CN103903675A - High-stability conductive slurry and preparation method thereof - Google Patents
High-stability conductive slurry and preparation method thereof Download PDFInfo
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- CN103903675A CN103903675A CN201210580547.4A CN201210580547A CN103903675A CN 103903675 A CN103903675 A CN 103903675A CN 201210580547 A CN201210580547 A CN 201210580547A CN 103903675 A CN103903675 A CN 103903675A
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Abstract
The invention discloses a high-stability conductive slurry. The conductive slurry comprises silver powder, a blinder, a stabilizer and a solvent. The silver power can be micrometer silver powder, nanometer silver powder or a combination of the two in any proportions; through adding the stabilizer, the slurry deposition layering phenomenon generated during the preparation, transportation and storage process of the conductive slurry, and the consistency of the conductive slurry, the distribution uniformity and flatness of the a conductive slurry on a base material are ensured; and the stability of the conductive slurry is effectively enhanced, the application and storage life of the conductive slurry is prolonged, and the high-stability conductive slurry and the preparation method are widely applied to conductive slurry fields such as an RFID antenna, a touch screen line, a flexible printed circuit (FPC), a film switch, a solar battery, a printed circuit board and the like.
Description
Technical field
The present invention relates to electrocondution slurry application, specifically the present invention relates to a kind of high stability electrocondution slurry and preparation method thereof.
Background technology
In recent years, electrocondution slurry, as a kind of base electronic material with specific function, is used widely in field of electronic circuitry such as printed circuit board, solar cell, surface mount, RFID radio-frequency antenna, touch-screen circuit, flexible print circuit FPC.The stability of electrocondution slurry in preparation, conveying and storage process can not be ignored in industrial production.Electrocondution slurry poor stability, active principle skewness in electrocondution slurry, the electronic circuit rough surface of printing, between conductive particle, adhesive is poor, causes the poorly conductive of circuit; Electrocondution slurry shifts and carries, while occurring that solid deposits is remaining in storage process, not only affect product quality, and can stop up various conveyance conduits, remains in not only polluted product but also affect material content calculating in electrocondution slurry of material on pipeline.In a word, electrocondution slurry is walked out of existing wild effect any one, need to drop into more man power and material's cost for the follow-up stability that need to again recover electrocondution slurry.
At present, improve electrocondution slurry stability approach and generally adopt physical method, comprise the methods such as simple and mechanical stirring, electromagnetic agitation, ultrasonic agitation, heating and thermal insulation.The electrocondution slurry that these class methods obtain has the stability in the short time, does not have problems for small-scale produced on-site; But, follow these class methods of large production scale not possess advantage, the obvious life period stability of electrocondution slurry weakens effect.
In the time that powder particle is distributed in polarizable medium (as water, containing electrolyte solution etc.), between the decentralized photo (powder particle) in dispersion, there are two kinds of power to interact, the one, the electrostatic repulsion forces of electric double layer, another is Van der Waals force.Double electrode layer repulsion is dominant, and dispersion tends towards stability; Van der Waals force is preponderated, and particle is tending towards assembling.Except Van der Waals force and double electrode layer repulsion, the stability of the dispersion that contains large molecular surface active material is also subject to the impact of the factor such as Desorption Energy, bridge effect.For example, in the dispersion of powder particle organic solvent, macromolecular substances is adsorbed on particle surface, and macromolecular chain will stretch in medium, in the time that particle is close to each other, causes the interaction of these keys, hinders the gathering of particle.The colloid-stabilised theory of Here it is so-called dispersion.
Summary of the invention
In order to solve electrocondution slurry unsettled problem in preparation, conveying and storage process in prior art, the invention provides a kind of high stability electrocondution slurry and preparation method thereof, by adding stabilizer, improve the stability of electrocondution slurry, extend use and the storage life of electrocondution slurry.
The present invention realizes in the following way: a kind of preparation method of high stability electrocondution slurry, comprises the following steps: according to mass ratio, first binding agent and stabilizer are joined in solvent, dispersed with stirring is dissolved; Then in above-mentioned mixed liquor, add silver powder, continue to be stirred to and mix; Finally adopt three-roll grinder ground and mixed.
Described electrocondution slurry comprises silver powder, binding agent, stabilizer and solvent; Described silver powder can be micro-silver powder, nano-silver powder or the combination of both arbitrary proportions.
Described micro-silver powder average grain diameter is 0.2～50 μ m; Described nano-silver powder average grain diameter is 1～200nm.
The quality percentage composition of the each component of described electrocondution slurry is: silver powder content is 40～80%, binder content is 5～30%, stabiliser content is 0.1～5%, solvent is 10～50%.
Described binding agent is one or both in polyester, polyacrylic resin, polyvinylpyrrolidone, polyethylene glycol, polyvinyl alcohol, phenolic resins, alkyd resins, epoxy resin, styrene and acrylic copolymer, polymethylacrylic acid and acrylate copolymer, butene dioic acid resin, polyamide, vinyl chloride-vinyl acetate resin, polyvinyl butyral resin, cellulose, organic siliconresin, gum arabic.
Described solvent is one or more in diethylene glycol monobutyl ether acetate, propandiol butyl ether acetate, DBE, dipropylene glycol monomethyl ether acetate, butyl glycol ether, terpinol or cyclohexanone.
Described stabilizer comprises one or more in inorganic molecules electrolyte, organic molecule electrolyte, polymer dielectric, surfactant, plasticizer or defoamer.
Described inorganic molecules electrolyte comprises inorganic acid, inorganic base and inorganic salts.Organic molecule electrolyte comprises small molecular organic acid, little molecule organic base and both sexes organic molecule.Polymer dielectric comprises poly-acids, poly-bases, macromolecule ampholytes.
Wherein polyelectrolyte comprises poly-acids: as polyacrylic, polymethylacrylic acid, polystyrolsulfon acid, polyvinyl sulfonic acid, polyethylene phosphoric acid etc.; Poly-bases: as polymine, polyvinylamine, polyvinyl pyridine etc.; Macromolecule ampholytes: natural nucleic acid, protein.
The optional fatty acid ester of described surfactant, neopelex; The optional polyol ester class of plasticizer; The optional SRE-2035A of described defoamer.
Electrocondution slurry of the present invention can be prepared electronic circuit layer by various mode of printings such as silk screen printing, ink jet printing, sprayings.
The present invention has following beneficial effect:
1, the present invention is by adding stabilizer, eliminate the slurry sediment lamination that electrocondution slurry occurs in preparation, conveying and storage process, extend use and the storage life of electrocondution slurry, ensured the consistency of electrocondution slurry and the uniformity distributing and evenness on base material.
2, stabilizer used in the present invention has the advantages such as the compatibility good with existing system, Costco Wholesale are lower, physics and chemistry stable performance, environmental protection is nontoxic, abundant raw material is easy to get.
Brief description of the drawings
Fig. 1 is the microphotograph of the circuit layer of preparation in embodiment 1.
Fig. 2 is the microphotograph of the circuit layer of preparation in embodiment 2.
Fig. 3 is the time dependent comparison diagram of electrocondution slurry specific viscosity that in embodiment 1, in conventional method and embodiment 2 prepared by new method.
Embodiment
Following embodiment can make those skilled in the art more fully understand the present invention, but does not limit the present invention in any way.
The experimental technique using in following embodiment if no special instructions, is conventional method.
Material, reagent etc. used in following embodiment, if no special instructions, all can obtain from commercial channels.
Embodiment 1
The present embodiment is blank assay, adopts conventional method preparation, is the preparation of conventional RFID antenna conductive silver paste, does not add stabilizer of the present invention.Only comprise silver powder, binding agent and solvent.
Its preparation method is as follows:
According to each constituent mass ratio in electrocondution slurry, the polyacrylic resin that takes 9.5g joins in 10.0g butyl glycol ether, and mechanical agitation is disperseed 30min; Then adding 80.0g average grain diameter is the micro-silver powder of 7 μ m, continues to be stirred to mix; Finally adopt three-roll grinder ground and mixed, to slurry particle diameter below 5 μ m.Be printed onto on TESLIN film by silk screen printing (250 order).The microphotograph of circuit layer as shown in Figure 1; Under the condition of room temperature (25 DEG C), use its viscosity of U.S. Brookfield rotary viscosity instrumentation, make specific viscosity and time chart, as shown in Figure 3.
Embodiment 2
According to each constituent mass ratio in electrocondution slurry, take successively the polyacrylic resin of 8.5g and the polymine of 1.0g and join in 10.0g butyl glycol ether, mechanical agitation is disperseed 30min; Then adding 80.0g average grain diameter is the micro-silver powder of 7 μ m, continues to be stirred to mix; Finally adopt three-roll grinder ground and mixed, to slurry particle diameter below 5 μ m.By preparing circuit layer on silk screen printing (250 order) printing TESLIN film, the microphotograph of circuit layer as shown in Figure 2.Under the condition of room temperature (25 DEG C), use its viscosity of U.S. Brookfield rotary viscosity instrumentation to change, make specific viscosity and time chart, as shown in Figure 3
Comparison diagram 1 and Fig. 2, obviously observe the electrocondution slurry adding after stabilizer and on printing element, distribute more evenly, and the circuit layer of preparation is more smooth smooth.
From Fig. 3, obviously can find out that the electrocondution slurry that adopts new method to obtain just has good stability, the viscosity of system is substantially unchanged in long-time.
Embodiment 3
According to each constituent mass ratio in electrocondution slurry, the neopelex that takes successively 8.0g epoxy resin (E-51) and 1.5g joins in 10.0g terpinol, and mechanical agitation is disperseed 30min; Then adding 80.0g average grain diameter is 10nm nano-silver powder, continues to be stirred to mix; Finally adopt three-roll grinder ground and mixed, to slurry particle diameter below 3 μ m.By preparing circuit layer on silk screen printing (400 order) printing PET film, the photo of circuit layer prepared by the microphotograph of circuit layer and embodiment 2, without essential difference, is evenly distributed on base material, and smooth in appearance is smooth; Under the condition of room temperature (25 DEG C), use its viscosity of U.S. Brookfield rotary viscosity instrumentation to change, obtain figure that specific viscosity and time chart and embodiment 2 obtain without essential distinction, the viscosity of system is substantially unchanged in for a long time.
Embodiment 4
According to each constituent mass ratio in electrocondution slurry, the polyvinylamine that takes successively 9.0g polyethylene glycol and 1.0g joins in 15.0g diethylene glycol monobutyl ether acetate, and mechanical agitation is disperseed 30min; Then adding 10.0g average grain diameter is that 5nm nano-silver powder and 50g average grain diameter are the micro-silver powder of 12 μ m, continues to be stirred to mix; Finally adopt three-roll grinder ground and mixed, to slurry particle diameter below 5 μ m.Be printed onto on PET film and prepared circuit layer by silk screen printing (250 order), the photo of circuit layer prepared by the microphotograph of circuit layer and embodiment 2, without essential difference, is evenly distributed on base material, and smooth in appearance is smooth; Under the condition of room temperature (25 DEG C), use its viscosity of U.S. Brookfield rotary viscosity instrumentation, the result that the specific viscosity obtaining and time chart and embodiment 2 obtain is without essential distinction, and the viscosity of system is substantially unchanged in long-time.
The above; be only three kinds of embodiments in the present invention, but protection scope of the present invention is not limited to this, is anyly familiar with those skilled in the art in the technical scope of the present invention's protection; the variation that can expect easily or replacement, within all should being encompassed in protection scope of the present invention.Therefore, protection scope of the present invention should be as the criterion with the protection range of claim.
Claims (9)
1. a high stability electrocondution slurry, described electrocondution slurry comprises silver powder, binding agent, stabilizer and solvent; Described silver powder can be micro-silver powder, nano-silver powder or the combination of both arbitrary proportions.
2. high stability electrocondution slurry according to claim 1, is characterized in that: described micro-silver powder average grain diameter is 0.2～50 μ m; Described nano-silver powder average grain diameter is 1～200nm.
3. high stability electrocondution slurry according to claim 1, it is characterized in that: taking electrocondution slurry quality percentage composition as benchmark, silver powder content is 40～80%, binder content is 5～30%, stabiliser content is 0.1～5%, solvent is 10～50%.
4. high stability electrocondution slurry according to claim 1, is characterized in that: described binding agent is one or both in polyester, polyacrylic resin, polyvinylpyrrolidone, polyethylene glycol, polyvinyl alcohol, phenolic resins, alkyd resins, epoxy resin, styrene and acrylic copolymer, polymethylacrylic acid and acrylate copolymer, butene dioic acid resin, polyamide, vinyl chloride-vinyl acetate resin, polyvinyl butyral resin, cellulose, organic siliconresin, gum arabic.
Described solvent is one or more in diethylene glycol monobutyl ether acetate, propandiol butyl ether acetate, DBE, dipropylene glycol monomethyl ether acetate, butyl glycol ether, terpinol or cyclohexanone.
5. high stability electrocondution slurry according to claim 4, is characterized in that: described stabilizer comprises one or more in inorganic molecules electrolyte, organic molecule electrolyte, polyelectrolyte, surfactant, plasticizer or defoamer.
6. high stability electrocondution slurry according to claim 5, is characterized in that: described inorganic molecules electrolyte comprises inorganic acid, inorganic base or inorganic salts.
Described organic molecule electrolyte comprises small molecular organic acid, little molecule organic base or organic amphiprotic molecule.
Described polyelectrolyte comprises poly-acid, poly-alkali or macromolecule ampholytes.
7. high stability electrocondution slurry according to claim 6, is characterized in that: described poly-acid comprises polyacrylic acid, polymethylacrylic acid, polystyrolsulfon acid, polyvinyl sulfonic acid or polyethylene phosphoric acid;
Described poly-alkali comprises polymine, polyvinylamine or polyvinyl pyridine;
Described macromolecule ampholytes comprises natural nucleic acid or protein.
8. a preparation method for high stability electrocondution slurry, comprises the following steps: according to mass ratio, first binding agent and auxiliary agent are joined in solvent, dispersed with stirring is dissolved; Then in above-mentioned mixed liquor, add silver powder, continue to be stirred to and mix; Finally adopt three-roll grinder ground and mixed.
9. according to the high stability electrocondution slurry described in above any one claim, it is characterized in that: comprise above-described high stability electrocondution slurry and preparation method thereof.
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Cited By (23)
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|---|---|---|---|---|
| CN104464881A (en) * | 2014-11-17 | 2015-03-25 | 昆明贵金属研究所 | Dual-function electric conduction silver paste for touch screen and preparation method and application thereof |
| CN104858437A (en) * | 2015-04-24 | 2015-08-26 | 昆明理工大学 | Nano silver paste for printing conducting circuit and preparation method of nano silver paste |
| CN104900296A (en) * | 2015-06-12 | 2015-09-09 | 江苏广信感光新材料股份有限公司 | Conductive silver paste for membrane switch, and preparation method for conductive silver paste |
| CN104952513A (en) * | 2015-03-06 | 2015-09-30 | 苏州深科微新材料科技有限公司 | Printing-way-based silver-nanowire transparent conductive slurry |
| CN105045457A (en) * | 2015-08-10 | 2015-11-11 | 东莞市通美电子科技有限公司 | Resistive touch screen printing silver pulp, preparing method of resistive touch screen printing silver pulp and use method of resistive touch screen printing silver pulp |
| CN105070349A (en) * | 2015-08-10 | 2015-11-18 | 东莞市通美电子科技有限公司 | Special conductive filament printing silver slurry for capacitive touch screen and preparation and application methods of special conductive filament printing silver slurry |
| CN105086813A (en) * | 2015-09-10 | 2015-11-25 | 苏州扬子江新型材料股份有限公司 | High-strength long-service-life titanium-silver backboard of household appliance |
| CN105139919A (en) * | 2015-08-10 | 2015-12-09 | 东莞市通美电子科技有限公司 | Laser silver paste used for capacitive touch screen as well as preparation method and use method for laser silver paste |
| CN105244076A (en) * | 2015-11-02 | 2016-01-13 | 云南师范大学 | Environment-friendly and low-filling conductive silver paste and preparation method thereof |
| CN105789629A (en) * | 2014-12-15 | 2016-07-20 | 中信国安盟固利动力科技有限公司 | Method for improving lasting stability of fluid |
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| CN106663494A (en) * | 2014-07-22 | 2017-05-10 | 阿尔法装配解决方案公司 | Stretchable interconnects for flexible electronic surfaces |
| CN106960693A (en) * | 2016-01-09 | 2017-07-18 | 湖南利德电子浆料股份有限公司 | A kind of touch-screen electrocondution slurry |
| CN107358990A (en) * | 2017-07-25 | 2017-11-17 | 合肥华盖光伏科技有限公司 | A kind of preparation method of crystal silicon solar back of the body aluminum conductor slurry |
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| CN109979639A (en) * | 2019-02-18 | 2019-07-05 | 英鸿纳米科技股份有限公司 | A kind of nano chips encapsulation mixed type conductive silver paste |
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| CN111261322A (en) * | 2020-02-13 | 2020-06-09 | 轻工业部南京电光源材料科学研究所 | Silk-screen conductive silver paste for touch screen and preparation method thereof |
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| CN106663494A (en) * | 2014-07-22 | 2017-05-10 | 阿尔法装配解决方案公司 | Stretchable interconnects for flexible electronic surfaces |
| CN106663494B (en) * | 2014-07-22 | 2018-11-30 | 阿尔法装配解决方案公司 | Stretchable interconnection for flexible electrical component surface |
| CN104464881A (en) * | 2014-11-17 | 2015-03-25 | 昆明贵金属研究所 | Dual-function electric conduction silver paste for touch screen and preparation method and application thereof |
| CN105789629A (en) * | 2014-12-15 | 2016-07-20 | 中信国安盟固利动力科技有限公司 | Method for improving lasting stability of fluid |
| CN104952513A (en) * | 2015-03-06 | 2015-09-30 | 苏州深科微新材料科技有限公司 | Printing-way-based silver-nanowire transparent conductive slurry |
| CN104858437A (en) * | 2015-04-24 | 2015-08-26 | 昆明理工大学 | Nano silver paste for printing conducting circuit and preparation method of nano silver paste |
| CN104900296A (en) * | 2015-06-12 | 2015-09-09 | 江苏广信感光新材料股份有限公司 | Conductive silver paste for membrane switch, and preparation method for conductive silver paste |
| CN105045457A (en) * | 2015-08-10 | 2015-11-11 | 东莞市通美电子科技有限公司 | Resistive touch screen printing silver pulp, preparing method of resistive touch screen printing silver pulp and use method of resistive touch screen printing silver pulp |
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| CN105244076A (en) * | 2015-11-02 | 2016-01-13 | 云南师范大学 | Environment-friendly and low-filling conductive silver paste and preparation method thereof |
| CN105244076B (en) * | 2015-11-02 | 2017-05-31 | 云南师范大学 | A kind of environment-friendly type, low loading conductive silver paste and preparation method thereof |
| CN106960693A (en) * | 2016-01-09 | 2017-07-18 | 湖南利德电子浆料股份有限公司 | A kind of touch-screen electrocondution slurry |
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| CN105969259B (en) * | 2016-05-17 | 2018-04-20 | 佛山市加恩新材料有限公司 | Hotmelt and preparation method for template heat transfer thermoprint |
| CN107358990A (en) * | 2017-07-25 | 2017-11-17 | 合肥华盖光伏科技有限公司 | A kind of preparation method of crystal silicon solar back of the body aluminum conductor slurry |
| CN111316458A (en) * | 2017-11-01 | 2020-06-19 | 株式会社Lg化学 | Organic-inorganic hybrid solar cell and method for manufacturing organic-inorganic hybrid solar cell |
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| CN108666000A (en) * | 2018-06-07 | 2018-10-16 | 太仓萃励新能源科技有限公司 | A kind of preparation method of N-type Halogen electrocondution slurry |
| CN111105932A (en) * | 2018-10-26 | 2020-05-05 | 南通宇华新材料科技有限公司 | Solid-state capacitance carbon foil nano conductive carbon paste and preparation method thereof |
| CN111105932B (en) * | 2018-10-26 | 2021-11-02 | 南通宇华新材料科技有限公司 | Solid-state capacitance carbon foil nano conductive carbon paste and preparation method thereof |
| CN109979639A (en) * | 2019-02-18 | 2019-07-05 | 英鸿纳米科技股份有限公司 | A kind of nano chips encapsulation mixed type conductive silver paste |
| CN111087248A (en) * | 2019-12-23 | 2020-05-01 | 厦门华信安电子科技有限公司 | Special adhesive for MLCC and preparation method thereof |
| CN111261322A (en) * | 2020-02-13 | 2020-06-09 | 轻工业部南京电光源材料科学研究所 | Silk-screen conductive silver paste for touch screen and preparation method thereof |
| CN113257458A (en) * | 2021-06-16 | 2021-08-13 | 西安宏星电子浆料科技股份有限公司 | Conductor paste for chip resistor electrode |
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| CN114210997A (en) * | 2021-11-05 | 2022-03-22 | 佛山科学技术学院 | Lead bonding method based on high-precision 3D printing |
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Application publication date: 20140702 |