CN104078098B - A kind of low silver content printed circuit board (PCB) silver slurry and preparation method thereof - Google Patents
A kind of low silver content printed circuit board (PCB) silver slurry and preparation method thereof Download PDFInfo
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- CN104078098B CN104078098B CN201410243998.8A CN201410243998A CN104078098B CN 104078098 B CN104078098 B CN 104078098B CN 201410243998 A CN201410243998 A CN 201410243998A CN 104078098 B CN104078098 B CN 104078098B
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Abstract
A kind of low silver content printed circuit board (PCB) silver slurry, is prepared by the raw materials in: glucose 12, nano-grade copper powder 20 30,1 20 μm flake silver powder 30 40, glass dust 13 16, Hyperbranched Polyester Resin 57, terpineol 58, Thiodiglycol 25, bisphenol A epoxide resin 24, butyl carbitol 68, ethyl acetate 79, nano titanium oxide 12, nanocrystal cellulose 12, nanometer tantalum carbide powder 35, nano silicon carbide niobium powder 35；The silver slurry of the present invention with the addition of nano-grade copper powder, nanometer tantalum carbide powder, nano silicon carbide niobium powder, not only maintains good electric conductivity, and has saved argentum powder consumption；Glass dust leadless environment-friendly of the present invention, caking property is good, and circuit is firm；Organic carrier solvent of the present invention volatilizees successively, more high temperature resistant, and printing is good so that circuit yield is high.
Description
Technical field
The invention belongs to electric slurry technical field, particularly relate to a kind of low silver content printed circuit board (PCB) silver slurry and preparation method thereof.
Background technology
In modern microelectronic industry, electronic devices and components are required more and more higher by people, produce uses procedure, standardization to carry out reducing cost more, printed circuit board (PCB) (PCB) is exactly to be suitable for this demand of microelectronics industry and be born, matching with printed circuit board (PCB) (PCB) with regard to the electric slurry such as the new conductor paste of requirement of demand, electrode slurry, dielectric paste and resistance slurry, grout slurry accordingly, the research carrying out new conductor paste is also the most imperative.
In general, the main component of electric slurry includes function mutually such as metal, noble metal powder etc., inorganic binder such as glass powder, oxide powder etc., organic binder bond, other solvent and additive.Generally, function in electric slurry plays electric action mutually, will have good electric conductivity, typically be served as by metal dust or noble metal powder, conventional metal dust has copper powder, aluminium powder, zinc powder, nikel powder etc., and conventional precious metal powder has bronze, argentum powder, platinum powder, palladium powder etc..Inorganic binder plays the effect to base material of the fixing electric slurry, is typically served as by oxide powder and glass powder, but this composition is relatively low at the proportion ratio of electric slurry, have even without；Organic binder bond acts primarily as and makes slurry have certain shape, be prone to printing or the effect of coating, macromolecule resin, little molecule resin etc. is mainly had to serve as, along with the effect in electric slurry of this part of progress of chemical industry technology is more and more prominent, especially when being applied to silk screen printing, the composition changing organic binder bond just can change the printing of electric slurry, dry, sintering character.
In existing electric slurry field, the features such as it is high that silver system slurry has conductivity, stable performance, big with substrate bond strength, it 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, relatively costly, and the silver powder major part in existing silver paste is micron-sized powder, and the thicknesses of layers of its slurry made, printing performance etc. have significant limitation for present high-end precision instrument；On the other hand, conventional printed circuit board (PCB) uses printing conductive copper paste to make conducting wire, but it is the most oxidized to there is conductive copper paste, reduces the service life of printed circuit board (PCB), and conductive copper paste can not be printed as the circuit that comparison is fine.It is thus desirable to the size of metal dust, shape, kind are to realize reducing cost, improving conductivity, the purpose of raising printing elaboration in research electrocondution slurry.
Binding agent in conductive silver paste has a significant impact for the yield rate of circuit printing, the printing performance of circuit all can be impacted by such as viscosity, caking property, adhesive force, levelability, film property, the volatility etc. of solvent, pore occurs, the phenomenons such as open circuit, there will be glass after Organic substance has volatilized the most sometimes the most not yet to start to melt, causing the phenomenon that conducting wire comes off from stock, make conducting wire scrap, therefore the performance need of organic binder bond improves.
The most a lot of inorganic binders use glass dust, glass dust is made up of the material such as metal-oxide, silicon oxide, if fusing point is too high, also occur Organic substance volatilized after glass the most not yet start mutually to melt, the phenomenon causing the conducting wire obtained by conductive silver paste to come off from stock, makes conducting wire scrap；And a lot of containing harmful substances such as lead, to environmentally undesirable in current glass dust, it is therefore desirable to develop the glass dust that performance is more excellent.
Summary of the invention
It is an object of the invention to provide a kind of low silver content printed circuit board (PCB) silver slurry and preparation method thereof, this silver slurry joint has good electric conductivity, and has saved argentum powder consumption, and more high temperature resistant, printing is good so that circuit yield is high.
Technical scheme is as follows:
A kind of low silver content printed circuit board (PCB) silver slurry, it is characterised in that be prepared by the raw materials in: glucose 1-2, nano-grade copper powder 20-30,1-20 μm flake silver powder 30-40, glass dust 13-16, Hyperbranched Polyester Resin 5-7, terpineol 5-8, Thiodiglycol 2-5, bisphenol A epoxide resin 2-4, butyl carbitol 6-8, ethyl acetate 7-9, nano titanium oxide 1-2, nanocrystal cellulose 1-2, nanometer tantalum carbide powder 3-5, nano silicon carbide niobium powder 3-5；
Described glass dust is prepared by the raw materials in: SiO2 10-13, V2O5 15-18, Sb2O3 5-7, gas phase aluminium sesquioxide 2-4, activated alumina 15-18, P2O5 4-6, anoxia cerium oxide 3-6, MgO2-3, four acicular type zinc oxide crystal whisker 2-4；Preparation method is: by SiO2, V2O5, Sb2O3, gas phase aluminium sesquioxide, activated alumina, P2O5, anoxia cerium oxide, MgO mixing, put into crucible and be fused into liquid 1100-1400 DEG C of heating, add four acicular type zinc oxide crystal whisker, vacuum defoamation is carried out after stirring, vacuum is 0.10-0.14MPa, and inclined heated plate is
6-9 minute, then pour sizing in mould into, then carry out shrend, feeding ball mill being pulverized, sieving, obtain 7-10 μm powder, to obtain final product.
The preparation method of described low silver content printed circuit board (PCB) silver slurry, it is characterised in that comprise the following steps:
(1) by terpineol, Thiodiglycol, butyl carbitol, ethyl acetate, glucose mixing, add Hyperbranched Polyester Resin, it is heated to 80-82 DEG C, stirring to resin all dissolves, it is down to room temperature and adds bisphenol A epoxide resin stirring to dissolving, filter with the gauze of 500 mesh, remove impurity and obtain organic carrier；
(2) by nano titanium oxide, nanocrystal cellulose, glass dust mixing, nanometer tantalum carbide powder, nano silicon carbide niobium powder is added under 6000-9000 rev/min of stirring, stir 10-20 minute, add nano-grade copper powder, stir 10-20 minute, add 1-20 μm flake silver powder, stir 10-20 minute, then add together with other residual componentss in organic carrier, mixing dispersion 30-50 minute in ball mill, ultrasonic disperse 6-8 minute again, obtains uniform slurry；
(3) slurry that step (2) obtains being carried out vacuum defoamation, vacuum is 0.06-0.09MPa, and inclined heated plate is 6-9 minute, is then ground in three-high mill, rolls, and is 10000-18000 centipoise to silver slurry viscosity, to obtain final product.
Beneficial effects of the present invention
The silver slurry of the present invention with the addition of nano-grade copper powder, nanometer tantalum carbide powder, nano silicon carbide niobium powder, not only maintains good electric conductivity, and has saved argentum powder consumption；Glass dust leadless environment-friendly of the present invention, caking property is good, and circuit is firm；Organic carrier solvent of the present invention volatilizees successively, more high temperature resistant, and printing is good so that circuit yield is high.
Detailed description of the invention
A kind of low silver content printed circuit board (PCB) silver slurry, is made up of the raw material of following weight portion (kilogram): glucose 1.5, nano-grade copper powder 25,1-20 μm flake silver powder 35, glass dust 15, Hyperbranched Polyester Resin 6, terpineol 7, Thiodiglycol 3, bisphenol A epoxide resin 3, butyl carbitol 7, ethyl acetate 8, nano titanium oxide 1.5, nanocrystal cellulose 1.5, nanometer tantalum carbide powder 4, nano silicon carbide niobium powder 4；
Described glass dust is made up of the raw material of following weight portion (kilogram): SiO2 11, V2O5 17, Sb2O3
6, gas phase aluminium sesquioxide 3, activated alumina 17, P2O5 5, anoxia cerium oxide 4, MgO2.5, four acicular type zinc oxide crystal whisker 3；Preparation method is: by SiO2, V2O5, Sb2O3, gas phase aluminium sesquioxide, activated alumina, P2O5, anoxia cerium oxide, MgO mixing, put into crucible, it is fused into liquid 1300 DEG C of heating, add four acicular type zinc oxide crystal whisker, vacuum defoamation is carried out after stirring, vacuum is 0.12MPa, and inclined heated plate is
7 minutes, then pour sizing in mould into, then carry out shrend, feeding ball mill being pulverized, sieving, obtain 9 μm powder, to obtain final product.
The preparation method of described low silver content printed circuit board (PCB) silver slurry, comprises the following steps:
(1) by terpineol, Thiodiglycol, butyl carbitol, ethyl acetate, glucose mixing, add Hyperbranched Polyester Resin, it is heated to 81, stirring to resin all dissolves, it is down to room temperature and adds bisphenol A epoxide resin stirring to dissolving, filter with the gauze of 500 mesh, remove impurity and obtain organic carrier；
(2) by nano titanium oxide, nanocrystal cellulose, glass dust mixing, nanometer tantalum carbide powder, nano silicon carbide niobium powder is added under 8000 revs/min of stirrings, stir 15 minutes, add nano-grade copper powder, stir 15 minutes, add 1-20 μm flake silver powder, stir 15 minutes, then add together with other residual componentss in organic carrier, mixing dispersion 40 minutes in ball mill, ultrasonic disperse 7 minutes again, obtain uniform slurry；
(3) slurry that step (2) obtains being carried out vacuum defoamation, vacuum is 0.07MPa, and inclined heated plate is 7 minutes, is then ground in three-high mill, rolls, and is 14000 centipoises to silver slurry viscosity, to obtain final product.
Test data:
The mode of the silver-colored slurry silk screen printing obtained by the present embodiment is printed onto in PCB, then heats to solidify 6 minutes formation conducting wires at 640 DEG C, thus obtains conducting wire plate.The wiring width recording conducting wire is 0.7mm, average film thickness 5 μm, and wire distribution distance is 0.7mm, and resistivity is 4.1 × 10-5Ω·m。
Batch production conducting wire plate 1000 pieces in the manner described above, conducting wire is well combined with PCB, svelteness, continuously, has the conducting wire of 2 pieces of circuit boards to come off from stock, yield rate 99.8%.
Claims (2)
1. one kind low silver content printed circuit board (PCB) silver slurry, it is characterised in that be prepared by the raw materials in: glucose 1-2, nano-grade copper powder 20-30,1-20 μm flake silver powder 30-40, glass dust 13-16, Hyperbranched Polyester Resin 5-7, terpineol 5-8, Thiodiglycol 2-5, bisphenol A epoxide resin 2-4, butyl carbitol 6-8, ethyl acetate 7-9, nano titanium oxide 1-2, nanocrystal cellulose 1-2, nanometer tantalum carbide powder 3-5, nano silicon carbide niobium powder 3-5；
Described glass dust is prepared by the raw materials in: SiO2 10-13、V2O5 15-18、Sb2O3
5-7, gas phase aluminium sesquioxide 2-4, activated alumina 15-18, P2O54-6, anoxia cerium oxide 3-6, MgO 2-3, four acicular type zinc oxide crystal whisker 2-4；Preparation method is: by SiO2、V2O5、Sb2O3, gas phase aluminium sesquioxide, activated alumina, P2O5, anoxia cerium oxide, MgO mixing, put into crucible and be fused into liquid 1100-1400 DEG C of heating, add four acicular type zinc oxide crystal whisker, carrying out vacuum defoamation after stirring, vacuum is 0.10-0.14MPa, and inclined heated plate is 6-9 minute, pour into again in mould and shape, carry out again shrend, feeding ball mill being pulverized, sieving, obtain 7-10 μm powder, to obtain final product.
The preparation method of low silver content printed circuit board (PCB) silver the most according to claim 1 slurry, it is characterised in that comprise the following steps:
(1) terpineol, Thiodiglycol, butyl carbitol, ethyl acetate, glucose being mixed, add Hyperbranched Polyester Resin, be heated to 80-82 DEG C, stirring is all dissolved to resin, is down to room temperature and adds bisphenol A epoxide resin stirring extremely dissolving, uses
The gauze of 500 mesh filters, and removes impurity and obtains organic carrier；
(2) by nano titanium oxide, nanocrystal cellulose, glass dust mixing, nanometer tantalum carbide powder, nano silicon carbide niobium powder is added under 6000-9000 rev/min of stirring, stir 10-20 minute, add nano-grade copper powder, stir 10-20 minute, add 1-20 μm flake silver powder, stir 10-20 minute, add in organic carrier, mixing dispersion 30-50 minute in ball mill, ultrasonic disperse 6-8 minute again, obtains uniform slurry；
(3) slurry that step (2) obtains being carried out vacuum defoamation, vacuum is 0.06-0.09MPa, and inclined heated plate is 6-9 minute, is then ground in three-high mill, rolls, and is 10000-18000 centipoise to silver slurry viscosity, to obtain final product.
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Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104392769A (en) * | 2014-10-17 | 2015-03-04 | 阜阳市节源照明电器有限责任公司 | Palygorskite-contained conductive silver paste and manufacturing method thereof |
| 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 |
| JP2019114370A (en) * | 2017-12-21 | 2019-07-11 | 住友金属鉱山株式会社 | Conductive composition, conductive paste, and electronic component |
| CN110232984B (en) * | 2018-03-05 | 2022-01-07 | 宁波柔印电子科技有限责任公司 | Printing conductive silver paste and preparation method thereof |
| CN108641123A (en) * | 2018-03-28 | 2018-10-12 | 山东建邦胶体材料有限公司 | The nanocrystalline organic carrier preparation method of containing cellulose and the application in silver paste |
| CN111132448B (en) * | 2019-12-30 | 2021-03-26 | 广德新三联电子有限公司 | Silver paste multilayer board for monitoring operation of generator set and preparation process thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101609850A (en) * | 2009-07-14 | 2009-12-23 | 中南大学 | Lead-free silver conductive paste used for positive electrode of solar battery and preparation technology thereof |
| CN102222536A (en) * | 2011-03-28 | 2011-10-19 | 彩虹集团公司 | Environment-friendly silver conductive paste for surface mounting of semiconductor chips and preparation method of environment-friendly silver conductive paste |
| CN102831949A (en) * | 2012-08-24 | 2012-12-19 | 合肥中南光电有限公司 | Efficient lead-free silver paste on back of solar cell and preparation method of silver paste |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101609850A (en) * | 2009-07-14 | 2009-12-23 | 中南大学 | Lead-free silver conductive paste used for positive electrode of solar battery and preparation technology thereof |
| CN102222536A (en) * | 2011-03-28 | 2011-10-19 | 彩虹集团公司 | Environment-friendly silver conductive paste for surface mounting of semiconductor chips and preparation method of environment-friendly silver conductive paste |
| CN102831949A (en) * | 2012-08-24 | 2012-12-19 | 合肥中南光电有限公司 | Efficient lead-free silver paste on back of solar cell and preparation method of silver paste |
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