CN110634620B - Preparation method of silver nanowire conductive film - Google Patents
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Abstract
The invention belongs to the technical field of nano materials, and particularly relates to a preparation method of a silver nanowire conductive film. The preparation method comprises the following steps: providing a substrate; coating silver nanowire ink on the substrate to form an initial silver nanowire film; and mixing the initial silver nanowire film with a solution containing ammonium ions and hydroboron ions, and then drying to obtain the silver nanowire conductive film. According to the preparation method of the silver nanowire conductive film, PVP (polyvinyl pyrrolidone) on the surface of the silver nanowire is effectively removed by combining ammonium ions and hydroboron ions, so that the silver nanowire can be well lapped, and the conductivity of the silver nanowire conductive film is finally improved.
Description
Technical Field
The invention belongs to the technical field of nano materials, and particularly relates to a preparation method of a silver nanowire conductive film.
Background
Silver Nanowires (AgNWs) generally refer to one-dimensional Silver metal materials with micrometer-scale length and nanometer-scale diameter, and currently, Silver Nanowires are mainly synthesized by a polyol reduction method, which inevitably adopts polyvinylpyrrolidone (PVP) as a structure directing agent to enable the Silver Nanowires to grow along a single direction and provide spatial stability so as to prevent aggregation and precipitation of the Silver Nanowires. The PVP can obstruct the lap joint of the silver nanowires and influence the conductivity of the silver nanowires, so that the PVP needs to be removed, but the PVP contains rich carbonyl which can be used as a ligand to generate a chemical complexing effect with the surfaces of the silver nanowires, so that the PVP and the silver nanowires are tightly combined together.
It has been reported that borohydride-containing ions [ BH4 ] can be used]-The PVP on the surface of the silver nanowire is removed by the aqueous solution. The carbonyl and the silver nanowire are connected by Ag-O bonds, and the binding energy is 50.9kCal/mol, [ BH4]-The aqueous solution can generate a large amount of hydride ions, the binding energy of the hydride ions with Ag is 81.71kCal/mol and is far higher than that of an Ag-O bond, so that carbonyl groups can be replaced by hydride, and PVP can be shed from the surface of the silver nanowire. However, since at room temperatureThe Ag-O substitution speed of Ag-H bond is slow under the condition of normal pressure without catalyst, and [ BH4 ]]-Unstable in aqueous solution and will react with water to release H2Result in [ BH4]-The concentration dropped dramatically. Thus [ BH4]-The practical effect of the aqueous solution to remove the PVP on the surface of the silver nanowire is not ideal, and the aqueous solution cannot be used for practical production.
Therefore, the prior art is in need of improvement.
Disclosure of Invention
The invention aims to provide a preparation method of a silver nanowire conductive film, and aims to solve the technical problem that PVP removing effect on the surface of the existing silver nanowire is not ideal.
In order to achieve the purpose, the invention adopts the following technical scheme:
the invention provides a preparation method of a silver nanowire conductive film, which comprises the following steps:
providing a substrate;
coating silver nanowire ink on the substrate to form an initial silver nanowire film;
and mixing the initial silver nanowire film with a solution containing ammonium ions and hydroboron ions, and then drying to obtain the silver nanowire conductive film.
The preparation method of the silver nanowire conductive film provided by the invention comprises the steps of forming an initial silver nanowire film on a substrate by silver nanowire ink, mixing the initial silver nanowire film with a solution containing ammonium ions and boron hydride ions, wherein in the mixing process, the ammonium ions in the solution have a strong complexing effect with Ag on the surface of the silver nanowire, so that Ag-O bonds on the surface of the silver nanowire can be quickly destroyed, and then the surface of the silver nanowire and [ BH4 ] are mixed]-The PVP is separated from the surface of the silver nanowire by combining a more stable chemical state, and the ammonium ions play a role in catalyzing the solution in the process, so that the silver nanowire is better matched with [ BH4 ]]-Bound, and ammonium ions can increase the OH of the solution-And the concentration of the PVP is reduced, so that the hydrolysis of borohydride ions is inhibited, borohydride ions can be more remained in the solution, and the PVP on the surface of the silver nanowire is more effectively removed.Therefore, the preparation method of the silver nanowire conductive film effectively removes PVP on the surface of the silver nanowire by combining ammonium ions and borohydride ions, so that the silver nanowire is better lapped, the impedance is reduced, and the conductivity of the silver nanowire conductive film is finally improved.
Drawings
Fig. 1 is a schematic flow chart of a method for preparing a silver nanowire conductive 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.
It is to be understood that the terms "first," "second," and "third" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or implicit ly indicating a number of technical features being indicated. Thus, features defined as "first", "second", "third" may explicitly or implicitly include one or more of the features.
The embodiment of the invention provides a preparation method of a silver nanowire conductive film, which comprises the following steps of:
s01: providing a substrate;
s02: coating silver nanowire ink on the substrate to form an initial silver nanowire film;
s03: and mixing the initial silver nanowire film with a solution containing ammonium ions and hydroboron ions, and then drying to obtain the silver nanowire conductive film.
The preparation method of the silver nanowire conductive film provided by the invention comprises the steps of forming an initial silver nanowire film on a substrate by silver nanowire ink, mixing the initial silver nanowire film with a solution containing ammonium ions and boron hydride ions, wherein in the mixing process, the ammonium ions in the solution and Ag on the surface of the silver nanowire have a strong complexing effectThe Ag-O bond on the surface of the silver nanowire is quickly destroyed, and then the surface of the silver nanowire is further mixed with [ BH4 ]]-The PVP is separated from the surface of the silver nanowire by combining a more stable chemical state, and the ammonium ions play a role in catalyzing the solution in the process, so that the silver nanowire is better matched with [ BH4 ]]-Bound, and ammonium ions can increase the OH of the solution-And the concentration of the PVP is reduced, so that the hydrolysis of borohydride ions is inhibited, borohydride ions can be more remained in the solution, and the PVP on the surface of the silver nanowire is more effectively removed. Therefore, the preparation method of the silver nanowire conductive film effectively removes PVP on the surface of the silver nanowire by combining ammonium ions and borohydride ions, so that the silver nanowire is better lapped, the impedance is reduced, and the conductivity of the silver nanowire conductive film is finally improved.
It should be noted that, in the method for preparing the silver nanowire conductive film provided by the embodiment of the present invention, the silver nanowire surface of the initial silver nanowire film is usually partially oxidized to produce the non-conductive Ag2O, thereby increasing contact resistance between the silver nanowires. And the solution containing ammonium ions contains a certain amount of NH3，NH3Ag capable of being attached to surface of silver nanowire2O reacts to form water soluble Ag (NH)3)2 +Thereby removing Ag2And O, the effects of improving the lap joint of the silver nanowires and reducing the sheet resistance are achieved.
The silver nanowire conductive film prepared by the embodiment of the invention is a transparent conductive film. In the step S01, the substrate for coating is a flexible substrate, and specifically, the substrate is any one of a PET (Polyethylene Terephthalate) film, a TAC (Triacetyl Cellulose) film, a PEN (Polyethylene Naphthalate) film, a PDMS (Polydimethylsiloxane) film, a CPI (Colorless transparent Polyimide) film, a COP (cyclic Olefin copolymer) film, and a glass film.
In the step S02, the silver nanowires in the silver nanowire ink for coating may be synthesized by a polyol reduction method, PVP is bonded to a portion of the surfaces of the silver nanowires, and the PVP blocks the silver nanowires from being overlapped to affect the conductivity of the silver nanowires. In the silver nanowire ink, the diameter of the silver nanowire is 15-95nm, the length-diameter ratio is 500-2500, and the concentration of the silver nanowire is 0.01-0.2%. The silver nanowire ink can contain assistants such as a thickening agent and a wetting dispersant besides the silver nanowires, wherein the thickening agent can be hydroxypropyl methyl cellulose, and the mass fraction of the thickening agent is 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%. 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 may be at least one of ethanol and isopropanol. The coating method for coating the silver nanowire ink on the substrate is any one selected from slot coating, dimple coating, blade coating and roller coating.
In one embodiment, the step of coating the silver nanowire ink on the substrate to form the initial silver nanowire thin film may comprise: coating silver nanowire ink on a clean flexible transparent substrate, and then drying in an oven, specifically, drying in an oven at 50-130 ℃ for 2-40 min.
In the step S03, the initial silver nanowire film and the solution containing ammonium ions and borohydride ions are mixed, and the initial silver nanowire film and the ammonium ions and the borohydride ions are fully contacted and reacted under the solution condition.
In one embodiment, the step of mixing the initial silver nanowire film with a solution containing ammonium ions and borohydride ions comprises: firstly, placing the initial silver nanowire film in a solution containing ammonium ions for first soaking treatment, and then adding borohydride for second soaking treatment. The initial silver nanowire film is firstly placed in a solution containing ammonium ions to be subjected to first soaking treatment, which is a pretreatment process, and the process can beThe ammonium ions are firstly complexed with Ag on the surface of the silver nanowire to destroy Ag-O bonds, so that PVP is dropped out to be the subsequent silver nanowire and [ BH4 ]]-Preparation for binding, after addition of borohydride, [ BH4]-Combines with silver nano-wire into more stable chemical state, thereby effectively removing PVP. The borohydride added may be a solution of borohydride, or may be a solid borohydride, such as a solid borohydride, which may be stirred to dissolve. In the above process, the solution containing ammonium ions is at least one selected from the group consisting of ammonia water, an ammonium fluoride solution and an ammonium chloride solution, and preferably ammonia water; the borohydride is at least one selected from lithium borohydride, sodium borohydride and potassium borohydride.
The first soaking time is 5-20s, and specifically 12-50 s; the time of the second soaking treatment is 10-300s, and specifically can be 150-200 s. In the solution containing ammonium ions, the concentration of the ammonium ions is 0.5-5 mol/L; after the borohydride is added, the concentration of borohydride ions in the solution is 0.01-0.5 mol/L.
In one embodiment, the step of mixing the initial silver nanowire film with a solution containing ammonium ions and borohydride ions comprises: and placing the initial silver nanowire film in a mixed solution containing ammonium ions and boron hydride ions, and performing third soaking treatment. Because the ammonium ions play a role in catalyzing the solution, the initial silver nanowire film can be directly soaked in the mixed solution containing the ammonium ions and the boron hydride ions, and the surface of the silver nanowire and the [ BH4 ] can be catalyzed]-Combine to a more stable chemical state. In the process, the mixed solution containing the ammonium ions and the borohydride ions is a mixed solution in which an ammonium ion compound and borohydride are dissolved. Specifically, the ammonium ion compound is selected from at least one of amine monohydrate, ammonium fluoride and ammonium chloride; the borohydride is at least one selected from lithium borohydride, sodium borohydride and potassium borohydride.
The time of the third soaking treatment is 10-300 s; in the mixed solution containing ammonium ions and borohydride ions, the concentration of the ammonium ions is 0.5-5mol/L, and the concentration of the borohydride ions is 0.01-0.5 mol/L.
In the above two embodiments, too low concentration of ammonium ions is not favorable for stabilization of borohydride ions in solution, too high concentration of ammonium ions is strongly alkaline and volatile, which is not favorable for industrial production, so that the ammonium ions in the above concentration range have the best effect. The PVP is not easy to effectively remove due to too low concentration of the hydroboron ions, demulsification can be caused due to too high and unstable concentration of the hydroboron ions, and the nano silver wires are subjected to coagulation. The borohydride ions in the above concentration range are therefore most effective.
In the step S03, the temperature of the drying treatment is 60-160 ℃; the drying time is 2-40 min; the drying treatment was performed in a nitrogen atmosphere. Specifically, mixing the initial silver nanowire film with a solution containing ammonium ions and boron hydride ions, taking out the initial silver nanowire film after mixing, putting the initial silver nanowire film into a nitrogen oven at the temperature of 60-130 ℃ for drying for 2-40min, and removing the solvent to obtain the dried silver nanowire conductive film.
And finally, after the step of mixing the initial silver nanowire film with the solution containing ammonium ions and boron hydride ions, cleaning the initial silver nanowire film to remove substances on the surface of the silver nanowire film, specifically, cleaning the initial silver nanowire film with an ethanol solution. In an embodiment, the initial silver nanowire film after the mixing treatment is taken out, and then washed with an ethanol aqueous solution for multiple times, for example, washed 3 times in sequence, so as to remove the residual ammonium ions and boron hydride ions, or PVP and other substances, on the surface of the silver nanowire film.
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 conductive film comprises the following steps:
spin-coating the prepared nano silver wire ink on clean PET to obtain an AgNWs film (in which PVP is combined on the surface of a part of silver nano wires); and (3) drying, soaking in a mixed solution of 0.01mol/L sodium borohydride and 0.5mol/L ammonia water for 200s, washing with water and ethanol for 3 times, and drying in a nitrogen atmosphere to obtain the AgNWs film with a clean surface.
Example 2
A preparation method of a silver nanowire conductive film comprises the following steps:
spin-coating the prepared nano silver wire ink on clean PET to obtain an AgNWs film (in which PVP is combined on the surface of a part of silver nano wires); and (3) drying, soaking in a mixed solution of 0.3M sodium borohydride and 2M ammonia water for 30s, washing with water and ethanol for 3 times, and drying in a nitrogen atmosphere to obtain the AgNWs film with a clean surface.
Example 3
A preparation method of a silver nanowire conductive film comprises the following steps:
spin-coating the prepared nano silver wire ink on clean PET to obtain an AgNWs film (in which PVP is combined on the surface of a part of silver nano wires); and (3) drying, soaking in a mixed solution of 0.5M potassium borohydride and 5M ammonia water for 10s, washing with water and ethanol for 3 times, and drying in a nitrogen atmosphere to obtain the AgNWs film with a clean surface.
Example 4
A preparation method of a silver nanowire conductive film comprises the following steps:
spin-coating the prepared silver nanowire-coated ink on clean PET to obtain an AgNWs film (in which PVP is combined on the surface of a part of silver nanowires); and after drying, soaking the AgNWs film in 0.5mol/L ammonia water for 20s, adding sodium borohydride, stirring and dissolving to enable the concentration of borohydride ions to reach 0.01mol/L, after soaking the AgNWs film in the mixed solution for 300s, washing the AgNWs film with water and ethanol for 3 times, and drying the AgNWs film in a nitrogen oven at the temperature of 60-130 ℃ for 2-40min to obtain the AgNWs film with a clean surface.
Example 5
A preparation method of a silver nanowire conductive film comprises the following steps:
spin-coating the prepared silver nanowire-coated ink on clean PET to obtain an AgNWs film (in which PVP is combined on the surface of a part of silver nanowires); and after drying, soaking the AgNWs film in 2.5mol/L ammonia water for 12s, adding sodium borohydride, stirring and dissolving to enable the concentration of borohydride ions to reach 0.25mol/L, after soaking the AgNWs film in the mixed solution for 150s, washing the AgNWs film with water and ethanol for 3 times, and drying the AgNWs film in a nitrogen oven at the temperature of 60-130 ℃ for 2-40min to obtain the AgNWs film with a clean surface.
Example 6
A preparation method of a silver nanowire conductive film comprises the following steps:
spin-coating the prepared silver nanowire-coated ink on clean PET to obtain an AgNWs film (in which PVP is combined on the surface of a part of silver nanowires); and after drying, soaking in 5mol/L ammonia water for 15s, adding a potassium borohydride solid, stirring and dissolving to enable the concentration of borohydride ions to reach 0.5mol/L, after soaking the AgNWs film in the mixed solution for 30s, washing with water and ethanol for 3 times, and drying in a nitrogen oven at 60-130 ℃ for 2-40min to obtain the AgNWs film with a clean surface.
Comparative example 1
A preparation method of a silver nanowire conductive film comprises the following steps:
spin-coating the prepared nano silver wire ink on clean PET to obtain an AgNWs film (in which PVP is combined on the surface of a part of silver nano wires); drying, and soaking in 0.01M NaBH4And (3) in the solution for 200s, washing with water and ethanol for 3 times, and drying in a nitrogen atmosphere to obtain the AgNWs film with a clean surface.
Comparative example 2
A preparation method of a silver nanowire conductive film comprises the following steps:
spin-coating the prepared nano silver wire ink on clean PET to obtain an AgNWs film (in which PVP is combined on the surface of a part of silver nano wires); drying, and soaking in 0.3M NaBH4And (3) in the solution for 30s, washing with water and ethanol for 3 times, and drying in a nitrogen atmosphere to obtain the AgNWs film with a clean surface.
Comparative example 3
A preparation method of a silver nanowire conductive film comprises the following steps:
spin coating the prepared nano silver wire ink on clean PET to obtain AgNWs film (part of which isPVP is bonded to the surface of the silver nanowire); drying, and soaking in 0.5M KBH4And (3) in the solution for 10s, then washing with water and ethanol for 3 times, and drying in a nitrogen atmosphere to obtain the AgNWs film with a clean surface.
The substrates used in the above examples and comparative examples were PET. In the silver nanowire ink, the mass fraction of silver nanowires is 0.01%, the mass fraction of hydroxypropyl methyl cellulose is 0.2%, the mass fraction of DISPERBYK-180 is 0.01%, and the balance is a mixture of isopropanol and water (the mass ratio is 3: 7).
Performance testing
(1) Spin coating apparatus: beijing Saidekais electronic Limited responsibility company (model: KW-4A desktop spin coater).
(2) Square resistance: the test was performed with a hand-held four-finger probe (model M-3, Suzhou lattice electronics, Inc.), and 5 points were randomly tested and averaged.
(3) Sheet resistance change rate: r% ([ square resistance ])After treatment-square resistanceBefore treatmentSquare resistanceBefore treatment*100％。
The final data are shown in table 1 below:
TABLE 1
From the data in table 1 above, it can be seen that: the sheet resistance of the silver nanowire conductive film prepared by the embodiment of the invention is obviously reduced compared with that of a comparative example, so that the conductive performance of the silver nanowire conductive film is better.
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 (5)
1. The preparation method of the silver nanowire conductive film is characterized by comprising the following steps:
providing a substrate;
coating silver nanowire ink on the substrate to form an initial silver nanowire film;
mixing the initial silver nanowire film with a solution containing ammonium ions and hydroboron ions, and then drying to obtain a silver nanowire conductive film; the step of mixing treatment comprises: firstly, placing the initial silver nanowire film in a solution containing ammonium ions for first soaking treatment, and then adding borohydride for second soaking treatment, wherein the solution containing the ammonium ions is selected from ammonia water;
wherein the ammonium ions catalyze the bonding of the borohydride ions to the surfaces of the silver nanowires in the initial silver nanowire film, and the ammonium ions generate NH3Ag on the surface of the silver nanowire2O reacts to generate water-soluble Ag (NH)3)2 +。
2. The method for preparing a silver nanowire conductive film according to claim 1, wherein the borohydride is at least one selected from the group consisting of lithium borohydride, sodium borohydride and potassium borohydride.
3. The method for preparing a silver nanowire conductive film according to claim 1, wherein the first soaking treatment is performed for 5 to 20 seconds; and/or the presence of a gas in the gas,
the time of the second soaking treatment is 10-300 s; and/or the presence of a gas in the gas,
in the solution containing ammonium ions, the concentration of the ammonium ions is 0.5-5 mol/L; and/or the presence of a gas in the gas,
after the borohydride is added, the concentration of borohydride ions in the solution is 0.01-0.5 mol/L.
4. The method for preparing a silver nanowire conductive film according to any one of claims 1 to 3, wherein the temperature of the drying process is 60 to 160 ℃; and/or the presence of a gas in the gas,
the drying time is 2-40 min; and/or the presence of a gas in the gas,
the drying treatment is carried out in a nitrogen atmosphere; and/or the presence of a gas in the gas,
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.
5. The method of preparing a silver nanowire conductive film according to any one of claims 1 to 3, wherein the step of mixing the initial silver nanowire film with a solution containing ammonium ions and boron hydride ions further comprises a washing treatment with an ethanol solution.
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