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.