CN104616721B - A kind of high adhesion force conductive silver paste - Google Patents
A kind of high adhesion force conductive silver paste Download PDFInfo
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- CN104616721B CN104616721B CN201510008182.1A CN201510008182A CN104616721B CN 104616721 B CN104616721 B CN 104616721B CN 201510008182 A CN201510008182 A CN 201510008182A CN 104616721 B CN104616721 B CN 104616721B
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Abstract
The invention discloses a kind of high adhesion force conductive silver paste, which is obtained by the raw material of following weight parts：Silver powder 55 70, dimethyl silicone polymer 0.8 1.0, amyl acetate 23, acetylacetone,2,4-pentanedione silver 25, C5 Petropols 24, polyester resin 5 15, dimethyl azelate 12, tetraethyl orthosilicate 0.3 0.6, isopropanol 18 22, modified glass powder 15 30, isophorone 10 12, butyl stearate 0.8 1.2.The add silver powder caused in conductive silver paste, powdered graphite of each additive can be disperseed after adding well, and improving adding for the electric conductivity of conductive silver paste, C5 Petropols etc. can be so that the present invention be good with the adhesive force of substrate.
Description
Technical field
A kind of the invention belongs to conductive silver paste field, more particularly to high adhesion force conductive silver paste.
Background technology
Slug type conductive silver slurry needs to sinter film forming, sintering temperature>500 DEG C, glass dust or oxide are used as bonding phase.
Silver powder is according to particle size classification, average grain diameter<0.1 μm (100nm) is nano-silver powder；0.1μm<Dav (average grain diameter)<10.0 μm it is
Micro silver powder；Dav (average grain diameter)>10.0 μm is raw Ag powder.The preparation method of powder has a lot, for silver, once can adopt
Physical (plasma, atomization), chemical method (silver nitrate thermal decomposition method, liquid-phase reduction).As silver is noble metal, easily it is reduced
And elemental stage is returned to, therefore liquid phase reduction is the topmost method for preparing silver powder at present.Will silver salt (silver nitrate etc.)
Soluble in water, add chemical reducing agent (such as hydrazine hydrate etc.), deposit silver powder, through washing, dry and obtain silver-colored reduced powder, put down
Between 0.1-10.0 μm, the selection of reducing agent, the control of reaction condition, the use of interfacial agent can be prepared particle diameter
Micro silver powder (particle shape, degree of scatter, average grain diameter and particle diameter distribution, specific surface area, the pine dress of different physicochemical characteristics
Density, tap density, grain size, crystallinity etc.), (ball milling etc.) is machined to reduced powder can be obtained Bright Silver Powder
(polished silver powder), flake silver powder (silver flake).
Content of the invention
It is an object of the invention to provide a kind of high adhesion force conductive silver paste.
The present invention is adopted the following technical scheme that to achieve these goals：
A kind of high adhesion force conductive silver paste, it is characterised in which is obtained by the raw material of following weight parts：Silver powder 55-
70th, dimethyl silicone polymer 0.8-1.0, amyl acetate 2-3, acetylacetone,2,4-pentanedione silver 2-5, C5 Petropols 2-4, polyester resin 5-
15th, dimethyl azelate 1-2, tetraethyl orthosilicate 0.3-0.6, isopropanol 18-22, modified glass powder 15-30, isophorone 10-
12nd, butyl stearate 0.8-1.2；
Modified glass powder is obtained by the raw material of following weight parts：Waste glass powder 10-15, Na2O 6-10,K2O 10-12、
Co2O310-12、SnO 2-4、Na3AlF64-8、TiO24-8, sodium aluminate 1-2, Tissuemat E 2-4, chlorinated paraffin 1-2, alkyl
Benzene sulfonic acid sodium salt 2-4, sodium metasilicate 3-5, turkey red oil 0.1-0.2, sodium hydrogensulfite 1-2, lecithin 1-2, deionized water
100-150；
The preparation method of described modified glass powder is：
(1) sodium aluminate, Tissuemat E, chlorinated paraffin and deionized water are added in reactor, 300-400 rev/min is stirred
Mix uniform, add sodium alkyl benzene sulfonate, sodium metasilicate, turkey red oil, sodium hydrogensulfite, lecithin, be warming up to 130-150
DEG C, stir under 200-500rpm, obtain modification liquid；
(2) waste glass powder and remaining raw material mix sintering, and sintering temperature is 1200-1400 DEG C, and the time is that 0.5-2 is little
When, obtain glass melt, quenching, ball milling, drying, sieve to obtain 10-15 μm of glass dust；
(3) by glass dust and modification liquid, mixing, at 50-60 DEG C, 3-5 hours are stirred, stand 7-8 hours, suction filtration is dried,
Obtain final product.
A kind of described high adhesion force conductive silver paste, it is characterised in that：Preparation method is comprised the following steps：
(1), dimethyl silicone polymer, C5 Petropols, polyester resin, dimethyl azelate, tetraethyl orthosilicate, isopropyl
Alcohol, isophorone, butyl stearate stir 30-50min under 40-50 DEG C, 45-60 rev/min, obtain organic carrier standby；
(2), modified glass powder is added in organic carrier, stirring is mixed, adds remaining raw material, mix 2-3 hours,
Obtain slurry；
(3), slurry ball milling, is ground to slurry fineness less than 10 μm, obtains final product after adjusting viscosity.
Beneficial effects of the present invention：
The addition of each additive is so that silver powder, powdered graphite in conductive silver paste can be divided after adding well
Dissipate, improve adding for the electric conductivity of conductive silver paste, C5 Petropols etc. and the present invention can be caused good with the adhesive force of substrate.
Specific embodiment
A kind of high adhesion force conductive silver paste, its are obtained by the raw material of following weight (kg)：
Silver powder 60, dimethyl silicone polymer 0.8, amyl acetate 2, acetylacetone,2,4-pentanedione silver 2, C5 Petropols 4, polyester resin
8th, dimethyl azelate 1, tetraethyl orthosilicate 0.3, isopropanol 22, modified glass powder 20, isophorone 12, butyl stearate 0.8；
Modified glass powder is obtained by the raw material of following weight (kg)：Waste glass powder 15, Na2O 10,K2O 12、Co2O310、
SnO 2-4、Na3AlF68、TiO26th, sodium aluminate 1, Tissuemat E 4, chlorinated paraffin 2, sodium alkyl benzene sulfonate 4, sodium metasilicate 3,
Turkey red oil 0.1, sodium hydrogensulfite 1, lecithin 2, deionized water 150；
The preparation method of described modified glass powder is：
(1) sodium aluminate, Tissuemat E, chlorinated paraffin and deionized water are added in reactor, 400 revs/min of stirrings are
Even, add sodium alkyl benzene sulfonate, sodium metasilicate, turkey red oil, sodium hydrogensulfite, lecithin, be warming up to 150 DEG C,
Stir under 500rpm, obtain modification liquid；
(2) waste glass powder and remaining raw material mix sintering, and sintering temperature is 1300 DEG C, and the time is 0.5 hour, obtains glass
Glass molten mass, quenching, ball milling, drying, sieve to obtain 10-15 μm of glass dust；
(3) by glass dust and modification liquid, mixing, stir 5 hours at 60 DEG C, stand 7 hours, suction filtration is dried, and is obtained final product.
A kind of described high adhesion force conductive silver paste, preparation method are comprised the following steps：
(1), dimethyl silicone polymer, C5 Petropols, polyester resin, dimethyl azelate, tetraethyl orthosilicate, isopropyl
Alcohol, isophorone, butyl stearate stir 50min under 50 DEG C, 60 revs/min, obtain organic carrier standby；
(2), modified glass powder is added in organic carrier, stirring is mixed, adds remaining raw material, mixed 3 hours, obtain
Arrive slurry；
(3), slurry ball milling, is ground to slurry fineness less than 10 μm, obtains final product after adjusting viscosity.
Silver paste is printed on 125mm × 125mm Si substrates using screen process press, then in 180 DEG C of dryings, then
880 DEG C carry out quick fired electrodes lead, and the contact conductor surface silvery white that makes after high temperature sintering, smooth zero defect are peeled off strong
14.6 N/cm are spent, soldering is functional, sheet resistance ＜ 10Siements/sq, the solar cell photoelectric transformation efficiency of preparation is
22.3%, tensile test result is adhesive force>15.2N/mm2.
Claims (2)
1. a kind of high adhesion force conductive silver paste, it is characterised in which is obtained by the raw material of following weight parts：Silver powder 55-
70th, dimethyl silicone polymer 0.8-1.0, amyl acetate 2-3, acetylacetone,2,4-pentanedione silver 2-5, C5 Petropols 2-4, polyester resin 5-
15th, dimethyl azelate 1-2, tetraethyl orthosilicate 0.3-0.6, isopropanol 18-22, modified glass powder 15-30, isophorone 10-
12nd, butyl stearate 0.8-1.2；
Modified glass powder is obtained by the raw material of following weight parts：Waste glass powder 10-15, Na2O 6-10、K2O 10-12、Co2O3
10-12、SnO 2-4、Na3AlF64-8、TiO24-8, sodium aluminate 1-2, Tissuemat E 2-4, chlorinated paraffin 1-2, benzene sulfonamide
Sour sodium 2-4, sodium metasilicate 3-5, turkey red oil 0.1-0.2, sodium hydrogensulfite 1-2, lecithin 1-2, deionized water 100-
150；
The preparation method of described modified glass powder is：
（1）Sodium aluminate, Tissuemat E, chlorinated paraffin and deionized water are added in reactor, 300-400 rev/min of stirring is
Even, add sodium alkyl benzene sulfonate, sodium metasilicate, turkey red oil, sodium hydrogensulfite, lecithin, be warming up to 130-150 DEG C,
Stir under 200-500rpm, obtain modification liquid；
（2）Waste glass powder and remaining raw material mix sintering, and sintering temperature is 1200-1400 DEG C, and the time is 0.5-2 hours, obtains
Glass melt, quenching, ball milling, drying, sieve to obtain 10-15 μm of glass dust；
（3）By glass dust and modification liquid, mixing, at 50-60 DEG C, 3-5 hours are stirred, stand 7-8 hours, suction filtration is dried, i.e.,
?.
2. a kind of high adhesion force conductive silver paste according to claim 1, it is characterised in that：Preparation method includes following step
Suddenly：（1）, dimethyl silicone polymer, C5 Petropols, polyester resin, dimethyl azelate, tetraethyl orthosilicate, isopropanol, different
Phorone, butyl stearate stir 30-50min under 40-50 DEG C, 45-60 rev/min, obtain organic carrier standby；
（2）, modified glass powder is added in organic carrier, stirring is mixed, and adds remaining raw material, is mixed 2-3 hours, is obtained
Slurry；
（3）, slurry ball milling, be ground to slurry fineness less than 10 μm, obtain final product after adjusting viscosity.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510008182.1A CN104616721B (en) | 2015-01-08 | 2015-01-08 | A kind of high adhesion force conductive silver paste |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510008182.1A CN104616721B (en) | 2015-01-08 | 2015-01-08 | A kind of high adhesion force conductive silver paste |
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| Publication Number | Publication Date |
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| CN104616721A CN104616721A (en) | 2015-05-13 |
| CN104616721B true CN104616721B (en) | 2017-03-15 |
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| CN201510008182.1A Expired - Fee Related CN104616721B (en) | 2015-01-08 | 2015-01-08 | A kind of high adhesion force conductive silver paste |
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Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107658046A (en) * | 2017-09-25 | 2018-02-02 | 江苏时瑞电子科技有限公司 | A kind of high adhesion force conductive silver paste and preparation method thereof |
| CN107887050A (en) * | 2017-11-27 | 2018-04-06 | 钦州学院 | A kind of crystal silicon solar energy battery high solderability front electrode silver slurry and preparation method |
| CN112820442B (en) * | 2021-04-19 | 2021-07-06 | 西安宏星电子浆料科技股份有限公司 | Strong-adhesion silver conductor paste for 5G ceramic dielectric filter |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101650982A (en) * | 2009-08-18 | 2010-02-17 | 深圳市中金岭南科技有限公司 | Conductive silver paste with low halogen content |
| CN102592710A (en) * | 2012-02-13 | 2012-07-18 | 江苏瑞德新能源科技有限公司 | Solar energy battery electrode-conducting silver slurry containing micron-size mixed silver powders |
| CN104143380A (en) * | 2014-07-05 | 2014-11-12 | 滁州恒恩光电科技有限公司 | Magnesia and zinc oxide composite conductive silver paste and manufacturing method thereof |
| CN104157323A (en) * | 2014-07-30 | 2014-11-19 | 安徽状元郎电子科技有限公司 | Silica powder corrosion-resistant conductive slurry and manufacturing method thereof |
-
2015
- 2015-01-08 CN CN201510008182.1A patent/CN104616721B/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101650982A (en) * | 2009-08-18 | 2010-02-17 | 深圳市中金岭南科技有限公司 | Conductive silver paste with low halogen content |
| CN102592710A (en) * | 2012-02-13 | 2012-07-18 | 江苏瑞德新能源科技有限公司 | Solar energy battery electrode-conducting silver slurry containing micron-size mixed silver powders |
| CN104143380A (en) * | 2014-07-05 | 2014-11-12 | 滁州恒恩光电科技有限公司 | Magnesia and zinc oxide composite conductive silver paste and manufacturing method thereof |
| CN104157323A (en) * | 2014-07-30 | 2014-11-19 | 安徽状元郎电子科技有限公司 | Silica powder corrosion-resistant conductive slurry and manufacturing method thereof |
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| CN104616721A (en) | 2015-05-13 |
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Effective date of registration: 20170210 Address after: Hangzhou City, Zhejiang province 310000 Jianggan District Garden 4 Building 3 unit on Bridge Applicant after: Ye Xiaoyu Address before: 233122 Anhui city of Chuzhou province Fengyang County town south of Fuxi Applicant before: ANHUI FENGYANG DECHENG TECHNOLOGY CO., LTD. |
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