CN108659623A - Composite conducting ink and preparation method thereof and conducting wire forming method - Google Patents
Composite conducting ink and preparation method thereof and conducting wire forming method Download PDFInfo
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- CN108659623A CN108659623A CN201810324975.8A CN201810324975A CN108659623A CN 108659623 A CN108659623 A CN 108659623A CN 201810324975 A CN201810324975 A CN 201810324975A CN 108659623 A CN108659623 A CN 108659623A
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- silver
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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
- C09D11/52—Electrically conductive inks
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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
-
- 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
-
- 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
- C09D11/14—Printing inks based on carbohydrates
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K1/00—Printed circuits
- H05K1/02—Details
- H05K1/09—Use of materials for the conductive, e.g. metallic pattern
- H05K1/092—Dispersed materials, e.g. conductive pastes or inks
Abstract
The present invention relates to touch screen technology field more particularly to composite conducting ink and preparation method thereof and conducting wire forming method, composite conducting ink includes the raw material of following parts by weight：40~50 parts of silver-colored complex conductive fillers, 8~12 parts of binder, 0.5~1 part of antifoaming agent, 0.5~1 part of dispersion stabilizer, 1.5~3 parts of surfactant, silver-colored complex conductive fillers are the compounds of titanium dioxide and nano silver wire.Wherein, titanium dioxide is the titania nanotube that aperture is 60~100nm, and nano silver wire is three-level bifurcated nano silver wire, one kind in level Four bifurcated nano silver wire or mixing.Nano silver wire and titania nanotube are effectively combined by the composite conducting ink of the present invention, reduce silver-colored electronics problem easy to migrate, and can reinforce the tie point between silver particles by bifurcated nano silver wire, are effectively reduced resistance, improve electric conductivity.
Description
Technical field
The present invention relates to touch screen technology field more particularly to composite conducting ink and preparation method thereof and conducting wire at
Type method.
Background technology
It is the hot spot studied both at home and abroad at present as the electrically conductive ink of one of the critical material for restricting touch screen technology development
And difficult point.Electrically conductive ink be electric conductor, bonding agent, solvent and auxiliary agent etc. by be specifically formulated and disperse means formed solution or
Suspension reaches the physical and chemical performances indexs such as defined dispersibility, viscosity, surface tension, solid content, to adapt to print or be coated with work
The requirement of skill.Electrically conductive ink is during sintering curing, volatile solvent volatilization, volume contraction, and filler particles are tight with bonding agent
Close links together, and particle space between each other becomes smaller, and can form electric current under the action of an external electric field, realizes conducting function.
Inorganic can pass the printing ink of the electric current has many advantages, such as that reliability is high, storge quality is high, stability is good, has been widely used in integrating
The electronic products such as circuit, RFID, wiring board, thin film switch are the hot spots of research and development recent years.According to the type of conductive material,
Inorganic can pass the printing ink of the electric current can be specifically divided into gold system, silver-colored system, copper system, carbon series conductive ink.The various performances of gold system electrically conductive ink are all very
It is excellent, but it is expensive, using significantly being limited, has particular/special requirement using thick film integrated circuit etc. is limited only to
Product；It is the electric conductivity slightly less than gold system of electrically conductive ink that silver powder, which has good high conduction performance and chemical stability, silver, but
Have a wide range of application, the printing molding China of the high appliance circuit of reliability can be largely used to, but that there are electronics is easy to migrate for silver system
The problem of, increase so as to cause the resistance of conducting wire, electric conductivity reduces.
Invention content
In view of this, the object of the present invention is to provide composite conducting ink and preparation method thereof and conducting wire molding side
Nano silver wire and titania nanotube are effectively combined by method, reduce silver-colored electronics problem easy to migrate, and by dividing
Fork nano silver wire can reinforce the tie point between silver particles, be effectively reduced resistance, improve electric conductivity.
The present invention solves above-mentioned technical problem by following technological means：
Composite conducting ink includes the raw material of following parts by weight：40~50 parts of silver-colored complex conductive fillers, binder 8~
12 parts, 0.5~1 part of antifoaming agent, 0.5~1 part of dispersion stabilizer, 1.5~3 parts of surfactant, it is described silver complex conductive fillers
It is the compound of titanium dioxide and nano silver wire.
Further, the titanium dioxide is the titania nanotube that aperture is 60~100nm.
Further, the nano silver wire is three-level bifurcated nano silver wire, one kind in level Four bifurcated nano silver wire or mixing.
Further, the binder be lead-free glass powder or sodium alginate, the antifoaming agent be dimethicone, described point
Dispersion stabilizer is sodium carboxymethylcellulose, and the surfactant is polyethylene glycol.
In addition, the invention also discloses the preparation method of above-mentioned composite conducting ink, include the following steps：
The preparation of silver-colored complex conductive fillers：Take titania nanotube and nano silver wire in mass ratio 1:3 are stirred, then
The isopropanol mixing of 0.1 times of titania nanotube quality is added, is transferred in ball grinder, it is cold in 80~95 DEG C of ball milling 8~12h
But it takes out and obtains silver-colored complex conductive fillers；
The preparation of composite conducting ink：By silver-colored complex conductive fillers, binder, antifoaming agent, dispersion stabilizer, surface-active
Agent is added in the isopropanol water solution of 20wt%, in 50~60 DEG C of 500~800rpm of rotating speed, temperature 1~2h of stirring, obtains compound
Electrically conductive ink.
Further, the nano silver wire is prepared by electrochemical deposition method with bifurcated alumina formwork.
Further, the condition of the electrochemical deposition is as follows：The concentrated sulfuric acid of silver nitrate and 15g/L that electrolyte is 5g/L is mixed
Close solution, the electrochemical deposition 5min under 18~20V alternating voltages, 40~48Hz frequencies.
In addition, the invention also discloses use above-mentioned composite conducting ink to form conducting wire forming method, the molding
Method is as follows：After base material successively to be carried out to neutral washing, non-contact AP cleanings, sprayed on base material using piezoelectric type nozzle compound
Electrically conductive ink sprays five times along conductive circuit pattern, is subsequently placed at 70~75 DEG C of baking 3min, then carry out flash of light sintering, i.e.,
Form conducting wire.
Flashing light sintering is that wide spectrum, the pulsed light of high-energy is utilized to be sintered nanometer ink or electrocondution slurry, energy
It is enough in the time range of millisecond so that nano-particle partly or completely fuses after absorbing energy, to reduce between silver particles
Gap, reduce the resistance of conducting wire to a certain extent, improve electric conductivity.
The nano silver wire of multistage bifurcated in the composite conducting ink of the present invention is interspersed in the sky of titanium dioxide carbon nanotube
In gap, multistage Y-shaped makes the connection contact that is superimposed with each other between nano silver wire, reduces the resistance of conducting wire at network structure,
Electric conductivity is improved, and the orderly hole of titania nanotube provides more spatial positions for the load of nano-silver thread, and be convenient for
Contacting with each other between nano silver wire, further improves electric conductivity.
Specific implementation mode
Below with reference to specific embodiment, the present invention is described in detail：
The composite conducting ink of the present invention includes the raw material of following parts by weight：40~50 parts of silver-colored complex conductive fillers glue
8~12 parts of agent, 0.5~1 part of antifoaming agent, 0.5~1 part of dispersion stabilizer, 1.5~3 parts of surfactant are tied, silver-colored composite conducting is filled out
Material is the compound of titanium dioxide and nano silver wire.Wherein, titanium dioxide is the nano titania that aperture is 60~100nm
Pipe, nano silver wire is that three-level bifurcated nano silver wire, one kind in level Four bifurcated nano silver wire or mixing, binder are crown glass
Powder or sodium alginate, antifoaming agent are dimethicone, and dispersion stabilizer is sodium carboxymethylcellulose, and surfactant is poly- second two
Alcohol.
Preparing for the composite conducting ink of the present invention is as follows：
Embodiment one
The preparation of nano silver wire：It takes high-purity aluminium flake to make electrolyte using the oxalic acid solution of 0.3mol/L, electricity is originated in 42V
Pressure, then withMultiple oxidation voltage is dropped into 15V and 10V successively from 42V, three-level bifurcated and four can be obtained respectively
The alumina formwork of grade bifurcated.Using the aluminium oxide of three-level or level Four bifurcated as template, with the dense sulphur of the silver nitrate of 5g/L and 15g/L
Sour mixed solution be electrolyte, 18V alternating voltages, 40Hz frequency under, electrochemical deposition 5min, the process of electrochemical deposition
Middle silver ion is attracted under the action of electric field on alumina formwork hole wall, and along being grown in hole wall, by alumina formwork
Shape copy completely come, obtain the nano silver wire of three-level or level Four bifurcated.
The preparation of titania nanotube：By titanium foil after liquid honing is smooth to surface, be first placed on acetone, go from
It is cleaned in sub- water and polishing solution, to remove the natural oxide and other impurities on surface, is then connected titanium foil and anode
Connect, platinum electrode is cathode, is placed in 400mL ethylene glycol electrolyte, in ethylene glycol electrolyte containing mass fraction be 2% go from
Sub- water and 0.4% ammonium fluoride, react 2h at electro-hydraulic 8V, be dried to obtain Nano tube array of titanium dioxide.
The preparation of silver-colored complex conductive fillers：It takes 2g titania nanotubes and 6g nano silver wires to be stirred, adds
0.2g isopropanol mixings, are transferred in ball grinder, and in 90 DEG C of ball milling 10h, cooling take out obtains silver-colored complex conductive fillers.
The preparation of composite conducting ink：48 parts of silver-colored complex conductive fillers, 10 parts of sodium alginate, 0.5 part of dimethicone, carboxylic
0.5 part of sodium carboxymethylcellulose pyce, 1.5 parts of polyethylene glycol are added in the isopropanol water solution of 20wt%, in rotating speed 700rpm, temperature 55
DEG C stirring 2h, obtain composite conducting ink.
Embodiment two
The preparation of nano silver wire：It takes high-purity aluminium flake to make electrolyte using the oxalic acid solution of 0.3mol/L, electricity is originated in 42V
Pressure, then withMultiple oxidation voltage is dropped into 15V and 10V successively from 42V, three-level bifurcated and four can be obtained respectively
The alumina formwork of grade bifurcated.Using the aluminium oxide of three-level or level Four bifurcated as template, with the dense sulphur of the silver nitrate of 5g/L and 15g/L
Sour mixed solution be electrolyte, 20V alternating voltages, 48Hz frequency under, electrochemical deposition 5min, the process of electrochemical deposition
Middle silver ion is attracted under the action of electric field on alumina formwork hole wall, and along being grown in hole wall, by alumina formwork
Shape copy completely come, obtain the nano silver wire of three-level or level Four bifurcated.
The preparation of titania nanotube：By titanium foil after liquid honing is smooth to surface, be first placed on acetone, go from
It is cleaned in sub- water and polishing solution, to remove the natural oxide and other impurities on surface, is then connected titanium foil and anode
Connect, platinum electrode is cathode, is placed in 400mL ethylene glycol electrolyte, in ethylene glycol electrolyte containing mass fraction be 2% go from
Sub- water and 0.6% ammonium fluoride, react 2h at electro-hydraulic 10V, be dried to obtain Nano tube array of titanium dioxide.
The preparation of silver-colored complex conductive fillers：It takes 2g titania nanotubes and 6g nano silver wires to be stirred, adds
0.2g isopropanol mixings, are transferred in ball grinder, and in 85 DEG C of ball milling 9h, cooling take out obtains silver-colored complex conductive fillers.
The preparation of composite conducting ink：45 parts of silver-colored complex conductive fillers, 10 parts of sodium alginate, 0.8 part of dimethicone, carboxylic
0.8 part of sodium carboxymethylcellulose pyce, 2 parts of polyethylene glycol addition 20wt% isopropanol water solution in, in 55 DEG C of rotating speed 600rpm, temperature
1.5h is stirred, composite conducting ink is obtained.
Embodiment three
The preparation of nano silver wire：It takes high-purity aluminium flake to make electrolyte using the oxalic acid solution of 0.3mol/L, electricity is originated in 42V
Pressure, then withMultiple oxidation voltage is dropped into 15V and 10V successively from 42V, three-level bifurcated and four can be obtained respectively
The alumina formwork of grade bifurcated.Using the aluminium oxide of three-level or level Four bifurcated as template, with the dense sulphur of the silver nitrate of 5g/L and 15g/L
Sour mixed solution be electrolyte, 19V alternating voltages, 45Hz frequency under, electrochemical deposition 5min, the process of electrochemical deposition
Middle silver ion is attracted under the action of electric field on alumina formwork hole wall, and along being grown in hole wall, by alumina formwork
Shape copy completely come, obtain the nano silver wire of three-level or level Four bifurcated.
The preparation of titania nanotube is the same as embodiment two.
The preparation of silver-colored complex conductive fillers：It takes 2g titania nanotubes and 6g nano silver wires to be stirred, adds
0.2g isopropanol mixings, are transferred in ball grinder, and in 95 DEG C of ball milling 12h, cooling take out obtains silver-colored complex conductive fillers.
The preparation of composite conducting ink：50 parts of silver-colored complex conductive fillers, 12 parts of lead-free glass powder, 1 part of dimethicone, carboxylic
1 part of sodium carboxymethylcellulose pyce, 3 parts of polyethylene glycol are added in the isopropanol water solution of 20wt%, are stirred in rotating speed 800rpm, temperature 60 C
2h is mixed, composite conducting ink is obtained.
Example IV
The preparation of nano silver wire：It takes high-purity aluminium flake to make electrolyte using the oxalic acid solution of 0.3mol/L, electricity is originated in 42V
Pressure, then withMultiple oxidation voltage is dropped into 15V and 10V successively from 42V, three-level bifurcated and four can be obtained respectively
The alumina formwork of grade bifurcated.Using the aluminium oxide of three-level or level Four bifurcated as template, with the silver nitrate of 5g/L and 15gThe dense sulphur of/L
Sour mixed solution be electrolyte, 20V alternating voltages, 48Hz frequency under, electrochemical deposition 10min, the mistake of electrochemical deposition
Silver ion is attracted under the action of electric field on alumina formwork hole wall in journey, and along being grown in hole wall, will aoxidize aluminum dipping form
The shape of plate copies completely to be come, and the nano silver wire of three-level or level Four bifurcated is obtained.
The preparation of titania nanotube：By titanium foil after liquid honing is smooth to surface, be first placed on acetone, go from
It is cleaned in sub- water and polishing solution, to remove the natural oxide and other impurities on surface, is then connected titanium foil and anode
Connect, platinum electrode is cathode, is placed in 400mL ethylene glycol electrolyte, in ethylene glycol electrolyte containing mass fraction be 2% go from
Sub- water and 0.3% ammonium fluoride, react 2h at electro-hydraulic 6V, be dried to obtain Nano tube array of titanium dioxide.
The preparation of silver-colored complex conductive fillers：It takes 2g titania nanotubes and 6g nano silver wires to be stirred, adds
0.2g isopropanol mixings, are transferred in ball grinder, and in 80 DEG C of ball milling 8h, cooling take out obtains silver-colored complex conductive fillers.
The preparation of composite conducting ink：40 parts of silver-colored complex conductive fillers, 8 parts of lead-free glass powder, 0.5 part of dimethicone,
0.5 part of sodium carboxymethylcellulose, 1.5 parts of polyethylene glycol are added in the isopropanol water solution of 20wt%, in rotating speed 500rpm, temperature
50 DEG C of stirring 1h, obtain composite conducting ink.
The composite conducting ink that above-described embodiment is prepared can be applied in the moulding process of touch screen conducting wire, at
Type method is as follows：After base material successively to be carried out to neutral washing, non-contact AP cleanings, sprayed again on base material using piezoelectric type nozzle
Electrically conductive ink is closed, is sprayed five times along conductive circuit pattern, is subsequently placed at 70~75 DEG C of baking 3min, then carry out flash of light sintering,
Form conducting wire.
The above examples are only used to illustrate the technical scheme of the present invention and are not limiting, although with reference to preferred embodiment to this hair
It is bright to be described in detail, it will be understood by those of ordinary skill in the art that, it can modify to technical scheme of the present invention
Or equivalent replacement should all cover the claim in the present invention without departing from the objective and range of technical solution of the present invention
In range.Technology that the present invention is not described in detail, shape, construction part are known technology.
Claims (8)
1. composite conducting ink, which is characterized in that include the raw material of following parts by weight：40~50 parts of silver-colored complex conductive fillers,
8~12 parts of binder, 0.5~1 part of antifoaming agent, 0.5~1 part of dispersion stabilizer, 1.5~3 parts of surfactant, the silver are compound
Conductive filler is the compound of titanium dioxide and nano silver wire.
2. composite conducting ink according to claim 1, which is characterized in that the titanium dioxide be aperture be 60~
The titania nanotube of 100nm.
3. composite conducting ink according to claim 2, which is characterized in that the nano silver wire is three-level bifurcated silver nanoparticle
Line, one kind in level Four bifurcated nano silver wire or mixing.
4. composite conducting ink according to claim 3, which is characterized in that the binder is lead-free glass powder or seaweed
Sour sodium, the antifoaming agent are dimethicone, and the dispersion stabilizer is sodium carboxymethylcellulose, and the surfactant is poly-
Ethylene glycol.
5. the preparation method of composite conducting ink according to claim 4, which is characterized in that include the following steps：
The preparation of silver-colored complex conductive fillers：Take titania nanotube and nano silver wire in mass ratio 1:3 are stirred, and add
The isopropanol mixing of 0.1 times of titania nanotube quality, is transferred in ball grinder, and in 80~95 DEG C of 8~12h of ball milling, cooling takes
Go out to obtain silver-colored complex conductive fillers；
The preparation of composite conducting ink：Silver-colored complex conductive fillers, binder, antifoaming agent, dispersion stabilizer, surfactant are added
In the isopropanol water solution for entering 20wt%, in 50~60 DEG C of 500~800rpm of rotating speed, temperature 1~2h of stirring, composite conducting is obtained
Ink.
6. the preparation method of composite conducting ink according to claim 5, which is characterized in that the nano silver wire is to divide
Alumina formwork is pitched, is prepared by electrochemical deposition method.
7. the preparation method of composite conducting ink according to claim 6, which is characterized in that the item of the electrochemical deposition
Part is as follows：Electrolyte is the concentrated sulfuric acid mixed solution of the silver nitrate and 15g/L of 5g/L, in 18~20V alternating voltages, 40~48Hz
Electrochemical deposition 5min under frequency.
8. conducting wire forming method, which is characterized in that the conducting wire is the composite guide being prepared by such as claim 7
Electric ink solidification is formed, and the forming method is as follows：After base material successively to be carried out to neutral washing, non-contact AP cleanings, using pressure
Electric-type nozzle sprays composite conducting ink on base material, is sprayed five times along conductive circuit pattern, is subsequently placed at 70~75 DEG C of bakings
Roasting 3min, then carry out flash of light sintering, that is, form conducting wire.
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| US20180022953A1 (en) * | 2012-08-16 | 2018-01-25 | Nthdegree Technologies Worldwide Inc. | Conductive Metallic and Semiconductor Ink Composition |
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2018
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| US20180022953A1 (en) * | 2012-08-16 | 2018-01-25 | Nthdegree Technologies Worldwide Inc. | Conductive Metallic and Semiconductor Ink Composition |
| CN104674215A (en) * | 2013-12-02 | 2015-06-03 | 天津大学 | Preparation method of nano silver particle loaded antimicrobial titanium dioxide coating |
| CN105692625A (en) * | 2014-11-24 | 2016-06-22 | 中国科学院上海硅酸盐研究所 | Preparation method of oxide nanotube and nanobelt |
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Application publication date: 20181016 |