CN111799034A - Preparation of polyethylene dioxythiophene-based nano silver wire transparent film - Google Patents
Preparation of polyethylene dioxythiophene-based nano silver wire transparent film Download PDFInfo
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- CN111799034A CN111799034A CN201910276541.XA CN201910276541A CN111799034A CN 111799034 A CN111799034 A CN 111799034A CN 201910276541 A CN201910276541 A CN 201910276541A CN 111799034 A CN111799034 A CN 111799034A
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- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 title claims abstract description 54
- 229920001609 Poly(3,4-ethylenedioxythiophene) Polymers 0.000 title claims abstract description 21
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 239000002042 Silver nanowire Substances 0.000 claims abstract description 20
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims abstract description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000000034 method Methods 0.000 claims abstract description 13
- 229920002799 BoPET Polymers 0.000 claims abstract description 11
- 239000008367 deionised water Substances 0.000 claims abstract description 10
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 10
- 239000000243 solution Substances 0.000 claims abstract description 8
- 229920001940 conductive polymer Polymers 0.000 claims abstract description 3
- 239000007864 aqueous solution Substances 0.000 claims abstract 3
- 239000003960 organic solvent Substances 0.000 claims abstract 2
- 229920005989 resin Polymers 0.000 claims abstract 2
- 239000011347 resin Substances 0.000 claims abstract 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 12
- 239000012528 membrane Substances 0.000 claims description 9
- 239000002244 precipitate Substances 0.000 claims description 8
- 239000007788 liquid Substances 0.000 claims description 5
- 239000000758 substrate Substances 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 4
- 239000000843 powder Substances 0.000 claims description 4
- 229910052709 silver Inorganic materials 0.000 claims description 4
- 239000004332 silver Substances 0.000 claims description 4
- 239000002904 solvent Substances 0.000 claims description 4
- 238000003756 stirring Methods 0.000 claims description 4
- 239000006228 supernatant Substances 0.000 claims description 4
- 238000003828 vacuum filtration Methods 0.000 claims description 4
- 238000007605 air drying Methods 0.000 claims description 3
- 238000007865 diluting Methods 0.000 claims description 3
- 238000001914 filtration Methods 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 239000002390 adhesive tape Substances 0.000 claims description 2
- 239000004372 Polyvinyl alcohol Substances 0.000 claims 8
- 229920002451 polyvinyl alcohol Polymers 0.000 claims 8
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims 6
- 239000000839 emulsion Substances 0.000 claims 4
- 239000004814 polyurethane Substances 0.000 claims 4
- 229920002635 polyurethane Polymers 0.000 claims 3
- 229920000139 polyethylene terephthalate Polymers 0.000 claims 2
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims 2
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims 2
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims 2
- 239000004925 Acrylic resin Substances 0.000 claims 1
- 229920000178 Acrylic resin Polymers 0.000 claims 1
- 229920000144 PEDOT:PSS Polymers 0.000 claims 1
- 229920003180 amino resin Polymers 0.000 claims 1
- 238000010438 heat treatment Methods 0.000 claims 1
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 claims 1
- 229910052753 mercury Inorganic materials 0.000 claims 1
- 229920000728 polyester Polymers 0.000 claims 1
- 238000000967 suction filtration Methods 0.000 claims 1
- 239000000463 material Substances 0.000 description 3
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 229910052738 indium Inorganic materials 0.000 description 2
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 description 2
- 239000010410 layer Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 239000000654 additive Substances 0.000 description 1
- 238000010923 batch production Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000004973 liquid crystal related substance Substances 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000009210 therapy by ultrasound Methods 0.000 description 1
- 238000002834 transmittance Methods 0.000 description 1
- 238000004383 yellowing Methods 0.000 description 1
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B13/00—Apparatus or processes specially adapted for manufacturing conductors or cables
- H01B13/0026—Apparatus for manufacturing conducting or semi-conducting layers, e.g. deposition of metal
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- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Manufacture Of Macromolecular Shaped Articles (AREA)
- Manufacturing Of Electric Cables (AREA)
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Abstract
The invention relates to a preparation method of a polyethylene dioxythiophene nano silver wire transparent film; according to the method, a water-soluble silver wire, an isopropanol-soluble silver wire and an ethanol-soluble silver wire are mixed with PEDOT under the same conditions according to the mass fraction: PSS solution, deionized water and isopropanol are mixed to form aqueous solution to improve the conductivity and the stability, and the ink comprises the following components in formula: 0.1% -8% of nano silver wire; 0.5 to 15 percent of water-based resin; 8 to 50 percent of organic solvent; a conductive polymer; 0.1% -8%; 30% -90.5% of deionized water; the content is 1.1-1.59%; and (3) respectively preparing AgNWs/MCE films, AgNWs/PET films and AgNWs/PVA films at the curing temperature of 120-145 ℃ on the basis of the MCE films.
Description
Technical Field
The invention relates to the technical field of preparation of more than two metal molecular elements deposited on a substrate in a liquid-solid state, in particular to preparation of a polyethylene dioxythiophene nano silver wire transparent film, belonging to a coated ion crystal nucleus synthesis technology.
Background
In recent years, with the widespread use of liquid crystal display screens and touch screens and the introduction of wearable and bendable screen concepts, the conventional ITO material has gradually failed to meet the market demand. Quantitatively, the world indium resource was surplus before 2009, but with the rapid expansion of the screen market after 2009, world indium has already seen a phenomenon of short supply and demand. In terms of performance, ITO has excellent light transmittance and conductivity, but as an oxide, ITO has problems of high brittleness, easy yellowing, and the like, and is difficult to apply to a flexible screen. On this basis, many novel transparent conductive materials have been reported, wherein the silver nanowires have been noticed by researchers in the field since being discovered. The nano silver wire has an absorption peak at about 380nm, belongs to an ultraviolet region, and basically has no absorption in a visible light range (400 nm-780 nm), so the nano silver wire is basically transparent, and simultaneously, the silver is the metal with the best conductivity. The high transparency and the good conductivity provide guarantee for the silver nanowires to become a new generation of transparent conductive film materials.
Although the nano silver wire is also reported as a transparent conductive film material, most of the nano silver wire is researched in a laboratory, is complex to operate, has high cost, is difficult to industrialize and meets the market.
Disclosure of Invention
In view of the above, the invention provides a preparation method of a polyethylene dioxythiophene-based nano silver wire transparent film; in order to realize the aim, the invention discloses a preparation method of a polyethylene dioxythiophene nano silver wire transparent film; which comprises the following steps:
s1, preparing a formula of nano transparent conductive silver wire powder and a solvent assistant;
s2, diluting, stirring, and ultrasonically dispersing for 30 min;
s3, centrifuging for 15min at the speed of 6000rmp, filtering out supernatant, dispersing the precipitate in a centrifugal tube by using a certain amount of ethanol, then repeatedly centrifuging for 25min at the speed of 6000rmp, finally dissolving the centrifuged precipitate in isopropanol, and quickly shaking to uniformly disperse silver wires;
s4, adding the mixture into deionized water, then carrying out vacuum filtration by adopting an MCE filter membrane, and fixing and air-drying the membrane;
s5, preparing transparent flexible nano silver wire films on different substrates by taking the MCE film as a basic film respectively, wherein the method comprises the following steps: AgNWs/MCE film, AgNWs/PET film, AgNWs/PVA film.
As a further improvement of the invention, the formula of the nano transparent conductive silver wire powder and the solvent assistant is prepared.
As a further improvement of the invention, the dispersion is uniformly dispersed by stirring after dilution and ultrasonic treatment for 30 min.
As a further improvement of the invention, the silver wire is centrifuged at the speed of 6000rmp for 15min, the supernatant is filtered, a certain amount of ethanol is used for dispersing the precipitate in a centrifuge tube, then the centrifugation at the speed of 6000rmp is repeated for 25min, and finally the centrifuged precipitate is dissolved in isopropanol and is quickly shaken to uniformly disperse the silver wire.
As a further improvement of the invention, the membrane is added into deionized water, then MCE filter membrane vacuum filtration is adopted, and the membrane is fixed and air-dried.
As a further improvement of the invention: the method for preparing the transparent flexible nano silver wire film on different substrates by taking the MCE film as a basic film comprises the following steps: AgNWs/MCE film, AgNWs/PET film, AgNWs/PVA film.
Compared with the prior art, the invention has the beneficial effects that: the synthesis method of the nano silver wire in the glycol solution, the formula research of the conductive ink formed by mixing the nano silver wire, the conductive polymer and some additives, and the coating method of the transparent conductive film are provided. The method is simple to operate and low in cost, aims to meet the rail of enterprises, and realizes batch production through a roll-to-roll coating mode. Under the combined action of solution volatilization and surface tension, the nano silver wires move towards the liquid surface and stay on the liquid surface, and as the concentration of the nano silver wires on the liquid surface increases, the nano silver wires are mutually extruded, and a layer of compact and orderly arranged film is gradually formed on the liquid surface. Then, the method of repeated stripping by the adhesive tape obtains a nearly single-layer and orderly arranged thin layer of nano silver wires.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments described in the present invention, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts.
Fig. 1 is a schematic flow chart of a method for preparing a specific embodiment of a polyethylene dioxythiophene-based silver nanowire transparent film according to the present invention.
Detailed Description
The invention discloses a preparation method of a polyethylene dioxythiophene nano silver wire transparent film, which comprises the following steps:
s1, preparing a formula of nano transparent conductive silver wire powder and a solvent assistant;
s2, diluting, stirring, and ultrasonically dispersing for 30 min;
s3, centrifuging for 15min at the speed of 6000rmp, filtering out supernatant, dispersing the precipitate in a centrifugal tube by using a certain amount of ethanol, then repeatedly centrifuging for 25min at the speed of 6000rmp, finally dissolving the centrifuged precipitate in isopropanol, and quickly shaking to uniformly disperse silver wires;
s4, adding the mixture into deionized water, then carrying out vacuum filtration by adopting an MCE filter membrane, and fixing and air-drying the membrane;
s5, preparing transparent flexible nano silver wire films on different substrates by taking the MCE film as a basic film respectively, wherein the method comprises the following steps: AgNWs/MCE film, AgNWs/PET film, AgNWs/PVA film.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein. Any reference sign in a claim should not be construed as limiting the claim concerned.
Furthermore, it should be understood that although the present description refers to embodiments, not every embodiment may contain only a single embodiment, and such description is for clarity only, and those skilled in the art will be able to make the description as a whole, and the embodiments may be appropriately combined to form other embodiments as will be apparent to those skilled in the art.
Claims (9)
1. The preparation method of the polyethylene dioxythiophene nano silver wire transparent film of claim 1, characterized in that the preparation method comprises the following steps:
s1, preparing a formula of nano transparent conductive silver wire powder and a solvent assistant;
s2, diluting, stirring, and ultrasonically dispersing for 30 min;
s3, centrifuging for 15min at the speed of 6000rmp, filtering out supernatant, dispersing the precipitate in a centrifugal tube by using a certain amount of ethanol, then repeatedly centrifuging for 25min at the speed of 6000rmp, finally dissolving the centrifuged precipitate in isopropanol, and quickly shaking to uniformly disperse silver wires;
s4, adding the mixture into deionized water, then carrying out vacuum filtration by adopting an MCE filter membrane, and fixing and air-drying the membrane;
s5, preparing transparent flexible nano silver wire films on different substrates by taking the MCE film as a basic film respectively, wherein the method comprises the following steps: AgNWs/MCE film, AgNWs/PET film, AgNWs/PVA film.
2. The preparation method of the transparent film of poly (ethylenedioxythiophene) nano-silver wire according to claim 1, wherein the preparation method comprises the following steps, and is characterized in that in step S1, water-soluble silver wire, isopropanol-soluble silver wire, ethanol-soluble silver wire and eighteen mega ohm mercury wire are mixed according to mass fraction ratio, and PEDOT under the same conditions: and the PSS solution, deionized water and isopropanol are mixed to form an aqueous solution.
3. The method for preparing a transparent film of poly (ethylenedioxythiophene) nano-silver wire according to claim 1, wherein in step S1, PEDOT under the same conditions: and (3) mixing the PSS solution, deionized water and isopropanol to form an aqueous solution, wherein when PEDoT: PSS + VDI): the Vxpa ratio is more than 1: 2 do not agglomerate.
4. The preparation method of the transparent film of poly (ethylenedioxythiophene) nano-silver wire as claimed in claim 1, wherein when the content of the nano-silver wire of step S1 is 2 wt%, the content of N nano-silver wire (10 mg.ml "1): N/PEDOT: (ii) Pss (2 wt%) is 1: o.5, l: 1. 1: 1.5, l: 2. 1: 2.5 ratio.
5. The method for preparing a transparent film of poly (ethylenedioxythiophene) nano-silver wires according to claim 1, wherein the ink comprises the following components in the formula of step S1: 0.1% -8% of nano silver wire; 05 to 15 percent of water-based resin; 8 to 50 percent of organic solvent; a conductive polymer; 0. 1% -8%; 30% -90.5% of deionized water; the content is 1.1-1.59%; the curing temperature is 120-145 ℃; the molecular weight of PVP (polyvinylpyrrolidone) is 50000-60000.
6. Preparing the transparent film of the polyethylene dioxythiophene nano silver wire according to claim 1; the method is characterized in that in the step S5, a layer of adhesive tape is pasted on the back of the MCE film, then the MCE film is steamed for 5min by acetone steam at 50-60 ℃ until the MCE film is completely transparent, the MCE film is taken out and placed for a few minutes, and the MCE film is dried and solidified to form the nano silver wire MCE film.
7. Preparing the transparent film of the polyethylene dioxythiophene nano silver wire according to claim 1; the method is characterized in that in the step S5, the PET film is cut, the PET film is washed for 3 times by ethanol and deionized water respectively, then the PET film is dried in an oven, the front surface of the MCE film after suction filtration is pasted on the PET, then the PET film is heated by a hot press at 80 ℃, the pressure is 0.5MPa15-25min, the MCE film is dried by acetone steam at 60 ℃ for 5min until the MCE is completely transparent, and then the MCE film is soaked in acetone liquid for 15min to completely dissolve the MCE.
8. Preparing a transparent film of polyethylene dioxythiophene nano silver wires according to claim 1; the method is characterized in that in the step S5, a proper amount of polyvinyl alcohol (PVA) is added into water with the temperature of 20-25 ℃, the PVA is heated and stirred by adopting water bath with the temperature of 80-100 ℃ after being stirred and expanded to be completely dissolved, the mixture is kept stand for 5-15min until bubbles are dispersed to obtain PVA solution, the PVA solution is coated on AgNWs/PET film (1000 rpm, 20S), then the AgNWs/PET film is placed on a heating plate with the temperature of 70-90 ℃ for 10min, the PVA film is dried and solidified, and the PVA film is peeled off from the PET.
9. The preparation method of the polyethylene dioxythiophene nano silver wire transparent film according to claim 1, wherein the step S5 is performed before film preparation: mixing polyurethane emulsion (PU), acrylic resin (PAA), amino resin (PA) and polyester emulsion; preferably, the adhesion is significantly improved by adding the polyurethane emulsion to the polyurethane emulsion ink, but the dry film needs to be washed with ethanol.
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| CN201910276541.XA CN111799034A (en) | 2019-04-08 | 2019-04-08 | Preparation of polyethylene dioxythiophene-based nano silver wire transparent film |
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| CN201910276541.XA CN111799034A (en) | 2019-04-08 | 2019-04-08 | Preparation of polyethylene dioxythiophene-based nano silver wire transparent film |
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