CN104575664A - Electric conduction silver paste with high adhesive force - Google Patents

Abstract

The invention discloses an electric conduction silver paste with high adhesive force. The silver paste consists of the following raw materials in parts by weight: 92-100 parts of cladding silver powder, 0.1-0.3 part of a nitrilotriacetic acid, 0.4-1 part of ferrous ammonium sulfate, 0.1-0.2 part of titanium nitride, 2-3 parts of graphite powder, 0.1-0.2 part of boron nitride, 1-2 parts of 2-butoxyethanol, 14-20 parts of polyamide, 2-3 parts of dibutyl maleate, 30-34 parts of 2(2-Ethoxyethoxy)ethanol acetic ester, 0.2-0.4 part of calcium aluminate, 0.1-0.2 part of hexafluoro- acetylacetone, and 10-13 parts of lead-free glass powder. The cladding silver powder is obtained by enabling nanometer silver powder to be uniformly and compactly cladded to the surfaces of macromolecular microspheres, so that the consumption of noble metal silver powder can be reduced, the production cost is reduced, and meanwhile the dispersibility and the stability of the nanometer silver powder are greatly improved.

Description

A kind of conductive silver paste of high adhesion force

Technical field

The present invention relates generally to conductive silver paste field, particularly relates to a kind of conductive silver paste of high adhesion force.

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 its conductivity is had no significant effect.

Summary of the invention

The object of the invention is just to provide a kind of conductive silver paste of high adhesion force.

The present invention is achieved by the following technical solutions:

A conductive silver paste for high adhesion force, is characterized in that what it was made up of the raw material of following weight parts:

Coated silver powder 92-100, NTA 0.1-0.3, iron ammonium sulfate 0.4-1, titanium nitride 0.1-0.2, graphite powder 2-3, boron nitride 0.1-0.2, butoxy ethanol 1-2, polyamide 14-20, dibutyl maleate 2-3, diethylene glycol ether acetate 30-34, calcium aluminate 0.2-0.4, hexafluoroacetylacetone 0.1-0.2, lead-free glass powder 10-13;

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 the conductive silver paste of described high adhesion force, is characterized in that comprising the following steps:

(1) joined in diethylene glycol ether acetate by polyamide, add dibutyl maleate after stirring, insulated and stirred 6-10 minute at 80-84 DEG C, obtains organic carrier;

(2) by titanium nitride, boron nitride, graphite powder mixing, add calcium aluminate, insulated and stirred 6-10 minute at 80-90 DEG C, adds lead-free glass powder, stirs, and obtains inorganic bond auxiliary agent;

(3) join in organic carrier by coated silver powder, mix, add inorganic bond auxiliary agent 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;

Conductive silver paste adhesive force of the present invention is good, and 3M600 adhesive tape vertically draws not dry linting, and the inorganic bond auxiliary agent added effectively can improve the resistance to fracture of silver slurry mold layer, and improve oxidation resistance, conductivity is good.

Embodiment

Embodiment 1

A conductive silver paste for high adhesion force, is characterized in that what it was made up of the raw material of following weight parts:

Coated silver powder 92, NTA 0.1, iron ammonium sulfate 0.4, titanium nitride 0.1, graphite powder 2, boron nitride 0.1, butoxy ethanol 1, polyamide 14, dibutyl maleate 2, diethylene glycol ether acetate 30, calcium aluminate 0.2, hexafluoroacetylacetone 0.1, lead-free glass powder 10;

Described coated silver powder is made up of the raw material of following weight parts:

Nano-sized iron oxide 4, lanthanum sulfate 0.1, deionized water 400, 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 35% of above-mentioned deionized water weight, sodium carboxymethylcellulose, after stirring, add benzoyl peroxide, reaction 10 hours are left standstill at 90 DEG C, add lanthanum sulfate, silane coupler KH560, magnetic agitation 15 minutes, obtains nanoemulsions;

By locust bean gum, sodium tetraborate mixing, add 30% 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 the conductive silver paste of described high adhesion force, comprises the following steps:

(1) joined in diethylene glycol ether acetate by polyamide, add dibutyl maleate after stirring, at 80 DEG C, insulated and stirred 6 minutes, obtains organic carrier;

(2) by titanium nitride, boron nitride, graphite powder mixing, add calcium aluminate, at 90 DEG C, insulated and stirred 10 minutes, adds lead-free glass powder, stirs, and obtains inorganic bond auxiliary agent;

(3) join in organic carrier by coated silver powder, mix, add inorganic bond auxiliary agent 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 5B;

Hardness 1H.

Claims (2)

1. a conductive silver paste for high adhesion force, is characterized in that what it was made up of the raw material of following weight parts:

Coated silver powder 92-100, NTA 0.1-0.3, iron ammonium sulfate 0.4-1, titanium nitride 0.1-0.2, graphite powder 2-3, boron nitride 0.1-0.2, butoxy ethanol 1-2, polyamide 14-20, dibutyl maleate 2-3, diethylene glycol ether acetate 30-34, calcium aluminate 0.2-0.4, hexafluoroacetylacetone 0.1-0.2, lead-free glass powder 10-13;

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 the conductive silver paste of high adhesion force as claimed in claim 1, is characterized in that comprising the following steps:

(1) joined in diethylene glycol ether acetate by polyamide, add dibutyl maleate after stirring, insulated and stirred 6-10 minute at 80-84 DEG C, obtains organic carrier;

(2) by titanium nitride, boron nitride, graphite powder mixing, add calcium aluminate, insulated and stirred 6-10 minute at 80-90 DEG C, adds lead-free glass powder, stirs, and obtains inorganic bond auxiliary agent;

(3) join in organic carrier by coated silver powder, mix, add inorganic bond auxiliary agent 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.