CN104143376A - Conductive silver paste containing nickel powder of PCB and preparation method thereof - Google Patents

Abstract

Conductive silver paste containing nickel powder of a PCB is prepared by the following raw materials, by weight: 3-5 parts of 10nm-20nm nickel powder, 3-5 parts of 30nm-60nm cobalt powder, 1-2 parts of tartaric acid, 50-60 parts of micro-sized silver powder, 1-2 parts of Carbomer resin, 0.4-0.8 parts of sodium lauroyl sarcosine, 0.8-1.2 parts of citric acid, 10-13 parts of glass powder, 1-2 parts of Arabic gum, 7-9 parts of hyperbranched polyester, 9-13 parts of acetic acid n-butyl ester, 1-2 parts of 2-ethyl-4-methyl imidazole, 3-5 parts of isophorone and 2-4 parts of cyclohexanone. The micro-sized nickel powder and the cobalt powder are added into the silver paste, holes are filled with the micro-sized nickel powder, the cobalt powder and the micro-sized silver powder alternatively, and therefore, conductivity is strengthened. The glass powder has a low fusing point, conductivity is not affected, and firm bonding and friction resistance are achieved.

Description

A kind of nickeliferous micro mist PCB circuit board conductive silver paste and preparation method thereof

Technical field

The invention belongs to electric slurry technical field, relate in particular to a kind of nickeliferous micro mist PCB 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 nickeliferous micro mist PCB circuit board conductive silver paste and preparation method thereof, this silver slurry good conductivity, bonding is firm, rub resistance.

Technical scheme of the present invention is as follows:

A kind of nickeliferous micro mist PCB circuit board conductive silver paste, is characterized in that being made up of the raw material of following weight portion: 10-20nm nickel powder 3-5,30-60nm cobalt powder 3-5, tartaric acid 1-2, micron order silver powder 50-60, carbomer 1-2, sodium lauroyl sarcosine 0.4-0.8, citric acid 0.8-1.2, glass dust 10-13, gum arabic 1-2, Hyperbranched Polyester Resin 7-9, n-butyl acetate 9-13,2-ethyl-4-methylimidazole 1-2, isophorone 3-5, cyclohexanone 2-4;

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 nickeliferous micro mist PCB circuit board conductive silver paste, is characterized in that comprising the following steps:

(1) n-butyl acetate, isophorone, cyclohexanone are mixed, add carbomer, gum arabic, Hyperbranched Polyester Resin, be heated to 80-84 DEG C, be stirred to resin and all dissolve, with 500 object gauzes filtrations, remove impurity and obtain organic carrier;

(2) glass dust, tartaric acid, citric acid, sodium lauroyl sarcosine are mixed, under 5000-7000 rev/min of stirring, add 10-20nm nickel powder, 30-60nm cobalt powder, stir 10-20 minute, add again micron order 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 0.08-0.11MPa, 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 nanoscale nickel powder and cobalt powder, interts and makes up hole mutually with micron order silver powder, has strengthened conductivity; The glass dust of the application of the invention, fusing point is low, does not affect conductivity, and bonding is firm, rub resistance.

Embodiment

A kind of nickeliferous micro mist PCB circuit board conductive silver paste, by following weight portion (kilogram) raw material make: 10-20nm nickel powder 4,30-60nm cobalt powder 4, tartaric acid 1.5, micron order silver powder 55, carbomer 1.5, sodium lauroyl sarcosine 0.6, citric acid 1.0, glass dust 12, gum arabic 1.5, Hyperbranched Polyester Resin 8, n-butyl acetate 11,2-ethyl-4-methylimidazole 1.5, isophorone 4, cyclohexanone 3;

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 nickeliferous micro mist PCB circuit board conductive silver paste, comprises the following steps:

(1) n-butyl acetate, isophorone, cyclohexanone are mixed, add carbomer, gum arabic, Hyperbranched Polyester Resin, be heated to 82 DEG C, be stirred to resin and all dissolve, with 500 object gauzes filtrations, remove impurity and obtain organic carrier;

(2) glass dust, tartaric acid, citric acid, sodium lauroyl sarcosine are mixed, under 6000 revs/min of stirrings, add 10-20nm nickel powder, 30-60nm cobalt powder, stir 15 minutes, add again micron order 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 0.11MPa, and the deaeration time is 8 minutes, then in three-high mill, grind, rolling, to silver-colored slurry viscosity be 14000 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 0.7mm, average film thickness 5 μ m, and wire distribution distance is 0.7mm, resistivity is 4.8 × 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 5 circuit boards to come off from stock, rate of finished products 99.5%.

Claims (2)

1. a nickeliferous micro mist PCB circuit board conductive silver paste, is characterized in that being made up of the raw material of following weight portion: 10-20nm nickel powder 3-5,30-60nm cobalt powder 3-5, tartaric acid 1-2, micron order silver powder 50-60, carbomer 1-2, sodium lauroyl sarcosine 0.4-0.8, citric acid 0.8-1.2, glass dust 10-13, gum arabic 1-2, Hyperbranched Polyester Resin 7-9, n-butyl acetate 9-13,2-ethyl-4-methylimidazole 1-2, isophorone 3-5, cyclohexanone 2-4;

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 nickeliferous micro mist PCB circuit board conductive silver paste according to claim 1, is characterized in that comprising the following steps:

(1) n-butyl acetate, isophorone, cyclohexanone are mixed, add carbomer, gum arabic, Hyperbranched Polyester Resin, be heated to 80-84 DEG C, be stirred to resin and all dissolve, with 500 object gauzes filtrations, remove impurity and obtain organic carrier;

(2) glass dust, tartaric acid, citric acid, sodium lauroyl sarcosine are mixed, under 5000-7000 rev/min of stirring, add 10-20nm nickel powder, 30-60nm cobalt powder, stir 10-20 minute, add again micron order 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 0.08-0.11MPa, 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.