CN103996433B - A kind of phosphorous copper alloy circuit board conductive silver paste and preparation method thereof - Google Patents
A kind of phosphorous copper alloy circuit board conductive silver paste and preparation method thereof Download PDFInfo
- Publication number
- CN103996433B CN103996433B CN201410167440.6A CN201410167440A CN103996433B CN 103996433 B CN103996433 B CN 103996433B CN 201410167440 A CN201410167440 A CN 201410167440A CN 103996433 B CN103996433 B CN 103996433B
- Authority
- CN
- China
- Prior art keywords
- powder
- silver
- phosphorous
- circuit board
- minute
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Abstract
A kind of phosphorous copper alloy circuit board conductive silver paste, is made up of the raw material of following weight portion: phosphorous copper alloyed powder 40-50, the glass dust 9-12 of nano-silver powder 20-30, cellulose acetate 13-17, expanded graphite powder 3-5, phosphorous 2-4%, ethyl acetate 11-13, APG 0.2-0.4, amyl acetate 2-3, BC 3-4, natrium citricum 1-2, dimethyl formamide 2-4, polyoxypropyleneglycol 1-2, wooden calcium 0.4-0.7; Silver slurry of the present invention uses phosphor copper powder, save the consumption of silver powder, by using nano-scale silver powder, ensure good electric conductivity, by using the solvent of different boiling and evaporation rate, make the successively volatilization in the processes such as printing, smooth and level, oven dry of silver slurry, be difficult for forming the defects such as pore, crack, silver slurry is connected firm with printed circuit board (PCB), improves bonding strength; By using natrium citricum, metal dust is difficult in high temperature process process oxidized, keep good electric conductivity.
Description
Technical field
The invention belongs to electric slurry technical field, relate in particular to a kind of phosphorous copper alloy circuit board conductive silver paste andIts preparation method.
Background technology
In modern microelectronics industry, people require more and more higher to electronic devices and components, the many employings of production procedures,Standardization is carried out reducing costs, and printed circuit board (PCB) (PCB) is exactly this demand that is applicable to microelectronics industryAnd be born, corresponding conductor paste, electrode slurry, dielectric paste and resistance slurry with regard to the new requirement of demand,The electric slurries such as grout slurry and printed circuit board (PCB) (PCB) match, and carry out the research of new conductor paste alsoJust imperative.
In general, the main component of electric slurry includes function mutually as metal, noble metal powder etc., inorganicBinding agent 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, generally by metal dust or expensiveMetal dust serves as, and conventional metal dust has copper powder, aluminium powder, zinc powder, nickel powder etc., conventional noble metalPowder has bronze, silver powder, platinum powder, palladium powder etc. Inorganic binder plays fixing electric slurry to base material, and oneAs served as by oxide powder and glass powder, but this composition is lower at the proportion of electric slurry, hasEven do not have; Organic binder bond mainly works the work that makes slurry have certain shape, be easy to printing or applyWith, mainly served as by macromolecule resin, little molecule resin etc., along with the progress of chemical industry technology this partEffect in electric slurry is more and more outstanding, especially, in the time being applied to serigraphy, changes organic binder bondComposition 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, is combined with substrateThe features such as intensity is large, are widely used in the life of the electronic devices and components such as integrated circuit, multi-chip module, thin film switchProduce. But silver is precious metal, cost is higher, and silver powder major part in existing silver paste is micro-The powder of meter level, thicknesses of layers, the printing performance etc. of its slurry of making is for present high-end precision instrumentThere is significant limitation; 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, reduce the service life of printed circuit board (PCB), conductive copper paste can notBe printed as meticulousr circuit. Therefore need to study size, shape, the kind of metal dust in electrocondution slurryThe object that reduce costs, improve conductance to realize, improves printing accuracy.
Binding agent in conductive silver paste has a significant impact for the yield rate of circuit printing, for example viscosity, caking property,The volatility of adhesive force, levelability, film forming, solvent etc. all can impact the printing performance of circuit, goes outExisting pore, the phenomenon such as open circuit, also there will be the organic matter glassy phase afterwards that volatilize not yet to start to melt sometimesChange, the phenomenon that causes conducting wire to come off from stock, scrap conducting wire, therefore organic binder bondPerformance need improves.
At present a lot of inorganic binders adopt glass dust, and glass dust is made up of the material such as metal oxide, silica,If fusing point is too high, also occur organic matter volatilized after glassy phase not yet start melt, cause by conductive silverThe phenomenon that the conducting wire that slurry obtains comes off from stock, scraps conducting wire; And current glass dustIn much contain the harmful substances such as plumbous, 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 phosphorous copper alloy circuit board conductive silver paste and preparation method thereof, this silverSlurry has been saved the consumption of silver powder, has ensured good electric conductivity, and bonding strength is high.
Technical scheme of the present invention is as follows:
A kind of phosphorous copper alloy circuit board conductive silver paste, is characterized in that being made up of the raw material of following weight portion: receiveThe phosphorous copper alloyed powder of rice silver powder 20-30, cellulose acetate 13-17, expanded graphite powder 3-5, phosphorous 2-4%40-50, glass dust 9-12, ethyl acetate 11-13, APG 0.2-0.4, amyl acetate 2-3, fourthBase carbitol 3-4, natrium citricum 1-2, dimethyl formamide 2-4, polyoxypropyleneglycol 1-2, wooden calcium0.4-0.7；
Described glass dust is made up of the raw material of following weight portion: bismuth telluride 15-17, SiO216-19、Bi2O37-9、BaO5-8、Al2O33-5、B2O317-23、V2O54-7、Na2O1-2, nano aluminum nitride powder 1-2; PreparationMethod is: by bismuth telluride, SiO2、Bi2O3、BaO、Al2O3、B2O3、V2O5、Na2O mixes, and puts into crucibleBecome liquid 1100-1400 DEG C of heat fused, then add nano aluminum nitride powder, after stirring, carry out vacuumDeaeration, vacuum is 0.10-0.14MPa, the deaeration time is 6-9 minute, then pours in mould and shape, thenCarry out shrend, send in ball mill and pulverize, sieve, obtain 9-13 μ m powder, to obtain final product.
The preparation method of described phosphorous copper alloy circuit board conductive silver paste, is characterized in that comprising the following steps:(1) ethyl acetate, amyl acetate, BC, dimethyl formamide, polyoxypropyleneglycol are mixed,Add cellulose acetate, be heated to 78-82 DEG C, be stirred to resin and all dissolve, then add wooden calcium to stir,With 500 object gauzes filtrations, remove impurity and obtain organic carrier;
(2) the phosphorous copper alloyed powder of natrium citricum, APG, phosphorous 2-4% is mixed, at 5000-7000Under rev/min stirring, add expanded graphite powder, stir 10-20 minute, then add nano-silver powder, stir 20-30Minute, then add in organic carrier together with other residual components, 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 is 0.06-0.09MPa, when deaerationBetween be 6-9 minute, then in three-high mill, grind, rolling, to silver-colored slurry viscosity be 10000-20000Centipoise, to obtain final product.
Beneficial effect of the present invention
Silver slurry of the present invention uses phosphor copper powder, has saved the consumption of silver powder, by using nano-scale silver powder,Ensured good electric conductivity, by using the solvent of different boiling and evaporation rate, make silver slurry printing,Successively volatilization in the processes such as smooth and level, oven dry, is difficult for forming the defects such as pore, crack, makes silver slurry and printed circuit board (PCB)It is firm to connect, and improves bonding strength; By using natrium citricum, make metal dust in high temperature process processBe difficult for oxidizedly, keep good electric conductivity; Glass dust of the present invention contains nano aluminum nitride powder, and heat conduction is fast,Fusing is fast, is easy to circuit curing molding.
Detailed description of the invention
A kind of phosphorous copper alloy circuit board conductive silver paste, by following weight portion (kilogram) raw material make: nanometerSilver powder 25, cellulose acetate 16, expanded graphite powder 4, the phosphorous copper alloyed powder 45 of phosphorous 2-4%, glass dust11, ethyl acetate 12, APG 0.3, amyl acetate 2.5, BC 3.5, natrium citricum1.5, dimethyl formamide 3, polyoxypropyleneglycol 1.5, wooden calcium 0.6;
Described glass dust by following weight portion (kilogram) raw material make: bismuth telluride 16, SiO217、Bi2O38、BaO7、Al2O34、B2O320、V2O56、Na2O1.5, nano aluminum nitride powder 1.5; Preparation method is: willBismuth telluride, SiO2、Bi2O3、BaO、Al2O3、B2O3、V2O5、Na2O mixes, and puts into crucible and adds at 1300 DEG CHot melt changes into liquid, then adds nano aluminum nitride powder, carries out vacuum defoamation after stirring, and vacuum is0.13MPa, the deaeration time is 7 minutes, then pours in mould and shape, then carries out shrend, sends in ball millPulverize, sieve, obtain 11 μ m powder, to obtain final product.
The preparation method of described phosphorous copper alloy circuit board conductive silver paste, comprises the following steps:
(1) ethyl acetate, amyl acetate, BC, dimethyl formamide, polyoxypropyleneglycol are mixed,Add cellulose acetate, be heated to 79 DEG C, be stirred to resin and all dissolve, then add wooden calcium to stir,With 500 object gauzes filtrations, remove impurity and obtain organic carrier;
(2) the phosphorous copper alloyed powder of natrium citricum, APG, phosphorous 2-4% is mixed, at 6000 revs/minUnder stirring, add expanded graphite powder, stir 15 minutes, then add nano-silver powder, stir 25 minutes, then withOther residual components add in organic carrier together, and in ball mill, mix and disperse 40 minutes, more ultrasonic dispersion 7Minute, obtain uniform slurry;
(3) slurry step (2) being obtained carries out vacuum defoamation, and vacuum is 0.08MPa, and the deaeration time is 7Minute, then in three-high mill, grind, rolling, to silver-colored slurry viscosity be 16000 centipoises, to obtain final product.
Test data:
The silver slurry mode of serigraphy that the present embodiment is obtained is printed onto on PCB circuit board, is then warming up toAt 640 DEG C, solidify and form conducting wire in 6 minutes, thereby obtain conducting wire plate. Record the wiring of conducting wireWidth is 0.7mm, average film thickness 5 μ m, and wire distribution distance is 1mm, resistivity is 5.1 × 10-5Ω·m。
Produce in the manner described above 1000 of conducting wire plates in batches, conducting wire is combined good with PCB circuit boardGood, svelteness, continuously, has the conducting wire of 5 circuit boards to come off from stock, yield rate 99.5%.
Claims (2)
1. a phosphorous copper alloy circuit board conductive silver paste, is characterized in that being made up of the raw material of following weight portion: phosphorous copper alloyed powder 40-50, the glass dust 9-12 of nano-silver powder 20-30, cellulose acetate 13-17, expanded graphite powder 3-5, phosphorous 2-4%, ethyl acetate 11-13, APG 0.2-0.4, amyl acetate 2-3, BC 3-4, natrium citricum 1-2, dimethyl formamide 2-4, polyoxypropyleneglycol 1-2, wooden calcium 0.4-0.7;
Described glass dust is made up of the raw material of following weight portion: bismuth telluride 15-17, Si0216-19、Bi2037-9、BaO5-8、Al2033-5、B2O317-23、V2O54-7、Na2O1-2, nano aluminum nitride powder 1-2; Preparation method is: by bismuth telluride, Si02、Bi203、BaO、Al203、B2O3、V2O5、Na2O 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 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. a preparation method for phosphorous copper alloy circuit board conductive silver paste as claimed in claim 1, is characterized in that comprising the following steps:
(1) ethyl acetate, amyl acetate, BC, dimethyl formamide, polyoxypropyleneglycol are mixed, add cellulose acetate, be heated to 78-82 DEG C, being stirred to resin all dissolves, add again wooden calcium to stir, with 500 object gauzes filtrations, remove impurity and obtain organic carrier;
(2) the phosphorous copper alloyed powder of natrium citricum, APG, phosphorous 2-4% is mixed, under 5000-7000 rev/min of stirring, add expanded graphite powder, stir 10-20 minute, add again nano-silver powder, stir 20-30 minute, then add in organic carrier together with other residual components, 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 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 |
|---|---|---|---|
| CN201410167440.6A CN103996433B (en) | 2014-04-24 | 2014-04-24 | A kind of phosphorous copper alloy circuit board conductive silver paste and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410167440.6A CN103996433B (en) | 2014-04-24 | 2014-04-24 | A kind of phosphorous copper alloy circuit board conductive silver paste and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN103996433A CN103996433A (en) | 2014-08-20 |
| CN103996433B true CN103996433B (en) | 2016-05-18 |
Family
ID=51310571
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410167440.6A Active CN103996433B (en) | 2014-04-24 | 2014-04-24 | A kind of phosphorous copper alloy circuit board conductive silver paste and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103996433B (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104575668B (en) * | 2015-01-08 | 2017-01-04 | 安徽凤阳德诚科技有限公司 | A kind of nanometer antiwear conductive silver paste |
| CN116189960B (en) * | 2023-04-19 | 2024-02-27 | 佛山科学技术学院 | Silver-copper composite conductive paste capable of being sintered at low temperature and preparation method and application thereof |
Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP4261786B2 (en) * | 2001-09-28 | 2009-04-30 | 三井金属鉱業株式会社 | Silver-coated copper powder manufacturing method, silver-coated copper powder obtained by the manufacturing method, conductive paste using the silver-coated copper powder, and printed wiring board using the conductive paste |
| JP4235887B2 (en) * | 2002-06-07 | 2009-03-11 | 日立化成工業株式会社 | Conductive paste |
| KR20130031414A (en) * | 2011-09-21 | 2013-03-29 | 삼성전기주식회사 | Conductive paste composition for low temperature firing |
| CN102831950B (en) * | 2012-08-24 | 2014-07-30 | 合肥中南光电有限公司 | Conductive lead-free silver paste mixed with copper powder and aluminum powder for solar cell and preparation method of conductive lead-free silver paste |
-
2014
- 2014-04-24 CN CN201410167440.6A patent/CN103996433B/en active Active
Also Published As
| Publication number | Publication date |
|---|---|
| CN103996433A (en) | 2014-08-20 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103985431B (en) | A kind of high intensity printed circuit board (PCB) conductive silver paste and preparation method thereof | |
| CN103996432B (en) | A kind of easily printed circuit board (PCB) silver slurry and preparation method thereof | |
| CN104078093B (en) | A kind of high-strength PC B circuit board conductive silver slurry and preparation method thereof | |
| CN104036842B (en) | A kind of leadless environment-friendly circuit board conductive silver slurry and preparation method thereof | |
| CN102262918B (en) | Grout silver paste used in PCB and preparation method thereof | |
| CN104078098B (en) | A kind of low silver content printed circuit board (PCB) silver slurry and preparation method thereof | |
| CN101950598A (en) | Conductor pulp for printed circuit board and preparation method thereof | |
| CN103996430A (en) | Highly-conductive PCB circuit board silver paste and preparation method thereof | |
| CN102426872A (en) | Low temperature solidified silver paste for keyboard lines and preparation method thereof | |
| CN104078097B (en) | A kind of grout printed circuit board (PCB) silver slurry and preparation method thereof | |
| CN104143377A (en) | PCB conductive silver paste and preparing method thereof | |
| CN103996433B (en) | A kind of phosphorous copper alloy circuit board conductive silver paste and preparation method thereof | |
| CN106128548B (en) | A kind of resistance slurry of high electric heating conversion ratio | |
| CN104318977A (en) | Sintering method for lead-free silver paste | |
| CN103996424A (en) | Wear-resistant printed circuit board silver slurry and preparation method thereof | |
| CN103996425A (en) | Nanometer carbon-containing circuit board conductive silver paste and preparation method thereof | |
| CN104143376A (en) | Conductive silver paste containing nickel powder of PCB and preparation method thereof | |
| CN103996434A (en) | Low-silver printed circuit board silver paste and preparation method thereof | |
| CN103985432B (en) | PCB silver paste and preparing method thereof | |
| CN104934095A (en) | Printed circuit board conductive silver paste and preparation method thereof | |
| CN104008790A (en) | Electricity-conducting silver paste for printed circuit board and preparing method thereof | |
| CN104955267A (en) | PCB (printed circuit board) silver paste containing silver coated nickel powder and preparation method of PCB silver paste | |
| CN104934096A (en) | Environment-friendly circuit board conductive silver paste and preparation method thereof | |
| CN104078099A (en) | Environmentally-friendly printed circuit board conductive silver paste and preparing method thereof | |
| CN113707359B (en) | Electrode paste, conductive thick film and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| TR01 | Transfer of patent right | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20210520 Address after: No.18-91, Gongye Road, South Taihu high tech Industrial Park, Wuxing District, Huzhou City, Zhejiang Province Patentee after: Zhejiang julibao Textile Technology Co., Ltd Address before: 242800 Matang Industrial Park, Dingqiao Town, Qingyang County, Chizhou City, Anhui Province Patentee before: ANHUI WEIMIN MAGNETIC TECHNOLOGY Co.,Ltd. |