CN107573876A - A kind of UV curing process of the filling-modified conductive adhesive of silver-coated copper powder - Google Patents
A kind of UV curing process of the filling-modified conductive adhesive of silver-coated copper powder Download PDFInfo
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- CN107573876A CN107573876A CN201710831780.8A CN201710831780A CN107573876A CN 107573876 A CN107573876 A CN 107573876A CN 201710831780 A CN201710831780 A CN 201710831780A CN 107573876 A CN107573876 A CN 107573876A
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Abstract
The invention discloses a kind of UV curing process of the filling-modified conductive adhesive of silver-coated copper powder, it is characterised in that ethanol, Ni-coated graphite, after impregnation, forced air drying are added into VTES；Absolute ethyl alcohol, KH550 are added into silver-coated copper powder, ultrasonic disperse processing, obtains slurry；Ball milling, vacuum drying；Distilled water, ethylene glycol are added into silver nitrate, stirring and dissolving, graphene oxide suspension is added, heating water bath, is slowly added to sodium borohydride solution, heating is heated to reflux, and is filtered, is washed, drying；Isooctyl acrylate monomer, trimethylolpropane trimethacrylate, benzoin ethyl ether, benzoyl peroxide are mixed, ultrasound, polyurethane prepolymer is added, stirs; it is ultrasonic again, add above resulting material, strong stirring; stand, be put into UV solidification cases and fully solidify, obtain the adhesive.
Description
Technical field
The present invention relates to conductive adhesive field, and in particular to a kind of UV of the filling-modified conductive adhesive of silver-coated copper powder
Curing process.
Background technology
With the fast development of microelectronics integrated technology and package technique, the volume of electronic component and logic circuit is more next
It is smaller, and working frequency sharply increases, the environment temperature of semiconductor is to high temperature direction change, to ensure electronic component for a long time
Reliably normal work, timely heat-sinking capability just turn into the restraining factors of its service life length.Highly thermally conductive polymeric base is compound
Material plays important in many manufacturing industry such as microelectronics, Aeronautics and Astronautics, military equipment, electrical equipment and electrical and high-tech area
Effect.Therefore excellent heat conductivility, and high heat-resisting, low dielectric loss, height are must assure that when preparing Heat Conduction Material
Anti-flammability and the performance such as good processability, so as to meet the requirement of electronic information industry.So it is excellent to develop combination property
Different Polymer Composites with High Thermal Conductivity becomes current study hotspot.
The content of the invention
The present invention solves the technical problem of the UV for providing a kind of filling-modified conductive adhesive of silver-coated copper powder to consolidate
Chemical industry skill, the conductive adhesive prepared according to the technique have good electric conductivity and mechanical property.
The technical problems to be solved by the invention are realized using following technical scheme：
The UV curing process of the filling-modified conductive adhesive of a kind of silver-coated copper powder, it is characterised in that carry out according to the following steps：
A. filler wet processed technique：
Into 0.5-1 parts by weight of ethylene ethyl triethoxy silicane alkane 1:15-20 adds ethanol, stirs, and adds 4-6 parts by weight and fills out
Expect Ni-coated graphite, after impregnation 2-3h, be put into forced air drying 3-4h, kept dry in 100-110 DEG C of baking oven；
B. pretreatment, vacuum drying and the ball-milling technology of silver-coated copper powder：
Into 4-7 parts by weight silver-coated copper powders 1:10-15 adds absolute ethyl alcohol, stirs 30-40min, adds 0.1-0.2 parts by weight silicon
Alkane coupling agent KH550, ultrasonic disperse processing 1-2h, obtains slurry；Ball milling 1-2h in ball mill is put it into, places into 90-100 DEG C
1-2h is dried in vacuum drying chamber；
C. the preparation of silver-colored graphene nano conductive filler is covered：
Into 3-6 parts by weight graphite oxides 1:5-10 adds ethylene glycol, sonic oscillation 50-60min, is vigorously agitated again 1-2h, obtains
Graphene oxide suspension；
Into 1-2 parts by weight silver nitrates 1:5:8-10 adds distilled water, ethylene glycol, stirring and dissolving, adds graphene oxide and suspends
Liquid, 1-2h is heated in 50-60 DEG C of water-bath, be slowly added to 1-2 parts by weight sodium borohydride solutions, be warming up to 110-120 DEG C of heating
Flow back 1-2h, filtering, washing 3-5 times, is dried at 70-80 DEG C；
D. UV curing process：
By the different monooctyl ester of the parts by weight of activated monomeric acrylics of 20-30,15-20 parts by weight of crosslinking agent trimethylolpropane tris acrylic acid
Ester, 2-4 parts by weight light triggers benzoin ethyl ether, the mixing of 0.5-1 parts by weight initiators benzoyl peroxide, ultrasonic 5-10min,
20-30 parts by weight of polyurethane prepolymers are added, are stirred, then ultrasonic 5-10min, resulting material in a, b, c is added, is strongly stirred
10-20min is mixed, stands 3-4h, fully solidification 10-20min is put into UV solidification cases, obtains the conductive adhesive.
Wherein, ball milling speed described in step b is 200-400r/min.Sodium borohydride solution concentration is described in step c
0.1-0.2mol/L.Polyurethane prepolymer described in step d is DH-318 (UAO), condition of cure 100-110mW/cm2Light
The wavelength of intensity, 315-400nm.
The present invention reaction mechanism and have the beneficial effect that：
Graphene oxide is mixed with silver nitrate, spent glycol and sodium borohydride reduce jointly, are made and cover silver-colored graphene nano and lead
Electric filler；During the course of the reaction, silver ion is reduced directly to Nano silver grain, and graphene sheet layer has big specific surface area,
Silver particles can be adsorbed on its surface；Filler silver-coated copper powder has dendritic structure, can improve the space contact probability of filler,
Reduce lumped resistance；Surface coated nano-Ag particles can improve inoxidizability, and high surface energy can reduce tunneling resistance, obtain
The conducting resinl of excellent electrical properties.
Traditional curing process needs high temperature or longer hardening time, and UV curing process can at room temperature in short-term
Interior completion, it is a kind of efficient curing mode；Stewing process before curing, conductive filler ordered arrangement can be made, increased
Conductive path so that the specific insulation of adhesive reduces；Ni-coated graphite surface is carried out with VTES
Processing, the electric conductivity and mechanical property of adhesive can be improved.
Embodiment
In order that the technical means, the inventive features, the objects and the advantages of the present invention are easy to understand, tie below
Specific embodiment is closed, the present invention is expanded on further.
Embodiment
The UV curing process of the filling-modified conductive adhesive of a kind of silver-coated copper powder, it is characterised in that enter according to the following steps
OK：
A. filler wet processed technique：
Into 0.5kg VTESs 1:15 add ethanol, stir, and add 6kg filler Ni-coated graphites, dipping
After handling 2h, forced air drying 3h, kept dry in 100-110 DEG C of baking oven are put into；
B. pretreatment, vacuum drying and the ball-milling technology of silver-coated copper powder：
Into 7kg silver-coated copper powders 1:15 add absolute ethyl alcohol, stir 35min, add 0.2kg Silane coupling agent KH550s, ultrasound point
Processing 1h is dissipated, obtains slurry；Ball milling 2h in ball mill is put it into, places into and 2h is dried in 90-100 DEG C of vacuum drying chamber；
C. the preparation of silver-colored graphene nano conductive filler is covered：
Into 6kg graphite oxides 1:10 add ethylene glycol, sonic oscillation 55min, are vigorously agitated again 1h, obtain graphene oxide suspension
Liquid；
Into 2kg silver nitrates 1:5:10 add distilled water, ethylene glycol, stirring and dissolving, graphene oxide suspension are added, in 50-
1h is heated in 60 DEG C of water-baths, is slowly added to 1kg sodium borohydride solutions, 110-120 DEG C is warming up to and is heated to reflux 1h, filtering, washing 3
It is secondary, dried at 70-80 DEG C；
D. UV curing process：
By 30kg activated monomers Isooctyl acrylate monomer, 15kg crosslinking agents trimethylolpropane trimethacrylate, 3kg light triggers peace
Fragrant ether, the mixing of 0.5kg initiators benzoyl peroxide are ceased, ultrasonic 10min, 30kg polyurethane prepolymers is added, stirs,
Ultrasonic 10min again, resulting material in a, b, c is added, strong stirring 20min, 3h is stood, is put into UV solidification cases and fully solidifies
15min, obtain the conductive adhesive.
Wherein, ball milling speed described in step b is 300r/min.Sodium borohydride solution concentration is described in step c
0.15mol/L.Polyurethane prepolymer described in step d is DH-318 (UAO), condition of cure 100-110mW/cm2Light intensity
Degree, 315-400nm wavelength.
Claims (5)
- A kind of 1. UV curing process of the filling-modified conductive adhesive of silver-coated copper powder, it is characterised in that：Ethanol, Ni-coated graphite, after impregnation, forced air drying are added into VTES；Into silver-coated copper powder Absolute ethyl alcohol, KH550 are added, ultrasonic disperse processing, obtains slurry；Ball milling, vacuum drying；Distilled water, second are added into silver nitrate Glycol, stirring and dissolving, graphene oxide suspension is added, heating water bath is slowly added to sodium borohydride solution, and heating is heated back Stream, filtering, washing, drying；By Isooctyl acrylate monomer, trimethylolpropane trimethacrylate, benzoin ethyl ether, benzoyl peroxide first Acyl mixes, and ultrasound, adds polyurethane prepolymer, stirs, then ultrasound, adds above resulting material, strong stirring, stands, It is put into UV solidification cases and fully solidifies, obtains the adhesive.
- A kind of 2. UV curing process of the filling-modified conductive adhesive of silver-coated copper powder, it is characterised in that：A. filler wet processed technique：Into 0.5-1 parts by weight of ethylene ethyl triethoxy silicane alkane 1:15-20 adds ethanol, stirs, and adds 4-6 parts by weight and fills out Expect Ni-coated graphite, after impregnation 2-3h, be put into forced air drying 3-4h, kept dry in 100-110 DEG C of baking oven；B. pretreatment, vacuum drying and the ball-milling technology of silver-coated copper powder：Into 4-7 parts by weight silver-coated copper powders 1:10-15 adds absolute ethyl alcohol, stirs 30-40min, adds 0.1-0.2 parts by weight silicon Alkane coupling agent KH550, ultrasonic disperse processing 1-2h, obtains slurry；Ball milling 1-2h in ball mill is put it into, places into 90-100 DEG C 1-2h is dried in vacuum drying chamber；C. the preparation of silver-colored graphene nano conductive filler is covered：Into 3-6 parts by weight graphite oxides 1:5-10 adds ethylene glycol, sonic oscillation 50-60min, is vigorously agitated again 1-2h, obtains Graphene oxide suspension；Into 1-2 parts by weight silver nitrates 1:5:8-10 adds distilled water, ethylene glycol, stirring and dissolving, adds graphene oxide and suspends Liquid, 1-2h is heated in 50-60 DEG C of water-bath, be slowly added to 1-2 parts by weight sodium borohydride solutions, be warming up to 110-120 DEG C of heating Flow back 1-2h, filtering, washing 3-5 times, is dried at 70-80 DEG C；D. UV curing process：By the different monooctyl ester of the parts by weight of activated monomeric acrylics of 20-30,15-20 parts by weight of crosslinking agent trimethylolpropane tris acrylic acid Ester, 2-4 parts by weight light triggers benzoin ethyl ether, the mixing of 0.5-1 parts by weight initiators benzoyl peroxide, ultrasonic 5-10min, 20-30 parts by weight of polyurethane prepolymers are added, are stirred, then ultrasonic 5-10min, resulting material in a, b, c is added, is strongly stirred 10-20min is mixed, stands 3-4h, fully solidification 10-20min is put into UV solidification cases, obtains the conductive adhesive.
- 3. a kind of UV curing process of the filling-modified conductive adhesive of silver-coated copper powder according to claim 2, its feature It is, ball milling speed described in step b is 200-400r/min.
- 4. a kind of UV curing process of the filling-modified conductive adhesive of silver-coated copper powder according to claim 2, its feature It is, sodium borohydride solution concentration described in step c is 0.1-0.2mol/L.
- 5. a kind of UV curing process of the filling-modified conductive adhesive of silver-coated copper powder according to claim 2, its feature It is, polyurethane prepolymer described in step d is DH-318 (UAO), condition of cure 100-110mW/cm2Luminous intensity, 315-400nm wavelength.
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| CN201710831780.8A CN107573876A (en) | 2017-09-15 | 2017-09-15 | A kind of UV curing process of the filling-modified conductive adhesive of silver-coated copper powder |
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Cited By (2)
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| CN109943252A (en) * | 2019-02-28 | 2019-06-28 | 苏州金枪新材料股份有限公司 | A kind of wicker copper conducting resinl and preparation method thereof |
| CN111205806A (en) * | 2020-01-20 | 2020-05-29 | 浙江多邦新材料有限公司 | High-conductivity conductive adhesive and synthesis process thereof |
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2017
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| CN102277109A (en) * | 2011-07-19 | 2011-12-14 | 彩虹集团公司 | Preparation method of environmentally-friendly photocuring silver conductive adhesive |
| CN106715615A (en) * | 2014-04-22 | 2017-05-24 | 沙特基础工业全球技术有限公司 | Ultraviolet curable transfer coating for applying nanometer sized metal particles to polymer surface |
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| CN109943252A (en) * | 2019-02-28 | 2019-06-28 | 苏州金枪新材料股份有限公司 | A kind of wicker copper conducting resinl and preparation method thereof |
| CN111205806A (en) * | 2020-01-20 | 2020-05-29 | 浙江多邦新材料有限公司 | High-conductivity conductive adhesive and synthesis process thereof |
| CN115386327A (en) * | 2020-01-20 | 2022-11-25 | 浙江多邦新材料有限公司 | High-conductivity conductive adhesive and preparation method and application thereof |
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Application publication date: 20180112 |