CN107622809A - A kind of copper electrode paste and preparation method thereof - Google Patents
A kind of copper electrode paste and preparation method thereof Download PDFInfo
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- CN107622809A CN107622809A CN201710872088.XA CN201710872088A CN107622809A CN 107622809 A CN107622809 A CN 107622809A CN 201710872088 A CN201710872088 A CN 201710872088A CN 107622809 A CN107622809 A CN 107622809A
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Abstract
The invention discloses a kind of copper electrode paste and preparation method thereof, the slurry is made up of by weight following compositions：Copper nanoparticle 80~110, glass dust 10~16, organic binder bond 20~30, wherein, average grain diameter≤50nm of the copper nanoparticle, specific surface area ＞ 18m2/g；The organic binder bond is made up of by weight percentage following each component：74~86% organic solvents, 11~20% resins, 1~2% coupling agent, 1~2% surfactant, 1~2% diluent.The slurry possesses good solderability and high adhesion force, silver is replaced using copper, reduce production cost, and after testing, electric conductivity is suitable with commercially available silver paste, better than the copper slurry of prior art, improve product quality, using nano-scale copper powder as raw material, while ensure that excellent electric property, also there is excellent oxidation resistance.
Description
Technical field
The invention belongs to electrocondution slurry field, and in particular to a kind of copper electrode paste and preparation method thereof.
Background technology
Electric slurry is a kind of new material, compared to other traditional circuit equipment have efficiently, environmental protection, energy-conservation, it is low into
This features such as, solar cell, space flight and aviation, sensing element, resistor network, display, lithium electronics electricity have been widely used in it
The technical fields such as the electrode material in pond.Electric slurry is passed through by solid metal powder, binding agent, organic solvent and other additives
Three-roll rolling is mixed into uniform paste, and form thickness by printing-sintering technology on substrate arrives some tens of pm for several microns
Film layer, can be used as manufacturing the basic materials of various electronic components.Conductive copper paste is by a kind of copper powder, a kind of thermosetting tree
The hybrid conductive coating of fat, a kind of organic solvent and other modifying agent composition.Compared to other base metal fillers, the volume electricity of copper
Resistance rate is with silver very close to and its price is only the 1/21 of silver-colored price, therefore is to prepare the preferable conductive filler of electrocondution slurry.It is conductive
Copper slurry has excellent electric conductivity, has been widely used in electronics industry, electrically-conducting paint, catalyst, lube oil additive etc.
Multiple fields, also there is potential application value in electromagnetic shielding and microelectronics Packaging field.The copper slurry of prior art is compared
Also it has been short of in silver paste electric conductivity, production cost, but product matter is although reduced using copper slurry as electrode slurry
Amount is also affected.
The B of CN 101364455 disclose a kind of base metal copper electrode paste and capacitor produced preparation, and the patent uses
Ball copper and piece copper are as raw material, and although the cost of sizing agent prepared reduces, but electric conductivity is general, oxidation resistance deficiency.
The content of the invention
The electric conductivity of copper and its crystal habit are closely related, and amorphous or nanocrystalline copper powder have excellent electrology characteristic and prevented
Oxidisability.It is an object of the invention to provide a kind of copper electrode paste and preparation method thereof, the slurry possess good solderability and
High adhesion force, electric conductivity is suitable with commercially available silver paste, higher than the copper slurry of prior art, also there is excellent anti-oxidant energy
Power, product quality is improved while reducing production cost.
The present invention is achieved by the following technical solutions：
A kind of copper electrode paste, it is made up of by weight following compositions：
Copper nanoparticle 80~110, glass dust 10~16, organic binder bond 20~30；
Wherein, average grain diameter≤50nm of the copper nanoparticle, specific surface area ＞ 18m2/g；
The organic binder bond is made up of by weight percentage following each component：74~86% organic solvents, 11~20%
Resin, 1~2% coupling agent, 1~2% surfactant, 1~2% diluent.
Preferably, the organic solvent is one in isopropanol, terpinol, butyl carbitol, dioctyl phthalate
Kind or any two kinds of mixed solvent.
Preferably, the resin is two kinds or two kinds in superchlorinated polyvinyl chloride resin, hydroxyethyl cellulose, melmac
Mixture above.
Preferably, the coupling agent is silane coupler KH792 or DL602.
Preferably, the surfactant is sodium n-alkylbenzenesulfonate or lauroyl glutamate.
Preferably, the diluent is toluene or dimethylbenzene.
The preparation method of above-mentioned copper electrode paste, comprises the following steps：
Organic solvent is placed in reactor by step 1) by part, adds deployed resin, normal temperature 100r/min thereto
After stirring and dissolving, then coupling agent and diluent are proportionally added into, are eventually adding surfactant, normal temperature 100r/min stirrings 20~
40min, obtain the organic binder bond；
Step 2) weighs copper nanoparticle and glass dust by part, is added sequentially in the organic binder bond of step 1) preparation, makes
Stirred evenly at a high speed under 1000~1200r/min with stirring dispersion machine, be then ground to 10 μm of fineness ＜ with three-roll grinder, obtain
To the copper electrode paste.
Beneficial effects of the present invention are as follows：
1st, silver is replaced using copper, reduces production cost, and after testing, electric conductivity is suitable with commercially available silver paste, is better than
The copper slurry of prior art, improves product quality.
2nd, the coupling agent in additive can improve the bonding strength of copper slurry coating and ceramic substrate, and test result shows
Show, copper slurry of the invention possesses good solderability and high adhesion force.
3rd, using copper nanoparticle as raw material, while ensure that excellent electric property, also have excellent anti-oxidant
Ability.
Embodiment
With reference to embodiment, the present invention is further elaborated.
Embodiment 1
A kind of copper electrode paste, the slurry are made up by weight of following material：
Copper nanoparticle 80, glass dust 10, isopropanol 14.8, superchlorinated polyvinyl chloride resin 2, hydroxyethyl cellulose 2, KH792 (silane
Coupling agent) 0.4, sodium n-alkylbenzenesulfonate 0.4, dimethylbenzene 0.4；
Wherein copper nanoparticle can use average grain diameter≤50nm, specific surface area ＞ 18m2/ g commercially available copper nanoparticle.
The preparation method of the copper electrode paste is as follows：
1st, 14.8 parts of isopropanols are placed in reactor, add 2 parts of superchlorinated polyvinyl chloride resins, 2 parts of hydroxy ethyl fibers thereto
Element, after normal temperature 100r/min stirring and dissolvings, then it is proportionally added into 0.4 part of KH792 silane coupler and 0.4 part of dimethylbenzene dilution
Agent, 0.4 part of sodium n-alkylbenzenesulfonate is eventually adding as surfactant, normal temperature 100r/min stirring 20min, is obtained organic
Binding agent；
2nd, 80 parts of copper nanoparticles and 10 parts of glass dust are weighed, is added sequentially in the organic binder bond of preparation, uses stirring
Dispersion machine stirs evenly at a high speed under 1000r/min, is then ground to 10 μm of fineness ＜ with three-roll grinder, obtains the copper electrode
Slurry.
Embodiment 2
A kind of copper electrode paste, the slurry are made up by weight of following material：
Copper nanoparticle 110, glass dust 16, terpinol 10.8, butyl carbitol 15, superchlorinated polyvinyl chloride resin 1.5, melamine
Resin 1.8, DL602 (silane coupler) 0.3, lauroyl glutamate 0.3, toluene 0.3；
Wherein copper nanoparticle can use average grain diameter≤50nm, specific surface area ＞ 18m2/ g commercially available copper nanoparticle.
The preparation method of the copper electrode paste is as follows：
1st, it is placed in after mixing 10.8 parts of terpinols, 15 parts of butyl carbitols in reactor, adds 1.5 parts thereto and cross chlorine
Vinyl, 1.8 parts of melmacs, after normal temperature 100r/min stirring and dissolvings, then it is proportionally added into 0.3 part of DL602 silane
Coupling agent and 0.3 part of dilution with toluene agent, 0.3 part of lauroyl glutamate is eventually adding as surfactant, normal temperature 100r/
Min stirs 40min, obtains organic binder bond；
2nd, 110 parts of copper nanoparticles and 16 parts of glass dust are weighed, is added sequentially in the organic binder bond of preparation, uses stirring
Dispersion machine stirs evenly at a high speed under 1200r/min, is then ground to 10 μm of fineness ＜ with three-roll grinder, obtains the copper electrode
Slurry.
Embodiment 3
A kind of copper electrode paste, the slurry are made up by weight of following material：
Copper nanoparticle 100, glass dust 12, isopropanol 10, dioctyl phthalate 10, hydroxyethyl cellulose 2, melamine
Polyimide resin 2, KH792 (silane coupler) 0.5, lauroyl glutamate 0.25, toluene 0.25；
Wherein copper nanoparticle can use average grain diameter≤50nm, specific surface area ＞ 18m2/ g commercially available copper nanoparticle.
The preparation method of the copper electrode paste is as follows：
1st, it is placed in after mixing 10 parts of isopropanols, 10 parts of dioctyl phthalates in reactor, adds 2 parts of hydroxyls thereto
Ethyl cellulose, 2 parts of melmacs, after normal temperature 100r/min stirring and dissolvings, then it is proportionally added into 0.5 part of KH792 silane
Coupling agent and 0.25 part of dilution with toluene agent, 0.25 part of lauroyl glutamate is eventually adding as surfactant, normal temperature 100r/
Min stirs 30min, obtains organic binder bond；
2nd, 100 parts of copper nanoparticles and 12 parts of glass dust are weighed, is added sequentially in the organic binder bond of preparation, uses stirring
Dispersion machine stirs evenly at a high speed under 1100r/min, is then ground to 10 μm of fineness ＜ with three-roll grinder, obtains the copper electrode
Slurry.
Embodiment 4
A kind of copper electrode paste, the slurry are made up by weight of following material：
Copper nanoparticle 90, glass dust 10, terpinol 8, dioctyl phthalate 7, superchlorinated polyvinyl chloride resin 2, ethoxy are fine
Dimension element 2, DL602 (silane coupler) 0.4, sodium n-alkylbenzenesulfonate 0.4, dimethylbenzene 0.2；
Wherein copper nanoparticle can use average grain diameter≤50nm, specific surface area ＞ 18m2/ g commercially available copper nanoparticle.
The preparation method of the copper electrode paste is as follows：
1st, it is placed in after mixing 8 parts of terpinols, 7 parts of dioctyl phthalates in reactor, adds 2 parts thereto and cross chlorine
Vinyl, 2 parts of hydroxyethyl celluloses, after normal temperature 100r/min stirring and dissolvings, then to be proportionally added into 0.4 part of DL602 silane even
Join agent and 0.4 part of diformazan benzene diluter, be eventually adding 0.2 part of sodium n-alkylbenzenesulfonate as surfactant, normal temperature 100r/
Min stirs 30min, obtains organic binder bond；
2nd, 90 parts of copper nanoparticles and 10 parts of glass dust are weighed, is added sequentially in the organic binder bond of preparation, uses stirring
Dispersion machine stirs evenly at a high speed under 1000r/min, is then ground to 10 μm of fineness ＜ with three-roll grinder, obtains the copper electrode
Slurry.
Embodiment 5
A kind of copper electrode paste, the slurry are made up by weight of following material：
Copper nanoparticle 100, glass dust 14, isopropanol 12.3, butyl carbitol 12.3, hydroxyethyl cellulose 2.1, melamine
Polyimide resin 2.1, DL602 (silane coupler) 0.3, sodium n-alkylbenzenesulfonate 0.3, dimethylbenzene 0.6；
Wherein copper nanoparticle can use average grain diameter≤50nm, specific surface area ＞ 18m2/ g commercially available copper nanoparticle.
The preparation method of the copper electrode paste is as follows：
1st, it is placed in after mixing 12.3 parts of isopropanols, 12.3 parts of butyl carbitols in reactor, adds 2.1 parts of hydroxyls thereto
Ethyl cellulose, 2.1 parts of melmacs, after normal temperature 100r/min stirring and dissolvings, then it is proportionally added into 0.3 part of DL602 silicon
Alkane coupling agent and 0.3 part of diformazan benzene diluter, 0.6 part of sodium n-alkylbenzenesulfonate is eventually adding as surfactant, normal temperature
100r/min stirs 40min, obtains organic binder bond；
2nd, 100 parts of copper nanoparticles and 14 parts of glass dust are weighed, is added sequentially in the organic binder bond of preparation, uses stirring
Dispersion machine stirs evenly at a high speed under 1100r/min, is then ground to 10 μm of fineness ＜ with three-roll grinder, obtains the copper electrode
Slurry.
Reference examples 1
1st, 20 parts of ethanol are placed in reactor, add 5 parts of bisphenol A type epoxy resins thereto, normal temperature 100r/min is stirred
After mixing dissolving, then 0.2 part of diformazan benzene diluter is proportionally added into, is eventually adding 0.2 part of sodium n-alkylbenzenesulfonate as surface
Activating agent, normal temperature 100r/min stirring 40min, obtains organic binder bond；
2nd, 90 parts of piece copper (average grain diameter is 20 μm or so) and 11 parts of glass dust are weighed, are added sequentially to the organic viscous of preparation
Tie in agent, stirred evenly at a high speed under 1000r/min using stirring dispersion machine, be then ground to the μ of fineness ＜ 10 with three-roll grinder
M, obtain copper electrode paste.
Reference examples 2
Take the commercially available chip ceramic capacitor conductive silver paste containing 65%Ag, silk-screen printing in ceramic substrate surface,
Sintered in air, prepare Y5V type chip ceramic capacitors.
By copper electrode paste silk-screen printing made from embodiment 1~5 and reference examples 1 in ceramic substrate surface, protected in N2 gas
Shield is lower to be sintered, and prepares Y5V type chip ceramic capacitors.
Obtained Y5V types chip ceramic capacitor is detected respectively, test result such as table 1.
The testing result of table 1
From the test result of table 1, copper electrode paste electric conductivity prepared by the present invention is suitable with commercially available Ag slurries, and shows
The copper electrode paste for having technology then shows slightly deficiency, and adhesive force is substantially better than the slurry of prior art after solderability and sintering, because
Not only electric conductivity and welding performance are excellent for this copper electrode paste of the invention, there is good inoxidizability, and cost is relatively low,
It is suitable to promote.
Claims (7)
1. a kind of copper electrode paste, it is characterised in that the slurry is made up of by weight following compositions：
Copper nanoparticle 80~110, glass dust 10~16, organic binder bond 20~30；
Wherein, average grain diameter≤50nm of the copper nanoparticle, specific surface area ＞ 18m2/g；
The organic binder bond is made up of by weight percentage following each component：74~86% organic solvents, 11~20% resins,
1~2% coupling agent, 1~2% surfactant, 1~2% diluent.
2. a kind of copper electrode paste according to claim 1, it is characterised in that the organic solvent is isopropanol, pine tar
One kind or any two kinds of mixed solvent in alcohol, butyl carbitol, dioctyl phthalate.
3. a kind of copper electrode paste according to claim 1, it is characterised in that the resin is superchlorinated polyvinyl chloride resin, hydroxyl
Two or more mixture in ethyl cellulose, melmac.
4. a kind of copper electrode paste according to claim 1, it is characterised in that the coupling agent is silane coupler
KH792 or DL602.
5. a kind of copper electrode paste according to claim 1, it is characterised in that the surfactant is linear alkylbenzene (LAB)
Sodium sulfonate or lauroyl glutamate.
6. a kind of copper electrode paste according to claim 1, it is characterised in that the diluent is toluene or dimethylbenzene.
7. based on a kind of preparation method of copper electrode paste described in claim 1, comprise the following steps：
Organic solvent is placed in reactor by step 1) by part, adds deployed resin, normal temperature 100r/min stirrings thereto
After dissolving, then coupling agent and diluent are proportionally added into, are eventually adding surfactant, normal temperature 100r/min stirrings 20~
40min, obtain the organic binder bond；
Step 2) weighs copper nanoparticle and glass dust by part, is added sequentially in the organic binder bond of step 1) preparation, using stirring
Mix dispersion machine to stir evenly at a high speed under 1000~1200r/min, be then ground to 10 μm of fineness ＜ with three-roll grinder, obtain institute
State copper electrode paste.
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| CN201710872088.XA CN107622809A (en) | 2017-09-25 | 2017-09-25 | A kind of copper electrode paste and preparation method thereof |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108899107A (en) * | 2018-05-23 | 2018-11-27 | 江苏时瑞电子科技有限公司 | A kind of Zinc-oxide piezoresistor carbon fiber-copper nanoparticle combination electrode slurry and preparation method thereof |
| CN108922652A (en) * | 2018-05-23 | 2018-11-30 | 江苏时瑞电子科技有限公司 | A kind of Zinc-oxide piezoresistor corrosion-resistant electrode slurry and preparation method thereof |
| CN110391042A (en) * | 2019-07-22 | 2019-10-29 | 广东风华高新科技股份有限公司 | A kind of copper conductor slurry and the preparation method and application thereof |
| CN113327721A (en) * | 2021-08-04 | 2021-08-31 | 西安宏星电子浆料科技股份有限公司 | Preparation method of low-temperature cured conductive copper paste |
| CN118380181A (en) * | 2024-05-08 | 2024-07-23 | 扬州虹运电子材料有限公司 | Air sintered antioxidation copper slurry and preparation method thereof |
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| CN106251929A (en) * | 2016-08-10 | 2016-12-21 | 中国科学院电工研究所 | Copper slurry for crystal silicon solar battery front side conductive layer electrode and preparation method thereof |
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| CN101136261A (en) * | 2007-07-06 | 2008-03-05 | 广东风华高新科技股份有限公司 | Copper electrode slurry material and manufacturing method thereof |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108899107A (en) * | 2018-05-23 | 2018-11-27 | 江苏时瑞电子科技有限公司 | A kind of Zinc-oxide piezoresistor carbon fiber-copper nanoparticle combination electrode slurry and preparation method thereof |
| CN108922652A (en) * | 2018-05-23 | 2018-11-30 | 江苏时瑞电子科技有限公司 | A kind of Zinc-oxide piezoresistor corrosion-resistant electrode slurry and preparation method thereof |
| CN110391042A (en) * | 2019-07-22 | 2019-10-29 | 广东风华高新科技股份有限公司 | A kind of copper conductor slurry and the preparation method and application thereof |
| CN113327721A (en) * | 2021-08-04 | 2021-08-31 | 西安宏星电子浆料科技股份有限公司 | Preparation method of low-temperature cured conductive copper paste |
| CN113327721B (en) * | 2021-08-04 | 2021-11-30 | 宁波维柔电子科技有限公司 | Preparation method of low-temperature cured conductive copper paste |
| CN118380181A (en) * | 2024-05-08 | 2024-07-23 | 扬州虹运电子材料有限公司 | Air sintered antioxidation copper slurry and preparation method thereof |
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