper amount of specific gas capable of oxidizing silver is introduced into the initial silver nanowire solution of the reaction kettle to oxidize the silver on the surface of the silver nanowires, so that the surface plasma resonance effect is inhibited, and finally the fog of the silver nanowire film can be reduced by 0.1-1.5%. The preparation method of the silver nanowire film provided by the embodiment of the invention has the advantages of simple process and low cost, and the product yield is not influenced under the condition of increasing the process steps, so that the preparation method can be used for preparing transparent conductive films by various conductive inks containing silver nanowires.
The silver nanowire film prepared by the embodiment of the invention is a transparent conductive film. The coated substrate is a flexible substrate, and specifically, the substrate is any one of PET (Polyethylene Terephthalate), TAC (Triacetyl Cellulose), PEN (Polyethylene naphthalate), PDMS (Polydimethylsiloxane), CPI (Colorless transparent Polyimide), COP (cyclic Olefin copolymer), and a glass film.
In an embodiment, the initial silver nanowire solution in step S01 is a silver nanowire ink prepared by a conventional method, wherein the silver nanowire can be obtained by a conventional synthesis method, and a specific preparation method can be any one of an alcoholic thermal method, a hydrothermal method and a polyol reduction method. After the initial silver nanowire solution is prepared, oxidizing gas is introduced, and then an oxidation reaction can be carried out on the surface of the silver nanowire. In one embodiment, the initial silver nanowire solution has a mass fraction of silver nanowires of 0.01% to 0.2%. The mass fraction of the silver nanowires in the initial silver nanowire solution is 0.01-0.2%. The primary silver nanowire solution in the concentration range can be better contacted with gas with oxidizing property, so that the silver nanowire solution can be oxidized.
In the initial silver nanowire solution, the diameter of the silver nanowire is 15-95nm, and the length-diameter ratio is 500-2500. The initial silver nanowire solution (or silver nanowire ink) may contain an additive such as a thickener and a wetting dispersant, and a pH adjuster, in addition to the silver nanowires. Wherein the thickener can be hydroxypropyl methylcellulose, and the mass fraction can be 0.01-0.8%. The wetting dispersant can be a high molecular type hyperdispersant, and is at least one of DISPERBYK-180, DISPERBYK-184, DISPERBYK-190, DISPERBYK-191, DISPERBYK-192, DISPERBYK-194, DISPERBYK-2010 and DISPERBYK-2015, and the mass fraction is 0.01-0.8%. The pH regulator is at least one of 2-amino-2-methyl-1-propanol, N-methylethanolamine, dimethylethanolamine, monoethanolamine, diethanolamine, triethanolamine, butylethanolamine, butyldiethanolamine, ammonia water, sodium hydroxide and potassium hydroxide, and has a mass fraction of 0.01-2%. And finally, the balance of the silver nanowire ink is a mixture of water and an alcohol solvent, wherein the mass of alcohol/the mass of water is (0.001-1): 1. the alcohol solvent is at least one of ethanol and isopropanol.
In one embodiment, in step S02, the carrier gas of the oxidizing gas is nitrogen, that is, nitrogen is used as the carrier gas, and the carrier gas contains a small amount of oxygen and/or hydrogen sulfide. Oxygen and hydrogen sulfide can be subjected to oxidation reaction on the surface of the silver nanowire. Accordingly, the silver nanowires showed that the silver metal compound formed by oxidation was Ag2O or Ag2S,Ag2o and Ag2S can inhibit the generation of surface plasmon resonance of silver nanowires, and Ag2O and Ag2S does not have metallic luster, so the reflection can be reduced, and the haze of the finally prepared silver nanowire film is obviously reduced. Therefore, the gas with oxidizing property introduced into the initial silver nano-wire solution is selected from at least one of oxygen and hydrogen sulfide.
And the silver nanowire solution after the oxidation is obtainedIn the liquid, the silver nanowires can realize surface oxidation to form an oxide layer (the component is silver metal compound, such as Ag)2O and/or Ag2S), in one embodiment, the thickness of the oxide layer on the surface of the silver nanowire is 1-20 nm. If the thickness of the oxide layer is too low, the haze reduction effect is not significant, and if the thickness of the oxide layer is too high, the bridging between the silver nanowires is affected, because of Ag2O or Ag2s is not conductive, so that the sheet resistance of the final silver nanowire film is increased. Therefore, silver nanowires within the above-mentioned range of oxide layer thickness work best.
In one embodiment, the concentration of the gas with oxidizability introduced into the initial silver nanowire solution is 0.1-100 mmol/L; in the concentration range, the oxidizing gas can be fully contacted with the silver nanowires in the primary silver nanowire solution for oxidation reaction, so that the haze of the transparent conductive film of the silver nanowires is effectively reduced.
specifically, the gas with the oxidizing property is oxygen, the concentration of the oxygen gas is 10-100mmol/L, and the pH value of the initial silver nanowire solution is 8-10 (through an alkaline pH regulator condition); therefore, in the oxygen concentration and the pH value range of the solution, the surface of the silver nanowire can be better oxidized, so that the haze of the silver nanowire film can be effectively reduced by 0.1-1.5%.
Or, the gas with the oxidizing property is hydrogen sulfide, the concentration of the hydrogen sulfide gas is 0.1-3mmol/L, the pH value of the silver nanowire solution is not limited too much, and the solution is neutral, so that the oxidation reaction can be carried out. Within the concentration range of the hydrogen sulfide gas, the haze of the silver nanowire film can be effectively reduced by 0.1-1.5%.
in one embodiment, a certain reaction condition may be selected for the oxidation reaction by introducing an oxidizing gas into the initial silver nanowire solution, and specifically, the flow rate of introducing the oxidizing gas is 50 to 500 ml/min; the temperature for carrying out oxidation reaction on the surface of the silver nanowire is 60-160 ℃; the time for oxidation reaction on the surface of the silver nanowire is 10-60 min. In the temperature and time range, the surface oxidation layer thickness of the silver nanowires can reach an optimal range. If it deviates from this range, there may be insufficient thickness of the oxide layer or excessive thickness of the oxide layer.
In S03, the oxidized silver nanowire solution may be coated on the substrate by a roll-to-roll coating method, specifically, two methods, i.e., a slit extrusion coating method and a micro gravure coating method, are included. The temperature for drying the oxidized silver nanowire solution coated on the substrate is 60-130 ℃; the time is 2-35 min. In this temperature and time range, the solvent in the silver nanowire solution can be better volatilized.
The invention is described in further detail with reference to a part of the test results, which are described in detail below with reference to specific examples.
Example 1
A preparation method of a silver nanowire film comprises the following steps:
S11, providing an initial silver nanowire solution; wherein, the pH is 10, the mass fraction of the silver nano-wire is 0.01 percent.
S12, introducing nitrogen containing oxygen into the initial silver nanowire solution, and carrying out oxidation reaction on the surface of the silver nanowire to obtain an oxidized silver nanowire solution; wherein the oxygen concentration is 10mmol/L, the flow rate is 500ml/min, the reaction temperature is 160 ℃, and the reaction time is 20 min.
s13, coating the oxidized silver nanowire solution on a PET film for drying treatment to obtain a silver nanowire film; wherein the drying temperature is 110 deg.C, and the drying time is 10 min.
Example 2
A preparation method of a silver nanowire film comprises the following steps:
S11, providing an initial silver nanowire solution; wherein, the pH value is 10, and the mass fraction of the silver nanowires is 0.08%.
S12, introducing nitrogen containing oxygen into the initial silver nanowire solution, and carrying out oxidation reaction on the surface of the silver nanowire to obtain an oxidized silver nanowire solution; wherein the oxygen concentration is 100mmol/L, the flow rate is 300ml/min, the reaction temperature is 130 ℃, and the reaction time is 60 min.
S13, coating the oxidized silver nanowire solution on a PET film for drying treatment to obtain a silver nanowire film; wherein the drying temperature is 130 deg.C, and the drying time is 5 min.
Example 3
A preparation method of a silver nanowire film comprises the following steps:
s11, providing an initial silver nanowire solution; wherein, the pH is 7, and the mass fraction of the silver nanowire is 0.13%.
S12, introducing nitrogen containing hydrogen sulfide into the initial silver nanowire solution, and carrying out oxidation reaction on the surface of the silver nanowire to obtain an oxidized silver nanowire solution; wherein the concentration of hydrogen sulfide is 3mmol/L, the flow rate is 50ml/min, the reaction temperature is 60 ℃, and the reaction time is 10 min.
S13, coating the oxidized silver nanowire solution on a PET film for drying treatment to obtain a silver nanowire film; wherein the drying temperature is 60 deg.C, and the drying time is 35 min.
Example 4
A preparation method of a silver nanowire film comprises the following steps:
S11, providing an initial silver nanowire solution; wherein, the pH is 7, and the mass fraction of the silver nanowire is 0.2%.
S12, introducing nitrogen containing hydrogen sulfide into the initial silver nanowire solution, and carrying out oxidation reaction on the surface of the silver nanowire to obtain an oxidized silver nanowire solution; wherein the concentration of hydrogen sulfide is 0.1mmol/L, the flow rate is 50ml/min, the reaction temperature is 100 ℃, and the reaction time is 20 min.
S13, coating the oxidized silver nanowire solution on a PET film for drying treatment to obtain a silver nanowire film; wherein the drying temperature is 100 deg.C, and the drying time is 15 min.
Comparative example
A preparation method of a silver nanowire film comprises the following steps:
e01: providing an initial silver nanowire solution; wherein the mass fraction of the silver nanowires is 0.13%.
e02: and coating the initial silver nanowire solution on a PET film for drying treatment to obtain the silver nanowire film. Wherein the temperature is 100 deg.C and the time is 15 min.
Performance testing
The silver nanowire films prepared in the above examples and comparative examples were subjected to sheet resistance and haze tests, which were as follows:
(1) Square resistance: the test was performed using a hand-held four-finger probe (model M3, suzhou crystal lattice electronics ltd) at 30 random points and averaged.
(2) Haze: the haze meter (model SGM-810, Shanghai apparatus electro-optical Shanghai apparatus electro-physical optical apparatus Co., Ltd.) automatically reads, randomly tests 10 points, and takes the average value.
The data are shown in table 1 below: from the data in table 1, it can be seen that: the haze of the silver nanowire film prepared by the embodiment of the invention is effectively reduced.
TABLE 1
the above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention are intended to be included within the scope of the present invention.
Claims (10)
1. the preparation method of the silver nanowire film is characterized by comprising the following steps:
Providing an initial silver nanowire solution;
Introducing gas with oxidability into the initial silver nanowire solution, and carrying out oxidation reaction on the surface of the silver nanowire to obtain an oxidized silver nanowire solution;
And coating the oxidized silver nanowire solution on a substrate for drying treatment to obtain the silver nanowire film.
2. The method for preparing a silver nanowire film as claimed in claim 1, wherein the carrier gas of the gas having the oxidizing property is nitrogen gas, and the flow rate is 50 to 500 ml/min; and/or the presence of a gas in the gas,
The gas having oxidizing property is at least one selected from oxygen and hydrogen sulfide.
3. The method for preparing the silver nanowire thin film as claimed in claim 2, wherein the oxidizing gas contains 10 to 100mmol/L of oxygen, and the initial silver nanowire solution has a pH of 8 to 10.
4. the method for preparing a silver nanowire thin film according to claim 2, wherein the oxidizing gas contains 0.1 to 5mmol/L of hydrogen sulfide.
5. The method for preparing a silver nanowire film according to claim 1, wherein the thickness of the oxide layer on the surface of the silver nanowire in the oxidized silver nanowire solution is 1 to 20 nm.
6. the method of preparing a silver nanowire film according to claim 1, wherein the mass fraction of the silver nanowires in the initial silver nanowire solution is 0.01% to 0.2%.
7. the method for preparing a silver nanowire film according to claim 1, wherein the temperature for performing the oxidation reaction on the surface of the silver nanowire is 60 to 160 ℃; and/or the presence of a gas in the gas,
The time for carrying out the oxidation reaction on the surface of the silver nanowire is 10-60 min.
8. The method for preparing a silver nanowire thin film as claimed in any one of claims 1 to 7, wherein the temperature of the drying process is 60 to 130 ℃; and/or the presence of a gas in the gas,
the drying time is 2-35 min.
9. The method for preparing a silver nanowire film as claimed in any one of claims 1 to 7, wherein the silver nanowire film is a transparent conductive film.
10. The method for preparing a silver nanowire film according to any one of claims 1 to 7, wherein the substrate is selected from any one of a PET film, a TAC film, a PEN film, a CPI film, a COP film, a PDMS film, and a glass film.
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