CN103996425A - Nanometer carbon-containing circuit board conductive silver paste and preparation method thereof - Google Patents
Nanometer carbon-containing circuit board conductive silver paste and preparation method thereof Download PDFInfo
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- CN103996425A CN103996425A CN201410167402.0A CN201410167402A CN103996425A CN 103996425 A CN103996425 A CN 103996425A CN 201410167402 A CN201410167402 A CN 201410167402A CN 103996425 A CN103996425 A CN 103996425A
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Abstract
A nanometer carbon-containing circuit board conductive silver paste is made of the following raw materials: by weight, 8-12 parts of indium tin oxide, 4-6 parts of 20-30nm silver powder, 55-60 parts of 10-20micron silver paste, 0.3-0.5 parts of lutein, 5-7 parts of diethylene glycol monoethylether, 4-7 parts of o-xylene, 1-2 parts of grape seed oil, 7-9 parts of glass powder, 1-2 parts of polyethylene glycol, 0.4-0.7 parts of casein, 2-3 parts of ethyl orthosilicate, 6-8 parts of ethanol, 7-9 parts of ethyl acetate, 3-4 parts of nanometer carbon, and 6-9 parts of melamine formaldehyde resin. Nanometer indium tin and nanometer carbon are added to the silver paste of the invention, the conductivity is high, and the use amount of silver powder is saved; by adding lutein and grape seed oil, the silver paste is resistant to oxidation, and silver powder can be prevented from oxidation during processing; and through the use of the glass powder, the melting point is low, the thermal expansion coefficient is small, circuit adhesion is firm, and the conductivity is stable.
Description
Technical field
The invention belongs to electric slurry technical field, relate in particular to a kind of containing nano-sized carbon circuit board conductive silver paste and preparation method thereof.
Background technology
In modern microelectronics industry, people require more and more higher to electronic devices and components, produce and adopt procedures, standardization to carry out reducing costs more, printed circuit board (PCB) (PCB) is exactly that this demand that is applicable to microelectronics industry is born, match with regard to the electric slurry such as conductor paste, electrode slurry, dielectric paste and resistance slurry, grout slurry and the printed circuit board (PCB) (PCB) of the new requirement of demand accordingly, the research of carrying out new conductor paste is also just imperative.
In general, the main component of electric slurry includes function mutually as metal, noble metal powder etc., and inorganic binder is as glass powder, oxide powder etc., organic binder bond, other solvent and additive.Conventionally, function in electric slurry plays electric action mutually, have good electric conductivity, is generally served as by metal dust or noble metal powder, conventional metal dust has copper powder, aluminium powder, zinc powder, nickel powder etc., and conventional precious metal powder has bronze, silver powder, platinum powder, palladium powder etc.Inorganic binder plays fixing electric slurry to base material, generally served as by oxide powder and glass powder, but this composition is lower at the proportion of electric slurry, and what have does not even have; Organic binder bond mainly plays a part to make slurry to have certain shape, is easy to printing or coating, mainly containing macromolecule resin, little molecule resin etc. serves as, along with this part effect in electric slurry of the progress of chemical industry technology is more and more outstanding, especially in the time being applied to silk screen printing, the composition that changes organic binder bond just can change the printing of electric slurry, dry, sintering character.
In existing electric slurry field, it is high that silver is that slurry has conductance, and stable performance, with the feature such as substrate bond strength is large, is widely used in the production of the electronic devices and components such as integrated circuit, multi-chip module, thin film switch.But silver is precious metal, cost is higher, and silver powder major part in existing silver paste is micron-sized powder, and thicknesses of layers, the printing performance etc. of its slurry of making has significant limitation for present high-end precision instrument; On the other hand, printed circuit board (PCB) adopted printing conductive copper slurry to make conducting wire more in the past, but it is easily oxidized to exist conductive copper paste, and in the useful life of having reduced printed circuit board (PCB), conductive copper paste can not be printed as meticulousr circuit.Therefore the size, shape, the kind that need to study metal dust in electrocondution slurry reduce costs, improve conductance to realize, improve the object of printing accuracy.
Binding agent in conductive silver paste has a significant impact for the rate of finished products of circuit printing, the such as volatility of viscosity, caking property, adhesive force, levelability, film forming, solvent etc. all can impact the printing performance of circuit, there is pore, the phenomenon such as open circuit, also there will be sometimes organic substance volatilized after glassy phase not yet start melt, the phenomenon that causes conducting wire to come off from stock, scraps conducting wire, and therefore the performance need of organic binder bond improves.
At present a lot of inorganic binders adopt glass dust, glass dust is made up of the material such as metal oxide, silica, if fusing point is too high, also occur organic substance volatilized after glassy phase not yet start melt, the phenomenon that causes the conducting wire being obtained by conductive silver paste to come off from stock, scraps conducting wire; And in current glass dust, much contain the harmful substances such as plumbous, and unfavorable to environment, therefore need to develop the glass dust that performance is more excellent.
Summary of the invention
The object of the present invention is to provide a kind of nano-sized carbon circuit board conductive silver paste and preparation method thereof that contains, this silver is starched good conductivity, and has saved the consumption of silver powder, and firmly, electric conductivity is stable for circuit bonding.
Technical scheme of the present invention is as follows:
A kind of containing nano-sized carbon circuit board conductive silver paste, it is characterized in that being made by the raw material of following weight portion: tin indium oxide 8-12,20-30nm silver powder 4-6,10-20 μ m silver powder 55-60, lutein 0.3-0.5, diethylene glycol ether 5-7, ortho-xylene 4-7, grape-kernel oil 1-2, glass dust 7-9, polyethylene glycol 1-2, casein 0.4-0.7, tetraethoxysilane 2-3, ethanol 6-8, ethyl acetate 7-9, nano-sized carbon 3-4, melamine resin 6-9;
Described glass dust is made up of the raw material of following weight portion: bismuth telluride 15-17, Si0
216-19, Bi
20
37-9, BaO5-8, Al
20
33-5, B
2o
317-23, V
2o
54-7, Na
2o1-2, nano aluminum nitride powder 1-2; Preparation method is: by bismuth telluride, Si0
2, Bi
20
3, BaO, Al
20
3, B
2o
3, V
2o
5, Na
2o mixes, put into crucible and become liquid 1100-1400 DEG C of heat fused, add again nano aluminum nitride powder, after stirring, carry out vacuum defoamation, vacuum degree is 0.10-0.14MPa, and the deaeration time is 6-9 minute, pour in mould and shape again, carry out again shrend, send in ball mill and pulverize, sieve, obtain 9-13 μ m powder, to obtain final product.
The described preparation method containing nano-sized carbon circuit board conductive silver paste, is characterized in that comprising the following steps:
(1) diethylene glycol ether, ortho-xylene, polyethylene glycol, grape-kernel oil, tetraethoxysilane, ethanol, ethyl acetate are mixed, add melamine resin, be heated to 80-84 DEG C, being stirred to resin all dissolves, add and stir again, with 500 object gauzes filtrations, remove impurity and obtain organic carrier;
(2) glass dust, tin indium oxide, nano-sized carbon are mixed, under 5000-7000 rev/min of stirring, add 20-30nm silver powder, stir 10-20 minute, add again 10-20 μ m silver powder, stir 10-20 minute, then add in organic carrier together with other residual componentss, in ball mill, mix and disperse 30-50 minute, ultrasonic dispersion 6-8 minute, obtains uniform slurry again;
(3) slurry step (2) being obtained carries out vacuum defoamation, and vacuum degree is 0.06-0.09MPa, and the deaeration time is 6-9 minute, then in three-high mill, grind, rolling, to silver-colored slurry viscosity be 10000-20000 centipoise, to obtain final product.
Beneficial effect of the present invention
Silver slurry of the present invention has added nano indium tin and nano-sized carbon, good conductivity, and saved the consumption of silver powder; By adding lutein and grape-kernel oil, can be anti-oxidant, prevent that silver powder is oxidized in process engineering; The glass dust of the application of the invention, fusing point is low, and thermal coefficient of expansion is little, and firmly, electric conductivity is stable for circuit bonding, and this glass dust contains nano aluminum nitride powder, and heat conduction is fast, and fusing is fast, is easy to circuit curing molding.
Embodiment
A kind of containing nano-sized carbon circuit board conductive silver paste, by following weight portion (kilogram) raw material make: tin indium oxide 10,20-30nm silver powder 5,10-20 μ m silver powder 58, lutein 0.4, diethylene glycol ether 6, ortho-xylene 5, grape-kernel oil 1.5, glass dust 8, polyethylene glycol 1.5, casein 0.6, tetraethoxysilane 2.5, ethanol 7, ethyl acetate 8, nano-sized carbon 3.5, melamine resin 7;
Described glass dust by following weight portion (kilogram) raw material make: bismuth telluride 16, Si0
217, Bi
20
38, BaO7, Al
20
34, B
2o
320, V
2o
56, Na
2o1.5, nano aluminum nitride powder 1.5; Preparation method is: by bismuth telluride, Si0
2, Bi
20
3, BaO, Al
20
3, B
2o
3, V
2o
5, Na
2o mixes, put into crucible and become liquid 1300 DEG C of heat fused, add again nano aluminum nitride powder, after stirring, carry out vacuum defoamation, vacuum degree is 0.13MPa, and the deaeration time is 7 minutes, pour in mould and shape again, carry out again shrend, send in ball mill and pulverize, sieve, obtain 11 μ m powder, to obtain final product.
The described preparation method containing nano-sized carbon circuit board conductive silver paste, comprises the following steps:
(1) diethylene glycol ether, ortho-xylene, polyethylene glycol, grape-kernel oil, tetraethoxysilane, ethanol, ethyl acetate are mixed, add melamine resin, be heated to 82 DEG C, being stirred to resin all dissolves, add and stir again, with 500 object gauzes filtrations, remove impurity and obtain organic carrier;
(2) glass dust, tin indium oxide, nano-sized carbon are mixed, under 6000 revs/min of stirrings, add 20-30nm silver powder, stir 15 minutes, add again 10-20 μ m silver powder, stir 15 minutes, then add in organic carrier together with other residual componentss, in ball mill, mix and disperse 40 minutes, ultrasonic dispersion 7 minutes, obtains uniform slurry again;
(3) slurry step (2) being obtained carries out vacuum defoamation, and vacuum degree is 0.08MPa, and the deaeration time is 7 minutes, then in three-high mill, grind, rolling, to silver-colored slurry viscosity be 15000 centipoises, to obtain final product.
Test data:
The silver slurry mode of silk screen printing that the present embodiment is obtained is printed onto on PCB circuit board, is then warming up at 630 DEG C and solidifies and form conducting wire in 6 minutes, thereby obtain conducting wire plate.The wiring width that records conducting wire is 0.7mm, average film thickness 5 μ m, and wire distribution distance is 0.8mm, resistivity is 3.7 × 10
-5Ω m.
Producing in the manner described above 1000 of conducting wire plates in batches, is combined well with PCB circuit board in conducting wire, and svelteness continuously, has the conducting wire of 1 circuit board to come off from stock, rate of finished products 99.9%.
Claims (2)
1. containing a nano-sized carbon circuit board conductive silver paste, it is characterized in that being made by the raw material of following weight portion: tin indium oxide 8-12,20-30nm silver powder 4-6,10-20 μ m silver powder 55-60, lutein 0.3-0.5, diethylene glycol ether 5-7, ortho-xylene 4-7, grape-kernel oil 1-2, glass dust 7-9, polyethylene glycol 1-2, casein 0.4-0.7, tetraethoxysilane 2-3, ethanol 6-8, ethyl acetate 7-9, nano-sized carbon 3-4, melamine resin 6-9;
Described glass dust is made up of the raw material of following weight portion: bismuth telluride 15-17, Si0
216-19, Bi
20
37-9, BaO5-8, Al
20
33-5, B
2o
317-23, V
2o
54-7, Na
2o1-2, nano aluminum nitride powder 1-2; Preparation method is: by bismuth telluride, Si0
2, Bi
20
3, BaO, Al
20
3, B
2o
3, V
2o
5, Na
2o mixes, put into crucible and become liquid 1100-1400 DEG C of heat fused, add again nano aluminum nitride powder, after stirring, carry out vacuum defoamation, vacuum degree is 0.10-0.14MPa, and the deaeration time is 6-9 minute, pour in mould and shape again, carry out again shrend, send in ball mill and pulverize, sieve, obtain 9-13 μ m powder, to obtain final product.
2. the preparation method containing nano-sized carbon circuit board conductive silver paste according to claim 1, is characterized in that comprising the following steps:
(1) diethylene glycol ether, ortho-xylene, polyethylene glycol, grape-kernel oil, tetraethoxysilane, ethanol, ethyl acetate are mixed, add melamine resin, be heated to 80-84 DEG C, being stirred to resin all dissolves, add and stir again, with 500 object gauzes filtrations, remove impurity and obtain organic carrier;
(2) glass dust, tin indium oxide, nano-sized carbon are mixed, under 5000-7000 rev/min of stirring, add 20-30nm silver powder, stir 10-20 minute, add again 10-20 μ m silver powder, stir 10-20 minute, then add in organic carrier together with other residual componentss, in ball mill, mix and disperse 30-50 minute, ultrasonic dispersion 6-8 minute, obtains uniform slurry again;
(3) slurry step (2) being obtained carries out vacuum defoamation, and vacuum degree is 0.06-0.09MPa, and the deaeration time is 6-9 minute, then in three-high mill, grind, rolling, to silver-colored slurry viscosity be 10000-20000 centipoise, to obtain final product.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410167402.0A CN103996425A (en) | 2014-04-24 | 2014-04-24 | Nanometer carbon-containing circuit board conductive silver paste and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410167402.0A CN103996425A (en) | 2014-04-24 | 2014-04-24 | Nanometer carbon-containing circuit board conductive silver paste and preparation method thereof |
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|---|---|
| CN103996425A true CN103996425A (en) | 2014-08-20 |
Family
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104392765A (en) * | 2014-10-17 | 2015-03-04 | 阜阳市节源照明电器有限责任公司 | Silicon-nitride-contained oxidation-resistant conductive silver paste and manufacturing method thereof |
| CN106653141A (en) * | 2016-11-18 | 2017-05-10 | 珠海特普力高精细化工有限公司 | Making method and application method of water-soluble conductive nano silver carbon paste |
| CN107880786A (en) * | 2017-11-30 | 2018-04-06 | 上海穗杉实业股份有限公司 | A kind of inorganic sealant and preparation method thereof and application method |
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| KR20080013787A (en) * | 2006-08-07 | 2008-02-13 | 주식회사 잉크테크 | Process for preparing silver nanoparticles or silver nanocolloid, and the compositions of silver ink containing the silver nanoparticles |
| CN101284928A (en) * | 2007-04-10 | 2008-10-15 | 国家淀粉及化学投资控股公司 | Electrically conductive UV-curable ink |
| CN101475781A (en) * | 2009-01-08 | 2009-07-08 | 华东师范大学 | Silver colloid material with high heat transfer efficiency and preparation thereof |
| CN103258584A (en) * | 2013-01-09 | 2013-08-21 | 深圳市创智材料科技有限公司 | Electric conductive silver paste and manufacturing method thereof |
| CN103500596A (en) * | 2013-09-30 | 2014-01-08 | 广州市尤特新材料有限公司 | Silver paste used for grapheme touch screen, and preparation method thereof |
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2014
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20080013787A (en) * | 2006-08-07 | 2008-02-13 | 주식회사 잉크테크 | Process for preparing silver nanoparticles or silver nanocolloid, and the compositions of silver ink containing the silver nanoparticles |
| CN101284928A (en) * | 2007-04-10 | 2008-10-15 | 国家淀粉及化学投资控股公司 | Electrically conductive UV-curable ink |
| CN101475781A (en) * | 2009-01-08 | 2009-07-08 | 华东师范大学 | Silver colloid material with high heat transfer efficiency and preparation thereof |
| CN103258584A (en) * | 2013-01-09 | 2013-08-21 | 深圳市创智材料科技有限公司 | Electric conductive silver paste and manufacturing method thereof |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104392765A (en) * | 2014-10-17 | 2015-03-04 | 阜阳市节源照明电器有限责任公司 | Silicon-nitride-contained oxidation-resistant conductive silver paste and manufacturing method thereof |
| CN106653141A (en) * | 2016-11-18 | 2017-05-10 | 珠海特普力高精细化工有限公司 | Making method and application method of water-soluble conductive nano silver carbon paste |
| CN106653141B (en) * | 2016-11-18 | 2018-06-29 | 珠海特普力高精细化工有限公司 | A kind of manufacture of water-soluble conducting nanometer silver carbon slurry and its application process |
| CN107880786A (en) * | 2017-11-30 | 2018-04-06 | 上海穗杉实业股份有限公司 | A kind of inorganic sealant and preparation method thereof and application method |
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| PB01 | Publication | ||
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Application publication date: 20140820 |