CN109166671A - A kind of preparation method of rapid draing low temperature silver paste - Google Patents
A kind of preparation method of rapid draing low temperature silver paste Download PDFInfo
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- CN109166671A CN109166671A CN201810957218.4A CN201810957218A CN109166671A CN 109166671 A CN109166671 A CN 109166671A CN 201810957218 A CN201810957218 A CN 201810957218A CN 109166671 A CN109166671 A CN 109166671A
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- resin
- silver paste
- low temperature
- preparation
- rapid draing
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B13/00—Apparatus or processes specially adapted for manufacturing conductors or cables
Abstract
The invention discloses a kind of preparation methods of rapid draing low temperature silver paste, include the following steps: S1, prepare raw material, prepare solvent, select resin, weigh silver powder, selected auxiliary agent；S2, solvent preheating are added first part's resin agitating and melt, form carrier；Silver powder and auxiliary agent are added into carrier, is stirred, forms thick slurry by S3；Surplus resin is added into thick slurry, then is filtered, is stirred under vacuum defoaming by S4, obtains slurry；S5 grinds slurry, is rolled, and finished product silver paste is obtained.By above-mentioned setting, resin is added in solvent in two times, so that resin and silver powder and auxiliary agent disperse more uniform, an entirety of homogeneous is capable of forming, reduces resistance value, reinforce the electric conductivity of finished product, while the also imparting good pliability of finished product.
Description
Technical field
The present invention relates to electronics connecting material technical field, in particular to a kind of preparation side of rapid draing low temperature silver paste
Method.
Background technique
In recent years, with the rapid development of electronics industry, thin film switch, flexible printed circuit board, electromagnetic shielding, potentiometer
And the demand of the products such as computor-keyboard also increases sharply, and conductive silver paste is as the crucial function for preparing such electronic component
Energy material, development and application are also constantly subjected to the extensive concern of people.But the conductive silver paste in China includes that low-temperature setting is led
Electric silver paste is most of still to rely on import, and the technology of preparing of the high quality conductive silver paste of domestic production is great prominent still without obtaining
It is broken, there can be more or less deficiency.
China if application publication number is CN101645318A applies for a patent that a kind of circuit of laptop keyboard is dedicated to lead
Electric silver paste and preparation method thereof, wherein silver paste includes silver powder, macromolecule resin, additive and solvent, and solvent is ester
Class solvent or ketone resins, additive include levelling agent, thickener and defoaming agent, and macromolecule resin is polyurethane resin or polyester
Resin.When preparation, each component first is taken by formula, then resin, solvent are mixed, heating is filtered after making it completely dissolved, and is obtained
Carrier；Silver powder is added again after obtaining carrier and stirs evenly to obtain silver paste, and finished product can be obtained and lead using grinding, rolling
Electric silver paste.
It is found that preparation process is still traditional from above scheme, although being made a change being formulated upper many enterprises and having
Attempt, but effect but also it is limited, and preparation process should be also adjusted accordingly more to adapt to the product of new formula
It is required that therefore, based on this, very it is necessary to propose a kind of preparation method of new silver paste.
Summary of the invention
In view of the deficiencies of the prior art, the present invention intends to provide a kind of preparation of rapid draing low temperature silver paste
Method.
Above-mentioned technical purpose of the invention has the technical scheme that a kind of rapid draing low temperature silver paste
Preparation method, include the following steps: S1, prepare raw material, prepare solvent, select resin, weigh silver powder, selected auxiliary agent；S2, it is molten
Agent preheating is added first part's resin agitating and melts, forms carrier；Silver powder and auxiliary agent are added into carrier, is stirred by S3,
Form thick slurry；Surplus resin is added into thick slurry, then is filtered, is stirred under vacuum defoaming by S4, obtains slurry；S5, to slurry
Material is ground, is rolled, and finished product silver paste is obtained.
By using above-mentioned technical proposal, resin is added in solvent in two times, so that resin and silver powder and auxiliary agent disperse
It is more uniform, be capable of forming an entirety of homogeneous, reduce resistance value, reinforce the electric conductivity of finished product, while being also given to
The good pliability of product.
The further setting of the present invention are as follows: solvent is using the arbitrary proportion of diethylene glycol ether acetate and DBE in S2
Compound, and it is 85-95 DEG C that the temperature of solvent is kept when preheating.
By using above-mentioned technical proposal, DBE be it is colourless, nontoxic and tasteless can be high by biodegradable environment-friendly type
Boiling point solvent, and diethylene glycol ether acetate is the very low solvent of colorless and transparent, toxicity, the solvent formed after the two mixing compared with
To be environmentally friendly, adaptation range is wider, moreover, mixed solvent boiling point is higher simultaneously, it is not volatile, it can effectively ensure that production
The original ingredient of product is relatively stable；On the other hand, the rate of drying of finished product slurry is very fast, is conducive to production and forms as early as possible.
The further setting of the present invention are as follows: resin includes polyvinyl acetate, polyamide and hydrogenated petroleum resin, and in S2
It is the 20%-30% of total resin weight when addition first part's resin.
By using above-mentioned technical proposal, polyvinyl acetate, polyamide are all more appropriate in production conductive silver paste
On the one hand resin, and after the hydrogenated petroleum resin added can significantly improve the viscous of carrier after macromolecule resin melting
Power and adhesion are tied, will closely be connected between conductive silver paste and substrate, due to being tied after hydrogenation in another aspect hydrogenated petroleum resin
Structure is stablized, it is difficult to aoxidize again, to can also have in the case where not using age resister even in hot environment
Standby good weatherability adapts to long-term use, while the addition of hydrogenated petroleum resin can also make whole resin system solid
Has good pliability after change.
The further setting of the present invention are as follows: the silver powder is diametrically 2-5 μm of sheet, and also added with accounting for silver powder in silver powder
Silver orthophosphate, silver pyrophosphate and the silver metaphosphate of total weight 2%-4%.
By using above-mentioned technical proposal, silver powder takes sheet, so that the contact area between adjacent silver particles is more
Greatly, be conducive to the transmission of electric signal, and resistance is smaller after film forming；
In the drying process, silver-colored phosphate can pass through slurry and substrate to silver orthophosphate, silver pyrophosphate and the silver metaphosphate of addition
Joint further reduces resistance to form Ohmic contact, strengthens electric conductivity.
The further setting of the present invention are as follows: use strainer mesh number for 850-900 mesh when being filtered in S4.
More impurity can be removed, guarantees the fineness of slurry by filtering by using above-mentioned technical proposal.
The further setting of the present invention are as follows: when carrying out being stirred under vacuum defoaming in S4, maintain air pressure in -0.1~-0.2MPa.
By using above-mentioned technical proposal, when stirring, negative pressure state is maintained, to lure that the bubble in slurry overflows into, is subtracted
Gap after few drying, reduces the resistance value of silver paste.
The further setting of the present invention is the component including following parts by weight:
16-20 parts of resin；65-78 parts of silver powder；10-15 parts of solvent；1-10 parts of auxiliary agent.
The further setting of the present invention are as follows: the resin includes the polyvinyl acetate that weight ratio is 1:1:0.2-0.5, gathers
Amide and hydrogenated petroleum resin.
The further setting of the present invention is that the auxiliary agent is grouped as by the group of following weight ratio:
Anti-settling agent 25-35%；
Defoaming agent 15-20%；
Adhesion promoter 20-25%；
Thixotropic agent 35-55%；
Wherein, thixotropic agent by ethyl cellulose, dibutyl phthalate, acrylic resin, polyvinylbutyrals extremely
A kind of few and castor oil is 1:3-5 composition according to weight ratio.
By using above-mentioned technical proposal, whether silver powder can be uniformly dispersed in resin and solvent, after film forming
The electric conductivity of conductive silver paste is particularly significant, and silver particles itself are relatively easy to there is a phenomenon where gathering, lower leaf in formation, or
At least electric conductivity sharp fall of side, therefore the sedimentation and accumulation of silver particles can be greatly reduced in the addition of anti-settling agent；
Conductive silver paste unavoidably needs to stir in process of production, and easily generates bubble not of uniform size during stirring, if
It is not taken out, bubble can cause strong influence to electric conductivity after the drying, increase resistance, therefore be properly added defoaming agent
Preferable effect can be obtained, is conducive to improve electric conductivity；Adhesion promoter and the adjustable slurry of thickener
Adhesion strength between matrix；
Thixotropic agent is by least one of ethyl cellulose, dibutyl phthalate, acrylic resin, polyvinylbutyrals
With castor oil according to weight ratio be 1:3-5 form, be stirred with resin and solvent after mixing, under the action of anti-settling agent uniformly
Be scattered in slurry system, and thixotropic agent can assign the good thixotropy of slurry and high viscosity so that finished product have compared with
High electric current, lesser resistance.
The further setting of the present invention are as follows: after thixotropic agent is added in S3, shear force is continuously applied to, until owning in S4
Resin dissolves completely.
By using above-mentioned technical proposal, constantly applies shear action after thixotropic agent is added, be not only to play stirring
Effect, while also being reinforced for the pliability of slurry entirety is further.
In conclusion the invention has the following advantages: resin is added in a point front and back twice, so that silver powder, solvent and tree
Rouge and auxiliary agent can disperse more uniform, and the performance of product is more stable, while be also beneficial to accelerate to be stirred in construction
Progress and improve stirring efficiency；Choosing suitable solvent, that resin and silver powder can be dispersed is uniform, and volatility is small
Be conducive to maintain to stablize, rate of drying is fast, is conducive to produce and process；Using addition defoaming agent and it is stirred under vacuum mutual cooperation, greatly
The air bubble content of amplitude reduced in finished product, the further electric conductivity for promoting product.
Specific embodiment
Embodiment 1-5, a kind of rapid draing low temperature silver paste, including component and its corresponding content it is as shown in table 1.Its
In, the weight ratio between polyvinyl acetate, polyamide and hydrogenated petroleum resin is 1:1:0.2；Anti-settling agent in auxiliary agent is
25%, defoaming agent 20%, adhesion promoter 20%, thixotropic agent 35, and thixotropic agent is the ethyl cellulose and castor oil group of 1:3
At.
Each component and its corresponding content (Kg) in 1 embodiment 1-5 of table
Embodiment 6, a kind of rapid draing low temperature silver paste, the difference from embodiment 1 is that, the anti-settling agent in auxiliary agent is
30%, defoaming agent 15%, adhesion promoter 20%, thixotropic agent 35, and thixotropic agent is the acrylic resin and polybutene alcohol of 1:4
Compound, the castor oil composition of butyral.
Embodiment 7, a kind of preparation method of rapid draing low temperature silver paste, the component and content contained such as 1 institute of embodiment
Include the following steps: when showing, and preparing
S1 prepares raw material, prepares solvent, selects resin, weighs silver powder, selected auxiliary agent；Wherein, resin includes polyvinyl acetate
Ester, polyamide and hydrogenated petroleum resin, silver powder are diametrically 2-5 μm of sheet, and also added with accounting for silver powder total weight in silver powder
Silver orthophosphate, silver pyrophosphate and the silver metaphosphate of 2%-4%；
S2, solvent use the compound of diethylene glycol ether acetate and the arbitrary proportion of DBE, and solvent heats temperature when preheating
And 90 DEG C are held in, the thawing of first part's resin agitating is added, carrier is formed, the resin of first part accounts for total weight resin
20%；
S3 keeps heating, and silver powder and auxiliary agent are added into carrier, is stirred, and forms thick slurry, after thixotropic agent is added, no
It is disconnected to apply shear force, until all resins dissolve completely；
S4 continues to heat, and surplus resin is added into thick slurry, then be filtered, be stirred under vacuum defoaming, obtains slurry；It crosses
It uses strainer mesh number for 900 mesh when filter, when carrying out being stirred under vacuum defoaming, maintains air pressure in -0.1~-0.2MPa；
S5 grinds slurry, is rolled, and finished product silver paste is obtained.
Comparative example 1, a kind of production method of silver paste, the difference with embodiment 7 are: whole trees is added at one time in S2
Rouge, and stir to whole thawings.
Comparative example 2, a kind of production method of silver paste, the difference with embodiment 7 are: directly being ground after filtering in S4
Mill, rolling, and obtain finished product silver paste.
Comparative example 3-7, a kind of silver paste, the difference from embodiment 1 is that comprising component and corresponding content such as table 2
It is shown.
Each component and its corresponding content (Kg) in 2 comparative example 3-7 of table
Test portion
Test 1, the test of silver paste end properties
Choosing embodiment 1-3, embodiment 7, comparative example 1-4 number consecutively is 1-8 group, wherein cuts out 8 groups of obtained silver paste finished products
It takes identical size as laboratory sample, and cohesive force test is carried out to 8 groups of laboratory samples, be with the cohesive force that embodiment 1 measures
Standard value, and by experiment value measured by 8 groups and the ratio (adhesion value) of standard value and corresponding experimental result record such as table 3.
The test of 3 silver paste end properties of table
Test 2, silver paste finished product void test
Test method: the product of each group in embodiment and comparative example or finished product obtained are cut into the identical code test of size
Block tests each piece of weight and is recorded as X, then is computed and obtains theoretical weight Y corresponding to standard block size, records every piece of examination
The porosity value Z of block is tested in table 4, wherein Z=100%* (Y-X)/Y.
4 silver paste finished product void test of table
Test 3, drying test
The product of each group in embodiment and comparative example or finished product obtained are cut into the identical code test block of size, each piece
Standard block size is 1cm*1cm*5 μm, and each group is placed in 80 DEG C of environment and carries out drying and processing, records experimental result such as table
Shown in 5.
5 drying time of table
Claims (10)
1. a kind of preparation method of rapid draing low temperature silver paste, which comprises the steps of:
S1 prepares raw material, prepares solvent, selects resin, weighs silver powder, selected auxiliary agent；
S2, solvent preheating are added first part's resin agitating and melt, form carrier；
S3 keeps heating, and silver powder and auxiliary agent are added into carrier, is stirred, forms thick slurry；
S4 continues to heat, and surplus resin is added into thick slurry, then be filtered, be stirred under vacuum defoaming, obtains slurry；
S5 grinds slurry, is rolled, and finished product silver paste is obtained.
2. a kind of preparation method of rapid draing low temperature silver paste according to claim 1, it is characterised in that: solvent is adopted in S2
With the compound of diethylene glycol ether acetate and the arbitrary proportion of DBE, and it is 85-95 DEG C that while preheating, which keeps the temperature of solvent,.
3. a kind of preparation method of rapid draing low temperature silver paste according to claim 2, it is characterised in that: resin includes poly-
Vinylacetate, polyamide and hydrogenated petroleum resin, and the 20%- in S2 when addition first part's resin for total resin weight
30%。
4. a kind of preparation method of rapid draing low temperature silver paste according to claim 3, it is characterised in that: the silver powder is in
The sheet that diameter is 2-5 μm, and also added with the silver orthophosphate, silver pyrophosphate and metaphosphoric acid for accounting for silver powder total weight 2%-4% in silver powder
Silver.
5. a kind of preparation method of rapid draing low temperature silver paste according to claim 4, it is characterised in that: carried out in S4
Use strainer mesh number for 850-900 mesh when filter.
6. a kind of preparation method of rapid draing low temperature silver paste according to claim 5, it is characterised in that: carried out in S4 true
When sky stirring defoaming, maintain air pressure in -0.1 ~ -0.2MPa.
7. a kind of preparation method of rapid draing low temperature silver paste according to claim 1, which is characterized in that including weighing as follows
Measure the component of number:
16-20 parts of resin；
65-78 parts of silver powder；
10-15 parts of solvent；
1-10 parts of auxiliary agent.
8. a kind of preparation method of rapid draing low temperature silver paste according to claim 7, it is characterised in that: the resin packet
Include polyvinyl acetate, polyamide and the hydrogenated petroleum resin that weight ratio is 1:1:0.2-0.5.
9. a kind of preparation method of rapid draing low temperature silver paste according to claim 8, which is characterized in that the auxiliary agent by
The group of following weight ratio is grouped as:
Anti-settling agent 25-35%；
Defoaming agent 15-20%；
Adhesion promoter 20-25%；
Thixotropic agent 35-55%；
Wherein, thixotropic agent by ethyl cellulose, dibutyl phthalate, acrylic resin, polyvinylbutyrals extremely
A kind of few and castor oil is 1:3-5 composition according to weight ratio.
10. a kind of preparation method of rapid draing low temperature silver paste according to claim 9, it is characterised in that: be added in S3
After thixotropic agent, it is continuously applied to shear force, until all resins dissolve completely in S4.
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| CN201810957218.4A CN109166671B (en) | 2018-08-22 | 2018-08-22 | Preparation method of quick-drying low-temperature silver paste |
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| CN201810957218.4A CN109166671B (en) | 2018-08-22 | 2018-08-22 | Preparation method of quick-drying low-temperature silver paste |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113077924A (en) * | 2021-04-13 | 2021-07-06 | 上海玖银电子科技有限公司 | Quick-drying silver paste for graphene heating film and preparation method thereof |
| CN114283964A (en) * | 2021-12-29 | 2022-04-05 | 苏州创印电子科技有限公司 | Conductive silver paste and preparation method thereof |
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Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5661041A (en) * | 1994-11-24 | 1997-08-26 | Murata Manufacturing Co., Ltd. | Conductive paste, solar cells with grid electrode made of the conductive paste, and fabrication method for silicon solar cells |
| CN101694872A (en) * | 2009-10-21 | 2010-04-14 | 保定风帆新能源有限公司 | Mixing preparation method of pulp of lithium ion battery |
| CN103094662A (en) * | 2013-01-21 | 2013-05-08 | 东莞市智源电子科技有限公司 | Low-temperature solidifying environment-friendly conductive silver paste and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113077924A (en) * | 2021-04-13 | 2021-07-06 | 上海玖银电子科技有限公司 | Quick-drying silver paste for graphene heating film and preparation method thereof |
| CN113077924B (en) * | 2021-04-13 | 2022-09-30 | 上海玖银电子科技有限公司 | Quick-drying silver paste for graphene heating film and preparation method thereof |
| CN114283964A (en) * | 2021-12-29 | 2022-04-05 | 苏州创印电子科技有限公司 | Conductive silver paste and preparation method thereof |
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| CN109166671B (en) | 2021-01-26 |
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