CN103965695B - A kind of electrically conductive ink containing micro-nano composition metal filler - Google Patents
A kind of electrically conductive ink containing micro-nano composition metal filler Download PDFInfo
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Abstract
The invention discloses a kind of electrically conductive ink containing micro-nano composition metal filler.The described electrically conductive ink containing micro-nano composition metal filler, it is characterised in that form and percentage composition is: main conductive filler: 10～60%；Auxiliary conductive filler: 1～10%；Binder: 1～5%；Additive: 1～5%；Bulk solvent: 30～85%.The present invention uses micro-nano complex technique, it is achieved that tightly packed between micron order and nanoscale metal particles, increases the contact area between metallic particles, improves conductive performance and the current capacity of printed circuit；Utilize the low-melting advantage of nano metal, can be at a relatively low sintering temperature, it is achieved excellent electric conductivity.The electrically conductive ink of the present invention can prepare conducting channel at multiple printing on substrates, the circuit layer of preparation has good electric conductivity, excellent adhesive force and higher hardness, can realize the regulation and control to electronics, have broad application prospects in the field such as electronic device, surface-mounted integrated circuit.
Description
Technical field
The present invention relates to a kind of electrically conductive ink containing micro-nano composition metal filler, prepare particularly to printing conductive inks
Circuit layer, belongs to printed circuit and manufactures field.
Background technology
Electrically conductive ink is a kind of specific function ink containing conductive compositions, on the basis of Conventional printing process, permissible
Realize the quick manufacture of conduction portion in electronic apparatus.Electrically conductive ink can be widely used for printing touch, Er Tongwan at present
Tool circuit, silicon solar battery electrode, sensor, electrode contacts, radio-frequency antenna, plating, multilayer circuit board grout
Etc. aspect.
One of core starting materials of electrically conductive ink or printed electronics circuit.In recent years, American-European, Japan, Korea S and
The ground such as China Taiwan are rising a revolutionary circuit board production techniques printed electronics circuit (Printed
Electronic Circuit), i.e. use functional ink directly to print out electronic circuit on printing plate, as having in flexibility
On machine film, printing conductive inks obtains conducting wire, and printed semiconductor ink obtains transistor or memory component etc..
The printed electronics circuit of this new generation is to contain electronics to connect circuit and the assembly of element, can substitute traditional printing
The function of circuit board mounting related components again.
Electrically conductive ink is mainly made up of following four parts: (1) conductive filler: provide the main part of conduction (to include gold
Belong to powder, metal oxide, nonmetal and other composite powders)；(2) binder: coating moiety (mainly has synthesis
Resin, photosensitive resin, low melting point lucite etc.)；(3) additive (also referred to as auxiliary agent): be adapted to printing and become
Films etc. (mainly have dispersant, conditioning agent, thickener, plasticizer, lubricant, inhibitor etc.)；(4) solvent is (main
Aromatic hydrocarbons to be had, alcohol, ketone, alcohol ether etc.) composition.Wherein conductive filler is the Core Feature composition of electrically conductive ink.
Currently, including the electrically conductive ink sold on market and use in electronics industry, its core conductive compositions is the most micro-
Meter level metallic particles, its grain shape mainly have circle and sheet (see Tong Li state CN101429358A mono-kind
The preparation method of electrically conductive ink, CN1741198 high-temperature sintered silver paste such as Wang Zisen and preparation method thereof；Quote document).
In recent years, along with the progress of nanometer technology, it is achieved that prepared by the scale of metal nano material, therefore, occur in that to receive
Rice metallic particles is electrically conductive ink (Beijing University of Chemical Technology, Wei Jie, the king CN101348634A mono-kind of functional stuffing
Photo-curing ink-jet nano conductive printing ink and preparation method thereof and using method；LG Co., Ltd. of Korea S Lee Zong Ze etc.
CN101522557A, for ink jet printing and used in the preparation method of metal nanoparticle；Draw
With document).
Connecting terminal between metallic particles is the most, i.e. contact area is the biggest, and its electric conductivity is the best.Micron particles
Owing to its size is relatively big, the gap between its particle increases the most accordingly, therefore, will increase its intergranular contact area,
One is that grain shape is changed into sheet by circle, and two are to increase the proportion of particle；Nanoscale metal particles not only can show
Write and increase contact area, and due to its small-size effect, it is possible to decrease the fusing point of metal, can be melted by low-temperature sintering
Merging into an organic whole, electric conductivity significantly improves.But at present nano-metal particle manufacturing cost is the highest, be also not suitable for completely by
Nano metal does conductive filler.
The present invention proposes using micrometer metal particles as main conductive filler, nano-metal particle as auxiliary conductive filler,
Under lower sintering temperature, utilize nano metal filler melted by integral for micrometer metal particles adhesion, it is achieved relatively low
Tenor, shows excellent conductive performance.
Summary of the invention
It is an object of the invention to provide a kind of electrically conductive ink containing micro-nano composition metal filler, this electrically conductive ink can be adopted
On different base materials, circuit is formed with different mode of printing printings.By micro-sized metal particle and nano level metal
Particles dispersed, it is achieved tightly packed between metallic particles, increases the contact area between metallic particles, improves printed
The conductive performance of circuit and current capacity；Utilize the low-melting advantage of nano metal, can at a relatively low sintering temperature,
Realize excellent electric conductivity.
The present invention realizes in the following way, a kind of electrically conductive ink containing micro-nano composition metal filler, its feature
It is: be made up of following component and mass percent:
Main conductive filler: 10～60%
Auxiliary conductive filler: 1～10%
Binder: 1～10%
Additive: 1～5%
Bulk solvent: 30～85%
Above-mentioned each constituent mass percentage composition sum is 100%；
Described main conductive filler is made up of micro-sized metal particle, wherein metal include but not limited to gold, silver, copper,
At least one in aluminum metal particle, its particle size range is 0.1 μm～10 μm.
Described auxiliary conductive filler is made up of nanoscale metal particles, wherein metal include but not limited to gold, silver, copper,
At least one in aluminum metal particle, its particle size range is 1nm～100nm.
Described binder includes but not limited to it is polyacrylic acid, polymethylacrylic acid, polyvinylpyrrolidone, poly-second
Glycol, polyvinyl alcohol, phenolic resin, alkyd resin, epoxy resin, styrene and copolymer-maleic anhydride, benzene second
Alkene and acrylic copolymer, acrylic acid and acrylate copolymer, polyvinyl formal, butene dioic acid resin, poly-
Amide resin, vinyl chloride-vinyl acetate resin, butyl etherified melamine resin, polyvinyl butyral resin, cellulose, heteroglycan,
One or both in organic siliconresin, gum arabic.
Described additive includes but not limited to levelling agent, pH value regulator, surfactant.
Described bulk solvent can be but not limited to ethanol, ethylene glycol, isopropanol, diethylene glycol (DEG), triethylene glycol, second two
Alcohol methyl ether, ethylene glycol ethyl ether, butyl glycol ether, ethylene glycol phenyl ether, ethylene glycol benzyl oxide, health alcohol, morpholine, diethylene glycol (DEG)
Methyl ether, DGDE, butyl carbitol, triethylene glycol methyl ether, diacetone alcohol, triethanolamine, sulfolane, diformazan
Sulfoxide, 1-METHYLPYRROLIDONE, dimethylacetylamide, carbitol acetate, linseed oil, high-boiling point kerosene, 13
Alcohol, tung oil, common colloid oil, tetradecyl alchohol, pentaerythrite, soybean oil, retinal, virtue camphor tree terpinol, adjacent benzene two
Formic acid dioctyl ester, ethyl acetate, butyl acetate, cyclohexanone, dimethylbenzene, bicyclohexyl, hexamethylene, n-butanol,
Butanone, deionized water, hydroxyethyl-pyrrolidone, repefral, oxirane, D-sorbite, salad
One or both in oil, palm oil, peppermint oil.
A kind of electrically conductive ink containing micro-nano composition metal filler, comprising step is:
(1) in bulk solvent, binder, levelling agent, pH adjusting agent and surfactant are added according to mass ratio,
Stirring 30min, mixes, obtains binder solution；
(2) in binder solution, it is separately added into main and auxiliary conductive filler according to mass ratio, continues to stir,
Electrically conductive ink to micro-nano composition metal filler；
(3) electrically conductive ink prepared forms circuit layer by different mode of printing printings on different base materials.
Wherein, in described step (1)
Described levelling agent is in polyacrylate, cellaburate, polymethyl siloxane and fluorocarbons
Kind；
Described pH value regulator is the one in ammoniacal liquor, NaOH, triethanolamine, sodium phosphate and azanol；
Described surfactant be aliphatic acid, fatty acid ester, neopelex, lauryl sodium sulfate,
One in polyoxyethylene alkylamide, polysiloxanes, polysorbate and Sodium perfluorooctanoate；
The ratio of described various additives is 1～5%.
In described step (2)
Weight ratio between described main conductive filler and auxiliary conductive filler is not less than 4: 1；
The grain shape of described conductive filler can be, but not limited to be the shapes such as spherical, sheet, disk, triangle；
The described ratio between conductive filler (including main conductive filler and auxiliary conductive filler) and binder is not less than 5: 1.
In described step (3)
Described mode of printing includes but not limited to serigraphy, offset printing, flexo and spray printing.
Described electrically conductive ink carries out property regulation according to printed substrate, suitably prints on different printed substrates after regulation,
Printed substrate include but not limited to polyimides, polyester, polyvinyl chloride, epoxy, pottery, papery, tetrafluoro, glass,
Half glass, bi-maleimide modified cyanate resin, polyimide resin, diphenylene ether resin, maleic anhydride are sub-
Amine, styrene resin, poly-cyanate ester resin, vistanex, polyether ketone resin, polysulfone resin flexible parent metal and nitrogen
At least one in SiClx, aluminium nitride, aluminum oxide, metal, glass rigid base material.
There is advantages that
1, use micro-nano complex technique, nano-sized metal particles can be filled between micro-sized metal particle, greatly
Adding the contact area between particle and particle, printing can greatly strengthen after making circuit layer leads its electric conductivity.
2, utilize the low-melting feature that nano metal is exclusive, nano particle can melt at a lower temperature, play chain
Connect the effect of big particle diameter micron metal, thus on the circuit layer of shaping, conducting wire is more continuous, smoother, electric conductivity
More preferably, and there is good adhesive force and hardness.
3, the electrically conductive ink preparation technology of the present invention is simple, reduces production cost, it is simple to large-scale production.
Detailed description of the invention
Embodiment 1:
The silk-screened conductive ink that micro-nano is compound, particular make-up: by 3.5g polymethylacrylic acid, 0.5g levelling agent, 1.0g pH
Value conditioning agent and 1.5g surfactant join in 20g hexamethylene, stir 30min, mix；By 20g
Particle diameter is the sheet metal copper of 5 μm and the circular metal silver that 4g particle diameter is 20nm joins in above-mentioned solution, continues
Stir, be configured to electrically conductive ink；Use the vertical screen printer of the white HD-3050 of reaching that this electrically conductive ink is printed onto polyene
On hydrocarbon resin film, sintering 10min under the conditions of 150 DEG C, the thickness recording circuit layer is 11 μm, and sheet resistance is 252m Ω/,
Hardness is 3H, and adhesive force is that (0A indicates that, without adhesive force, 1A, 2A, 3A, 4A, 5A represent that adhesive force depends on to 4A
Secondary enhancing, adhesive force optimum is expressed as 5A).
Embodiment 2:
The offset printing electrically conductive ink that micro-nano is compound, particular make-up: by 5.0g butene dioic acid resin, 1.5g levelling agent, 1.5g pH
Value conditioning agent and 1.0g surfactant join in 25g oxirane, stir 30min, mix；By 25g
Particle diameter is the disk metallic aluminium of 8 μm and the circular metal silver that 5g particle diameter is 30nm joins in above-mentioned solution, continues
Stir, be configured to electrically conductive ink；Use Heidelberg print despot's PM52 offset press by this ink printing to 250g/m2
On art paper, sintering 30min under the conditions of 150 DEG C, the thickness recording circuit layer is 2 μm, and sheet resistance is 285m Ω/, firmly
Degree is 3H, and adhesive force is 5A.
Embodiment 3:
The spray printing electrically conductive ink that micro-nano is compound, particular make-up: by 3g styrene and acrylic copolymer, 0.8g levelling agent,
0.8g pH value regulator and 0.7g surfactant join in 30g diacetone alcohol, stir 30min, mix；
Triangle metal gold and the circular metal copper that 3g particle diameter is 10nm that 15g particle diameter is 2 μm are joined above-mentioned solution
In, continue to stir, be configured to electrically conductive ink；Use safe prestige flat board jet printer by this ink printing to polyvinyl chloride
On resin film, sintering 3min under the conditions of 200 DEG C, the thickness recording circuit layer is 1 μm, and sheet resistance is 180m Ω/,
Hardness is 4H, and adhesive force is 5A.
Embodiment 4
Micro-nano compound silk-screened conductive ink, particular make-up: by 3.0g alkyd resin, 0.6g levelling agent, 0.6g pH
Value conditioning agent and 0.8g surfactant join in 20g hexamethylene, the mixing of butyl carbitol solution, stir 30min,
Mix；Sheet metal gold and the circular metal silver that 5g particle diameter is 80nm that 24g particle diameter is 10 μm are added
In above-mentioned solution, continue to stir, be configured to electrically conductive ink；Use white reach the vertical screen printer of HD-3050 should
Ink printing, on sheet glass, sinters 10min under the conditions of 150 DEG C, the thickness recording circuit layer is 10 μm, and sheet resistance is
16.5m Ω/, hardness is 3H, and adhesive force is 5A.
Embodiment 5
The offset printing electrically conductive ink that micro-nano is compound, particular make-up: by 6.0g phenolic resin, 0.9g levelling agent, 1.2g pH value
Conditioning agent and 1.3g surfactant join in 35g 1-METHYLPYRROLIDONE, dimethylacetylamide mixed solution,
Stirring 30min, mixes；It is the circle of 100nm by disk metallic copper and 6.0g particle diameter that 28g particle diameter is 9 μm
Shape argent joins in above-mentioned solution, continues to stir, is configured to electrically conductive ink；Use Heidelberg print despot PM52
Offset press is by this ink printing to 200g/m2On art paper, sinter 30min under the conditions of 150 DEG C, record the thickness of circuit layer
Degree is 2.5 μm, and sheet resistance is 112m Ω/, and hardness is 3H, and adhesive force is 4A.
Embodiment 6
The spray printing electrically conductive ink that micro-nano is compound, particular make-up: by 3g butyl etherified melamine resin, 0.6g levelling agent,
0.8g pH value regulator and 0.6g surfactant join in 24g diacetone alcohol, stir 30min, mix；
Circular metal gold and the circular metal silver that 3.5g particle diameter is 1.0nm that 16g particle diameter is 0.1 μm are joined above-mentioned molten
In liquid, continue to stir, be configured to electrically conductive ink；Use safe prestige flat-plate ink jet printer by this ink printing to EPSON
On fine fleece waterproof RC printing paper, sintering 25min under the conditions of 200 DEG C, the thickness recording circuit layer is 2.5 μm, and sheet resistance is
86m Ω/, hardness is 3H, and adhesive force is 5A.
Embodiment 7
The flexo electrically conductive ink that micro-nano is compound, particular make-up: by 5g polyethylene glycol, 0.6g levelling agent, 0.8g pH value
Conditioning agent and 0.6g surfactant join in 34g hexamethylene, n-butanol, butanone mixed solution, stir 30min,
Mix；Sheet metal aluminium and the circular metal silver that 5g particle diameter is 100nm that 30g particle diameter is 6 μm are joined
In above-mentioned solution, continue to stir, be configured to electrically conductive ink；Beiren's BFR-500 printing machine is used to be printed by this ink
Brushing on EPSON fine fleece waterproof RC printing paper, sinter 20min under the conditions of 180 DEG C, the thickness recording circuit layer is 2.5 μm,
Sheet resistance is 252m Ω/, and hardness is 3H, and adhesive force is 5A.
Claims (10)
1. the electrically conductive ink containing micro-nano composition metal filler, it is characterised in that: by following component and mass percent
Composition:
Main conductive filler: 10～60%
Auxiliary conductive filler: 1～10%
Binder: 1～10%
Additive: 1～5%
Bulk solvent: 30～85%
Above-mentioned each constituent mass percentage composition sum is 100%；
Wherein micrometer metal particles as auxiliary conductive filler, utilizes nm of gold as main conductive filler, nano-metal particle
Belong to low-melting advantage, can be under relatively low tenor and relatively low sintering temperature, it is achieved excellent electric conductivity.
Electrically conductive ink containing micro-nano composition metal filler the most according to claim 1, it is characterised in that: described master
Conductive filler is made up of micro-sized metal particle, during wherein metal includes but not limited to gold, silver, copper, aluminum metal particle
At least one, its particle size range is 0.1 μm～10 μm.
Electrically conductive ink containing micro-nano composition metal filler the most according to claim 1, it is characterised in that: described is auxiliary
Conductive filler is made up of nanoscale metal particles, during wherein metal includes but not limited to gold, silver, copper, aluminum metal particle
At least one, its particle size range is 1nm～100nm.
Electrically conductive ink containing micro-nano composition metal filler the most according to claim 1, it is characterised in that: described adds
Add agent and include but not limited to levelling agent, pH value regulator and surfactant.
Electrically conductive ink containing micro-nano composition metal filler the most according to claim 1, it is characterised in that: comprise step
For:
(1) in bulk solvent, binder, levelling agent, pH value regulator and surfactant are added according to mass ratio,
Stirring 30min, mixes, obtains binder solution；
(2) in above-mentioned binder solution, it is separately added into main and auxiliary conductive filler according to mass ratio, continues to stir,
Obtain the electrically conductive ink of micro-nano composition metal filler；
(3) electrically conductive ink of above-mentioned preparation forms circuit layer by different mode of printing printings on different base materials.
Electrically conductive ink containing micro-nano composition metal filler the most according to claim 5, it is characterised in that: described step
Suddenly in (1), levelling agent is the one in polyacrylate, cellaburate, polymethyl siloxane and fluorocarbons.
Electrically conductive ink containing micro-nano composition metal filler the most according to claim 5, it is characterised in that: described step
Suddenly in (1), pH value regulator is the one in ammoniacal liquor, NaOH, triethanolamine, sodium phosphate and azanol.
Electrically conductive ink containing micro-nano composition metal filler the most according to claim 5, it is characterised in that: described step
Suddenly in (1), surfactant is aliphatic acid, fatty acid ester, neopelex, lauryl sodium sulfate, gathers
One in oxygen vinyl alkyl acid amides, polysiloxanes, polysorbate and Sodium perfluorooctanoate.
Electrically conductive ink containing micro-nano composition metal filler the most according to claim 5, it is characterised in that: described step
Suddenly in (2) mass ratio between main conductive filler and auxiliary conductive filler not less than 4: 1.
Contain the electrically conductive ink of micro-nano composition metal filler the most according to claim 1 or 5, it is characterised in that: institute
The electrically conductive ink stated carries out property regulation according to printed substrate, suitably prints on different printed substrates, printing after regulation
Base material include but not limited to polyimides, polyester, polyvinyl chloride, epoxy, pottery, papery, tetrafluoro, glass, half
Glass, bi-maleimide modified cyanate resin, polyimide resin, diphenylene ether resin, maleic anhydride imines,
Styrene resin, poly-cyanate ester resin, vistanex, polyether ketone resin, polysulfone resin flexible parent metal and silicon nitride,
At least one in aluminium nitride, aluminum oxide, metal, glass rigid base material.
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| CN105670384A (en) * | 2016-03-31 | 2016-06-15 | 广东南海启明光大科技有限公司 | Nano silver gravure ink and preparation method thereof |
| CN105778626A (en) * | 2016-05-27 | 2016-07-20 | 佛山市智巢电子科技有限公司 | Nanometer metal powder ink for ink-jet printing and preparation method thereof |
| TWI629337B (en) * | 2016-07-29 | 2018-07-11 | 余琬琴 | High-adhesion conductive copper colloid and screen printing application method thereof |
| CN107793864A (en) * | 2017-10-30 | 2018-03-13 | 汪涛 | A kind of preparation method of conducting paint composite |
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| JP2019172862A (en) * | 2018-03-29 | 2019-10-10 | セイコーエプソン株式会社 | Inkjet composition and recorded matter |
| CN109021711B (en) * | 2018-08-02 | 2021-06-18 | 苏州蓝沛光电科技有限公司 | Printing ink for manufacturing touch screen with metal-containing grid structure |
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| 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 |
| CN113422084B (en) * | 2021-04-30 | 2023-02-03 | 上海交通大学 | A kind of titanium alloy surface micro-nano particle composite conduction enhancement structure and preparation method thereof |
| CN114025489B (en) * | 2021-10-27 | 2024-05-24 | 深圳市贝加电子材料有限公司 | Microetching solution for copper surface treatment, application of microetching solution in PCB (printed circuit board) manufacturing process and PCB production flow |
| CN115020119A (en) * | 2022-07-22 | 2022-09-06 | 寰宇新材料科技(江苏)有限公司 | A kind of multilayer composite electrode and preparation method thereof |
| CN117866484B (en) * | 2024-03-12 | 2024-06-04 | 成都先进金属材料产业技术研究院股份有限公司 | Liquid metal printing ink and preparation method thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101580660A (en) * | 2009-06-26 | 2009-11-18 | 无锡晶睿光电新材料有限公司 | Electrically conductive printing ink for printing circuit strips on flexible circuit board |
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101580660A (en) * | 2009-06-26 | 2009-11-18 | 无锡晶睿光电新材料有限公司 | Electrically conductive printing ink for printing circuit strips on flexible circuit board |
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