CN106297949B - High conductivity low temperature silver paste - Google Patents
High conductivity low temperature silver paste Download PDFInfo
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- CN106297949B CN106297949B CN201510282011.8A CN201510282011A CN106297949B CN 106297949 B CN106297949 B CN 106297949B CN 201510282011 A CN201510282011 A CN 201510282011A CN 106297949 B CN106297949 B CN 106297949B
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Abstract
The invention discloses a kind of high conductivity low temperature silver paste and preparation method thereof, high tenacity resin, thickener, toughener, curing agent, organic solvent is mixed successively scattered；Low-melting alloy, scaling powder, conductive silver powder are sequentially added, high-speed stirred, obtains slurry；Gained slurry is ground into 5~10 μm of fineness with three-roll grinder, up to conductive silver paste.Conductive silver paste prepared by the present invention has the advantages that high conductivity, high-mechanical property.Electrical conductivity performance and hardness performance are improved significantly after introducing low-melting alloy.By adding suitable thickener and toughener, diffusion and the bending performance of silver wire bar can be effectively controlled.Low temperature silver paste prepared by the invention, can effectively reduce silver content, improve electrical conductivity and mechanical performance, finished product is greatly saved, can be widely applied in the industries such as thin film switch, capacitance electrode, touch-screen.
Description
Technical field
The present invention relates to silver paste technical field, more particularly to a kind of high conductivity low temperature silver paste, available for thin film switch, electricity
Hold electrode, touch-screen.
Background technology
Electrocondution slurry is as a kind of feature print material because its good physical property obtains extensively in electronics and IT products
Application, as electronic product is more powerful and more environmentally friendly direction is developed to lighter, thinner, feature, to its performance it is also proposed that
The requirement of higher.Wherein low temperature Halogen conductive silver paste is widely used in film because of its excellent electric conductivity, thermal conductivity and practicality
Switch, capacitance electrode, touch-screen etc..Low-temperature conductive silver paste be using conductive silver powder as conductive filler, with polymeric resin,
Agitated, the scattered and manufactured uniform sizing material such as solvent, curing agent, auxiliary agent.After conductive silver paste is coated on base material, in low temperature ring
Drying (generally below 160 DEG C) under border, after solvent release, resin and curing agent step-reaction, curing, ultimately form densification
Conductive film layer.
In the raw material of conductive silver paste, resin etc. is insulator, and silver powder particles can be enveloped after curing, make silver powder with
It is spaced between silver powder by resin, the electric conductivity that result in whole film layer is greatly reduced.In order to meet the height in electronics industry
Electric conductivity, at present, the only effective method that research worker can take are exactly to improve the loading of silver powder particles in slurry,
In low-temperature conductive silver paste currently on the market, the Argent grain loading (hereinafter referred to as silver content) of Halogen silver paste is typically greater than
55%, some low temperature silver pastes have been even up to more than 70%, this just forces conductive silver paste to be substantially improved in cost, serious to hinder
The fast development of related industry.
In addition, in electronics industry, in order to meet the high intensity of product, high-mechanical property demand, low-temperature conductive silver paste is solid
Conductive film layer after change generally has mechanical requirement (film hardness, film layer and base material adhesive force etc.).Conductive silver powder is metal
Powder, hardness is of a relatively high, but the hardness of the high polymer such as resin is then general poor.And work as in a manner of improving silver powder loading to expire
During sufficient high rigidity demand, the resin of relatively small amount cannot fully, effectively coat silver powder, cause top layer silver powder absorption loosely to occur
Obscission.
Low-melting alloy, is the lead-free alloy that scientific worker's sight is gradually introduced after lead and its compound are forbidden
Compound, eutectic point is relatively low, its particle size and granularity point can effectively be controlled by preparing low-melting alloy powder by aqua-solution method
Cloth, this just makes it possible low-melting alloy powder being introduced in conductive ink systems；But the prior art is found because introducing
Low-melting alloy, system may be brought after curing spreads the unfavorable factors such as larger and brittleness is big, limits low-melting alloy
Using low-melting alloy is introduced in low-temperature conductive silver slurry system by seldom researcher at present.
The content of the invention
The object of the present invention is to provide a kind of high conductivity low temperature silver paste, it combines inorganic material and high molecular material is compound
Material technology, design is unique, and composition is reasonable, and it is convenient to prepare, and has excellent electric conductivity, and good with substrate compatibility, attached
Put forth effort, environmental pollution is small；And low-temperature setting technique can be used for, flow to be simple, and production efficiency is high, avoids manual operation
The damage brought, product rejection is few, beneficial to reducing cost.
To reach above-mentioned purpose, the technical solution adopted by the present invention is：A kind of high conductivity low temperature silver paste, by weight
Meter, it is composed of the following components：
The high tenacity resin is saturated polyester resin, the one or more in polyacrylic resin, polyurethane；
The boiling point of the organic solvent is 100~250 DEG C；
The conductive silver powder particle diameter is 0.1~20 μm.
The high tenacity resin of the present invention is toughness polymeric resin, and this area thinks that the resin of elongation ＞ 200% can claim
For high tenacity resin；One or more in saturated polyester resin, polyacrylic resin or polyurethane, its glass transition temperature
It it is preferably 10-40 DEG C for 0-50 DEG C；And containing the polymer resin for having excellent flexibility that can be rolled into a ball with reactivity hat, it is described anti-
Answer functional group to be selected from hydroxyl, carboxyl, epoxy group or isocyanate group, be preferably hydroxyl.
In above-mentioned technical proposal, selected organic solvent boiling point is 100~250 DEG C, is preferably 180~210 DEG C；Volatility is small
In 0.1,0.03 is preferably less than, is preferably esters and ketones solvent.In the present invention, organic solvent can with regulation system viscosity,
Silver paste application property is adjusted, each component is uniformly dispersed, improves the concertedness of system, so as to obtain the highly conductive of high comprehensive performance
Low temperature silver paste.
In above-mentioned technical proposal, the conductive silver powder is spherical, near-spherical, sheet, dendroid etc., preferably sheet；Institute
Conductive silver powder particle diameter is stated as 0.1~20 μm, is preferably 0.5~6 μm.
In above-mentioned technical proposal, the thickener is selected from hydroxyethyl cellulose, modified alta-mud or aerosil
In one or more.Thickener is mixed in resin system, adjusts the viscosity of system, there is provided excellent paintability, is beneficial to
The processability of silver paste improves；Good with resin infiltration at the same time, its surface dipole effect can produce interface interaction with resin, improve tree
Performance after the curing of fat, increases the wearability of system.
In above-mentioned technical proposal, the toughener is selected from a kind of liquid nitrile rubber.
In above-mentioned technical proposal, the curing agent is selected from the blocked isocyanate that deblocking temperature is less than 150 DEG C.
In above-mentioned technical proposal, the low-melting alloy selects the Sn of different-grain diameter58Bi42Alloy powder, preferable particle size
For less than 10 μm powders.
In above-mentioned technical proposal, the scaling powder is selected from a kind of disposable halogen-free scaling powder, by rosin resin derivative, has
Machine acid activators and organic solvent etc. form.
Invention introduces the Sn that fusing point is 138 DEG C58Bi42Powder, introduce scaling powder make its melted under heating environment and
Metallurgical connection is formed, reduces the silver content of system, reduces cost, while is obstructed from resin, ensures electric conductivity.Overcome existing
The technical barrier that resin declines the electric conductivity that conductive particle wrap comes in technology.
But due under aerobic conditions, Sn58Bi42The top layer of powder is oxidized easily and coats one layer of oxide, these
The fusing point of oxide is apparently higher than Sn58Bi42The fusing point of powder, reaches after fusing point is melted into liquid, these oxides are still in powder
The Sn of liquid is surrounded in the form of " spherical shell "58Bi42, without can be uniformly dispersed in silver powder and commercial resin；The present invention passes through introducing
The scaling powder of Halogen disperses after strengthening powder body melting, is effectively formed metallurgical connection, improves electrical conductivity, improves mechanical performance.
Additionally, due to Sn58Bi42Into liquid after thawing, mobility is strong, and diffusion can be more serious after being printed as lines, and when cold
But after curing, brittleness is big, can influence its bending resistance；Present invention introduces the auxiliary agents such as thickener and toughener to improve silver paste flowing
State and after curing top layer compliance, that improves silver wire bar the performance such as spreads, is resistant to bending.
The electric conductivity of silver paste derives from conducting metal and the concertedness of conducting metal and resin system.Selected by the present invention
High tenacity polymeric resin with reactive group, while silver paste electric conductivity is improved, ensures that coating has good attachment
Power and abrasion resistance.Wherein conductive silver powder dosage is low, far below silver powder dosage in existing low-temperature conductive silver paste, effectively reduces
The cost of system, strength promote the development of related industry.The present invention by low-melting alloy introduce silver paste system, reduce silver paste into
This while, ensured the due high conduction performance of silver paste system, by the coordinated with the auxiliary agent such as scaling powder, solves existing
There is the defects of low-melting alloy is brought in technology mechanicalness is worse so that low-melting alloy can really be applied to low-temperature conductive
Silver paste system, achieves unexpected technique effect.
In above-mentioned technical proposal, silver powder content is low, can effectively be infiltrated by resin, ensure that the compatible of organic-inorganic thing
Property, also improves the adhesive force of silver paste coating and base material；Simultaneously because low melting point electrical conductivity alloy forms metallurgical connection so that silver paste
Density of connecting in system, between metal is high, ensure that the electric conductivity of whole film layer.So silver powder content of the present invention is low, drop significantly
While inexpensive, the electric conductivity of system ensure that, overcome and silver powder is only significantly increased in the prior art could improve conduction
The technology prejudice of property.
Preferably, by weight, the high conductivity low temperature silver paste is composed of the following components：
The invention also discloses the preparation method of above-mentioned high conductivity low temperature silver paste, comprise the following steps：
High tenacity resin, thickener, toughener, curing agent, organic solvent are mixed successively scattered；Sequentially add
Low-melting alloy, scaling powder, conductive silver powder, high-speed stirred, obtains slurry；Gained slurry is ground into fineness with three-roll grinder
5~10 μm, up to conductive silver paste.
In above-mentioned technical proposal, high-speed stirred rotating speed turns/min, time 10-15min for 1000-1200.
For low-temperature conductive silver paste in addition to high conductivity requirement, its bonding force to base material, mechanical property are also key
Can, the prior art does not meet the method for the requirement well, and only in production, constantly modification adjusts formula, meets a certain
Performance and reduce other performances；But so cause that a batch is small, and production batch is more, cause product quality inhomogeneities
More, multiple batches of production easily produces formula and obscures, and shipment link also tends to have mistake；Final result takes time and effort, produces for production
Product quality discrepancy is big, and yield rate is low.The present invention is except designing new conductive silver paste system, the creative association by each component
Effect is adjusted, highly conductive, high bonding, excellent mechanical performance and inexpensive needs can not be met at the same time in the prior art by solving
Problem.The highly conductive low temperature silver paste of excellent combination property is made public for the first time, can be produced in batches, time power is saved, reduces cost, and
And will not malfunction, one pot of properties of product equilibrium.
Resin is the major embodiment person of coating property, it not only plays the basic nature such as the bonding of itself, heat shock resistance, weather-proof
Can, more important is the compatibility for coordinating all components in coating, make to play interfacial effect between each component, reach collaboration and make
With avoiding a certain component incompatible the defects of bringing overall performance to decline.The resin system composition of the present invention is reasonable, high tenacity tree
Fat is used as matrix resin, and curing reaction is high with the crosslink density of curing agent soon, is conducive to improve the curing performance of silver paste, tool
There are excellent wearability and solvent resistance, there is excellent adhesion performance to base material, it is attached to material highly conductive silver paste to be solved
The problem of force difference, while also have good quick-drying, to improve the rate of drying of film, is used in combination with curing agent etc.,
Assign conductive silver paste the effect good, wear-resisting, mechanical property is excellent to material adhesive force.
Conductive silver paste is constructing and some physics, chemical change can occur in film forming procedure, these changes and silver paste are in itself
Property, construction and the application performance of silver paste will be significantly affected.After silver paste construction, it may appear that new interface, if silver paste and bottom
The interfacial tension at the liquid/solid interface between material is higher than the critical surface tension of ground, and silver paste can not just be sprawled on ground, natural
The defects of flake, shrinkage cavity will be produced；Silver paste cure when solvent volatilization can cause between film surface and inside produce temperature,
Density and surface tension are poor, these differences so that cause produce film inside turbulent motion, form so-called vortex, vortex can cause
Produce tangerine peel；In the system of the component containing more than one, if there is some difference for the motility of each component, vortex is also likely led
Loose colour and floating, vertical surface construction is caused to cause silking；In curing system, resin there is more than, it is possible in solidification process
Insoluble micelle is produced, causes surface tension gradient to be formed.After particle adds silver paste system, it is above-mentioned that silver paste system can be aggravated
Flowing and bonding agent solidification defect, not only influence appearance, while also damage safeguard function, such as formed shrinkage cavity cause silver slurry layer thickness low LCL,
The discontinuity of silver slurry layer can be caused by forming pin hole, and it is bonding with base material that these can all reduce silver paste, can substantially reduce whole body
The cementability of system, electric conductivity.
The invention devises new highly conductive silver paste system, resin and additive, particularly phase between metal
Capacitive is good, avoids silver paste and produces appearance, boundary defect when flowing is with curing, it is bonding with ground to effectively increase silver paste
Power；Silver paste system stability is good, is unlikely to deteriorate, and viscosity change is small after storage, on performance without influence；Reactivity is good during curing, right
In having good workability for base material；Solvent resistant after curing corrodes, and the mechanical property having had；Silver slurry layer after curing has excellent
Different electric conductivity (sheet resistance as low as 6.8 milliohms), hardness, resistant to bending, adhesive force height (3M600 adhesive tapes, >=5B), diffusivity.Solve
Electric conductivity existing for existing silver paste is low, folding is poor, adhesive force is weak problem.
In addition, the prior art reduces drawbacks described above to the greatest extent, can print silver to improve the interfacial effect of silver paste and base material
Base material is pre-processed before slurry；The present invention is without pre-processing base material, directly by the construction of newly-designed silver paste after base material, curing
Film layer is good with substrate bonding, no boundary defect, while ensure that product appearance U.S., effectively increases mechanical property.
Since above-mentioned technical proposal is used, the present invention has following advantages compared with prior art：
1. the first public high conductivity low temperature silver paste of the present invention, design is unique, and composition is reasonable, and it is convenient to prepare, and has excellent
Different electric conductivity, and it is good with base material adhesive force, while conductive coating, mechanical performance is improved, it ensure that the viscous of coating
Connecing property, workability, hardness, diffusivity, while environmental pollution is small.
2. high conductivity low temperature silver paste disclosed by the invention only needs the amount of low amounts silver powder filler, excellent lead still is achieved
Electrical property, overcomes existing the defects of needing the amount of a large amount of silver powder fillers still to improve electric conductivity, avoids existing product
The weak film layer defect of existing bonding force difference, folding；And silver paste film layer is thin, you can has excellent electric conductivity, sheet resistance is as low as
6.8 milliohms, far more than existing conductive silver paste, achieve unexpected technique effect.
3. high conductivity low temperature silver paste each component compatibility provided by the invention is good, organic matter fills out inorganic material, micro mist
Expect that wellability is good, no aggregation phenomenon, avoids the defects of a certain component film overall performance that collaboration belt does not come declines；At the same time solid
Under the interfacial effect effect of body filler, resin system solidification effect is good, obtains certain toughness reinforcing, enhancing, and mechanical property improves,
So as to obtain the highly conductive low temperature silver paste of the excellent combination properties such as adhesive force, folding, hardness, conduction.
4. the invention by adding low-melting alloy, by introducing low melting point Sn58Bi42Alloy powder is to low
After in warm conductive silver paste system, fusing point is reached by alloy powder after heating, is melted under the action of halogen-free scaling powder, with silver powder
Metallurgical connection is formed between particle, greatly enhances the electrical conductivity of system；And by its synergistic effect with other components, solve
Low-melting alloy can not be applied to the problem of low-temperature conductive silver paste in the prior art；Product can be produced in batches, save the time
Power, reduces cost, and will not malfunction, one pot of properties of product equilibrium.
5. the introducing thickener of the invention, makes the alloy of melting effectively be adsorbed in its effect in silver powder particles and increasing
Around thick powder, it ensure that the integrality of printing lines, be effectively controlled the diffusion of silver paste；By introducing toughener, make
Soft segment is introduced after curing, makes the pliability enhancing of silver paste top layer, is effectively guaranteed the bending resistance of silver paste；By drawing
Enter the metallurgical connection of low-melting alloy formation, significantly improve the conductive film layer mechanical performance after curing, it is attached to possess high rigidity, height
Put forth effort, high bending performance.
It is convenient that 6. high conductivity low temperature silver paste provided by the invention is used and stored, and before highly conductive requirement is met
Put, only need one-step print, thickness is thin, and dosage is few, the pollution smaller to environment, and the injury to human body is lower；And due to adding
Add agent dosage low, wellability is good in resin system, is conducive to the lifting of product appearance, is more suitable for industrialized production.
Brief description of the drawings
Fig. 1 is the front and rear figure of adhesive force test after one product of embodiment cures；
The front and rear figure of bending test after Fig. 2 cures for three line width 0.3mm silver wires bar of embodiment.
Embodiment
The invention will be further described with reference to the accompanying drawings and embodiments：
The preparation of high conductivity low temperature silver paste
By the formula of table 1, high tenacity resin, thickener, toughener, curing agent, organic solvent are mixed divide successively
Dissipate；Low-melting alloy, scaling powder, conductive silver powder are sequentially added, 1200 turns/min stirring 15min, obtain slurry；Ground with three rollers
Gained slurry is ground into 5~10 μm of fineness by grinding machine, up to conductive silver paste.
With screen printing mode on PET even print conductive silver paste, PET film material is dried in 150 DEG C of convection oven
Taken out after roasting 50min, cooling, the performance such as measurement line thickness (thickness is 4~6 microns), line resistor, hardness, attachment, bending
As a result.According to thickness, line resistor, line thickness, line length, after conductive silver paste baking is calculated with sheet resistance calculation formula
Sheet resistance.Corresponding the performance test results are shown in Table 2.From the data of table 2：Conductive silver paste prepared by the present invention has high conductance
The advantages that rate, high-mechanical property.By comparison example result, electrical conductivity performance and hardness performance after low-melting alloy are introduced
It is improved significantly.By adding suitable thickener and toughener, the diffusion and bending of silver wire bar can be effectively controlled
Performance.Low temperature silver paste prepared by the invention, can effectively reduce silver content, improve electrical conductivity and mechanical performance, be greatly saved into
Product, can be widely applied in the industries such as thin film switch, capacitance electrode, touch-screen.
Attached drawing 1 is (A) (B) figure afterwards before adhesive force test after one paint solidification of embodiment, it can be seen that coating of the present invention
Adhesive force is big after curing, reaches 5B.
(A) (B) figure afterwards before test resistant to bending after attached drawing 2 cures for three line width 0.3mm silver pastes of embodiment, it can be seen that this
Bending resistance is splendid after invention paint solidification.
1 conductive silver paste of table forms
Performance after the curing of 2 conductive silver paste of table
Claims (6)
1. a kind of high conductivity low temperature silver paste, it is characterised in that by weight, composed of the following components：
The high tenacity resin is saturated polyester resin, the one or more in polyacrylic resin, polyurethane；
The boiling point of the organic solvent is 100-250 DEG C；
The conductive silver powder particle diameter is 0.1-20 μm；
The low-melting alloy is less than 10 μm of Sn for particle diameter58Bi42Alloy powder；
One or more of the thickener in hydroxyethyl cellulose, modified alta-mud or aerosil；The increasing
Tough dose is liquid nitrile rubber；The curing agent is less than 150 DEG C of blocked isocyanate for deblocking temperature；The scaling powder is
Halogen-free scaling powder, is made of rosin resin derivative, organic acid for activating agent and organic solvent.
2. high conductivity low temperature silver paste according to claim 1, it is characterised in that：The glass transition of the high tenacity resin
Temperature is 0-50 DEG C.
3. high conductivity low temperature silver paste according to claim 1, it is characterised in that：The organic solvent is esters and/or ketone
Class solvent.
4. high conductivity low temperature silver paste according to claim 1, it is characterised in that：The conductive silver powder particle diameter is micro- for 0.5-6
Rice；The pattern of conductive silver powder is spherical, near-spherical, sheet or dendroid.
5. high conductivity low temperature silver paste according to claim 1, it is characterised in that：By weight, the high conductivity is low
Warm silver paste is composed of the following components：
6. high conductivity low temperature silver paste according to claim 1, it is characterised in that the preparation of the high conductivity low temperature silver paste
Method comprises the following steps：High tenacity resin, thickener, toughener, curing agent, organic solvent are mixed successively scattered；
Low-melting alloy, scaling powder, conductive silver powder are sequentially added, high-speed stirred, obtains slurry；With three-roll grinder by gained slurry
5~10 μm of fineness is ground into, up to conductive silver paste.
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
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| CN201810260835.9A CN108538442B (en) | 2015-05-27 | 2015-05-27 | Preparation method of high-conductivity low-temperature silver paste |
| CN201510282011.8A CN106297949B (en) | 2015-05-27 | 2015-05-27 | High conductivity low temperature silver paste |
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| CN201510282011.8A CN106297949B (en) | 2015-05-27 | 2015-05-27 | High conductivity low temperature silver paste |
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| CN108130036B (en) * | 2017-12-18 | 2021-02-02 | 深圳市思迈科新材料有限公司 | Flexible bonding conductive adhesive and preparation method thereof |
| CN110097998B (en) * | 2018-01-31 | 2021-06-15 | 上海宝银电子材料有限公司 | Conductive silver paste for transfer printing process touch screen and preparation method thereof |
| CN108565041B (en) * | 2018-04-20 | 2020-04-28 | 四川省银河化学股份有限公司 | High-conductivity soldering-resistant low-temperature silver paste and preparation method thereof |
| CN108962496A (en) * | 2018-07-19 | 2018-12-07 | 佛山腾鲤新能源科技有限公司 | A kind of preparation method of solar battery specific complex transparent conductive film |
| CN108962437A (en) * | 2018-07-25 | 2018-12-07 | 佛山腾鲤新能源科技有限公司 | A kind of preparation method of graphene oxide composite conductive film |
| CN110079035B (en) * | 2019-04-15 | 2020-04-28 | 华南理工大学 | Rubber/low-melting-point alloy/nano-carbon composite material with three-dimensional conductive network and preparation method thereof |
| CN110534229A (en) * | 2019-08-30 | 2019-12-03 | 湖南诺尔得材料科技有限公司 | A kind of conductive silver paste and the preparation method and application thereof that sintering temperature is low |
| CN110783013B (en) * | 2019-11-06 | 2021-06-15 | 英利能源（中国）有限公司 | Solar cell electrode slurry, cell and preparation method of assembly of cell |
| CN110993149A (en) * | 2019-12-26 | 2020-04-10 | 无锡晶睿光电新材料有限公司 | Silver paste for metal grid capacitive flexible touch screen and preparation method and application thereof |
| CN113484393B (en) * | 2021-09-08 | 2021-12-14 | 北京华益精点生物技术有限公司 | Electrode quality control method |
| CN114141404A (en) * | 2021-11-22 | 2022-03-04 | 苏州市贝特利高分子材料股份有限公司 | High-conductivity high-flexibility low-temperature silver paste |
| CN114496402A (en) * | 2022-02-15 | 2022-05-13 | 西安英诺维特新材料有限公司 | Preparation method of fast curing UV silver paste for ITO film of touch screen |
| CN114864132A (en) * | 2022-04-18 | 2022-08-05 | 湖南省国银新材料有限公司 | Low-temperature quick-drying mask silver paste for gravure printing and preparation method thereof |
| CN116313226B (en) * | 2023-05-12 | 2023-08-04 | 浙江飞宜光电能源科技有限公司 | Low-temperature curing silver paste and preparation method thereof |
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|---|---|---|---|---|
| JP2003249735A (en) * | 2002-02-15 | 2003-09-05 | E I Du Pont De Nemours & Co | Improved method for embedding thick film component |
| CN101593568A (en) * | 2008-05-30 | 2009-12-02 | 三星电机株式会社 | The electrocondution slurry and the printed circuit board (PCB) that uses it that contain carbon nano-tube |
| CN102197444A (en) * | 2008-10-22 | 2011-09-21 | 东曹株式会社 | Composition for producing metal film, method for producing metal film, and method for producing metal powder |
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Also Published As
| Publication number | Publication date |
|---|---|
| CN108538442B (en) | 2020-07-17 |
| CN108538442A (en) | 2018-09-14 |
| CN106297949A (en) | 2017-01-04 |
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