CN104575676A - Low-temperature electric conduction silver paste - Google Patents
Low-temperature electric conduction silver paste Download PDFInfo
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- CN104575676A CN104575676A CN201410809756.0A CN201410809756A CN104575676A CN 104575676 A CN104575676 A CN 104575676A CN 201410809756 A CN201410809756 A CN 201410809756A CN 104575676 A CN104575676 A CN 104575676A
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Abstract
The invention discloses a low-temperature electric conduction silver paste. The silver paste consists of the following raw materials in parts by weight: 80-90 parts of cladding silver powder, 6-10 parts of ethyl cellulose, 6-8 parts of methyl cellulose, 10-13 parts of ethylene glycol butyl ether, 10-12 parts of carbitol, 0.1-0.2 part of a phenol-4-sulfonic acid solution, 0.5-1 part of polyoxyethylene poly propylene propylene alcohol ether, 0.6-1 part of titanium nitride, 0.8-1 part of polyethylene, 0.4-1 part of gluconolactone, 1-2 parts of sa-hao seed gum, 10-13 parts of lead-free glass powder, 1-2 parts of alumina, 0.2-0.3 part of a methyl silicone oil, and 2-3 parts of butyl benzyl phthalate. The cladding silver powder is obtained by enabling nanometer silver powder to be uniformly and compactly clad to the surfaces of macromolecular microspheres, so that not only can the consumption of noble metal silver powder be reduced and the production cost be lowered, but also the dispersibility and the stability of the nanometer silver powder are greatly improved.
Description
Technical field
The present invention relates generally to conductive silver paste field, particularly relates to a kind of low-temperature conductive silver paste.
Background technology
Conductive silver slurry refers to and is printed on conduction stock, and making it the silver slurry having conduction current and get rid of accumulate static charge ability, is generally be imprinted on the non-conductive stocks such as plastics, glass, pottery or cardboard.Printing process is very wide, as silk screen printing, letterpress, flexographic printing, intaglio printing and offset printing etc. all can adopt.Then resistance, Solder resistance and rub resistance etc. are also different can to select different printing processes, thickness difference according to the requirement of thickness.This silver slurry has thick film mill base and resin type two kinds.The former is that the high temperature of binder burns till type with frit, the latter take synthetic resin as the low temperature drying of binder or the silk screen silver slurry of radiation-curable, and in conductive filler conductivity it is preferred that silver powder and copper powder, but cost is relatively high, therefore find through experiment, adopt silver-colored coated particle just can to effectively reduce cost as conductive filler, and its conductivity is had no significant effect.
Summary of the invention
The object of the invention is just to provide a kind of low-temperature conductive silver paste.
The present invention is achieved by the following technical solutions:
A kind of low-temperature conductive silver paste, is characterized in that what it was made up of the raw material of following weight parts:
Coated silver powder 80-90, ethyl cellulose 6-10, methylcellulose 6-8, ethylene glycol monobutyl ether 10-13, carbitol 10-12, p-hydroxybenzenyl sulfonate 0.1-0.2, polyoxyethylene polyoxypropylene propylene glycol 0.5-1, titanium nitride 0.6-1, poly-adipate glycol 0.8-1, gluconolactone 0.4-1, Artemisia Glue 1-2, lead-free glass powder 10-13, aluminium oxide 1-2, methyl-silicone oil 0.2-0.3, phthalandione butyl benzyl ester 2-3;
Described coated silver powder is made up of the raw material of following weight parts:
Nano-sized iron oxide 4-6, lanthanum sulfate 0.1-0.2, deionized water 300-400, butyl acrylate 10-13, sodium carboxymethylcellulose 0.9-2, silane coupler KH560 0.06-0.1, benzoyl peroxide 0.01-0.02, ascorbic acid 45-60, locust bean gum 1-2, sodium tetraborate 0.1-0.14, silver nitrate 100-110;
By nano-sized iron oxide, butyl acrylate mixing, add 31-35%, the sodium carboxymethylcellulose of above-mentioned deionized water weight, benzoyl peroxide is added after stirring, reaction 6-10 hour is left standstill at 70-90 DEG C, add lanthanum sulfate, silane coupler KH560, magnetic agitation 10-15 minute, obtains nanoemulsions;
By locust bean gum, sodium tetraborate mixing, add the 20-30% of residue deionized water weight, drip ammoniacal liquor, adjustment PH is 6.8-7, adds ascorbic acid, stirs, obtain reducing solution;
The mixing of each raw material will be remained, stir, obtain oxidation solution;
Above-mentioned oxidation solution is added drop-wise in reducing solution, nanoemulsions is added after dropwising, rotating speed be 1200-1500rmp, temperature be 20-25 DEG C at dispersed with stirring 25-30 minute, after sedimentation 1-2 hour, supernatant is gone to get its sediment, wash 3-5 time with deionized water and ethanol, dry, abrasive dust.
The preparation method of described low-temperature conductive silver paste, comprises the following steps:
(1) ethyl cellulose is joined in ethylene glycol monobutyl ether, stir; Methylcellulose is joined in carbitol, stir; By each raw material mixing after above-mentioned process, add phthalandione butyl benzyl ester, p-hydroxybenzenyl sulfonate, raised temperature is 75-80 DEG C, is uniformly mixed 10-13 minute, obtains organic carrier;
(2) Artemisia Glue is mixed with poly-adipate glycol, after stirring, add gluconolactone, at 50-60 DEG C, be uniformly mixed 7-10 minute, obtain dispersant;
(3) join in organic carrier by coated silver powder, mix, add above-mentioned dispersant and each raw material of residue, high speed dispersion, send on three-roll grinder and mix, ground slurry granularity, to 8-15 micron, gets product.
Advantage of the present invention is:
The nano-silver powder that coated silver powder of the present invention is evenly and is densely coated on the surface of polymer microsphere, not only can reduce the consumption of noble metal silver powder, reduce production cost, also substantially increase dispersiveness and the stability of nano-silver powder simultaneously, adopt the mixing of locust bean gum, sodium tetraborate as dispersant, viscosity is low, is convenient to washing and filtering, good dispersion, not easily forms reunion;
Dispersant of the present invention can effectively reduce reunion, and can not affect the conductivity of coated silver powder itself, conductive silver paste modest viscosity of the present invention, has high bending resistance folding endurance, high conductivity and superior meticulous printability, stable performance.
Embodiment
Embodiment 1
A kind of low-temperature conductive silver paste, is characterized in that what it was made up of the raw material of following weight parts:
Coated silver powder 80, ethyl cellulose 10, methylcellulose 6, ethylene glycol monobutyl ether 10, carbitol 10, p-hydroxybenzenyl sulfonate 0.2, polyoxyethylene polyoxypropylene propylene glycol 0.5, titanium nitride 0.6, poly-adipate glycol 0.8, gluconolactone 0.4, Artemisia Glue 1, lead-free glass powder 10, aluminium oxide 1, methyl-silicone oil 0.2, phthalandione butyl benzyl ester 2;
Described coated silver powder is made up of the raw material of following weight parts:
Nano-sized iron oxide 4, lanthanum sulfate 0.2, deionized water 300, butyl acrylate 10, sodium carboxymethylcellulose 0.9, silane coupler KH560 0.06, benzoyl peroxide 0.01, ascorbic acid 45, locust bean gum 1, sodium tetraborate 0.1, silver nitrate 100;
By nano-sized iron oxide, butyl acrylate mixing, add 31% of above-mentioned deionized water weight, sodium carboxymethylcellulose, after stirring, add benzoyl peroxide, reaction 6 hours are left standstill at 70 DEG C, add lanthanum sulfate, silane coupler KH560, magnetic agitation 10 minutes, obtains nanoemulsions;
By locust bean gum, sodium tetraborate mixing, add 20% of residue deionized water weight, drip ammoniacal liquor, regulate PH to be 6.8, add ascorbic acid, stir, obtain reducing solution;
The mixing of each raw material will be remained, stir, obtain oxidation solution;
Above-mentioned oxidation solution is added drop-wise in reducing solution, add nanoemulsions after dropwising, rotating speed be 1200rmp, temperature be 20 DEG C at dispersed with stirring 25 minutes, supernatant goes after 1 hour to get its sediment by sedimentation, 3 times are washed, dry, abrasive dust with deionized water and ethanol.
The preparation method of described low-temperature conductive silver paste, comprises the following steps:
(1) ethyl cellulose is joined in ethylene glycol monobutyl ether, stir; Methylcellulose is joined in carbitol, stir; By each raw material mixing after above-mentioned process, add phthalandione butyl benzyl ester, p-hydroxybenzenyl sulfonate, raised temperature is 75 DEG C, is uniformly mixed 10 minutes, obtains organic carrier;
(2) Artemisia Glue is mixed with poly-adipate glycol, after stirring, add gluconolactone, at 50 DEG C, be uniformly mixed 7 minutes, obtain dispersant;
(3) join in organic carrier by coated silver powder, mix, add above-mentioned dispersant and each raw material of residue, high speed dispersion, send on three-roll grinder and mix, ground slurry granularity to 15 micron, gets product.
Performance test:
Without lump, in uniform state after stirring;
Fineness≤15 μm;
Adhesive force 4.7B;
Hardness 1H.
Claims (2)
1. a low-temperature conductive silver paste, is characterized in that what it was made up of the raw material of following weight parts:
Coated silver powder 80-90, ethyl cellulose 6-10, methylcellulose 6-8, ethylene glycol monobutyl ether 10-13, carbitol 10-12, p-hydroxybenzenyl sulfonate 0.1-0.2, polyoxyethylene polyoxypropylene propylene glycol 0.5-1, titanium nitride 0.6-1, poly-adipate glycol 0.8-1, gluconolactone 0.4-1, Artemisia Glue 1-2, lead-free glass powder 10-13, aluminium oxide 1-2, methyl-silicone oil 0.2-0.3, phthalandione butyl benzyl ester 2-3;
Described coated silver powder is made up of the raw material of following weight parts:
Nano-sized iron oxide 4-6, lanthanum sulfate 0.1-0.2, deionized water 300-400, butyl acrylate 10-13, sodium carboxymethylcellulose 0.9-2, silane coupler KH560 0.06-0.1, benzoyl peroxide 0.01-0.02, ascorbic acid 45-60, locust bean gum 1-2, sodium tetraborate 0.1-0.14, silver nitrate 100-110;
By nano-sized iron oxide, butyl acrylate mixing, add 31-35%, the sodium carboxymethylcellulose of above-mentioned deionized water weight, benzoyl peroxide is added after stirring, reaction 6-10 hour is left standstill at 70-90 DEG C, add lanthanum sulfate, silane coupler KH560, magnetic agitation 10-15 minute, obtains nanoemulsions;
By locust bean gum, sodium tetraborate mixing, add the 20-30% of residue deionized water weight, drip ammoniacal liquor, adjustment PH is 6.8-7, adds ascorbic acid, stirs, obtain reducing solution;
The mixing of each raw material will be remained, stir, obtain oxidation solution;
Above-mentioned oxidation solution is added drop-wise in reducing solution, nanoemulsions is added after dropwising, rotating speed be 1200-1500rmp, temperature be 20-25 DEG C at dispersed with stirring 25-30 minute, after sedimentation 1-2 hour, supernatant is gone to get its sediment, wash 3-5 time with deionized water and ethanol, dry, abrasive dust.
2. a preparation method for low-temperature conductive silver paste as claimed in claim 1, is characterized in that comprising the following steps:
(1) ethyl cellulose is joined in ethylene glycol monobutyl ether, stir; Methylcellulose is joined in carbitol, stir; By each raw material mixing after above-mentioned process, add phthalandione butyl benzyl ester, p-hydroxybenzenyl sulfonate, raised temperature is 75-80 DEG C, is uniformly mixed 10-13 minute, obtains organic carrier;
(2) Artemisia Glue is mixed with poly-adipate glycol, after stirring, add gluconolactone, at 50-60 DEG C, be uniformly mixed 7-10 minute, obtain dispersant;
(3) join in organic carrier by coated silver powder, mix, add above-mentioned dispersant and each raw material of residue, high speed dispersion, send on three-roll grinder and mix, ground slurry granularity, to 8-15 micron, gets product.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201410809756.0A CN104575676A (en) | 2014-12-23 | 2014-12-23 | Low-temperature electric conduction silver paste |
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| CN201410809756.0A CN104575676A (en) | 2014-12-23 | 2014-12-23 | Low-temperature electric conduction silver paste |
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| CN104575676A true CN104575676A (en) | 2015-04-29 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106024100A (en) * | 2016-07-20 | 2016-10-12 | 苏州顾氏新材料有限公司 | Low-temperature conductive silver paste and preparation method and application thereof |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH01107592A (en) * | 1987-10-20 | 1989-04-25 | Tanaka Massey Kk | Electric circuit board |
| CN101473386A (en) * | 2006-06-22 | 2009-07-01 | 三菱制纸株式会社 | Method for producing conductive material |
| CN102592706A (en) * | 2012-03-16 | 2012-07-18 | 上海交通大学 | Solar cell anode silver paste and preparation method thereof |
| CN103000250A (en) * | 2012-11-07 | 2013-03-27 | 宁波广博纳米新材料股份有限公司 | Back silver paste for low-silver-content crystalline silicon solar battery and preparation method thereof |
| CN103192074A (en) * | 2013-04-10 | 2013-07-10 | 张宇 | Highly dispersed sliver powder and conductive silver paste for film batteries |
| CN103537708A (en) * | 2013-09-09 | 2014-01-29 | 烟台同立高科新材料股份有限公司 | Hyperpure silver powder for solar cell conductive silver paste and preparing method of hyperpure silver powder |
-
2014
- 2014-12-23 CN CN201410809756.0A patent/CN104575676A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH01107592A (en) * | 1987-10-20 | 1989-04-25 | Tanaka Massey Kk | Electric circuit board |
| CN101473386A (en) * | 2006-06-22 | 2009-07-01 | 三菱制纸株式会社 | Method for producing conductive material |
| CN102592706A (en) * | 2012-03-16 | 2012-07-18 | 上海交通大学 | Solar cell anode silver paste and preparation method thereof |
| CN103000250A (en) * | 2012-11-07 | 2013-03-27 | 宁波广博纳米新材料股份有限公司 | Back silver paste for low-silver-content crystalline silicon solar battery and preparation method thereof |
| CN103192074A (en) * | 2013-04-10 | 2013-07-10 | 张宇 | Highly dispersed sliver powder and conductive silver paste for film batteries |
| CN103537708A (en) * | 2013-09-09 | 2014-01-29 | 烟台同立高科新材料股份有限公司 | Hyperpure silver powder for solar cell conductive silver paste and preparing method of hyperpure silver powder |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106024100A (en) * | 2016-07-20 | 2016-10-12 | 苏州顾氏新材料有限公司 | Low-temperature conductive silver paste and preparation method and application thereof |
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Application publication date: 20150429 |