CN104505144B - A kind of low-temperature conductive silver paste of heat generating component - Google Patents
A kind of low-temperature conductive silver paste of heat generating component Download PDFInfo
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- CN104505144B CN104505144B CN201410776839.4A CN201410776839A CN104505144B CN 104505144 B CN104505144 B CN 104505144B CN 201410776839 A CN201410776839 A CN 201410776839A CN 104505144 B CN104505144 B CN 104505144B
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Abstract
The invention discloses a kind of low-temperature conductive silver paste of heat generating component, it is made up of the raw material of following weight parts:High dispersive conductive silver powder 80 90, vinyl chloride vinyl acetate 15 17, dimethylformamide 20 25, cyclohexanone 35, dimethyl silicone polymer 0.3 1, BBP(Butyl Benzyl Phthalate 23, ammonium metaborate 0.1 0.2, potassium titanate 0.1 0.2, particle diameter is 10 15 μm of graphite powder 23, linolenic acid 0.6 1, dimethyl succinate 0.5 1, glass dust 10 12, polyethylene glycol 12, the nano-silver powder that the high dispersive conductive silver powder of the present invention is uniformly and is densely coated on the surface of polymer microsphere, the consumption of noble metal silver powder can not only be reduced, reduce production cost, the dispersiveness and stability of nano-silver powder are also substantially increased simultaneously.
Description
Technical field
The invention mainly relates to conductive silver paste field, more particularly to a kind of low-temperature conductive silver paste of heat generating component.
Background technology
Using main component of the metallic silver particles as silver paste in traditional conductive silver paste, its electric conductivity is also to come real by it
Existing, it is uniformly distributed in bonding agent, before printing, slurries is constituted the print material of certain viscosity, after printing, is made silver paste
Stable combination is formed between particulate and base material, but is due to that silver metal price is relatively expensive, it is possible to silver-colored cladding is considered as
Mode reduce the cost of metallic silver particles.
The content of the invention
The object of the invention is just to provide a kind of low-temperature conductive silver paste of heat generating component.
The present invention is achieved by the following technical solutions:
A kind of low-temperature conductive silver paste of heat generating component, it is characterised in that it is made up of the raw material of following weight parts:
High dispersive conductive silver powder 80-90, vinyl chloride vinyl acetate 15-17, dimethylformamide 20-25, cyclohexanone 3-5,
Dimethyl silicone polymer 0.3-1, BBP(Butyl Benzyl Phthalate 2-3, ammonium metaborate 0.1-0.2, potassium titanate 0.1-0.2, particle diameter are
10-15 μm of graphite powder 2-3, linolenic acid 0.6-1, dimethyl succinate 0.5-1, glass dust 10-12, polyethylene glycol 1-2;
What described high dispersive conductive silver powder was made up of the raw material of following weight parts:
Nano aluminium oxide 5-10, di-n-octyl sebacate 0.1-0.2, deionized water 300-400, styrene 4-7, alkyl phenol gather
Oxygen vinethene 0.8-1, silane coupler KH560 1-2, ammonium persulfate 0.01-0.02, silver nitrate 131-140, polyvinyl pyrrole
Alkanone 1-2, sodium hypophosphite 30-40, three (nonyl phenyl) phosphite 2-3;
Nano aluminium oxide, di-n-octyl sebacate, silane coupler KH560 are mixed, 500-700 revs/min of stirring mixing 20-
30 minutes, addition styrene, APES, the 30-35% of deionized water weight, magnetic agitation 40-50 minutes, plus
Enter ammonium persulfate, ultrasonic oscillation 10-15h obtains nanoemulsions;
Silver nitrate, polyvinylpyrrolidone are mixed, the 40-50% of remaining deionized water weight is added, stirs,
Obtain oxidation solution;
Remaining each raw material is mixed, ammoniacal liquor is added dropwise, regulation PH is 10-10.5, is reducing solution;
Above-mentioned oxidation solution is added drop-wise in reducing solution, nanoemulsions are added after completion of dropping, stirring reaction 30-50 minutes,
Centrifuge, washed 3-5 times with deionized water and ethanol, dry, produce.
A kind of preparation method of the low-temperature conductive silver paste of heat generating component, it is characterised in that comprise the following steps:
(1)Ammonium metaborate, linolenic acid are mixed, BBP(Butyl Benzyl Phthalate is stirring evenly and then adding into, at 60-65 DEG C
Insulated and stirred 3-5 minutes, obtains esterification dispersant;
(2)In the mixed liquor that vinyl chloride vinyl acetate is added to dimethylformamide and cyclohexanone, add after stirring
Enter to be esterified dispersant, stirring mixing 10-20 minutes, obtain organic carrier at 70-75 DEG C;
(3)Dimethyl succinate, polyethylene glycol are mixed, insulated and stirred 4-6 minutes at 50-60 DEG C adds poly dimethyl
Siloxanes, stirs to normal temperature, obtains activating agent;
(4)High dispersive conductive silver powder is added in organic carrier, is well mixed, activating agent and remaining each raw material is added,
It is scattered at a high speed, mixed on feeding three-roll grinder, ground slurry granularity is got product to 8-15 microns.
It is an advantage of the invention that:
The high dispersive conductive silver powder of the present invention is the surface that nano-silver powder uniformly and is densely coated on to polymer microsphere,
Can not only reduce the consumption of noble metal silver powder, reduce production cost, at the same also substantially increase nano-silver powder dispersiveness and
Stability;
The organic carrier of the present invention, the processing through over-churning dispersant can effectively improve slurry viscosity, obtained
Slurry is more stable, prevented from caking, precipitation and layering, reduces the baking temperature of silver paste, improves adhesive force;
The activating agent of addition can effectively improve the electric conductivity of silver paste, improve the printing quality of silver paste.
Embodiment
Embodiment 1
A kind of low-temperature conductive silver paste of heat generating component, it is characterised in that it is made up of the raw material of following weight parts:
High dispersive conductive silver powder 90, vinyl chloride vinyl acetate 17, dimethylformamide 25, cyclohexanone 5, polydimethylsiloxanes
Graphite powder 3, the linolenic acid of alkane 0.3, BBP(Butyl Benzyl Phthalate 3, ammonium metaborate 0.2, potassium titanate 0.2, particle diameter for 15 μm
0.6th, dimethyl succinate 0.5, glass dust 12, polyethylene glycol 2;
What described high dispersive conductive silver powder was made up of the raw material of following weight parts:
Nano aluminium oxide 10, di-n-octyl sebacate 0.2, deionized water 400, styrene 7, APES 0.8,
Silane coupler KH560 2, ammonium persulfate 0.02, silver nitrate 140, polyvinylpyrrolidone 1, sodium hypophosphite 40, three (nonylbenzenes
Base) phosphite 3;
Nano aluminium oxide, di-n-octyl sebacate, silane coupler KH560 are mixed, 700 revs/min of stirrings are mixed 30 minutes,
Styrene, APES, the 35% of deionized water weight are added, magnetic agitation 50 minutes adds ammonium persulfate, surpassed
Sound wave shock 10-15h, obtains nanoemulsions;
Silver nitrate, polyvinylpyrrolidone are mixed, the 50% of remaining deionized water weight is added, stirs, obtain oxygen
Change liquid;
Remaining each raw material is mixed, ammoniacal liquor is added dropwise, regulation PH is 10.5, is reducing solution;
Above-mentioned oxidation solution is added drop-wise in reducing solution, nanoemulsions, stirring reaction 50 minutes, centrifugation are added after completion of dropping
Separation, is washed 3 times with deionized water and ethanol, is dried, is produced.
A kind of preparation method of the low-temperature conductive silver paste of heat generating component, it is characterised in that comprise the following steps:
(1)Ammonium metaborate, linolenic acid are mixed, BBP(Butyl Benzyl Phthalate is stirring evenly and then adding into, protected at 65 DEG C
Temperature stirring 3 minutes, obtains esterification dispersant;
(2)In the mixed liquor that vinyl chloride vinyl acetate is added to dimethylformamide and cyclohexanone, add after stirring
Enter to be esterified dispersant, stirring mixing 20 minutes, obtain organic carrier at 75 DEG C;
(3)Dimethyl succinate, polyethylene glycol are mixed, insulated and stirred 4 minutes at 60 DEG C adds polydimethylsiloxanes
Alkane, stirs to normal temperature, obtains activating agent;
(4)High dispersive conductive silver powder is added in organic carrier, is well mixed, activating agent and remaining each raw material is added,
It is scattered at a high speed, mixed on feeding three-roll grinder, ground slurry granularity is got product to 8-15 microns.
Performance test:
Without lump, in uniform state after stirring;
Fineness≤15 μm;
Adhesive force 4.7B;
Hardness 1.2H.
Claims (1)
1. a kind of low-temperature conductive silver paste of heat generating component, it is characterised in that it is prepared from by the raw material of following weight parts:
High dispersive conductive silver powder 80-90, vinyl chloride vinyl acetate 15-17, dimethylformamide 20-25, cyclohexanone 3-5, poly- two
Methylsiloxane 0.3-1, BBP(Butyl Benzyl Phthalate 2-3, ammonium metaborate 0.1-0.2, potassium titanate 0.1-0.2, particle diameter are 10-15
μm graphite powder 2-3, linolenic acid 0.6-1, dimethyl succinate 0.5-1, glass dust 10-12, polyethylene glycol 1-2;
Described high dispersive conductive silver powder is prepared from by the raw material of following weight parts:Nano aluminium oxide 5-10, decanedioic acid
Dioctyl ester 0.1-0.2, deionized water 300-400, styrene 4-7, APES 0.8-1, silane coupler KH560
1-2, ammonium persulfate 0.01-0.02, silver nitrate 131-140, polyvinylpyrrolidone 1-2, sodium hypophosphite 30-40, three (nonylbenzenes
Base) phosphite 2-3;
Nano aluminium oxide, di-n-octyl sebacate, silane coupler KH560 are mixed, 500-700 revs/min of 20-30 points of stirring mixing
Clock, adds styrene, APES, the 30-35% of deionized water weight, and magnetic agitation 40-50 minutes was added
Ammonium sulfate, ultrasonic oscillation 10-15h, obtains nanoemulsions;
Silver nitrate, polyvinylpyrrolidone are mixed, the 40-50% of remaining deionized water weight is added, stirs, obtain oxygen
Change liquid;
Remaining each raw material is mixed, ammoniacal liquor is added dropwise, regulation pH is 10-10.5, is reducing solution;
Above-mentioned oxidation solution is added drop-wise in reducing solution, nanoemulsions, stirring reaction 30-50 minutes, centrifugation are added after completion of dropping
Separation, is washed 3-5 times with deionized water and ethanol, is dried, is produced;
The preparation method of the low-temperature conductive silver paste of described heat generating component, comprises the following steps:
(1)Ammonium metaborate, linolenic acid are mixed, BBP(Butyl Benzyl Phthalate is stirring evenly and then adding into, is incubated at 60-65 DEG C
Stirring 3-5 minutes, obtains esterification dispersant;
(2)In the mixed liquor that vinyl chloride vinyl acetate is added to dimethylformamide and cyclohexanone, ester is stirring evenly and then adding into
Change dispersant, stirring mixing 10-20 minutes, obtain organic carrier at 70-75 DEG C;
(3)Dimethyl succinate, polyethylene glycol are mixed, insulated and stirred 4-6 minutes at 50-60 DEG C adds polydimethylsiloxanes
Alkane, stirs to normal temperature, obtains activating agent;
(4)High dispersive conductive silver powder is added in organic carrier, is well mixed, activating agent and remaining each raw material is added, at a high speed
It is scattered, mixed on feeding three-roll grinder, ground slurry granularity is got product to 8-15 microns.
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Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN1785558A (en) * | 2005-11-21 | 2006-06-14 | 东南大学 | Preparation method of micron grade ball shape silver powder for conductive silver paste |
CN1870180A (en) * | 2006-06-28 | 2006-11-29 | 华东微电子技术研究所合肥圣达实业公司 | Environment pretection leadless surface silver coating for PTC ceramic and its preparation method |
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US7718092B2 (en) * | 2005-10-11 | 2010-05-18 | E.I. Du Pont De Nemours And Company | Aluminum thick film composition(s), electrode(s), semiconductor device(s) and methods of making thereof |
JP4737249B2 (en) * | 2008-08-12 | 2011-07-27 | ソニー株式会社 | Thin film manufacturing method and apparatus, and electronic device manufacturing method |
CN103379973A (en) * | 2011-03-31 | 2013-10-30 | 户田工业株式会社 | Silver-coated copper powder and method for producing same, silver-coated copper powder-containing conductive paste, conductive adhesive agent, conductive film, and electric circuit |
CN104078102A (en) * | 2014-06-30 | 2014-10-01 | 合肥中南光电有限公司 | Modified nanometer carbon conductive silver paste and preparation method thereof |
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Patent Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
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CN1785558A (en) * | 2005-11-21 | 2006-06-14 | 东南大学 | Preparation method of micron grade ball shape silver powder for conductive silver paste |
CN1870180A (en) * | 2006-06-28 | 2006-11-29 | 华东微电子技术研究所合肥圣达实业公司 | Environment pretection leadless surface silver coating for PTC ceramic and its preparation method |
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