CN104538084A - High-temperature-resistant electric conducting silver paste - Google Patents
High-temperature-resistant electric conducting silver paste Download PDFInfo
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- CN104538084A CN104538084A CN201510007837.3A CN201510007837A CN104538084A CN 104538084 A CN104538084 A CN 104538084A CN 201510007837 A CN201510007837 A CN 201510007837A CN 104538084 A CN104538084 A CN 104538084A
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- silver
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Abstract
The invention discloses high-temperature-resistant electric conducting silver paste. The silver paste is prepared from, by weight, 45 parts of silver powder of 10-20 micrometers, 20 parts of modified glass powder, 0.5 part of nanometer carbon, 2 parts of 1-4-Butanediol, 3.5 parts of nickel powder of 10-20 nm, 0.4-0.6 part of silver acetate, 0.2-0.4 part of silver benzoate, 0.1-0.2 part of phosphotriester, 0.1-0.3 part of dibutyltin dilaurate, 0.6-0.8 part of epoxidized soybean oil, 25-33 parts of styrene, 4.5-8.5 parts of novolac epoxy, 0.5-2 parts of rosin, 0.5-1 part of stearic acid and 2-3 parts of silane coupling agent KH602. The glass powder is modified, an organic carrier is compounded, and therefore the silver paste is good in electrical conductivity, abrasion resistance and high-temperature resistance.
Description
Technical field
The invention belongs to conductive silver paste field, particularly relate to a kind of high temperature resistant 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 temperature resistant conductive silver paste.
The present invention adopts following technical scheme to achieve these goals:
A kind of high temperature resistant conductive silver paste, it is characterized in that, it is obtained by the raw material of following weight parts:
10-20 μm of silver powder 42-55, modified glass powder 15-20, nano-sized carbon 0.3-0.5,1.4-butanediol 1-2,10-20nm nickel powder 3-5, silver acetate 0.4-0.6, silver benzoate 0.2-0.4, phosphotriester 0.1-0.2, dibutyl tin laurate 0.1-0.3, epoxidized soybean oil 0.6-0.8, styrene 25-33, novolac epoxy resin 4.5-8.5, rosin 0.5-2, stearic acid 0.5-1, silane coupler KH602 2-3;
Modified glass powder is obtained by the raw material of following weight parts: nano silicon 15-20, PbO 5-7, SnO 2-4, CuO 8-10, P
2o
51-3, Bi
2o
37-10, SrO1-5, 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) 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 1-5 μm of glass dust;
(3) glass dust and modification liquid are mixed, at 30-50 DEG C, stir 30-40 minute, leave standstill 15-18 hour, suction filtration is dry, to obtain final product.
Described one is high temperature resistant conductive silver paste, is characterized in that: preparation method comprises the following steps:
(1) by nano-sized carbon, 1.4-butanediol, silver acetate, silver benzoate, phosphotriester, dibutyl tin laurate, epoxidized soybean oil, styrene, novolac epoxy resin, rosin, after stearic acid, silane coupler KH602 mixing, obtains 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, is ground to slurry fineness and is less than 10 μm, and adjust viscosity, viscosity is 120-150Pas.
Beneficial effect of the present invention:
Conductive silver paste of the present invention passes through glass dust modification, and composite organic carrier, makes conductivity of the present invention good, wear-resisting, high temperature resistant.
Embodiment
A kind of high temperature resistant conductive silver paste, it is obtained by the raw material of following weight (kg):
10-20 μm of silver powder 45, modified glass powder 20, nano-sized carbon 0.5,1.4-butanediol 2,10-20nm nickel powder 3.5, silver acetate 0.4, silver benzoate 0.4, phosphotriester 0.2, dibutyl tin laurate 0.1, epoxidized soybean oil 0.6, styrene 28, novolac epoxy resin 7.5, rosin 2, stearic acid 0.5, silane coupler KH602 2;
Modified glass powder is obtained by the raw material of following weight (kg): nano silicon 18, PbO 5, SnO 2, CuO 10, P
2o
51, Bi
2o
37, SrO
4, sodium aluminate 1, Tissuemat E 2, chlorinated paraffin wax 1, sodium alkyl benzene sulfonate 2, sodium metasilicate 3, turkey red oil 0.1, sodium hydrogensulfite 1, lecithin 1, 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 200rpm, obtain modification liquid;
(2) all the other raw material blendings sintering, sintering temperature is 1400 DEG C, and the time is 1 hour, obtains glass melt quenching, ball milling, drying, and sieve to obtain 1-5 μm of glass dust;
(3) glass dust and modification liquid are mixed, stir 40 minutes at 40 DEG C, leave standstill 15 hours, suction filtration is dry, to obtain final product.
Described one is high temperature resistant conductive silver paste, preparation method comprises the following steps:
(1) by nano-sized carbon, 1.4-butanediol, silver acetate, silver benzoate, phosphotriester, dibutyl tin laurate, epoxidized soybean oil, styrene, novolac epoxy resin, rosin, after stearic acid, silane coupler KH602 mixing, 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 2 hours, obtain slurry;
(3) slurry ball milling, is ground to slurry fineness and is less than 10 μm, and adjust viscosity, viscosity is 120-150Pas.
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 12.8N/cm, soldering is functional, sheet resistance < 10 Siements/sq, the solar cell photoelectric transformation efficiency of preparation is 21.9%, and tensile test result is adhesive force >13.2N/mm
2.
Claims (2)
1. a high temperature resistant conductive silver paste, is characterized in that, it is obtained by the raw material of following weight parts:
10-20 μm of silver powder 42-55, modified glass powder 15-20, nano-sized carbon 0.3-0.5,1.4-butanediol 1-2,10-20nm nickel powder 3-5, silver acetate 0.4-0.6, silver benzoate 0.2-0.4, phosphotriester 0.1-0.2, dibutyl tin laurate 0.1-0.3, epoxidized soybean oil 0.6-0.8, styrene 25-33, novolac epoxy resin 4.5-8.5, rosin 0.5-2, stearic acid 0.5-1, silane coupler KH602 2-3;
Modified glass powder is obtained by the raw material of following weight parts: nano silicon 15-20, PbO 5-7, SnO 2-4, CuO 8-10, P
2o
51-3, Bi
2o
37-10, SrO1-5, 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) 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 1-5 μm of glass dust;
(3) glass dust and modification liquid are mixed, at 30-50 DEG C, stir 30-40 minute, leave standstill 15-18 hour, suction filtration is dry, to obtain final product.
2. the high temperature resistant conductive silver paste of one according to claim 1, is characterized in that: preparation method comprises the following steps:
(1) by nano-sized carbon, 1.4-butanediol, silver acetate, silver benzoate, phosphotriester, dibutyl tin laurate, epoxidized soybean oil, styrene, novolac epoxy resin, rosin, after stearic acid, silane coupler KH602 mixing, obtains 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, is ground to slurry fineness and is less than 10 μm, and adjust viscosity, viscosity is 120-150Pas.
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CN201510007837.3A CN104538084A (en) | 2015-01-08 | 2015-01-08 | High-temperature-resistant electric conducting silver paste |
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CN201510007837.3A CN104538084A (en) | 2015-01-08 | 2015-01-08 | High-temperature-resistant electric conducting silver paste |
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Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN104934096A (en) * | 2015-05-25 | 2015-09-23 | 铜陵宏正网络科技有限公司 | Environment-friendly circuit board conductive silver paste and preparation method thereof |
CN106028640A (en) * | 2016-06-15 | 2016-10-12 | 杭州升达电子有限公司 | Dual-layer through hole printed circuit board with silver paste through holes and manufacturing technology of dual-layer through hole printed circuit board |
CN106971769A (en) * | 2017-04-10 | 2017-07-21 | 台山市都斛亚美化工有限公司 | A kind of high-temperature electric conduction silver paste |
CN109686498A (en) * | 2018-12-25 | 2019-04-26 | 深圳市欧科力科技有限公司 | A kind of preparation method of photoactive electrode slurry |
WO2020009200A1 (en) * | 2018-07-06 | 2020-01-09 | Hitachi Chemical Company, Ltd. | Print-on pastes with metal-based additives for modifying material properties of metal particle layers |
Citations (3)
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JPS5333752B1 (en) * | 1966-11-12 | 1978-09-16 | ||
CN102015884A (en) * | 2008-04-21 | 2011-04-13 | 三键株式会社 | Conductive resin composition |
CN103021570A (en) * | 2012-12-18 | 2013-04-03 | 安徽金大仪器有限公司 | Method for preparing conductive paste containing rosin resin |
-
2015
- 2015-01-08 CN CN201510007837.3A patent/CN104538084A/en active Pending
Patent Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPS5333752B1 (en) * | 1966-11-12 | 1978-09-16 | ||
CN102015884A (en) * | 2008-04-21 | 2011-04-13 | 三键株式会社 | Conductive resin composition |
CN103021570A (en) * | 2012-12-18 | 2013-04-03 | 安徽金大仪器有限公司 | Method for preparing conductive paste containing rosin resin |
Cited By (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN104934096A (en) * | 2015-05-25 | 2015-09-23 | 铜陵宏正网络科技有限公司 | Environment-friendly circuit board conductive silver paste and preparation method thereof |
CN106028640A (en) * | 2016-06-15 | 2016-10-12 | 杭州升达电子有限公司 | Dual-layer through hole printed circuit board with silver paste through holes and manufacturing technology of dual-layer through hole printed circuit board |
CN106028640B (en) * | 2016-06-15 | 2018-09-18 | 杭州升达电子有限公司 | A kind of silver paste hole filled double-deck perforation printed wiring board and its manufacturing process |
CN106971769A (en) * | 2017-04-10 | 2017-07-21 | 台山市都斛亚美化工有限公司 | A kind of high-temperature electric conduction silver paste |
WO2020009200A1 (en) * | 2018-07-06 | 2020-01-09 | Hitachi Chemical Company, Ltd. | Print-on pastes with metal-based additives for modifying material properties of metal particle layers |
CN109686498A (en) * | 2018-12-25 | 2019-04-26 | 深圳市欧科力科技有限公司 | A kind of preparation method of photoactive electrode slurry |
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Application publication date: 20150422 |