CN102079847A - Photosensitive silver slurry conductive adhesive and preparation method thereof - Google Patents
Photosensitive silver slurry conductive adhesive and preparation method thereof Download PDFInfo
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- CN102079847A CN102079847A CN2009101942004A CN200910194200A CN102079847A CN 102079847 A CN102079847 A CN 102079847A CN 2009101942004 A CN2009101942004 A CN 2009101942004A CN 200910194200 A CN200910194200 A CN 200910194200A CN 102079847 A CN102079847 A CN 102079847A
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Abstract
The invention belongs to the technical field of micro-electronic packaging. The photosensitive silver slurry conductive adhesive provided by the invention is composed of a photosensitive resin, conducting particles, a dispersing agent, a photoinitiator, an antioxidant and a defoaming agent. The photosensitive resin is an epoxy acrylic resin generated by the reaction of butyl acrylate, acrylic acid, an epoxy resin, N,N-methylene bis-acrylamide and hydroquinone, acrylic acid isoborneol ester serves as the dispersing agent, the conducting particles are micrometer aluminum powder, nanometer aluminum powder and silvered glass powder; a silane coupling agent (3-glycidol ether oxygen acyl propyl trimethoxy silane) serves as the nanometer Ag dispersing agent; benzoin ether serves as the photoinitiator; and hydroxybenzene methyl ether serves as the antioxidant, and dibutyl phosphate is adopted as the defoaming agent. The photosensitive Ag slurry conductive adhesive provided by the invention has good ultraviolet light curing property, high bonding strength, low resistivity, and can satisfy the requirement of micro-electronic packaging technologies of a film circuit, a circuit board, a ceramic capacitor and the like.
Description
Technical field
The present invention relates to a kind of photosensitive silver slurry conductive resin and preparation method thereof, belong to the microelectronic packaging technology field.
Background technology
In recent years, along with microelectronic product transforms to aspects such as low-cost, portable, high-performance, multi-functional, environmental friendliness, the electronics assembling is also progressively striding forward to system-level integrated assembling.The Sn/Pb scolder is the employed a kind of basic connection material of Electronic Packaging industry, and its composition Pb belongs to heavy metal element, has very big toxicity, and the welding temperature of scolder is too high, also damages device and substrate easily; Exist in the scolder " build bridge ' phenomenon, can not be used for the defective of aspects such as high density integrated circuit, limited the application of Sn/Pb scolder.In electronics assembly industry, conductive resin replaces original methods such as welding and is used for the electroconductibility connection, has obtained good progress, and conductive resin has become a kind of requisite type material, the conductive resin huge market demand in electronic industry.
Conductive resin is the matrix material of high molecular polymer and conducting particles combination, and polymkeric substance is given switching performance, and conductive particle is given conductivity, and conductive resin has certain toughness, can reduce, eliminate thermal stresses, improves device reliability; Conductive resin connects the resolving power height, can satisfy fine rule and connect technology.Conductive resin has two kinds of curing modes: thermofixation and photocuring, heat curing temperature is generally at 150～180 ℃, and about time 30min, photocuring has curing speed fast (in the 5min), advantage that solidification value is low, with the thermofixation ratio, photocuring conserve energy about 70%.The characteristics of photocuring technology are that curing speed is fast, the production efficiency height, be fit to streamline production, solvent-free discharging, photocuring does not need to force to be heating and curing, and is particularly favourable to the curing of thermo-sensitive material, can effectively reduce thermal stresses, avoid in the solidification process variation of temperature to the destruction of liquid crystal material and glass substrate, improve device reliability and yield rate.
Conductive resin is to form conductive network by the conducting particles of filling in resin matrix to conduct electricity, the quality that network forms has very big influence to the electric property of conductive resin, the quality of network depends primarily on kind, pattern, size, electroconductibility of filled conductive particle etc., the present invention can form conductive network with micro-silver powder, nano-silver powder and silvered glass powder better as the conductive filler material of conductive resin in the resin matrix of conductive resin, give full play to a tunnel conduction effect and an emission conductive effect of Nano silver grain.Adopt micro-silver powder, nano-silver powder and silvered glass powder stuff and other stuff to prepare the photosensitive silver slurry of a kind of high-performance conductive resin as conductive filler material.This conductive resin that makes has good electric property and very high shear strength.
Summary of the invention:
One, material mixture ratio:
The preparation photosensitive resin, preparation nano-silver powder and silvered glass powder.With the isobornyl acrylate is dispersion agent, and micro-silver powder, nano-silver powder and silvered glass powder are conducting particles; Silane coupling agent (3 one glycidyl ether oxygen base propyl trimethoxy silicane) is as the nanometer silver dispersion agent; Benzoin ether is as light trigger; MEHQ is as antioxidant, and dibutyl phosphate is as defoamer.Conducting particles, dispersion agent, light trigger, antioxidant, defoamer are dispersed in the photosensitive resin, stir, vacuum is removed small molecules and is promptly obtained photosensitive silver slurry conductive resin.Its system component weight percent consists of: 15～30 parts of photosensitive resins, 60～80 parts of conducting particless, 0.1～2 part of dispersion agent, 0.5～2.0 part of light trigger, 0.1～1.0 part of antioxidant, 0.5～5 part of defoamer.
Two, preparation process:
1, with AgNO
3Be dissolved in the N-vinyl pyrrolidone that (weight percent is respectively 10 parts in the ethylene glycol, 2 parts, 30 parts), add 20% sodium hypophosphite solution sonic oscillation 20min after, heated constant temperature causes 80～90 ℃ of temperature, backflow 80min, add 3-glycidyl ether oxygen base propyl trimethoxy silicane (weight percent is respectively 0.2 part) then, backflow 30min adds washing with acetone then in solution, last centrifugation obtains the nano-silver powder of surface modification.
2, at 5% AgNO
3Solution drips 10% NaOH solution (weight percent was respectively 100: 1), produce white precipitate immediately, dropwise splash into ammoniacal liquor subsequently, till precipitation has just disappeared, must colourless silver ammino solution, 3 parts of silver ammino solutions are poured in 1 part of glass powder, add 2 parts of 10% glucose solutions, constant temperature 20min under 85～95 ℃ of conditions, last centrifugation obtains the silvered glass powder.
3, photosensitive resin is by butyl acrylate, vinylformic acid, Resins, epoxy, N, the epoxy acrylic resin that N-methylene-bisacrylamide and Resorcinol polyreaction form, wherein 20～50 parts of butyl acrylates, 10～30 parts in vinylformic acid, 5～20 parts of Resins, epoxy, N, 2～10 parts of N-methylene-bisacrylamides, 10～20 parts of Resorcinol.Resins, epoxy and butyl acrylate are mixed, be heated to 80 ℃ then, stir down slowly dropping and be dissolved with Resorcinol, N, the vinylformic acid mixing solutions of N-methylene-bisacrylamide, behind the reaction 90min, temperature is increased to 85 ℃ and reacts 30min again, and cooling promptly obtains the epoxy acrylic photosensitive resin.
4, according to photosensitive sliver-powder conducting glue prescription, be dispersion agent with the isobornyl acrylate, micro-silver powder, nano-silver powder and silvered glass powder are conducting particles; Silane coupling agent (3-glycidyl ether oxygen base propyl trimethoxy silicane) is as the nanometer silver dispersion agent; Benzoin ether is as light trigger; MEHQ is as antioxidant, dibutyl phosphate is as defoamer, photosensitive resin, conducting particles, dispersion agent, light trigger, antioxidant, defoamer are dispersed in the photosensitive resin, stir, vacuum is removed small molecules and is promptly obtained photosensitive silver slurry conductive resin.
Advantage of the present invention:
Adopt the Nano silver grain of chemical reduction method preparation, with 3-glycidyl ether oxygen base propyl trimethoxy silicane to the Nano silver grain surface modification, improved the dispersiveness of Nano silver grain in photosensitive resin, adopted the toughner of chemical silvering glass powder as conductive resin.Advantages such as it is low that this conductive resin has resistivity than conventional conductive glue, and mechanical property is good, and preparation method's cost is low, method is simple, and controllability is good, has very high practical value for the development of Electronic Packaging industry.
Examples of implementation:
The photosensitive sliver-powder conducting glue of (%) formulated as following weight percent:
The conductive resin initial viscosity is 37000mPas, and volume specific resistance is 1.8x10
-4Ω cm, 100w ultraviolet light polymerization time 110s, the shear strength when being substrate with Al are 22MPa.The conductive resin initial viscosity is 39600mPas after 90 days, and volume specific resistance is 1.9x10
-4Ω cm, 100w ultraviolet light polymerization time 140s, the shear strength when being substrate with Al are 20MPa.
Claims (3)
1. a photosensitive silver slurry conductive resin is made up of photosensitive resin, conducting particles, dispersion agent, light trigger, antioxidant, defoamer, it is characterized in that with the isobornyl acrylate being dispersion agent, and micro-silver powder, nano-silver powder and silvered glass powder are conducting particles; Silane coupling agent (3 one glycidyl ether oxygen base propyl trimethoxy silicane) is as the nanometer silver dispersion agent; Benzoin ether is as light trigger; MEHQ is as antioxidant, and dibutyl phosphate is as defoamer.Photosensitive resin, conducting particles, dispersion agent, light trigger, antioxidant, defoamer weight percent consist of: 15～30 parts of photosensitive resins, 60～80 parts of conducting particless, 0.1～2 part of dispersion agent, 0.5～2.0 part of light trigger, 0.1～1.0 part of antioxidant, 0.5～5 part of defoamer.
2. according to the described photosensitive silver slurry conductive resin of claim 1, photosensitive resin is by butyl acrylate, vinylformic acid, Resins, epoxy, N, the epoxy acrylic resin that N-methylene-bisacrylamide and Resorcinol polyreaction form, it is characterized in that their weight percent consist of: 20～50 parts of butyl acrylates, 10～30 parts in vinylformic acid, 5～20 parts of Resins, epoxy, N, 2～10 parts of N-methylene-bisacrylamides, 10～20 parts of Resorcinol.
3. according to the described photosensitive silver slurry conductive resin of claim 1, conducting particles is made up of micro-silver powder, nano-silver powder and silvered glass powder, it is characterized in that their weight percent consist of: 50～70 parts of micro-silver powders, 5～25 parts of nano-silver powders, 10～35 parts in silvered glass powder.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009101942004A CN102079847A (en) | 2009-11-27 | 2009-11-27 | Photosensitive silver slurry conductive adhesive and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009101942004A CN102079847A (en) | 2009-11-27 | 2009-11-27 | Photosensitive silver slurry conductive adhesive and preparation method thereof |
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| CN102079847A true CN102079847A (en) | 2011-06-01 |
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| CN2009101942004A Pending CN102079847A (en) | 2009-11-27 | 2009-11-27 | Photosensitive silver slurry conductive adhesive and preparation method thereof |
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Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20110192633A1 (en) * | 2010-02-05 | 2011-08-11 | Cambrios Technologies Corporation | Photosensitive ink compositions and transparent conductors and method of using the same |
| CN103165215A (en) * | 2011-12-14 | 2013-06-19 | 上海宝银电子材料有限公司 | Silver paste for mobile phone shielding and preparation method thereof |
| CN103555251A (en) * | 2013-10-18 | 2014-02-05 | 中山职业技术学院 | High-heat-conductivity high-reliability ultraviolet-curing LED (light-emitting diode) electrically-conductive silver adhesive and preparation method thereof |
| CN103854853A (en) * | 2012-12-03 | 2014-06-11 | 六和电子（江西）有限公司 | Epoxy resin one-step packaging production technology of foil-type capacitor |
| CN104143373A (en) * | 2014-07-30 | 2014-11-12 | 安徽状元郎电子科技有限公司 | Oyster shell/fluorapatite composite conductive silver paste and preparation method thereof |
| CN105006272A (en) * | 2015-08-03 | 2015-10-28 | 佛山市顺德区百锐新电子材料有限公司 | Ultraviolet conductive silver slurry, and preparation method and application thereof |
| CN105073939A (en) * | 2013-04-02 | 2015-11-18 | 昭和电工株式会社 | Conductive adhesive, anisotropic conductive film and electronic devices using both |
| CN106520010A (en) * | 2016-11-08 | 2017-03-22 | 铜陵中锐电子科技有限公司 | An electrically conductive adhesive used for LEDs and a preparing method thereof |
| CN107393811A (en) * | 2017-07-24 | 2017-11-24 | 北京时代民芯科技有限公司 | A kind of silver paste bonding die ceramic package device takes chip method |
| CN109628042A (en) * | 2018-12-26 | 2019-04-16 | 深圳日高胶带新材料有限公司 | A kind of photo-crosslinking adhesive |
| CN109929490A (en) * | 2019-02-24 | 2019-06-25 | 北京氦舶科技有限责任公司 | A kind of normal temperature cure conducting resinl and preparation method thereof |
| CN110337191A (en) * | 2019-07-03 | 2019-10-15 | 常州轻工职业技术学院 | A method of the 3D printing great power LED printed circuit board based on Graphene conductive ink |
| JP2020097713A (en) * | 2018-12-18 | 2020-06-25 | ニホンハンダ株式会社 | Production method of conductive filler, conductive filler, conductive addition reaction-curable silicone elastomer composition and semiconductor device |
| WO2023092575A1 (en) * | 2021-11-29 | 2023-06-01 | 广州市白云化工实业有限公司 | Modified epoxy acrylate prepolymer, photo-thermal dual-curing conductive adhesive, and preparation method therefor |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1984002423A1 (en) * | 1982-12-11 | 1984-06-21 | Kennedy John W | Formable polymer composition |
| US6942824B1 (en) * | 2002-05-22 | 2005-09-13 | Western Digital (Fremont), Inc. | UV curable and electrically conductive adhesive for bonding magnetic disk drive components |
| CN1699492A (en) * | 2005-07-11 | 2005-11-23 | 大连轻工业学院 | Photo-curable conductive adhesive and method for making same |
| CN101441382A (en) * | 2007-11-19 | 2009-05-27 | 中国科学院理化技术研究所 | One-step cover closing method of electronic paper micro-cup and cover closing material |
-
2009
- 2009-11-27 CN CN2009101942004A patent/CN102079847A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1984002423A1 (en) * | 1982-12-11 | 1984-06-21 | Kennedy John W | Formable polymer composition |
| US6942824B1 (en) * | 2002-05-22 | 2005-09-13 | Western Digital (Fremont), Inc. | UV curable and electrically conductive adhesive for bonding magnetic disk drive components |
| CN1699492A (en) * | 2005-07-11 | 2005-11-23 | 大连轻工业学院 | Photo-curable conductive adhesive and method for making same |
| CN101441382A (en) * | 2007-11-19 | 2009-05-27 | 中国科学院理化技术研究所 | One-step cover closing method of electronic paper micro-cup and cover closing material |
Cited By (20)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US9534124B2 (en) * | 2010-02-05 | 2017-01-03 | Cam Holding Corporation | Photosensitive ink compositions and transparent conductors and method of using the same |
| US20110192633A1 (en) * | 2010-02-05 | 2011-08-11 | Cambrios Technologies Corporation | Photosensitive ink compositions and transparent conductors and method of using the same |
| CN103165215A (en) * | 2011-12-14 | 2013-06-19 | 上海宝银电子材料有限公司 | Silver paste for mobile phone shielding and preparation method thereof |
| CN103854853A (en) * | 2012-12-03 | 2014-06-11 | 六和电子（江西）有限公司 | Epoxy resin one-step packaging production technology of foil-type capacitor |
| CN105073939B (en) * | 2013-04-02 | 2018-11-09 | 昭和电工株式会社 | Conductive adhesive, anisotropic conductive film and use their electronic equipment |
| CN105073939A (en) * | 2013-04-02 | 2015-11-18 | 昭和电工株式会社 | Conductive adhesive, anisotropic conductive film and electronic devices using both |
| US9701874B2 (en) | 2013-04-02 | 2017-07-11 | Showa Denko K.K. | Conductive adhesive, anisotropic conductive film, and electronic device using same |
| CN103555251A (en) * | 2013-10-18 | 2014-02-05 | 中山职业技术学院 | High-heat-conductivity high-reliability ultraviolet-curing LED (light-emitting diode) electrically-conductive silver adhesive and preparation method thereof |
| CN103555251B (en) * | 2013-10-18 | 2015-03-11 | 中山职业技术学院 | High-heat-conductivity high-reliability ultraviolet-curing LED (light-emitting diode) electrically-conductive silver adhesive and preparation method thereof |
| CN104143373A (en) * | 2014-07-30 | 2014-11-12 | 安徽状元郎电子科技有限公司 | Oyster shell/fluorapatite composite conductive silver paste and preparation method thereof |
| CN104143373B (en) * | 2014-07-30 | 2016-07-20 | 安徽状元郎电子科技有限公司 | Conductive silver paste that a kind of Concha Ostreae/fluor-apatite is compound and preparation method thereof |
| CN105006272A (en) * | 2015-08-03 | 2015-10-28 | 佛山市顺德区百锐新电子材料有限公司 | Ultraviolet conductive silver slurry, and preparation method and application thereof |
| CN106520010A (en) * | 2016-11-08 | 2017-03-22 | 铜陵中锐电子科技有限公司 | An electrically conductive adhesive used for LEDs and a preparing method thereof |
| CN107393811A (en) * | 2017-07-24 | 2017-11-24 | 北京时代民芯科技有限公司 | A kind of silver paste bonding die ceramic package device takes chip method |
| CN107393811B (en) * | 2017-07-24 | 2019-07-23 | 北京时代民芯科技有限公司 | A kind of silver paste bonding die ceramic package device takes chip method |
| JP2020097713A (en) * | 2018-12-18 | 2020-06-25 | ニホンハンダ株式会社 | Production method of conductive filler, conductive filler, conductive addition reaction-curable silicone elastomer composition and semiconductor device |
| CN109628042A (en) * | 2018-12-26 | 2019-04-16 | 深圳日高胶带新材料有限公司 | A kind of photo-crosslinking adhesive |
| CN109929490A (en) * | 2019-02-24 | 2019-06-25 | 北京氦舶科技有限责任公司 | A kind of normal temperature cure conducting resinl and preparation method thereof |
| CN110337191A (en) * | 2019-07-03 | 2019-10-15 | 常州轻工职业技术学院 | A method of the 3D printing great power LED printed circuit board based on Graphene conductive ink |
| WO2023092575A1 (en) * | 2021-11-29 | 2023-06-01 | 广州市白云化工实业有限公司 | Modified epoxy acrylate prepolymer, photo-thermal dual-curing conductive adhesive, and preparation method therefor |
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Application publication date: 20110601 |