CN104008790A - Electricity-conducting silver paste for printed circuit board and preparing method thereof - Google Patents
Electricity-conducting silver paste for printed circuit board and preparing method thereof Download PDFInfo
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- CN104008790A CN104008790A CN201410170300.4A CN201410170300A CN104008790A CN 104008790 A CN104008790 A CN 104008790A CN 201410170300 A CN201410170300 A CN 201410170300A CN 104008790 A CN104008790 A CN 104008790A
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Abstract
The invention provides an electricity-conducting silver paste for a printed circuit board. The electricity-conducting silver paste comprises, by weight, 10-20 parts of silver powder of 1-10nm, 10-20 parts of silver powder of 40-50nm, 30-40 parts of silver powder of 20-30Mum, 5-10 parts of nanoscale flaky silver powder, 1-2 parts of zinc stearate, 5-8 parts of chloroethylene vinyl acetate, 3-4 parts of bismuth oxide, 6-7 parts of DBE, 2-3 parts of isophorone, 3-5 parts of furfural resin, 3-5 parts of E-12 epoxy resin, 2-3 parts of propylene glycol, 2-3 parts of dipropylene glycol butyl ether, 2-3 parts of petroleum ether, 1-2 parts of turpentine and 10-13 parts of glass powder. According to the silver paste, by matching the silver powder of different grain diameters and shapes, the silver powder is combined closely, and therefore the conductivity is excellent; the glass powder is added, so that electricity-conducting silver paste is free of lead and environmentally friendly; the melting point is low, and solidifying and forming are easy to carry out; the viscosity of the silver paste is moderate, the printing property is good, the printing precision is high, the circuit is safe and reliable, and the silver paste can not be broken easily.
Description
Technical field
The invention belongs to electric slurry technical field, relate in particular to a kind of printed circuit board (PCB) 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 printed circuit board (PCB) conductive silver paste and preparation method thereof, this silver slurry electric conductivity excellence, modest viscosity, printing is good, and printing precision is high, and circuit safety is firm, not easy fracture.
Technical scheme of the present invention is as follows:
A kind of printed circuit board (PCB) conductive silver paste, is characterized in that being made up of the raw material of following weight portion: 1-10nm silver powder 10-20,40-50nm silver powder 10-20,20-30 μ m silver powder 30-40, nano-grade silver powder 5-10, zinc stearate 1-2, vinyl chloride vinyl acetate 5-8, bismuth oxide 3-4, DBE 6-7, isophorone 2-3, chaff carbamide resin 3-5, E-12 epoxy resin 3-5, propylene glycol 2-3, DPG n-butyl ether 2-3, benzinum 2-3, turpentine oil 1-2, glass dust 10-13;
Described glass dust is made up of the raw material of following weight portion: SiO2 10-13, V2O5 15-18, Sb2O3 5-7, gas phase alundum (Al2O3) 2-4, activated alumina 15-18, P2O5 4-6, anoxic cerium oxide 3-6, MgO2-3, four acicular type zinc oxide crystal whisker 2-4; Preparation method is: SiO2, V2O5, Sb2O3, gas phase alundum (Al2O3), activated alumina, P2O5, anoxic cerium oxide, MgO are mixed, put into crucible and become liquid 1100-1400 DEG C of heat fused, add again four acicular type zinc oxide crystal whisker, 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 7-10 μ m powder, to obtain final product.
The preparation method of described printed circuit board (PCB) conductive silver paste, is characterized in that comprising the following steps:
(1) DBE, isophorone, propylene glycol, DPG n-butyl ether, benzinum, turpentine oil are mixed, add vinyl chloride vinyl acetate, chaff carbamide resin, be heated to 80-82 DEG C, being stirred to resin all dissolves, add again E-12 epoxy resin to stir, with 500 object gauzes filtrations, remove impurity and obtain organic carrier;
(2) bismuth oxide, glass dust, zinc stearate are mixed, under 5000-7000 rev/min of stirring, add 1-10nm silver powder, 40-50nm silver powder, stir 10-20 minute, add again 20-30 μ m silver powder, nano-grade 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 10000-15000 centipoise, to obtain final product.
Beneficial effect of the present invention
Silver-colored slurry of the present invention is by collocation different-grain diameter, difform silver powder, and silver powder combination is tight, electric conductivity excellence, and by adding glass dust of the present invention, leadless environment-friendly, fusing point is low, easily curing molding; This silver slurry viscosity is moderate, and printing is good, and printing precision is high, and circuit safety is firm, not easy fracture.
Embodiment
A kind of printed circuit board (PCB) conductive silver paste, by following weight portion (kilogram) raw material make: 1-10nm silver powder 15,40-50nm silver powder 15,20-30 μ m silver powder 35, nano-grade silver powder 8, zinc stearate 1.5, vinyl chloride vinyl acetate 7, bismuth oxide 3.5, DBE 6.6, isophorone 2.5, chaff carbamide resin 4, E-12 epoxy resin 4, propylene glycol 2.5, DPG n-butyl ether 2.5, benzinum 2.5, turpentine oil 1.5, glass dust 12;
Described glass dust by following weight portion (kilogram) raw material make: SiO2 11, V2O5 17, Sb2O3 6, gas phase alundum (Al2O3) 3, activated alumina 17, P2O5 5, anoxic cerium oxide 4, MgO2.5, four acicular type zinc oxide crystal whisker 3; Preparation method is: SiO2, V2O5, Sb2O3, gas phase alundum (Al2O3), activated alumina, P2O5, anoxic cerium oxide, MgO are mixed, put into crucible, become liquid 1300 DEG C of heat fused, then add four acicular type zinc oxide crystal whisker, after stirring, carry out vacuum defoamation, vacuum degree is 0.12MPa, the deaeration time is 7 minutes, then pours in mould and shape, then carries out shrend, sends in ball mill and to pulverize, to sieve, obtain 9 μ m powder, to obtain final product.
The preparation method of described printed circuit board (PCB) conductive silver paste, is characterized in that comprising the following steps:
(1) DBE, isophorone, propylene glycol, DPG n-butyl ether, benzinum, turpentine oil are mixed, add vinyl chloride vinyl acetate, chaff carbamide resin, be heated to 81 DEG C, being stirred to resin all dissolves, add again E-12 epoxy resin to stir, with 500 object gauzes filtrations, remove impurity and obtain organic carrier;
(2) bismuth oxide, glass dust, zinc stearate are mixed, under 6000 revs/min of stirrings, add 1-10nm silver powder, 40-50nm silver powder, stir 16 minutes, add again 20-30 μ m silver powder, nano-grade silver powder, stir 16 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 0.09MPa, and the deaeration time is 7 minutes, then in three-high mill, grind, rolling, to silver-colored slurry viscosity be 12000 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 640 DEG C and solidifies and form conducting wire in 6 minutes, thereby obtain conducting wire plate.The wiring width that records conducting wire is 0.9mm, average film thickness 5 μ m, and wire distribution distance is 0.9mm, resistivity is 4.9 × 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. a printed circuit board (PCB) conductive silver paste, is characterized in that being made up of the raw material of following weight portion: 1-10nm silver powder 10-20,40-50nm silver powder 10-20,20-30 μ m silver powder 30-40, nano-grade silver powder 5-10, zinc stearate 1-2, vinyl chloride vinyl acetate 5-8, bismuth oxide 3-4, DBE 6-7, isophorone 2-3, chaff carbamide resin 3-5, E-12 epoxy resin 3-5, propylene glycol 2-3, DPG n-butyl ether 2-3, benzinum 2-3, turpentine oil 1-2, glass dust 10-13;
Described glass dust is made up of the raw material of following weight portion: SiO2 10-13, V2O5 15-18, Sb2O3 5-7, gas phase alundum (Al2O3) 2-4, activated alumina 15-18, P2O5 4-6, anoxic cerium oxide 3-6, MgO2-3, four acicular type zinc oxide crystal whisker 2-4; Preparation method is: SiO2, V2O5, Sb2O3, gas phase alundum (Al2O3), activated alumina, P2O5, anoxic cerium oxide, MgO are mixed, put into crucible and become liquid 1100-1400 DEG C of heat fused, add again four acicular type zinc oxide crystal whisker, 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 7-10 μ m powder, to obtain final product.
2. the preparation method of printed circuit board (PCB) conductive silver paste according to claim 1, is characterized in that comprising the following steps:
(1) DBE, isophorone, propylene glycol, DPG n-butyl ether, benzinum, turpentine oil are mixed, add vinyl chloride vinyl acetate, chaff carbamide resin, be heated to 80-82 DEG C, being stirred to resin all dissolves, add again E-12 epoxy resin to stir, with 500 object gauzes filtrations, remove impurity and obtain organic carrier;
(2) bismuth oxide, glass dust, zinc stearate are mixed, under 5000-7000 rev/min of stirring, add 1-10nm silver powder, 40-50nm silver powder, stir 10-20 minute, add again 20-30 μ m silver powder, nano-grade 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 10000-15000 centipoise, to obtain final product.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201410170300.4A CN104008790A (en) | 2014-04-25 | 2014-04-25 | Electricity-conducting silver paste for printed circuit board and preparing method thereof |
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| CN201410170300.4A CN104008790A (en) | 2014-04-25 | 2014-04-25 | Electricity-conducting silver paste for printed circuit board and preparing method thereof |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104934100A (en) * | 2015-05-25 | 2015-09-23 | 铜陵宏正网络科技有限公司 | Easy-to-sinter PCB silver paste and preparation method thereof |
| CN104955267A (en) * | 2015-05-25 | 2015-09-30 | 铜陵宏正网络科技有限公司 | PCB (printed circuit board) silver paste containing silver coated nickel powder and preparation method of PCB silver paste |
| CN111372434A (en) * | 2020-03-09 | 2020-07-03 | 广东四维新材料有限公司 | Preparation method of 5G ceramic filter electrosilvering-simulated electromagnetic wave shield |
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| EP2363864A1 (en) * | 2010-02-12 | 2011-09-07 | Giga Solar Materials Corporation | Conductive aluminum paste and the fabrication method thereof, the solar cell and the module thereof |
| CN102262918A (en) * | 2011-07-19 | 2011-11-30 | 彩虹集团公司 | Grout silver paste used in PCB and preparation method thereof |
| CN102324263A (en) * | 2011-07-04 | 2012-01-18 | 江苏瑞德新能源科技有限公司 | Silver paste for solar cells and preparation method thereof |
| CN102831951A (en) * | 2012-08-24 | 2012-12-19 | 合肥中南光电有限公司 | Silver paste for environmental-friendly lead-free silicon solar cell electrode and preparation method of silver paste |
| TW201303893A (en) * | 2011-07-06 | 2013-01-16 | Taiwan Mao Cheng Electronic Material Co Ltd | Conductive slurry |
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2014
- 2014-04-25 CN CN201410170300.4A patent/CN104008790A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP2363864A1 (en) * | 2010-02-12 | 2011-09-07 | Giga Solar Materials Corporation | Conductive aluminum paste and the fabrication method thereof, the solar cell and the module thereof |
| CN102324263A (en) * | 2011-07-04 | 2012-01-18 | 江苏瑞德新能源科技有限公司 | Silver paste for solar cells and preparation method thereof |
| TW201303893A (en) * | 2011-07-06 | 2013-01-16 | Taiwan Mao Cheng Electronic Material Co Ltd | Conductive slurry |
| CN102262918A (en) * | 2011-07-19 | 2011-11-30 | 彩虹集团公司 | Grout silver paste used in PCB and preparation method thereof |
| CN102831951A (en) * | 2012-08-24 | 2012-12-19 | 合肥中南光电有限公司 | Silver paste for environmental-friendly lead-free silicon solar cell electrode and preparation method of silver paste |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104934100A (en) * | 2015-05-25 | 2015-09-23 | 铜陵宏正网络科技有限公司 | Easy-to-sinter PCB silver paste and preparation method thereof |
| CN104955267A (en) * | 2015-05-25 | 2015-09-30 | 铜陵宏正网络科技有限公司 | PCB (printed circuit board) silver paste containing silver coated nickel powder and preparation method of PCB silver paste |
| CN111372434A (en) * | 2020-03-09 | 2020-07-03 | 广东四维新材料有限公司 | Preparation method of 5G ceramic filter electrosilvering-simulated electromagnetic wave shield |
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Application publication date: 20140827 |
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