CN103996429A - Low-temperature conductive printed circuit board silver slurry and preparation method thereof - Google Patents

Low-temperature conductive printed circuit board silver slurry and preparation method thereof Download PDF

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Publication number
CN103996429A
CN103996429A CN201410152266.8A CN201410152266A CN103996429A CN 103996429 A CN103996429 A CN 103996429A CN 201410152266 A CN201410152266 A CN 201410152266A CN 103996429 A CN103996429 A CN 103996429A
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China
Prior art keywords
parts
slurry
powder
silver powder
silver
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Pending
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CN201410152266.8A
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Chinese (zh)
Inventor
胡萍
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Chizhou City Electronic Science And Technology Co Ltd Of Asus
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Chizhou City Electronic Science And Technology Co Ltd Of Asus
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Priority to CN201410152266.8A priority Critical patent/CN103996429A/en
Publication of CN103996429A publication Critical patent/CN103996429A/en
Pending legal-status Critical Current

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Abstract

Disclosed is a low-temperature conductive printed circuit board silver slurry. The slurry is prepared by use of the following raw materials in parts by weight: 6-9 parts of indium tin oxide, 4-6 parts of 1-10 nm sheet-like silver powder, 4-6 parts of 40-50 nm spherical silver powder, 50-60 parts of 1-10 [mu]m sheet-like silver powder, 5-7 parts of an E-12 epoxy resin, 1-2 parts of a silicone resin, 12-15 parts of xylene, 7-10 parts of n-butanol, 1-2 parts of a polyurethane resin, 0.4-0.8 parts of isophorone diamine, 1-2 parts of dipentene, 2-4 parts of lignine, 0.4-0.8 parts of ethylene bis oleamide, and 11-14 parts of glass powder. According to the invention, the indium tin oxide is added to the slurry, less silver powder is consumed, the conductivity is good under the condition of a low temperature, and excellent conducting effect is achieved through matching of the silver powder in different particle sizes and different shapes; and the glass powder is low in melting point and small in heat expansion ratio, such that the circuit printing yield is high, and the conducting performance is good.

Description

A kind of low-temperature conductive printed circuit board (PCB) silver slurry and preparation method thereof
Technical field
The invention belongs to electric slurry technical field, relate in particular to a kind of low-temperature conductive printed circuit board (PCB) silver slurry 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 low-temperature conductive printed circuit board (PCB) silver slurry and preparation method thereof, this silver slurry has been saved the consumption of silver powder, and under low temperature condition, electric conductivity is good.
Technical scheme of the present invention is as follows:
A low-temperature conductive printed circuit board (PCB) silver slurry, is characterized in that being made up of the raw material of following weight portion: tin indium oxide 6-9, the spherical silver powder 4-6 of 1-10nm flake silver powder 4-6,40-50nm, 1-10 μ m flake silver powder 50-60, E-12 epoxy resin 5-7, silicones 1-2, dimethylbenzene 12-15, n-butanol 7-10, polyurethane resin 1-2, IPD 0.4-0.8, dipentene 1-2, lignin 2-4, ethylene two oleamide 0.4-0.8, glass dust 11-14;
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 preparation method of described low-temperature conductive printed circuit board (PCB) silver slurry, is characterized in that comprising the following steps:
(1) dimethylbenzene, n-butanol, dipentene are mixed, add E-12 epoxy resin, silicones, lignin, be heated to 78-85 DEG C, being stirred to resin all dissolves, add again polyurethane resin to stir, with 500 object gauzes filtrations, remove impurity and obtain organic carrier;
(2) glass dust, tin indium oxide, the two oleamides of ethylene are mixed, under 8000-10000 rev/min of stirring, add 1-10nm flake silver powder, the spherical silver powder of 40-50nm, stir 10-20 minute, add again 1-10 μ m flake 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 8-10 minute, then in three-high mill, grind, rolling, to silver-colored slurry viscosity be 10000-18000 centipoise, to obtain final product.
Beneficial effect of the present invention
Silver slurry of the present invention has added tin indium oxide, saved the consumption of silver powder, and electric conductivity is good under low temperature condition, by collocation different-grain diameter, difform silver powder, has reached excellent conductive effect; Glass dust of the present invention, fusing point is low, and coefficient of thermal expansion is little, makes circuit printing rate of finished products high, conduct electricity very well, 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 low-temperature conductive printed circuit board (PCB) silver slurry, by following weight portion (kilogram) raw material make: tin indium oxide 7,1-10nm flake silver powder 5, the spherical silver powder 5 of 40-50nm, 1-10 μ m flake silver powder 55, E-12 epoxy resin 6, silicones 1.6, dimethylbenzene 14, n-butanol 8, polyurethane resin 1.5, IPD 0.6, dipentene 1.5, lignin 3, the two oleamides 0.6 of ethylene, glass dust 13;
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 preparation method of described low-temperature conductive printed circuit board (PCB) silver slurry, comprises the following steps:
(1) dimethylbenzene, n-butanol, dipentene are mixed, add E-12 epoxy resin, silicones, lignin, be heated to 82 DEG C, being stirred to resin all dissolves, add again polyurethane resin to stir, with 500 object gauzes filtrations, remove impurity and obtain organic carrier;
(2) glass dust, tin indium oxide, the two oleamides of ethylene are mixed, under 9000 revs/min of stirrings, add 1-10nm flake silver powder, the spherical silver powder of 40-50nm, stir 15 minutes, add again 1-10 μ m flake 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 0.07MPa, and the deaeration time is 9 minutes, then in three-high mill, grind, rolling, to silver-colored slurry viscosity be 13000 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 0.5mm, average film thickness 5 μ m, and wire distribution distance is 0.5mm, resistivity is 4.7 × 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. a low-temperature conductive printed circuit board (PCB) silver slurry, is characterized in that being made up of the raw material of following weight portion: tin indium oxide 6-9, the spherical silver powder 4-6 of 1-10nm flake silver powder 4-6,40-50nm, 1-10 μ m flake silver powder 50-60, E-12 epoxy resin 5-7, silicones 1-2, dimethylbenzene 12-15, n-butanol 7-10, polyurethane resin 1-2, IPD 0.4-0.8, dipentene 1-2, lignin 2-4, ethylene two oleamide 0.4-0.8, glass dust 11-14;
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 of low-temperature conductive printed circuit board (PCB) silver slurry according to claim 1, is characterized in that comprising the following steps:
(1) dimethylbenzene, n-butanol, dipentene are mixed, add E-12 epoxy resin, silicones, lignin, be heated to 78-85 DEG C, being stirred to resin all dissolves, add again polyurethane resin to stir, with 500 object gauzes filtrations, remove impurity and obtain organic carrier;
(2) glass dust, tin indium oxide, the two oleamides of ethylene are mixed, under 8000-10000 rev/min of stirring, add 1-10nm flake silver powder, the spherical silver powder of 40-50nm, stir 10-20 minute, add again 1-10 μ m flake 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 8-10 minute, then in three-high mill, grind, rolling, to silver-colored slurry viscosity be 10000-18000 centipoise, to obtain final product.
CN201410152266.8A 2014-04-16 2014-04-16 Low-temperature conductive printed circuit board silver slurry and preparation method thereof Pending CN103996429A (en)

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Application Number Priority Date Filing Date Title
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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105788700A (en) * 2014-12-18 2016-07-20 上海宝银电子材料有限公司 Quick-dry type silver paste used for PCB through hole and preparation method for quick-dry type silver paste
CN109754903A (en) * 2018-12-13 2019-05-14 东莞市银屏电子科技有限公司 A kind of solar energy HIT battery main grid low-temperature conductive silver paste and preparation method thereof

Citations (4)

* Cited by examiner, † Cited by third party
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
CN102653453A (en) * 2011-03-01 2012-09-05 同和电子科技有限公司 Silver-coated glass powder for conduction and manufacture method thereof and conductive paste
TW201303893A (en) * 2011-07-06 2013-01-16 Taiwan Mao Cheng Electronic Material Co Ltd Conductive slurry
CN103021512A (en) * 2011-09-21 2013-04-03 三星电机株式会社 Conductive paste composition for low temperature firing

Patent Citations (4)

* Cited by examiner, † Cited by third party
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
CN102653453A (en) * 2011-03-01 2012-09-05 同和电子科技有限公司 Silver-coated glass powder for conduction and manufacture method thereof and conductive paste
TW201303893A (en) * 2011-07-06 2013-01-16 Taiwan Mao Cheng Electronic Material Co Ltd Conductive slurry
CN103021512A (en) * 2011-09-21 2013-04-03 三星电机株式会社 Conductive paste composition for low temperature firing

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105788700A (en) * 2014-12-18 2016-07-20 上海宝银电子材料有限公司 Quick-dry type silver paste used for PCB through hole and preparation method for quick-dry type silver paste
CN105788700B (en) * 2014-12-18 2017-08-11 上海宝银电子材料有限公司 It is a kind of for quick-dry type silver paste of PCB perforations and preparation method thereof
CN109754903A (en) * 2018-12-13 2019-05-14 东莞市银屏电子科技有限公司 A kind of solar energy HIT battery main grid low-temperature conductive silver paste and preparation method thereof

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Application publication date: 20140820