CN104861776A - Anti-settling and self-leveling silver nanowire conductive printing ink and method for preparing transparent conducting thin film by using same - Google Patents
Anti-settling and self-leveling silver nanowire conductive printing ink and method for preparing transparent conducting thin film by using same Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D11/00—Inks
- C09D11/02—Printing inks
- C09D11/10—Printing inks based on artificial resins
- C09D11/102—Printing inks based on artificial resins containing macromolecular compounds obtained by reactions other than those only involving unsaturated carbon-to-carbon bonds
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D11/00—Inks
- C09D11/02—Printing inks
- C09D11/03—Printing inks characterised by features other than the chemical nature of the binder
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- 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
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Abstract
The invention discloses an anti-settling and self-leveling silver nanowire conductive printing ink which is composed of the following components by weight percent: 0.1 to 5 percent of silver nanowire, 1 to 10 percent of water-base resin, 0.1 to 5 percent of conductive macromolecule, 10 to 45 percent of an organic solvent and 35 to 88.5 percent of deionized water. The invention further provides a method for preparing a transparent conducting thin film by using the anti-settling and self-leveling silver nanowire conductive printing ink. The method comprises the following steps: coating a PET transparent substrate with the silver nanowire conductive printing ink, drying and curing, so as to obtain the transparent conducting thin film. The transparent conducting thin film prepared is 50 to 100 Ohm/sq in surface electrical resistivity, 88.5 to 90.1 percent in light transmittance, and 1.1 to 1.5 percent in haze. Moreover, the printing ink is simple in components, low in cost and suitable for large scale production.
Description
Technical field
The invention belongs to the preparing technical field of electrically conductive ink and conductive film.
Background technology
Current touch-control display electronic product mainly designs based on tin indium oxide semiconductor material (ITO), but this technology is but faced with indium scarcity of resources, the course of processing is complicated, energy consumption is high, preservation is difficult, easily the problems such as yellow occur, especially ITO is as a kind of oxide compound, its fragility is large, and snappiness difference is difficult to the demand of satisfied touch-control technique of display of new generation to the aspect such as flexibility, bendable folding endurance of product.Novel transparent conductive film based on nano-silver thread electrically conductive ink then shows superior performance as a class substitute technology, especially it has good electroconductibility, snappiness, light transmission, and silver reserves on earth will enrich relative to indium, tooling cost is low, energy consumption is little, pollution is few.It is trend of the times that the nano-silver thread transparent conductive film therefore with high transmittance, extremely strong electroconductibility and the advantage such as flexible replaces ito thin film.
The current transparent conductive film based on nano-silver thread and its ink have multinomial patent application, but common complete processing more complicated, through a few step transfer printing or the result repeatedly needed for the final realization of coating process ability.Or in ink formulation process, introduce the auxiliary agents such as a large amount of macromolecule resin, tensio-active agent, flow agent, anti-settling agent and dispersion agent.The introducing of this multiple auxiliary agent not only makes ink formulation become complicated, and to a great extent the menu cost adding ink.The present invention chooses optimized formula, only in nano-silver thread stoste, adds minority component, just can prepare transparent conductive film easily and the film obtained is reached even to surmount existing data target.
Summary of the invention
A first aspect of the present invention provides a kind of nano-silver thread electrically conductive ink with anti-settling and Self-leveling performance, and it is made up of nano-silver thread, water-base resin, conducting polymer, organic solvent and deionized water, and its weight consists of:
Nano-silver thread 0.1% ~ 5%;
Water-base resin 1% ~ 10%;
Conducting polymer 0.1% ~ 5%;
Organic solvent 10% ~ 45%;
Deionized water 35% ~ 88.5%.
The weight of wherein said nano-silver thread refers to the weight of this nano-silver thread itself, does not comprise the weight of solvent in nano-silver thread suspension or suspension medium.
In preferred embodiments, described nano-silver thread length is 5 ~ 60 μm, and diameter is 20 ~ 60nm.
In preferred embodiments, described water-base resin is waterborne polyurethane resin.
In preferred embodiments, conducting polymer is poly-3,4-ethylene dioxythiophene: poly styrene sulfonate (being abbreviated as PEDOT:PSS).
In preferred embodiments, described organic solvent is selected from one or more in methyl alcohol, ethanol, Virahol, dimethyl sulfoxide (DMSO), tetrahydrofuran (THF), N,N-dimethylacetamide.
A second aspect of the present invention provides a kind of preparation method of transparent conductive film, and it comprises the following steps:
A. the nano-silver thread electrically conductive ink with anti-settling and Self-leveling performance as shown in first aspect present invention is prepared;
B. described nano-silver thread electrically conductive ink is applied to PET transparent substrates, baking and curing by line rod rolling process, obtains transparent conductive film.
In preferred embodiments, the temperature of described baking and curing is 110 ~ 130 DEG C, and the time is 1 ~ 5 minute.
The concrete steps of method of the present invention are: first at room temperature the nano-silver thread of corresponding amount, water-base resin, organic solvent, conducting polymer and deionized water are added to beaker, and with stirring, make it mix completely.Deployed droplets of ink is added in PET base, excellent with certain speed roller coating by line subsequently, obtain electrically conductive ink wet film.Wet film is placed in vacuum drying oven, treats the deionized water in wet film, organic solvent volatilizees completely, take out PET and obtain dry film, i.e. above-mentioned transparent conductive film.
Because nano-silver thread surface is coated by polyvinylpyrrolidone (PVP), make produce a large amount of contact resistances between overlap joint process nano-silver thread, therefore in order to reduce contact resistance, introduce conducting polymer in ink and gather 3,4-ethylene dioxythiophene: poly styrene sulfonate (PEDOT:PSS).Wherein gather 3, sulphur in 4-ethylenedioxy thiophene (PEDOT) in thiphene ring can pass through chemical bonds with the silver on nano-silver thread, and poly-3, π-pi-conjugated the structure of 4-ethylenedioxy thiophene (PEDOT) can conduction electron, thus to a great extent reduce contact resistance, improve the electroconductibility of diaphragm.Poly styrene sulfonate (PSS) and poly-3,4-ethylene dioxythiophene (PEDOT) combine and improve that it is water-soluble.
The effect of waterborne polyurethane resin is the binding property improving nano-silver thread and substrate PET, prevents nano-silver thread from coming off, obtains reliable nano-silver thread film.
Thickness and the planeness of nano-silver thread conductive layer effectively can be controlled by the coating method of line rod roller coating.
Compared with prior art, the present invention has the following advantages and beneficial effect:
Electrically conductive ink is water color ink, and unharmful substance volatilizees, and has no irritating odor, asepsis environment-protecting.
Electrically conductive ink composition is simple, is not adding complicated additive, as: under the condition of the auxiliary agents such as flow agent, anti-settling agent, tensio-active agent, still there is self-leveling and anti-settling performance, and still can obtain excellent electroconductibility and light transmission.
Due to adding of conducting polymer, greatly reducing the consumption of silver-colored line, e.g., under the silver content of only 0.17wt%, the transparent conductive film that surface resistivity is 100ohm/sq can be obtained.
Waterborne polyurethane resin can make nano-silver thread firmly adhere in PET base, there will not be the phenomenon that nano-silver thread comes off.
Transparent conductive film take PET as substrate, can arbitrarily bend, distortion, meets the requirement of following flexible screen completely.
For the above and other object of the present invention, feature and advantage can be become apparent, cited below particularly go out preferred embodiment, and coordinate institute's accompanying drawings, be described in detail below.
Accompanying drawing explanation
Fig. 1 is that in the embodiment of the present invention 1, diameter is scanning electron microscope (SEM) photo of transparent conductive film prepared by 40nm silver line.
Fig. 2 is that in the embodiment of the present invention 1, diameter is 40nm silver line sweep electron microscope (SEM) photo.
Embodiment
Below in conjunction with embodiment, the present invention is described in further detail, but embodiments of the present invention are not limited thereto.
Embodiment 1
(1) allotment of nano-silver thread electrically conductive ink:
Deionized water 500g is added in the 1000mL there-necked flask of agitator, and then add waterborne polyurethane resin 10g, (wherein PEDOT:PSS massfraction is 1wt% to PEDOT:PSS solution 200g, solvent is water: Virahol 1:1), nano-silver thread aqueous isopropanol 150g (nano-silver thread strength of solution is 10mg/ml), nano-silver thread mean diameter 40nm, mean length 40 μm, length-to-diameter ratio is about 1000.Stir 30min, namely obtain nano-silver thread electrically conductive ink after mixing, in obtained nano-silver thread electrically conductive ink, nano-silver thread concentration is 0.17wt%.
(2) transparent conductive film and performance test is prepared:
Take PET as transparent flexible base material, himself transmittance is 92.1%, and thickness is 100 μm.The above-mentioned nano-silver thread electrically conductive ink prepared evenly is coated on PET in the mode of line rod roller coating, its center line interrod spacing is 15 μm, roller coating speed is 80cm/min, substrate surface forms the uniform wet film of one deck, at the dry 3min of 130 DEG C of vacuum drying ovens, treat that deionized water in wet film and organic solvent volatilize completely, take out the PET dry film with nano-silver thread network, i.e. described transparent conductive film.Four-point probe is adopted to measure the sheet resistance of gained film, the transmittance of the prepared film of photoelectricity haze meter test and mist degree.Its preparation-obtained transparent conductive film transmittance is 89.9 ± 0.1%, and sheet resistance is 100 ± 10 Ω/, and mist degree is 1.3%.
Fig. 1 is that in the embodiment of the present invention 1, diameter is scanning electron microscope (SEM) photo of transparent conductive film prepared by 40nm silver line, and display nano-silver thread is coated by conducting polymer.
Fig. 2 is that in the embodiment of the present invention 1, diameter is 40nm silver line sweep electron microscope (SEM) photo, and showing its diameter is 20 ~ 60nm, and length is 5 ~ 60 μm.
Table 1 is each component concentration and property indices.
Embodiment 2
(1) allotment of nano-silver thread electrically conductive ink:
Deionized water 350g is added in the 1000mL there-necked flask of agitator, and then add waterborne polyurethane resin 20g, (wherein PEDOT:PSS massfraction is 2wt% to PEDOT:PSS solution 200g, solvent is water: Virahol 1:1), nano-silver thread aqueous isopropanol 300g (nano-silver thread strength of solution is 10mg/ml), nano-silver thread mean diameter 40nm, mean length 40 μm, length-to-diameter ratio is about 1000.Stir 30min, namely obtain nano-silver thread electrically conductive ink after mixing, in obtained nano-silver thread electrically conductive ink, nano-silver thread concentration is 0.34wt%.
(2) transparent conductive film and performance test is prepared:
Take PET as transparent flexible base material, himself transmittance is 92.1%, and thickness is 100 μm.The above-mentioned nano-silver thread electrically conductive ink prepared evenly is coated on PET in the mode of line rod roller coating, its center line interrod spacing is 15 μm, roller coating speed is 80cm/min, substrate surface forms the uniform wet film of one deck, at the dry 3min of 130 DEG C of vacuum drying ovens, treat that deionized water in wet film and organic solvent volatilize completely, take out the PET dry film with nano-silver thread network, i.e. described transparent conductive film.Four-point probe is adopted to measure the sheet resistance of gained film, the transmittance of the prepared film of photoelectricity haze meter test and mist degree.Its preparation-obtained transparent conductive film transmittance is 88.1 ± 0.1%, and sheet resistance is 50 ± 5 Ω/, and mist degree is 1.5%.Table 1 is each component concentration and property indices.
Comparative example 1
(1) allotment of nano-silver thread electrically conductive ink:
Deionized water 500g is added in the 1000mL there-necked flask of agitator, (wherein PEDOT:PSS massfraction is 1wt% to PEDOT:PSS solution 200g, solvent is water: Virahol 1:1), nano-silver thread aqueous isopropanol 150g (nano-silver thread strength of solution is 10mg/ml), nano-silver thread mean diameter 40nm, mean length 40 μm, length-to-diameter ratio is about 1000.Stir 30min, namely obtain nano-silver thread electrically conductive ink after mixing, in obtained nano-silver thread electrically conductive ink, nano-silver thread concentration is 0.18wt%.
(2) transparent conductive film and performance test is prepared:
Take PET as transparent flexible base material, himself transmittance is 92.1%, and thickness is 100 μm.The above-mentioned nano-silver thread electrically conductive ink prepared evenly is coated on PET in the mode of line rod roller coating, its center line interrod spacing is 15 μm, roller coating speed is 80cm/min, substrate surface forms the uniform wet film of one deck, at the dry 3min of 130 DEG C of vacuum drying ovens, treat that deionized water in wet film and organic solvent volatilize completely, take out the PET dry film with nano-silver thread network, i.e. described transparent conductive film.Four-point probe is adopted to measure the sheet resistance of gained film, the transmittance of the prepared film of photoelectricity haze meter test and mist degree.Its preparation-obtained transparent conductive film transmittance is 89.9 ± 0.1%, and sheet resistance is 100 ± 10 Ω/, and mist degree is 1.3%.Table 1 is each component concentration and property indices.
Comparative example 2
(1) allotment of nano-silver thread electrically conductive ink:
Deionized water 500g is added in the 1000mL there-necked flask of agitator, Virahol 100g, and then add aqueous polyurethane 10g, nano-silver thread aqueous isopropanol 150g (nano-silver thread strength of solution is 10mg/ml), nano-silver thread mean diameter 40nm, mean length 40 μm, length-to-diameter ratio is about 1000.Stir 30min, namely obtain nano-silver thread electrically conductive ink after mixing, in obtained nano-silver thread electrically conductive ink, nano-silver thread concentration is 0.17wt%.
(2) transparent conductive film and performance test is prepared:
Take PET as transparent flexible base material, himself transmittance is 92.1%, and thickness is 100 μm.The above-mentioned nano-silver thread electrically conductive ink prepared evenly is coated on PET in the mode of line rod roller coating, its center line interrod spacing is 15 μm, roller coating speed is 80cm/min, substrate surface forms the uniform wet film of one deck, at the dry 3min of 130 DEG C of vacuum drying ovens, treat that deionized water in wet film and organic solvent volatilize completely, take out the PET dry film with nano-silver thread network, i.e. described transparent conductive film.Four-point probe is adopted to measure the sheet resistance of gained film, the transmittance of the prepared film of photoelectricity haze meter test and mist degree.Its preparation-obtained transparent conductive film transmittance is 89.9 ± 0.1%, and sheet resistance is greater than 3000 Ω/, and mist degree is 1.4%.Table 1 is each component concentration and property indices.
Comparative example 3
(1) allotment of nano-silver thread electrically conductive ink:
Deionized water 600g is added in the 1000mL there-necked flask of agitator, Virahol 100, nano-silver thread aqueous isopropanol 150g (nano-silver thread strength of solution is 10mg/ml), nano-silver thread mean diameter 40nm, mean length 40 μm, length-to-diameter ratio is about 1000.Stir 30min, namely obtain nano-silver thread electrically conductive ink after mixing, in obtained nano-silver thread electrically conductive ink, nano-silver thread concentration is 0.17wt%.
(2) transparent conductive film and performance test is prepared:
Take PET as transparent flexible base material, himself transmittance is 92.1%, and thickness is 100 μm.The above-mentioned nano-silver thread electrically conductive ink prepared evenly is coated on PET in the mode of line rod roller coating, its center line interrod spacing is 15 μm, roller coating speed is 80cm/min, substrate surface forms the uniform wet film of one deck, at the dry 3min of 130 DEG C of vacuum drying ovens, treat that deionized water in wet film and organic solvent volatilize completely, take out the PET dry film with nano-silver thread network, i.e. described transparent conductive film.Four-point probe is adopted to measure the sheet resistance of gained film, the transmittance of the prepared film of photoelectricity haze meter test and mist degree.Its preparation-obtained transparent conductive film transmittance is 89.8 ± 0.1%, and sheet resistance is for being greater than 3000 Ω/, and mist degree is 1.3%.Table 1 is each component concentration and property indices.
Table 1:
From table 1, add waterborne polyurethane resin and significantly can improve the tack of ink on PET, add poly-3,4-ethylene dioxythiophene: poly styrene sulfonate (PEDOT:PSS) can promote the electroconductibility of PET film.
Uniformity test:
Comparative example 4
The transparent conductive film that size is 10cm*10cm is prepared according to the method for embodiment 1 in application publication number CN 103627255 A " a kind of Nano silver conductive ink and the conductive film adopting this ink to prepare ", and on this transparent conductive film, randomly draw 140 points, test the sheet resistance of these 140 points, calculate its mean and variance.Simultaneously under equivalent environment, prepare according to the method in the embodiment of the present invention 1 transparent conductive film that size is 10cm*10cm, carry out aforesaid operations, result is as table 2:
Table 2:
Embodiment is numbered | Mean value | Variance | Maximum value | Minimum value |
Comparative example 4 | 99.25ohm/sq | 7.07ohm/sq | 108.5ohm/sq | 93.1ohm/sq |
Embodiment 1 | 99.79ohm/sq | 3.77ohm/sq | 105.1ohm/sq | 93.5ohm/sq |
Be evenly distributed by table 2 this membrane resistance visible, i.e. silver-colored line uniform content under per surface.This is beyond expectation, because do not use dispersion agent and flow agent in nano-silver thread electrically conductive ink of the present invention, can also realize uniform distribution of resistance in comparative example 4, estimable.
Comparative example 5
According to the method allotment nano-silver thread electrically conductive ink of embodiment 1 in application publication number CN 103627255 A " a kind of Nano silver conductive ink and the conductive film adopting this ink to prepare ", static placement 10 days, 15 days, 20 days, 25 days and 30 days, observes its sedimentation situation.Mix electrically conductive ink according to nano-silver thread electrically conductive ink concocting method in the embodiment of the present invention 1 simultaneously, under similarity condition, observe its sedimentation situation.Obtain result as shown in table 3:
Table 3:
Project | 10 days | 15 days | 20 days | 25 days | 30 days | 60 days |
Comparative example 5 | Evenly | Evenly | Evenly | There is sedimentation | Sediment increases | Severe delamination |
Embodiment 1 | Evenly | Evenly | Evenly | There is sedimentation | Sediment increases | Layering slightly |
From table 3, the present invention still can reach and surmount in comparative example 5 the anti-settling effect adding anti-settling agent (dibutyl phthalate) under the prerequisite not adding any anti-settling agent.This also illustrates the superiority of nano-silver thread electrically conductive ink of the present invention on formula.
Claims (7)
1. have a nano-silver thread electrically conductive ink for anti-settling and Self-leveling performance, it is made up of nano-silver thread, water-base resin, conducting polymer, organic solvent and deionized water, and its weight consists of:
Nano-silver thread 0.1% ~ 5%;
Water-base resin 1% ~ 10%;
Conducting polymer 0.1% ~ 5%;
Organic solvent 10% ~ 45%;
Deionized water 35% ~ 88.5%.
2. method according to claim 1, wherein said nano-silver thread length is 5 ~ 60 μm, and diameter is 20 ~ 60nm.
3. method according to claim 1, wherein said water-base resin is waterborne polyurethane resin.
4. method according to claim 1, wherein said conducting polymer is poly-3,4-ethylene dioxythiophene: poly styrene sulfonate, it is abbreviated as PEDOT:PSS.
5. method according to claim 1, wherein said organic solvent be selected from methyl alcohol, ethanol, Virahol, dimethyl sulfoxide (DMSO), tetrahydrofuran (THF), N,N-dimethylacetamide one or more.
6. a preparation method for transparent conductive film, comprises the following steps:
A. the nano-silver thread electrically conductive ink as claimed in claim 1 with anti-settling and Self-leveling performance is prepared;
B. described nano-silver thread electrically conductive ink is applied to PET transparent substrates, baking and curing by line rod rolling process, obtains transparent conductive film.
7. method according to claim 6, the temperature of wherein said baking and curing is 110 ~ 130 DEG C, and the time is 1 ~ 5 minute.
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CN105273471A (en) * | 2015-12-07 | 2016-01-27 | 苏州艾达仕电子科技有限公司 | Water-soluble nano-silver conductive coating |
CN105679394A (en) * | 2016-01-27 | 2016-06-15 | 广州中国科学院先进技术研究所 | UV conductive paste and method for printing silver nanowire flexible transparent conductive film from same |
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CN105679394A (en) * | 2016-01-27 | 2016-06-15 | 广州中国科学院先进技术研究所 | UV conductive paste and method for printing silver nanowire flexible transparent conductive film from same |
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