CN106046918A - Conductive ink and preparation method thereof - Google Patents
Conductive ink and preparation method thereof Download PDFInfo
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- CN106046918A CN106046918A CN201610596686.4A CN201610596686A CN106046918A CN 106046918 A CN106046918 A CN 106046918A CN 201610596686 A CN201610596686 A CN 201610596686A CN 106046918 A CN106046918 A CN 106046918A
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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
- C09D11/023—Emulsion inks
- C09D11/0235—Duplicating inks, e.g. for stencil printing
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- 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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- 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
- C09D11/033—Printing inks characterised by features other than the chemical nature of the binder characterised by the solvent
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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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- 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
- C09D11/52—Electrically conductive inks
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Abstract
The invention belongs to the field of conductive ink and discloses transparent conductive ink and a preparation method thereof. The transparent conductive ink is prepared from, by weight, 0.5-50 parts of nano silver wire dispersion liquid, 15-35 parts of poly(3,4-ethylenedioxy thiophene)-poly(styrene sulfonic acid), 5-40 parts of an organic solvent, 5-40 parts of deionized water, 1-8 parts of dimethyl sulfoxide, 0.1-5 parts of a viscosity modifier, 0.01-1 part of a pH regulator, 0.01-2 parts of a surfactant, 0.01-1 part of a leveling agent and 0.1-0.5 part of an adhesion promoter. The solid content of the transparent conductive ink is no more than 2%; due to addition of dimethyl sulfoxide in a formulation of the conductive ink, conductivity of a PEDOT/PSS and nano silver wire combined system is effectively improved; a prepared transparent conductive film has advantages of high optical transmittance, low haze and low surface square resistance and is excellent in adhesion, conductivity and environmental stability.
Description
Technical field
The invention belongs to electrically conductive ink field, specifically a kind of silk-screen electrically conducting transparent ink and preparation method thereof.
Background technology
Along with the raising day by day of levels of substance, consumer to the requirement of electronic product toward lightening and flexibility, visualization
Aspect fast-developing.Flexible display technologies makes display have the characteristic that can bend or be curled into arbitrary shape, has light, thin
And the feature such as it is convenient for carrying.Personal consumption electronic product on existing market mainly uses the hard such as tin indium oxide (ITO)
Inorganic oxide material as handset touch panel, solar energy, electromagnetic shielding, light-emitting diode display, electroluminescent device, thin film switch,
The core of the products such as cold light film, tin indium oxide is because its fragility is big and is difficult to the defect of bending, it is difficult at flexible optoelectronic
Device is applied.High plus the processing cost of tin indium oxide, energy consumption big, graphically need through mask, expose, develop, etch,
The loaded down with trivial details processing steps such as washing, bring many puzzlements to electron trade.At present those skilled in the art are devoted to develop novel
Substitution material be applied to transparent conductive film.Wherein, metal nano material particularly nano silver material become have at present most uncommon
Hope and realize commercial alternative material.
It is currently based on the existing multinomial patent application of electrically conducting transparent ink of nano-silver thread, but electric conductivity and still need to be changed
Kind, mist degree is the highest, light transmittance is on the low side, and major part use be coated with, spray, the non-patterned technique for applying such as blade coating, it is impossible to lead to
Cross volume to volume typography easy, efficient to realize.Electrically conducting transparent ink for silk-screen printing technique must be provided simultaneously with height
Viscosity, low haze, the feature of high transmission rate.The mode of printing of main flow has intaglio printing, letterpress, lithographic printing, silk at present
Wire mark brush etc..Silk-screen i.e. refers to silk screen printing, and by the extruding of scraper plate during printing, the ink being is transferred to hold by areas
On print thing, screen printing apparatus is simple and convenient to operate, print, make a plate simple and with low cost, flexibility or rigidity base material is the most permissible
Printing.Chinese patent application 201510096067.4 discloses a kind of electrically conducting transparent ink, its preparation method and nesa coating
Production method.The method is also by carrying out photocuring gained after silk screen printing, but owing to resin content is high, ink solid content
High (more than 60%), and it is thicker to carry out the film layer of silk-screen printing acquisition according to current screen thickness, ultimately results in sheet resistance bigger than normal, saturating
Light rate is on the low side, mist degree is higher.Chinese patent application 201510526785.0 disclose a kind of transparent conductive nano silver wire ink and
The preparation method of nesa coating, this ink equally exists the feature that light transmittance is on the low side, mist degree is higher, and transparency conducting layer uses
Coating process cannot be graphical.Chinese patent application 201510296650.X discloses a kind of anti-settling, Self-leveling nano-silver thread
Electrically conductive ink and the method being prepared transparent conductive film by it, this ink can use bar roll coating process, but be not used to silk screen
Printing.Therefore develop a kind of novel, excellent performance, can the silk-screen electrically conducting transparent ink of mass application be very urgent and must
Want.
Summary of the invention
It is an object of the invention to provide that a kind of preparation technology is simple, stable conductivity, energy-conserving and environment-protective silk screen printing transparent
Electrically conductive ink.
Another object of the present invention provides the preparation method of this electrically conducting transparent ink.
For reaching one of above-mentioned purpose, the present invention by the following technical solutions:
A kind of electrically conducting transparent ink, according to parts by weight, described electrically conducting transparent ink includes that 0.5～50 part of nano-silver thread divides
Dissipate liquid, 15～35 parts of poly-(3,4-Ethylenedioxy Thiophene)-poly-(styrene sulfonic acids), 5～40 parts of organic solvents, 5～40 parts go
Live in ionized water, 1～8 part of dimethyl sulfoxide, 0.1～5 part of viscosity modifier, 0.01～1 part of pH adjusting agent, 0.01～2 part of surface
Property agent, 0.01～1 part of levelling agent, 0.1～0.5 part of adhesion promoter.
Further, described nano-silver thread dispersion liquid is that nano-silver thread is scattered in methanol, ethanol, isopropanol, normal propyl alcohol, second
Glycol, propylene glycol, glycerol, water, propylene glycol monomethyl ether, dipropylene glycol methyl ether or propandiol butyl ether and obtain.
Further, the draw ratio of described nano-silver thread is 50～5000.
Further, the concentration of described nano-silver thread dispersion liquid is 1～100mg/mL.
Preferably nano-silver thread specification is:
Specification 1: average line footpath is 30nm, a length of 30 μm of average line, draw ratio 1000；
Specification 2: average line footpath is 40nm, a length of 40 μm of average line, draw ratio 1000；
Specification 3: average line footpath is 70nm, a length of 40 μm of average line, draw ratio about 570.
Along with the raising of nano-silver thread draw ratio, the mist degree of transparent conductive film reduces, and electric conductivity makes moderate progress.Nanometer silver
Line function as conductive filler, by the conductive network of nano-silver thread overlap joint, give ink film good electric conductivity.
Further, the solid content of described poly-(3,4-Ethylenedioxy Thiophene)-poly-(styrene sulfonic acid) be 1.0～
1.5%, electrical conductivity is 50～1000S/cm, and solvent is deionized water.Its effect is the electric conductivity improving ink, simultaneously works as adjusting
The effect of whole viscosity.
Further, described organic solvent be methanol, ethanol, isopropanol, normal propyl alcohol, ethylene glycol, propylene glycol, glycerol,
N-butyl alcohol, ethyl acetate, n-propyl acetate, isopropyl acetate, n-butyl acetate, sec-butyl acetate, propylene glycol monomethyl ether, dipropyl two
At least one in alcohol methyl ether, propandiol butyl ether, propylene glycol methyl ether acetate, isophorone and terpineol.Its effect is to reduce
Ink surface tension, it is provided that dissolubility, levelability the most widely.
Further, described viscosity modifier is hydroxypropyl methyl cellulose, hydroxypropyl cellulose, methylcellulose, second
The non-poly-ammonia of base cellulose, hydroxyethyl cellulose, xanthan gum, guar gum, polyurethane thickener, alkali solubility thickening agent, hydrophobically modified
At least one in ester thickener, poly-methyl pyrrole alkanone, aerosil and organobentonite.Its effect is to improve ink
Viscosity, improve printing adaptability.
Polyurethane thickener chemical composition is polyurethane resin, as Akzo Nobel Bermodol PUR 2102,
Bermodol PUR2110, Bermodol PUR2130, Bermodol PUR2150, the ACRYSOLRM-8 of ROHM AND HAAS,
ACRYSOLRM-8W, ACRYSOLRM-2020MPR, the Tego Viscoplus 3000 of Di Gao company, Tego Viscoplus
3030、Tego Viscoplus 3060。
Alkali solubility thickening agent is generally acrylic resin, such as ROHM AND HAAS AP-10, AP-50, ASE-60, TT-615, TT-
935；The modest Rheolate 125 of this moral of hamming, Rheolate 150, Rheolate 425, Rheolate450.
The non-polyurethane thickener of hydrophobically modified is generally hydrophobically modified polyethers, the DSX2000 of as peaceful in section of Germany (Cognis),
DSX3000, DSX3075, DSX3220, L100, L150, M200, H600 of Lockwood (Rockwood).
Further, described pH adjusting agent be ammonia, sodium hydroxide, diethanolamine, triethanolamine, 2-amino-2-methyl-
1-propanol or ethylenediamine.
Further, described surfactant is Tego dispers740w, Tego dispers750w, Tego
Dispers760w, BYK-151, BYK-180, BYK-181, BYK-190, BYK-194, TRITON (x45, x100, x140) and
At least one in FSO-100.Surfactant is used for reconciliation statement surface tension, plays humidification.
TRITON (x45, x100, x140) be the Polyethylene Glycol that produces of U.S. TritonX to isooctyl phenyl ether, from Guangzhou
Xi Lu Chemical Co., Ltd. buys；FSO-100 is the ethyoxyl fluorocarbon surfactant of E.I.Du Pont Company's exploitation, converges from Guangzhou and is coated with trade
Easily company limited buys.
Further, described levelling agent is BYK-307, BYK-333, BYK-341, BYK-345, BYK-346, Tego
At least one in Glid110, Tego Glid410, Tego Glid450, the modest W-461 of this moral of hamming and the modest FS-444 of moral.Stream
Flat agent is used for improving levelability, prevents shrinkage cavity, grows dim.
Further, described adhesion promoter be aqueous polyurethane, water-borne acrylic resin, polyvinyl alcohol, aqueous gather
Ester, aqueous alkide resin, polyacrylamide, polyethylene glycol oxide, styrenemaleic acid resin, aqueous epoxy resins and tripolycyanamide
At least one in resin.Its effect is to improve ink film scratch resistance, adhesive force, and improves nano-silver thread dispersibility and stability.
A kind of method preparing above-mentioned electrically conducting transparent ink, specifically: at room temperature by nano-silver thread dispersion liquid, poly-
(3,4-Ethylenedioxy Thiophene)-poly-(styrene sulfonic acid), dimethyl sulfoxide, viscosity modifier, surfactant, levelling agent,
Adhesion promoter, organic solvent, deionized water are sequentially added in beaker under 100～1000r/min stirrings, disperse 25
～35min, it being subsequently adding pH value regulator, regulation pH value, between 8～9, i.e. makes electrically conducting transparent ink.
This electrically conducting transparent ink may be used for preparing transparent conductive film, specifically: by above-mentioned electrically conducting transparent ink silk
Being printed on base material, drying solidification obtains transparent conductive film, and described base material is polyethylene terephthalate (PET), gathers
Carbonic ester, polyimides, glass, polypropylene or polyethylene.
The condition dried is: 90～180 DEG C, 1～10min.This drying condition regards temperature tolerance and the solidification of ink of base material
Depending on temperature.
The process of silk-screen is: take 20mL electrically conducting transparent ink in silk-screen half tone, starts screen printer, by scraper ink
It is printed on base material.Silk-screen half tone can make all types of pattern (lines, square, circular, point-like etc.), silk-screen half tone mesh number in advance
Can be 200 mesh, 250 mesh, 300 mesh, 350 mesh, 400 mesh, use nylon, terylene, braided steel wire exposure imaging to form, thickness 40
～100 μm.
The method have the advantages that
1, the solid content of tradition silk-screened conductive ink is more than 60% and opaque after film forming.The electrically conducting transparent of the present invention
Ink solid content is less than 2%；Can be used for any transparent conductive pattern of design and printing, after silk-screen, form one layer 100～800nm
Transparent conductive film, has the advantages that optical transmittance is high, mist degree is low, sheet resistivity is low, is provided simultaneously with good adhesive force, leads
Electrically, environmental stability, the most alternative traditional ITO conductive film of properties.
2, in the electrically conducting transparent ink composition of the present invention, dimethyl sulfoxide is as high bp polar solvent, it is possible to significantly carry
The electrical conductivity of high product.PEDOT/PSS and nano-silver thread are as main conductive materials, and the situation of film forming can make electric conductivity have
The biggest difference.PEDOT/PSS film forming to unfold degree the highest, electric conductivity is the best, and vice versa；And the electric conductivity of nano-silver thread takes
The certainly probability of overlap joint between line and line, this probability can be improved by the concentration strengthening nano-silver thread.Dimethyl sulfoxide energy
The PEDOT/PSS macromolecular chain being enough effectively improved a ball of string unfolds degree, improves taking of line and line after nano-silver thread film forming simultaneously
Connect probability, reduce surface roughness, thus be effectively improved PEDOT/PSS and the electrical conductivity of nano-silver thread compound system.
3, ink is water-based system, environment friendly and pollution-free, unharmful substance, by relevant detection certification.
4, ink has good oxidative resistance, weatherability, it is adaptable to for solar module, be also applied for large-scale from
The dynamic successional silk screen printing of screen printer.
5 need the subtractive process etched by justifying different from the transparent conductive film of tradition ITO, and this ink can pass through silk
Net typography a step addition process can directly prepare patterned transparent conductive film, and technique is simple, production efficiency improves, cost is big
Amplitude reduction.
6, when the present invention uses the flexible parent metal such as PET, polyimides, meet flexible touch screen requirement, can arbitrarily bend, turn round
Bent.
In sum, the electrically conducting transparent ink of the present invention be a kind of with nano-silver thread as conductive filler low admittedly containing silk-screen saturating
Bright electrically conductive ink, makes a patterned flex electronic device be possibly realized, and generally has the feelings of screen printing device in electron trade
Under condition, it is not necessary to add other equipment, so that it may carry out technological transformation, product up-gradation.For promoting that China leads at novel touch technology
The development in territory, break away from Japan on high-end ITO, monopolize the situation of continental market, grasp independent intellectual property right, there is long-range warp
Ji benefit and social benefit.
Accompanying drawing explanation
Fig. 1 is 10,000 times of enlarged drawings of scanning electron microscope of nano-silver thread used by embodiment 1；
Fig. 2 is 100,000 times of enlarged drawings of scanning electron microscope of nano-silver thread used by embodiment 1；
Fig. 3 is the transparent conductive film after embodiment 1 silk screen printing；
Fig. 4 is 100 times of enlarged drawings of microscope of embodiment 1 transparent conductive film；
Fig. 5 is 800 times of enlarged drawings of microscope of embodiment 1 transparent conductive film；
Fig. 6 is 2000 times of enlarged drawings of microscope of embodiment 1 transparent conductive film.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is described further:
Embodiment 1
Prepare electrically conducting transparent ink in accordance with the following methods:
Take 250gPEDOT/PSS (Germany congratulates Li Shi PH1000) in 2000mL beaker, to add under the stirring of 500r/min
(wherein nano-silver thread concentration is 10mg/mL, and average line footpath is 40nm, average line length to enter the aqueous isopropanol of 250g nano-silver thread
Being 40 μm, draw ratio 1000, Fig. 1 is 10,000 times of enlarged drawings of scanning electron microscope of nano-silver thread, and Fig. 2 is the scanning electron microscope of nano-silver thread
100000 times of enlarged drawings), after dispersion 10min, it is sequentially added into dimethyl sulfoxide 50g, alkali solubility thickening agent 20g (ROHM AND HAAS ASE-
60), surfactant (Tego dispers740w) 5g, levelling agent (Tego Glid410) 5g, aqueous polyurethane 5g, continue point
Dissipate 10min, be subsequently adding isopropanol: deionized water=1: the mixed solvent 415g of 1, continuation disperses 10min, is subsequently adding 5g ammonia
Water, regulation pH value, between 8～9, prepares silk-screen electrically conducting transparent ink after mix homogeneously.
Prepare transparent conductive film in accordance with the following methods:
With PET as flexible parent metal (light transmittance 92%, mist degree 0.3%, thickness 100 μm), by the above-mentioned conductive oil prepared
Ink semi-automatic silk-screen machine is printed on PET in silk-screen mode, then the base material being printed on silk-screen electrically conducting transparent ink is put in 130
DEG C vacuum drying oven 3min, treat solvent volatilization completely, ink film solidifies, and i.e. prepares patterned transparent conductive film, such as Fig. 3～6
Shown in, Fig. 4 is 100 times of enlarged drawings of microscope, and Fig. 5 is 800 times of enlarged drawings of microscope, and Fig. 6 is 2000 times of enlarged drawings of microscope.
Embodiment 2
Prepare electrically conducting transparent ink in accordance with the following methods:
Take 350gPEDOT/PSS (Germany congratulates Li Shi PH1000) in 2000mL beaker, to add under the stirring of 500r/min
(wherein nano-silver thread concentration is 10mg/mL, and average line footpath is 30nm, average line length to enter the aqueous isopropanol of 150g nano-silver thread
It is 30 μm, draw ratio 1000), after dispersion 10min, it is sequentially added into dimethyl sulfoxide 50g, hydroxypropyl methyl cellulose 20g, surface
Activating agent (TRITONx100) 5g, levelling agent (Tego Glid410) 5g, water-borne acrylic resin 5g, continue dispersion 10min, so
Rear addition isopropanol: deionized water=1: the mixed solvent 415g of 1, continues dispersion 10min, is subsequently adding 4g diethanolamine, adjust
Joint pH value between 8～9, ultrasonic vibration 5min, after mix homogeneously prepare silk-screen electrically conducting transparent ink.
Prepare transparent conductive film in accordance with the following methods:
With PET as flexible parent metal (light transmittance 92%, mist degree 0.3%, thickness 100 μm), by the above-mentioned conductive oil prepared
Ink semi-automatic silk-screen machine is printed on PET in silk-screen mode, then the base material being printed on silk-screen electrically conducting transparent ink is put in 120
DEG C vacuum drying oven 5min, treat solvent volatilization completely, ink film solidifies, and i.e. prepares patterned transparent conductive film.
Embodiment 3
Prepare electrically conducting transparent ink in accordance with the following methods:
Take 350gPEDOT/PSS (purchased from Shanghai Chun Yuan phytochemistry company limited) in 2000mL beaker, at 500r/
(wherein nano-silver thread concentration is 10mg/mL to the propylene glycol monomethyl ether solution of the stirring lower addition 150g nano-silver thread of min, average line
Footpath is 30nm, a length of 30 μm of average line, draw ratio 1000), after dispersion 10min, it is sequentially added into dimethyl sulfoxide 50g, hydrophobic changes
Property non-polyurethane thickener (L100 of Lockwood Rockwood) 20g, surfactant (BYK-151) 5g, levelling agent (Tego
Glid410) 5g, water-borne acrylic resin 5g, continues dispersion 10min, is subsequently adding ethylene glycol: deionized water=1: the mixing of 1
Solvent 415g, continues dispersion 10min, is subsequently adding 5g triethanolamine, regulation pH value between 8～9, ultrasonic vibration 5min, mixed
Silk-screen electrically conducting transparent ink is prepared after closing uniformly.
Prepare transparent conductive film in accordance with the following methods:
With PET as flexible parent metal (light transmittance 91%, mist degree 0.3%, thickness 100 μm), by the above-mentioned conductive oil prepared
Ink semi-automatic silk-screen machine is printed on PET in silk-screen mode, then the base material being printed on silk-screen electrically conducting transparent ink is put in 150
DEG C vacuum drying oven 10min, treat solvent volatilization completely, ink film solidifies, and i.e. prepares patterned transparent conductive film.
Embodiment 4
Prepare electrically conducting transparent ink in accordance with the following methods:
Take 350gPEDOT/PSS (Germany congratulates Li Shi PH1000) in 2000mL beaker, to add under the stirring of 500r/min
(wherein nano-silver thread concentration is 10mg/mL, and average line footpath is 70nm, averagely to enter the propylene glycol monomethyl ether solution of 150g nano-silver thread
Line length is 40 μm, draw ratio about 600), after dispersion 10min, it is sequentially added into dimethyl sulfoxide 50g, organobentonite 20g, surface
Activating agent (BYK-190) 5g, levelling agent (BYK-333) 5g, water-borne acrylic resin 5g, continue dispersion 10min, be subsequently adding second
Glycol: deionized water=1: the mixed solvent 415g of 1, continues dispersion 10min, is subsequently adding 1g sodium hydroxide, and regulation pH value is 8
～between 9, ultrasonic vibration 5min, prepare silk-screen electrically conducting transparent ink after mix homogeneously.
Prepare transparent conductive film in accordance with the following methods:
With polycarbonate as flexible parent metal (light transmittance 92%, thickness 125 μm), the above-mentioned electrically conductive ink prepared is used
Semi-automatic silk-screen machine is printed on PET in silk-screen mode, then the base material being printed on silk-screen electrically conducting transparent ink is put in 150 DEG C
Vacuum drying oven 10min, treats solvent volatilization completely, and ink film solidifies, and i.e. prepares patterned transparent conductive film.
Embodiment 5
Prepare electrically conducting transparent ink in accordance with the following methods:
Take 150gPEDOT/PSS (Germany congratulates Li Shi PH1000) in 2000mL beaker, to add under the stirring of 500r/min
(wherein nano-silver thread concentration is 10mg/mL, and average line footpath is 70nm, averagely to enter the propylene glycol monomethyl ether solution of 350g nano-silver thread
Line length is 40 μm, draw ratio about 600), after dispersion 10min, it is sequentially added into dimethyl sulfoxide 50g, the non-polyurethane of hydrophobically modified
Thick dose of (L100 of Lockwood) 20g, surfactant (TRITONx140) 5g, levelling agent (BYK-345) 5g, water soluble acrylic acid
5g, continues dispersion 10min, is subsequently adding ethylene glycol: deionized water=1: the mixed solvent 415g of 1, continuation disperses 10min, so
Rear addition 2g 2-amino-2-methyl-1-propanol, regulation pH value between 8～9, ultrasonic vibration 5min, after mix homogeneously prepare
Silk-screen electrically conducting transparent ink.
Prepare transparent conductive film in accordance with the following methods:
With glass as rigid substrate (light transmittance 90%, thickness 3mm), by the above-mentioned semi-automatic silk of the electrically conductive ink prepared
Print machine is printed on glass in silk-screen mode, and the vacuum that then base material being printed on silk-screen electrically conducting transparent ink is put in 150 DEG C is done
Dry case 10min, treats solvent volatilization completely, and ink film solidifies, and i.e. prepares patterned transparent conductive film.
Embodiment 6
Prepare electrically conducting transparent ink in accordance with the following methods:
Take 250gPEDOT/PSS (solid content is 1.3%, and electrical conductivity is 1000S/cm, and solvent is deionized water) in
In 2000mL beaker, under the stirring of 400r/min, add glycerin solution (the wherein nano-silver thread concentration of 100g nano-silver thread
For 5mg/mL, average line footpath is 70nm, a length of 40 μm of average line, draw ratio 570), after dispersion 10min, it is sequentially added into dimethyl
Sulfoxide 30g, xanthan gum 1g, surfactant (BYK-194) 1g, levelling agent (Tego Glid450) 1g, melmac 1g,
Continue dispersion 10min, be subsequently adding 200g propandiol butyl ether, 200g deionized water, continue dispersion 5min, be subsequently adding 1g ammonia
Water, regulation pH value, between 8～9, prepares silk-screen electrically conducting transparent ink after mix homogeneously.
Prepare transparent conductive film in accordance with the following methods:
With polyimides as flexible parent metal, the above-mentioned electrically conductive ink semi-automatic silk-screen machine prepared is printed in silk-screen mode
It is formed on polyimides, then the base material being printed on silk-screen electrically conducting transparent ink is put in the vacuum drying oven 1min of 180 DEG C, treats molten
Completely, ink film solidifies, and i.e. prepares patterned transparent conductive film in agent volatilization.
Embodiment 7
Prepare electrically conducting transparent ink in accordance with the following methods:
Take 200gPEDOT/PSS (solid content is 1.3%, and electrical conductivity is 1000S/cm, and solvent is deionized water) in
In 2000mL beaker, under the stirring of 600r/min, add ethylene glycol solution (the wherein nano-silver thread concentration of 450g nano-silver thread
For 20mg/mL, average line footpath is 80nm, a length of 40 μm of average line, draw ratio 500), after dispersion 10min, it is sequentially added into dimethyl
Sulfoxide 40g, aerosil 5g, surfactant (Tego dispers750w) 2g, levelling agent (the modest W-461 of this moral of hamming)
2g, aqueous alkide resin 4g, continue dispersion 15min, be subsequently adding 400g terpineol, 400g deionized water, continue dispersion
10min, is subsequently adding 3g ethylenediamine, and regulation pH value, between 8～9, prepares silk-screen electrically conducting transparent ink after mix homogeneously.
Prepare transparent conductive film in accordance with the following methods:
With polyethylene as base material, the above-mentioned electrically conductive ink semi-automatic silk-screen machine prepared is printed on poly-in silk-screen mode
On ethylene, then the base material being printed on silk-screen electrically conducting transparent ink is put in the vacuum drying oven 8min of 90 DEG C, treats that solvent is evaporated completely
Entirely, ink film solidifies, and i.e. prepares patterned transparent conductive film.
Embodiment 8
Prepare electrically conducting transparent ink in accordance with the following methods:
Take 200gPEDOT/PSS in 2000mL beaker, under the stirring of 500r/min, add the third of 200g nano-silver thread
(wherein nano-silver thread concentration is 12mg/mL to glycol butyl ether solution, and average line footpath is 50nm, a length of 40 μm of average line, draw ratio
800), after dispersion 10min, it is sequentially added into dimethyl sulfoxide 30g, ethyl cellulose 10g, surfactant (Tego
Dispers760w) 4g, levelling agent (Tego Glid110) 3g, polyethylene glycol oxide 2g, continues dispersion 10min, is subsequently adding 300g
Dipropylene glycol methyl ether, 350g deionized water, continue dispersion 10min, is subsequently adding 3g ammonia, and regulation pH value is between 8～9, mixed
Silk-screen electrically conducting transparent ink is prepared after closing uniformly.
Prepare transparent conductive film in accordance with the following methods:
With polypropylene as base material, the above-mentioned electrically conductive ink semi-automatic silk-screen machine prepared is printed on poly-in silk-screen mode
On propylene, then the base material being printed on silk-screen electrically conducting transparent ink is put in the vacuum drying oven 3min of 100 DEG C, treats that solvent is evaporated completely
Entirely, ink film solidifies, and i.e. prepares patterned transparent conductive film.
Performance test
Comparative example 1: removed by the dimethyl sulfoxide in embodiment 1 electrically conducting transparent ink formulations, other component and deal are protected
Hold constant, according to embodiment 1 preparation method, prepare transparent conductive film.
For embodiment 1～8 and the product of comparative example 1, use four-point probe resolution chart transparent conductive film
Sheet resistance, photoelectricity haze meter resolution chart transparent conductive film light transmittance, mist degree, use 3M610 adhesive tape test adhesive force, pencil
Durometer test hardness, the results are shown in Table 1.
Table 1 the performance test results
| Base material | Sheet resistance (Ω/) | Total light transmittance (%) | Mist degree (%) | Adhesive force | Hardness | |
| Embodiment 1 | PET | 50 | 90 | 1.5 | 5B | H |
| Embodiment 2 | PET | 60 | 91 | 0.7 | 5B | H |
| Embodiment 3 | PET | 45 | 92 | 1.5 | 5B | H |
| Embodiment 4 | PC | 100 | 94 | 2.0 | 5B | H |
| Embodiment 5 | Glass | 10 | 83 | 4 | 5B | H |
| Embodiment 6 | PI | 80 | 80 | 3.5 | 5B | H |
| Embodiment 7 | PE | 100 | 90 | 12 | 5B | H |
| Embodiment 8 | PP | 60 | 90 | 1.8 | 5B | H |
| Comparative example 1 | PET | 80 | 82 | 3.0 | 5B | H |
As seen from the above table, when using same substrate, transparent obtained by the electrically conducting transparent ink containing dimethyl sulfoxide is led
Conductive film, has a higher optical transmittance, and lower mist degree and sheet resistivity.
The above, the only detailed description of the invention of the present invention, but protection scope of the present invention is not limited thereto, and any
Belong to those skilled in the art in the technical scope that the invention discloses, the change that can readily occur in or replacement, all answer
Contain within protection scope of the present invention.Therefore, protection scope of the present invention should be as the criterion with scope of the claims.
Claims (8)
1. an electrically conducting transparent ink, it is characterised in that according to parts by weight, described electrically conducting transparent ink includes that 0.5 ~ 50 part is received
Rice silver wire dispersion liquid, 15 ~ 35 parts of poly-(3,4-Ethylenedioxy Thiophene)-poly-(styrene sulfonic acids), 5 ~ 40 parts of organic solvents, 5 ~ 40
Live in part deionized water, 1 ~ 8 part of dimethyl sulfoxide, 0.1 ~ 5 part of viscosity modifier, 0.01 ~ 1 part of pH adjusting agent, 0.01 ~ 2 part of surface
Property agent, 0.01 ~ 1 part of levelling agent, 0.1 ~ 0.5 part of adhesion promoter.
Electrically conducting transparent ink the most according to claim 1, it is characterised in that described nano-silver thread dispersion liquid is nano-silver thread
It is scattered in methanol, ethanol, isopropanol, normal propyl alcohol, ethylene glycol, propylene glycol, glycerol, water, propylene glycol monomethyl ether, dipropylene glycol methyl ether
Or propandiol butyl ether and obtain.
Electrically conducting transparent ink the most according to claim 2, it is characterised in that the draw ratio of described nano-silver thread is 50 ~
5000。
Electrically conducting transparent ink the most according to claim 1, it is characterised in that described organic solvent is methanol, ethanol, isopropyl
The positive fourth of alcohol, normal propyl alcohol, ethylene glycol, propylene glycol, glycerol, n-butyl alcohol, ethyl acetate, n-propyl acetate, isopropyl acetate, acetic acid
Ester, sec-butyl acetate, propylene glycol monomethyl ether, dipropylene glycol methyl ether, propandiol butyl ether, propylene glycol methyl ether acetate, isophorone and
At least one in terpineol.
Electrically conducting transparent ink the most according to claim 1, it is characterised in that described viscosity modifier is that hydroxypropyl methyl is fine
Dimension element, hydroxypropyl cellulose, methylcellulose, ethyl cellulose, hydroxyethyl cellulose, xanthan gum, guar gum, polyurethane thickening
Agent, alkali solubility thickening agent, the non-polyurethane thickener of hydrophobically modified, poly-methyl pyrrole alkanone, aerosil and organic swelling
At least one in soil.
Electrically conducting transparent ink the most according to claim 1, it is characterised in that described pH adjusting agent be ammonia, sodium hydroxide,
Diethanolamine, triethanolamine, 2-amino-2-methyl-1-propanol or ethylenediamine.
Electrically conducting transparent ink the most according to claim 1, it is characterised in that described adhesion promoter is the poly-ammonia of aqueous
Ester, water-borne acrylic resin, polyvinyl alcohol, waterborne polyester, aqueous alkide resin, polyacrylamide, polyethylene glycol oxide, styrene
At least one in maleic acid resin, aqueous epoxy resins and melmac.
8. the method for the electrically conducting transparent ink that one kind is prepared described in any one of claim 1 ~ 7, it is characterised in that at room temperature will
Nano-silver thread dispersion liquid, poly-(3,4-Ethylenedioxy Thiophene)-poly-(styrene sulfonic acid), organic solvent, deionized water, dimethyl
Sulfoxide, viscosity modifier, surfactant, levelling agent, adhesion promoter add under 100 ~ 1000r/min stirring successively
Entering in beaker, disperse 25 ~ 35min, be subsequently adding pH value regulator, regulation pH value, between 8 ~ 9, i.e. makes electrically conducting transparent oil
Ink.
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| CN104861776A (en) * | 2015-06-02 | 2015-08-26 | 北京化工大学 | Anti-settling and self-leveling silver nanowire conductive printing ink and method for preparing transparent conducting thin film by using same |
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