CN107118620A - A kind of preparation method of conductive silver ink - Google Patents
A kind of preparation method of conductive silver ink Download PDFInfo
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- CN107118620A CN107118620A CN201710559121.3A CN201710559121A CN107118620A CN 107118620 A CN107118620 A CN 107118620A CN 201710559121 A CN201710559121 A CN 201710559121A CN 107118620 A CN107118620 A CN 107118620A
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- conductive 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
- C09D11/30—Inkjet printing inks
- C09D11/38—Inkjet printing inks characterised by non-macromolecular additives other than solvents, pigments or dyes
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- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Wood Science & Technology (AREA)
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- Conductive Materials (AREA)
- Inks, Pencil-Leads, Or Crayons (AREA)
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
Abstract
The invention discloses a kind of preparation method of conductive silver ink, by solvent and dispersant, stirring is well mixed to dispersant with solvent, obtains solution；Under the conditions of ultrasonic disperse, nano-Ag particles are added, nano silver dispersion is obtained；PH adjusting agent is added, pH adjusting agent is completely dispersed；Surface tension modifier and tackifier are added, is stirred；Preservative, defoamer and adhesive are added, stirring obtains mixed liquor to well mixed；Mixed liquor is filtered, the conductive silver ink that precipitation obtains stable dispersion is removed.Nano-tourmaline particle is added the pH environment of ink is adjusted.This method preparation technology is simple, and the stability of ink prepared is good, can be preserved with the long period.
Description
Technical field
The invention belongs to technical field of nano material, specifically a kind of preparation method of conductive silver ink.
Background technology
Printed electronics refer to conductive ink is selectively deposited at into printing using means such as intaglio printing, silk-screen printings
On thing, and the emerging interleaving techniques by post-processing with electric conductivity.Printed electronics overcome conventional etch preparation
The problems such as complex process present in wiring board process, waste of resource and generation a large amount of chemical contaminations, the spirit of its simple production process
Living, cost is low, meets the development trend of " green production ", is the mainstream technology of following printed wiring board.Current printed electronic skill
Art has been successfully applied to electronic tag (RFID), OTFT (OTFT), PCB editions, the field such as solar energy grid, has
Vast potential for future development.
In numerous ink deposition process, 3D printing technique is due to high and can be with noncontact, without mask, yields
Cause the extensive concern of people in three dimensions the advantages of selective deposition multiple material.High-precision 3D printer can be by circuit
The precision of plate is brought up in micrometer range；3D printing relies on digital information to be processed, can be quickly real by computer software
Now to the adjustment of deposited picture；In addition, 3D printing equipment has simultaneous well with extensive volume to volume (R2R) production technology
Capacitive, can quickly put among large-scale production after the completion of being manufactured experimently in laboratory.
The difficult point that 3D printing technique is applied into printed electronic production at present is the preparation of 3D printing conductive ink.
In metal nano conductive ink, silver ink have concurrently conduct electricity very well, it is not oxidizable, moderate the advantages of turn at present gold
Belong to the emphasis of nanometer conductive ink research.Application number 201010166965.X discloses a kind of preparation side of nano silver conductive ink
Method, can make below particle diameter 10nm nano-Ag particles stable dispersion in the ink.But used in the preparation process of ink
Organic acid destroys the pH value of ink and is adjusted, it is necessary to add alkaline complexing agent, reduce Nano Silver as protective agent
Mass content, and the stability to ink is not described in detail.
Conductive ink needs to take into account ink rheological properties, stability, sintering temperature, conductive materials in preparation process to be contained
Many-sided parameter such as amount, wherein stability of ink are particularly important for evaluating drop mass.Due to silver in nano silver conductive ink
Scattered with form of nanoparticles, the specific surface energy of ink is high, and nano-Ag particles can be sent to bulky grain aggregation certainly to reduce system
Surface energy, this aggregation can make particle heavy poly-, reduce the stability of ink.The particle reunited in ink can influence print pattern matter
Amount, or even block shower nozzle.Therefore it is that 3D printing technique is applied into extensive print to prepare the ink that can disperse steadily in the long term
The essential condition of brush electronics production.
The content of the invention
In view of the shortcomings of the prior art, the technical problem that the present invention is intended to solve is to provide a kind of preparation of conductive silver ink
Method.This method preparation technology is simple, and the stability of ink prepared is good, can be preserved with the long period.
The technical scheme that the present invention solves the technical problem is to provide a kind of preparation method of conductive silver ink, and it is special
Levy and be that the method includes the steps of：
(1) by the solvent of 10-18 mass parts and the dispersant of 0.1-0.4 mass parts, stirring to dispersant and solvent
It is well mixed, obtain solution；
(2) under the conditions of ultrasonic disperse, the nano-Ag particles of 2-5 mass parts are added into step 1) in obtained solution, obtain
To nano silver dispersion；
(3) to step 2) pH adjusting agents of 0.1-0.2 mass parts is added in obtained nano silver dispersion, make pH adjusting agent
It is completely dispersed；
(4) surface tension modifier of 0.02-1 mass parts and the tackifier of 0.8-2 mass parts are added, is stirred；
(5) preservative, the defoamer and 0.02-0.1 of 0.02-0.1 mass parts of 0.002-0.02 mass parts are separately added into
The adhesive of mass parts, stirring obtains mixed liquor to well mixed；
(6) mixed liquor is filtered, removes the conductive silver ink that precipitation obtains stable dispersion；
The solvent be ethanol, isopropanol, butanol, ethylene glycol, pentane, n-hexane, normal heptane, normal octane, n -nonane,
N-dodecane, pentamethylene, hexamethylene, methyl cyclopentane, hexahydrotoluene, petroleum ether, tetrahydrofuran, benzene,toluene,xylene,
At least one of carbon tetrachloride, ethyl acetate or butyl acetate；
The dispersant be selected from polyvinylpyrrolidone, polyvinyl alcohol, polyethylene glycol, polyamide, polyurethane, polycarboxylic acids,
At least one in diethanol amine, commodity Disper 9170, commodity BYK-180, commodity BYK-190 or commodity Spredox D-260
Kind；
The pH adjusting agent is schorl, dravite, elbaite, chromium dravite, buergerite, iron magnesium electricity
At least one of gas stone, alum dravite, calcium elbaite, uvite, alkali-free elbaite or alkali-free iron tourmaline.
Compared with prior art, beneficial effect of the present invention is：Add pH environment of the nano-tourmaline particle to ink
It is adjusted.PH is to influence the key factor of stability of ink：Adhesive such as acrylate in ink etc. is relatively low in pH
In the environment of be insoluble, the dispersibility of part dispersant also changes with pH change.Meanwhile, tourmaline to negative and positive from
The absorption of son can reduce the presence of free charge in ink, prevent the stabilizer on nano-Ag particles by ion substitution.It is based on
Both the above mechanism, nano-Ag particles can be significantly improved in ink by adding nano-scaled electric stone particle in silver ink
Dispersion effect in water, improves the holding time of ink.Tourmaline has a permanent spontaneous polarization effect, its two ends band respectively
There are the different electric charges of both positive and negative.Tourmaline can absorb negative electrical charge by positive electrode, and electric charge can be delivered into negative electricity by itself
Pole, while negative electrode discharges anion again, forms electric field.Based on spontaneous polarization effect, tourmaline particle can assist Nano Silver
Electronics is transmitted, the electric conductivity of printing wire is improved.
Embodiment
The specific embodiment of the present invention is given below.Specific embodiment is only used for that the present invention is further described, and does not limit
The application scope of the claims processed.
The invention provides a kind of preparation method of conductive silver ink (abbreviation method), it is characterised in that this method include with
Lower step：
(1) by the solvent of 10-18 mass parts and the dispersant of 0.1-0.4 mass parts, stirring 1-5min to dispersant
It is well mixed with solvent, obtains solution；
(2) under the conditions of ultrasonic disperse, the nano-Ag particles of 2-5 mass parts are added into step 1) in obtained solution, surpass
Sound 30-60min obtains nano silver dispersion；
(3) to step 2) pH adjusting agents of 0.1-0.2 mass parts is added in obtained nano silver dispersion, make ink pH value
For 7 or so, ultrasonic 30-60min is completely dispersed pH adjusting agent；
(4) surface tension modifier of 0.02-1 mass parts and the tackifier of 0.8-2 mass parts are added, 1- is stirred
5min, control surface tension force is in 25-30dyn/cm, viscosity 3-20cP；
(5) preservative, the defoamer and 0.02-0.1 of 0.02-0.1 mass parts of 0.002-0.02 mass parts are separately added into
The adhesive of mass parts, stirring 1-5min obtains mixed liquor to well mixed；
(6) it is 0.22 μm or 0.45 μm of micro-filtrate membrane filtration by mixed liquor aperture, removes precipitation and obtain leading for stable dispersion
Electric silver inks water.
The nano-Ag particles are ball-type nano-Ag particles, and particle diameter is 20-1000nm；
The solvent be ethanol, isopropanol, butanol, ethylene glycol, pentane, n-hexane, normal heptane, normal octane, n -nonane,
N-dodecane, pentamethylene, hexamethylene, methyl cyclopentane, hexahydrotoluene, petroleum ether, tetrahydrofuran, benzene,toluene,xylene,
At least one of carbon tetrachloride, ethyl acetate or butyl acetate；
The dispersant be selected from polyvinylpyrrolidone, polyvinyl alcohol, polyethylene glycol, polyamide, polyurethane, polycarboxylic acids,
At least one in diethanol amine, commodity Disper 9170, commodity BYK-180, commodity BYK-190 or commodity Spredox D-260
Kind；
The pH adjusting agent is nano-scaled electric stone particle, and particle size range is 10-1000nm；The nano-scaled electric stone
Grain is schorl, dravite, elbaite, chromium dravite, buergerite, iron dravite, alum dravite, calcium
At least one of elbaite, uvite, alkali-free elbaite or alkali-free iron tourmaline；
The surface tension modifier is APES -10, dodecyl sodium sulfate, polyacrylamide, poly-
Acrylate, ether modified dimethyl polysiloxane, triethanolamine, commodity GSK511, commodity AK505, commodity CFL7260, commodity
At least one of Surfynol 465, commodity Dynol 607；
The tackifier are terpinol or nylon acid methyl esters；
The preservative is benzoic acid or dehydroactic acid；
The defoamer is at least one of 2-Ethyl Hexanol, isooctanol, isoamyl alcohol or diisobutyl carbinol (DIBC)；
Described adhesive is cellulose acetate, nitrocellulose, hydroxypropyl methyl cellulose, acetylbutyrylcellulose, ring
At least one of oxygen tree fat, acrylate, polyester resin, polyamide or polyimide resin；
The conductive silver ink prepared according to this method is applied to the technologies such as 3D printing, inkjet printing and aerosol spray printing
In；
Embodiment 1
(1) 1g polyvinylpyrrolidones are dissolved in 50ml ethanol solutions, 5min is stirred under room temperature environment to poly- second
Alkene pyrrolidone is completely dissolved.
(2) 8g particle diameters 35nm nano-Ag particles are slowly added in whipping process, then sonic oscillation 30min is to receiving
Rice Argent grain is completely dispersed, and obtains nano silver dispersion.
(3) 0.5g particle diameters 35nm dravite particle is slowly added into nano silver dispersion in whipping process,
Then sonic oscillation 30min is completely dispersed to tourmaline particle.
(4) 0.5g dodecyl sodium sulfates and 2.5g terpinols are added, 5min is stirred so that solution surface tension is
25.2dyn/cm, viscosity is 3.2cP, meets 3D printing ink rheological property requirement.
(5) 0.1g benzoic acid, 0.1g 2-Ethyl Hexanols and 0.1g polyimide resins are added, stirring 5min is equal to mixing
It is even.
(6) filtered using 0.22 μm of filter membrane, remove precipitation, obtain the 3D printing nano-silver conductive ink of stable dispersion
Water.
Ink can stablize preservation more than 90 days at normal temperatures, and conductance improves 43% compared with without tourmaline.
Embodiment 2
(1) 1g polyvinyl alcohol is dissolved in 50ml ethanol solutions, 5min is stirred under room temperature environment complete to polyvinyl alcohol
Fully dissolved.
(2) 8g particle diameters 35nm nano-Ag particles are slowly added in whipping process, then sonic oscillation 30min is to receiving
Rice Argent grain is completely dispersed, and obtains nano silver dispersion.
(3) 0.5g particle diameters 35nm uvite particle is slowly added into nano silver dispersion in whipping process
In, then sonic oscillation 30min is completely dispersed to tourmaline particle.
(4) 0.8g APESs -10 and 2.5g terpinols are added, 5min is stirred so that solution surface tension
For 25.7dyn/cm, viscosity is 3.4cP, meets 3D printing ink rheological property requirement.
(5) 0.1g benzoic acid, 0.1g 2-Ethyl Hexanols and 0.1g polyimide resins are added, stirring 5min is equal to mixing
It is even.
(6) filtered using 0.45 μm of filter membrane, remove precipitation, obtain the 3D printing nano-silver conductive ink of stable dispersion
Water.
Ink can stablize preservation more than 65 days at normal temperatures, and conductance improves 35% compared with without tourmaline.
Embodiment 3
(1) 1g polyvinylpyrrolidones are dissolved in 25ml ethanol and 25ml ethylene glycol mixed solutions, in room temperature environment
Lower stirring 5min is completely dissolved to polyvinylpyrrolidone.
(2) 8g particle diameters 35nm nano-Ag particles are slowly added in mixed solution in whipping process, then ultrasound is shaken
Swing 30min to be completely dispersed to nano-Ag particles, obtain nano silver dispersion.
(3) 0.5g particle diameters 35nm buergerite particle is slowly added into nano silver dispersion in whipping process
In, then sonic oscillation 30min is completely dispersed to tourmaline particle.
(4) 0.5g dodecyl sodium sulfates and 2g nylon acid methyl esters are added, 5min is stirred so that solution surface tension is
27.1dyn/cm, viscosity is 5.7cP, meets ink jet ink for printing rheological property requirement.
(5) 0.1g benzoic acid, 0.1g 2-Ethyl Hexanols and 0.1g polyimide resins are added, stirring 5min is equal to mixing
It is even.
(6) filtered using 0.22 μm of filter membrane, remove precipitation, obtain the inkjet printing nano-silver conductive of stable dispersion
Ink.
Ink can stablize preservation more than 70 days at normal temperatures, and conductance improves 39% compared with without tourmaline.
Embodiment 4
(1) 1g polyvinylpyrrolidones are dissolved in 20ml ethanol and 30ml ethylene glycol mixed solutions, in room temperature environment
Lower stirring 5min is completely dissolved to polyvinylpyrrolidone.
(2) 8g particle diameters 35nm nano-Ag particles are slowly added in whipping process, then sonic oscillation 30min is to receiving
Rice Argent grain is completely dispersed, and obtains nano silver dispersion.
(3) 0.5g particle diameters 35nm alkali-free elbaite particle is slowly added into nano silver dispersion in whipping process
In, then sonic oscillation 30min is completely dispersed to tourmaline particle.
(4) 0.5g polyacrylamides and 2g terpinols stirring 5min are added so that solution normal temperature lower surface tension force is
29.6dyn/cm, viscosity is 7.8cP, meets aerosol spray printing ink rheological property requirement.
(5) 0.1g benzoic acid, 0.1g 2-Ethyl Hexanols and 0.1g cellulose acetates are added, stirring 5min is to well mixed.
(6) filtered using 0.22 μm of filter membrane, remove precipitation, the aerosol spray printing for obtaining stable dispersion is led with Nano Silver
Electric ink.
Ink can stablize preservation more than 70 days at normal temperatures, and conductance improves 40% compared with without tourmaline.
The present invention does not address part and is applied to prior art.
Claims (9)
1. a kind of preparation method of conductive silver ink, it is characterised in that the method includes the steps of：
(1) by the solvent of 10-18 mass parts and the dispersant of 0.1-0.4 mass parts, stirring to dispersant is mixed with solvent
Uniformly, solution is obtained；
(2) under the conditions of ultrasonic disperse, the nano-Ag particles of 2-5 mass parts are added into step 1) in obtained solution, received
The silver-colored dispersion liquid of rice；
(3) to step 2) pH adjusting agents of 0.1-0.2 mass parts is added in obtained nano silver dispersion, make pH adjusting agent complete
It is scattered；
(4) surface tension modifier of 0.02-1 mass parts and the tackifier of 0.8-2 mass parts are added, is stirred；
(5) preservative, the defoamer of 0.02-0.1 mass parts and 0.02-0.1 mass of 0.002-0.02 mass parts are separately added into
The adhesive of part, stirring obtains mixed liquor to well mixed；
(6) mixed liquor is filtered, removes the conductive silver ink that precipitation obtains stable dispersion；
The solvent is ethanol, isopropanol, butanol, ethylene glycol, pentane, n-hexane, normal heptane, normal octane, n -nonane, positive ten
Dioxane, pentamethylene, hexamethylene, methyl cyclopentane, hexahydrotoluene, petroleum ether, tetrahydrofuran, benzene,toluene,xylene, tetrachloro
Change at least one of carbon, ethyl acetate or butyl acetate；
The dispersant is selected from polyvinylpyrrolidone, polyvinyl alcohol, polyethylene glycol, polyamide, polyurethane, polycarboxylic acids, diethyl
At least one of hydramine, commodity Disper 9170, commodity BYK-180, commodity BYK-190 or commodity Spredox D-260；
The pH adjusting agent is that schorl, dravite, elbaite, chromium dravite, buergerite, iron magnesium are electric
At least one of stone, alum dravite, calcium elbaite, uvite, alkali-free elbaite or alkali-free iron tourmaline.
2. the preparation method of conductive silver ink according to claim 1, it is characterised in that the nano-Ag particles are ball-type
Nano-Ag particles, particle diameter is 20-1000nm.
3. the preparation method of conductive silver ink according to claim 1, it is characterised in that the pH adjusting agent is nanoscale
Tourmaline particle, particle size range is 10-1000nm.
4. the preparation method of conductive silver ink according to claim 1, it is characterised in that the surface tension modifier is
APES -10, dodecyl sodium sulfate, polyacrylamide, polyacrylate, ether modified polydimethyl silica
In alkane, triethanolamine, commodity GSK511, commodity AK505, commodity CFL7260, commodity Surfynol 465, commodity Dynol 607
At least one.
5. the preparation method of conductive silver ink according to claim 1, it is characterised in that the tackifier be terpinol or
Nylon acid methyl esters.
6. the preparation method of conductive silver ink according to claim 1, it is characterised in that the defoamer be diethyl oneself
At least one of alcohol, isooctanol, isoamyl alcohol or diisobutyl carbinol (DIBC).
7. the preparation method of conductive silver ink according to claim 1, it is characterised in that described adhesive is acetate fiber
Element, nitrocellulose, hydroxypropyl methyl cellulose, acetylbutyrylcellulose, epoxy resin, acrylate, polyester resin,
At least one of polyamide or polyimide resin.
8. the preparation method of conductive silver ink according to claim 1, it is characterised in that the preservative be benzoic acid or
Dehydroactic acid.
9. the conductive silver ink that a kind of preparation method of any described conductive silver inks of claim 1-8 is prepared, it is special
Levy and be that the conductive silver ink is applied to 3D printing, inkjet printing or aerosol spray printing.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107446413A (en) * | 2017-09-14 | 2017-12-08 | 中国科学院深圳先进技术研究院 | A kind of electrically conductive ink and preparation method thereof |
| CN109535849A (en) * | 2018-12-18 | 2019-03-29 | 盐城工学院 | A kind of ink-jet nano silver conductive ink and preparation method thereof |
| CN109777202A (en) * | 2017-11-10 | 2019-05-21 | 上海宝银电子材料有限公司 | A kind of electronic tag electrically conductive ink and preparation method thereof |
| CN110894381A (en) * | 2019-12-19 | 2020-03-20 | 河北工业大学 | Preparation method of nano-silver ink |
| CN110982349A (en) * | 2019-12-05 | 2020-04-10 | 陕西科技大学 | Preparation method of 3D printing conductive ink used on paper |
| CN111180107A (en) * | 2020-01-06 | 2020-05-19 | 青岛理工大学 | Preparation method for electric field driven injection of micro-nano 3D printing nano silver paste |
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| CN105694596A (en) * | 2016-04-08 | 2016-06-22 | 苏州捷德瑞精密机械有限公司 | Low-silver copper-base conductive ink and preparation method thereof |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107446413A (en) * | 2017-09-14 | 2017-12-08 | 中国科学院深圳先进技术研究院 | A kind of electrically conductive ink and preparation method thereof |
| CN109777202A (en) * | 2017-11-10 | 2019-05-21 | 上海宝银电子材料有限公司 | A kind of electronic tag electrically conductive ink and preparation method thereof |
| CN109535849A (en) * | 2018-12-18 | 2019-03-29 | 盐城工学院 | A kind of ink-jet nano silver conductive ink and preparation method thereof |
| CN110982349A (en) * | 2019-12-05 | 2020-04-10 | 陕西科技大学 | Preparation method of 3D printing conductive ink used on paper |
| CN110894381A (en) * | 2019-12-19 | 2020-03-20 | 河北工业大学 | Preparation method of nano-silver ink |
| CN111180107A (en) * | 2020-01-06 | 2020-05-19 | 青岛理工大学 | Preparation method for electric field driven injection of micro-nano 3D printing nano silver paste |
| CN111180107B (en) * | 2020-01-06 | 2021-09-21 | 青岛理工大学 | Preparation method for electric field driven injection of micro-nano 3D printing nano silver paste |
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| CN107118620B (en) | 2020-12-29 |
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