CN104616721A - High adhesive force of conductive silver paste - Google Patents

High adhesive force of conductive silver paste Download PDF

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Publication number
CN104616721A
CN104616721A CN201510008182.1A CN201510008182A CN104616721A CN 104616721 A CN104616721 A CN 104616721A CN 201510008182 A CN201510008182 A CN 201510008182A CN 104616721 A CN104616721 A CN 104616721A
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parts
silver paste
conductive silver
powder
glass powder
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CN201510008182.1A
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CN104616721B (en
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王乐乐
刘战
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ANHUI FENGYANG DECHENG TECHNOLOGY Co Ltd
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Abstract

The invention discloses high adhesive force of conductive silver paste. The high adhesive force of conductive silver paste is produced through following materials of, by weight, 55 to 70 parts of silver powder, 0.8 to 1.0 part of poly dimethyl siloxane, 2 to 3 parts of amyl acetate, 2 to 5 parts of silver acetylacetonate, 2 to 4 parts of C5 petroleum resin, 5 to 15 parts of polyester resin, 1 to 2 parts of acelaic acid dimethyl ester, 0.3 to 0.6 part of ethyl orthosilicate, 18 to 22 parts of isopropyl alcohol, 15 to 30 parts of modified glass powder, 10 to 12 parts of isophorone and 0.8 to 1.2 parts of butyl stearate. According to the high adhesive force of conductive silver paste, the silver powder and graphite powder in the conductive silver paste can be well dispersed after being added due to the adding of additives and accordingly the conductivity of the conductive silver paste is improved and the adhesive force of the conductive silver paste and a substrate can be good due to the adding of the C5 petroleum resin and the like.

Description

A kind of high adhesion force conductive silver paste
Technical field
The invention belongs to conductive silver paste field, particularly relate to a kind of high adhesion force conductive silver paste.
Background technology
Slug type conductive silver slurry needs to sinter film forming, and sintering temperature >500 DEG C, glass dust or oxide are as bonding phase.Silver powder is according to particle size classification, and average grain diameter <0.1 μm (100nm) is nano-silver powder; 0.1 μm of < Dav (average grain diameter) <10.0 μm is micro silver powder; Dav (average grain diameter) > 10.0 μm is raw Ag powder.The preparation method of powder has a lot, with regard to silver, once can adopt Physical (plasma, atomization), chemical method (silver nitrate thermal decomposition method, liquid-phase reduction).Because silver is noble metal, be easily reduced and get back to elemental stage, therefore liquid phase reduction is the topmost method preparing silver powder at present.Soluble in water by silver salt (silver nitrate etc.), add chemical reducing agent (as hydrazine hydrate etc.), deposit silver powder, through washing, dry and obtain silver-colored reduced powder, average grain diameter is between 0.1-10.0 μm, the selection of reducing agent, the control of reaction condition, the use of interfacial agent, micro silver powder (the particle shape of different physicochemical characteristics can be prepared, degree of scatter, average grain diameter and domain size distribution, specific area, apparent density, tap density, grain size, crystallinity etc.), machining (ball milling etc.) is carried out to reduced powder and can obtain Bright Silver Powder (polished silver powder), flake silver powder (silver flake).
Summary of the invention
The object of this invention is to provide a kind of high adhesion force conductive silver paste.
The present invention adopts following technical scheme to achieve these goals:
A kind of high adhesion force conductive silver paste, it is characterized in that, it is obtained by the raw material of following weight parts:
Silver powder 55-70, dimethyl silicone polymer 0.8-1.0, amyl acetate 2-3, acetylacetone,2,4-pentanedione silver 2-5, C5 Petropols 2-4, mylar 5-15, dimethyl azelate 1-2, tetraethoxysilane 0.3-0.6, isopropyl alcohol 18-22, modified glass powder 15-30, isophorone 10-12, butyl stearate 0.8-1.2;
Modified glass powder is obtained by the raw material of following weight parts: waste glass powder 10-15, Na 2o 6-10, K 2o 10-12, Co 2o 310-12, SnO 2-4, NA 3aLF 64-8, TiO 24-8, sodium aluminate 1-2, Tissuemat E 2-4, chlorinated paraffin wax 1-2, sodium alkyl benzene sulfonate 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 wax and deionized water are added in reactor, 300-400 rev/min stirs, add sodium alkyl benzene sulfonate, sodium metasilicate, turkey red oil, sodium hydrogensulfite, lecithin again, be warming up to 130-150 DEG C, stir under 200-500rpm, obtain modification liquid;
(2) waste glass powder and all the other raw material blendings sintering, sintering temperature is 1200-1400 DEG C, and the time is 0.5-2 hour, obtains glass melt quenching, ball milling, drying, and sieve to obtain 10-15 μm of glass dust;
(3) by glass dust and modification liquid, mixing, at 50-60 DEG C, stir 3-5 hour, leave standstill 7-8 hour, suction filtration is dry, to obtain final product.
Described a kind of high adhesion force conductive silver paste, is characterized in that: preparation method comprises the following steps:
(1), dimethyl silicone polymer, C5 Petropols, mylar, dimethyl azelate, tetraethoxysilane, isopropyl alcohol, isophorone, butyl stearate in 40-50 DEG C, stir 30-50min under 45-60 rev/min, obtain organic carrier for subsequent use;
(2), join in organic carrier by modified glass powder, stir mixed, then add all the other raw materials, mixed 2-3 hour, obtains slurry;
(3), slurry ball milling, be ground to slurry fineness and be less than 10 μm, adjust after viscosity and get final product.
Beneficial effect of the present invention:
Each additive add the silver powder made in conductive silver paste, powdered graphite can well be disperseed after adding, and improves the conductivity of conductive silver paste, C5 Petropols etc. to add the adhesive force that can make the present invention and substrate good.
Embodiment
A kind of high adhesion force conductive silver paste, it is 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, mylar 8, dimethyl azelate 1, tetraethoxysilane 0.3, isopropyl alcohol 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, Na 2o10, K 2o 12, Co 2o 310, SnO 2-4, NA 3aLF 68, TiO 26, sodium aluminate 1, Tissuemat E 4, chlorinated paraffin wax 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 wax and deionized water are added in reactor, 400 revs/min stir, add sodium alkyl benzene sulfonate, sodium metasilicate, turkey red oil, sodium hydrogensulfite, lecithin again, be warming up to 150 DEG C, stir under 500rpm, obtain modification liquid;
(2) waste glass powder and all the other raw material blendings sintering, sintering temperature is 1300 DEG C, and the time is 0.5 hour, obtains glass melt quenching, ball milling, drying, and sieve to obtain 10-15 μm of glass dust;
(3) by glass dust and modification liquid, mixing, stir 5 hours at 60 DEG C, leave standstill 7 hours, suction filtration is dry, to obtain final product.
Described a kind of high adhesion force conductive silver paste, preparation method comprises the following steps:
(1), dimethyl silicone polymer, C5 Petropols, mylar, dimethyl azelate, tetraethoxysilane, isopropyl alcohol, isophorone, butyl stearate stir 50min under 50 DEG C, 60 revs/min, obtains organic carrier for subsequent use;
(2), modified glass powder is joined in organic carrier, stir mixed, then add all the other raw materials, mixed 3 hours, obtain slurry;
(3), slurry ball milling, be ground to slurry fineness and be less than 10 μm, adjust after viscosity and get final product.
Screen process press is adopted to be printed on 125mm × 125mm Si substrate by silver slurry, then 180 DEG C of dryings, quick fired electrodes lead-in wire is carried out again at 880 DEG C, the contact conductor surface silvery white made after high temperature sintering, smooth zero defect, peel strength 14.6 N/cm, soldering is functional, sheet resistance < 10 Siements/sq, the solar cell photoelectric transformation efficiency of preparation is 22.3%, and tensile test result is adhesive force >15.2N/mm 2.

Claims (2)

1. a high adhesion force conductive silver paste, is characterized in that, it is obtained by the raw material of following weight parts:
Silver powder 55-70, dimethyl silicone polymer 0.8-1.0, amyl acetate 2-3, acetylacetone,2,4-pentanedione silver 2-5, C5 Petropols 2-4, mylar 5-15, dimethyl azelate 1-2, tetraethoxysilane 0.3-0.6, isopropyl alcohol 18-22, modified glass powder 15-30, isophorone 10-12, butyl stearate 0.8-1.2;
Modified glass powder is obtained by the raw material of following weight parts: waste glass powder 10-15, Na 2o 6-10, K 2o 10-12, Co 2o 310-12, SnO 2-4, NA 3aLF 64-8, TiO 24-8, sodium aluminate 1-2, Tissuemat E 2-4, chlorinated paraffin wax 1-2, sodium alkyl benzene sulfonate 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 wax and deionized water are added in reactor, 300-400 rev/min stirs, add sodium alkyl benzene sulfonate, sodium metasilicate, turkey red oil, sodium hydrogensulfite, lecithin again, be warming up to 130-150 DEG C, stir under 200-500rpm, obtain modification liquid;
(2) waste glass powder and all the other raw material blendings sintering, sintering temperature is 1200-1400 DEG C, and the time is 0.5-2 hour, obtains glass melt quenching, ball milling, drying, and sieve to obtain 10-15 μm of glass dust;
(3) by glass dust and modification liquid, mixing, at 50-60 DEG C, stir 3-5 hour, leave standstill 7-8 hour, suction filtration is dry, to obtain final product.
2. a kind of high adhesion force conductive silver paste according to claim 1, is characterized in that: preparation method comprises the following steps:
(1), dimethyl silicone polymer, C5 Petropols, mylar, dimethyl azelate, tetraethoxysilane, isopropyl alcohol, isophorone, butyl stearate in 40-50 DEG C, stir 30-50min under 45-60 rev/min, obtain organic carrier for subsequent use;
(2), join in organic carrier by modified glass powder, stir mixed, then add all the other raw materials, mixed 2-3 hour, obtains slurry;
(3), slurry ball milling, be ground to slurry fineness and be less than 10 μm, adjust after viscosity and get final product.
CN201510008182.1A 2015-01-08 2015-01-08 A kind of high adhesion force conductive silver paste Expired - Fee Related CN104616721B (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
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
CN112820442A (en) * 2021-04-19 2021-05-18 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)

* Cited by examiner, † Cited by third party
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

Patent Citations (4)

* Cited by examiner, † Cited by third party
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

Cited By (4)

* Cited by examiner, † Cited by third party
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
CN112820442A (en) * 2021-04-19 2021-05-18 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
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

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Inventor after: Ye Xiaoyu

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Address after: Hangzhou City, Zhejiang province 310000 Jianggan District Garden 4 Building 3 unit on Bridge

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Address before: 233122 Anhui city of Chuzhou province Fengyang County town south of Fuxi

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