CN104505140B - A kind of conductive silver paste of effective thickening - Google Patents
A kind of conductive silver paste of effective thickening Download PDFInfo
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- CN104505140B CN104505140B CN201410775486.6A CN201410775486A CN104505140B CN 104505140 B CN104505140 B CN 104505140B CN 201410775486 A CN201410775486 A CN 201410775486A CN 104505140 B CN104505140 B CN 104505140B
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- conductive silver
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- silver powder
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- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 title claims abstract description 39
- 230000008719 thickening Effects 0.000 title claims abstract description 11
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims abstract description 20
- SWXVUIWOUIDPGS-UHFFFAOYSA-N diacetone alcohol Chemical compound CC(=O)CC(C)(C)O SWXVUIWOUIDPGS-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000002994 raw material Substances 0.000 claims abstract description 13
- 239000002562 thickening agent Substances 0.000 claims abstract description 13
- 239000003822 epoxy resin Substances 0.000 claims abstract description 7
- 150000002617 leukotrienes Chemical class 0.000 claims abstract description 7
- DITXJPASYXFQAS-UHFFFAOYSA-N nickel;sulfamic acid Chemical compound [Ni].NS(O)(=O)=O DITXJPASYXFQAS-UHFFFAOYSA-N 0.000 claims abstract description 7
- 229920000647 polyepoxide Polymers 0.000 claims abstract description 7
- 239000004814 polyurethane Substances 0.000 claims abstract description 7
- 229920002635 polyurethane Polymers 0.000 claims abstract description 7
- UCQFCFPECQILOL-UHFFFAOYSA-N diethyl hydrogen phosphate Chemical compound CCOP(O)(=O)OCC UCQFCFPECQILOL-UHFFFAOYSA-N 0.000 claims abstract description 6
- 229920002301 cellulose acetate Polymers 0.000 claims abstract description 5
- 108010010803 Gelatin Proteins 0.000 claims abstract description 4
- 235000021302 avocado oil Nutrition 0.000 claims abstract description 4
- 239000008163 avocado oil Substances 0.000 claims abstract description 4
- 239000000428 dust Substances 0.000 claims abstract description 4
- 229920000159 gelatin Polymers 0.000 claims abstract description 4
- 239000008273 gelatin Substances 0.000 claims abstract description 4
- 235000019322 gelatine Nutrition 0.000 claims abstract description 4
- 235000011852 gelatine desserts Nutrition 0.000 claims abstract description 4
- 239000011521 glass Substances 0.000 claims abstract description 4
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 18
- 238000003756 stirring Methods 0.000 claims description 14
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 claims description 12
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims description 12
- 239000008367 deionised water Substances 0.000 claims description 12
- 229910021641 deionized water Inorganic materials 0.000 claims description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 12
- 238000002156 mixing Methods 0.000 claims description 10
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims description 10
- 229910052709 silver Inorganic materials 0.000 claims description 7
- 239000004332 silver Substances 0.000 claims description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- 230000003213 activating effect Effects 0.000 claims description 6
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims description 6
- 239000003795 chemical substances by application Substances 0.000 claims description 6
- MIMDHDXOBDPUQW-UHFFFAOYSA-N dioctyl decanedioate Chemical compound CCCCCCCCOC(=O)CCCCCCCCC(=O)OCCCCCCCC MIMDHDXOBDPUQW-UHFFFAOYSA-N 0.000 claims description 6
- 239000007908 nanoemulsion Substances 0.000 claims description 6
- 239000002002 slurry Substances 0.000 claims description 6
- BPSIOYPQMFLKFR-UHFFFAOYSA-N trimethoxy-[3-(oxiran-2-ylmethoxy)propyl]silane Chemical compound CO[Si](OC)(OC)CCCOCC1CO1 BPSIOYPQMFLKFR-UHFFFAOYSA-N 0.000 claims description 6
- 230000003647 oxidation Effects 0.000 claims description 5
- 238000007254 oxidation reaction Methods 0.000 claims description 5
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 5
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 5
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 5
- 229910001961 silver nitrate Inorganic materials 0.000 claims description 5
- 241001272567 Hominoidea Species 0.000 claims description 4
- -1 alkyl phenol Chemical compound 0.000 claims description 4
- KWSLGOVYXMQPPX-UHFFFAOYSA-N 5-[3-(trifluoromethyl)phenyl]-2h-tetrazole Chemical compound FC(F)(F)C1=CC=CC(C2=NNN=N2)=C1 KWSLGOVYXMQPPX-UHFFFAOYSA-N 0.000 claims description 3
- 238000013019 agitation Methods 0.000 claims description 3
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 3
- 230000033228 biological regulation Effects 0.000 claims description 3
- 238000005119 centrifugation Methods 0.000 claims description 3
- 238000006243 chemical reaction Methods 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 3
- 239000012467 final product Substances 0.000 claims description 3
- 238000002360 preparation method Methods 0.000 claims description 3
- 239000000047 product Substances 0.000 claims description 3
- 229910001379 sodium hypophosphite Inorganic materials 0.000 claims description 3
- GPOGLVDBOFRHDV-UHFFFAOYSA-N (2-nonylphenyl) dihydrogen phosphite Chemical compound CCCCCCCCCC1=CC=CC=C1OP(O)O GPOGLVDBOFRHDV-UHFFFAOYSA-N 0.000 claims description 2
- 230000010355 oscillation Effects 0.000 claims description 2
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims 2
- 229920006221 acetate fiber Polymers 0.000 claims 1
- 150000001336 alkenes Chemical class 0.000 claims 1
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 claims 1
- 239000000843 powder Substances 0.000 abstract description 4
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 239000004005 microsphere Substances 0.000 abstract description 2
- 229910000510 noble metal Inorganic materials 0.000 abstract description 2
- 229920000642 polymer Polymers 0.000 abstract description 2
- 238000007639 printing Methods 0.000 description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- KAESVJOAVNADME-UHFFFAOYSA-N Pyrrole Chemical compound C=1C=CNC=1 KAESVJOAVNADME-UHFFFAOYSA-N 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 230000006641 stabilisation Effects 0.000 description 2
- 238000011105 stabilization Methods 0.000 description 2
- QYKIQEUNHZKYBP-UHFFFAOYSA-N Vinyl ether Chemical compound C=COC=C QYKIQEUNHZKYBP-UHFFFAOYSA-N 0.000 description 1
- 239000013543 active substance Substances 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 239000007767 bonding agent Substances 0.000 description 1
- 238000005253 cladding Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- LIXVMPBOGDCSRM-UHFFFAOYSA-N nonylbenzene Chemical class CCCCCCCCCC1=CC=CC=C1 LIXVMPBOGDCSRM-UHFFFAOYSA-N 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- OJMIONKXNSYLSR-UHFFFAOYSA-N phosphorous acid Chemical compound OP(O)O OJMIONKXNSYLSR-UHFFFAOYSA-N 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 229920002554 vinyl polymer Polymers 0.000 description 1
Abstract
The invention discloses a kind of conductive silver paste of effective thickening, it is made up of the raw material of following weight parts:High dispersive conductive silver powder 100 104, epoxy resin E51 14 17, acetone 20 25, leukotrienes 0.5 1, diethyl phosphate 12, cellulose acetate 0.5 1, gelatin 0.3 0.5, diacetone alcohol 0.6 1, nickel sulfamic acid 1 1.2, avocado oil 0.2 0.3, polyurethane levelling thickener pu 8,080 0.4 0.6, glass dust 10 14, the nano-silver powder that high dispersive conductive silver powder of the 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 conductive silver paste of effective thickening.
Background technology
Metallic silver particles are used in traditional conductive silver paste as the main component of 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, makes silver paste
The combination of stabilization is formed between particulate and base material, but because silver metal price is relatively expensive, it is possible to it is considered as silver-colored cladding
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 conductive silver paste of effective thickening.
The present invention is achieved by the following technical solutions:
A kind of conductive silver paste of effective thickening, it is characterised in that it is made up of the raw material of following weight parts:
High dispersive conductive silver powder 100-104, epoxy resin E51 14-17, acetone 20-25, leukotrienes 0.5-1, di(2-ethylhexyl)phosphate
Ethyl ester 1-2, cellulose acetate 0.5-1, gelatin 0.3-0.5, diacetone alcohol 0.6-1, nickel sulfamic acid 1-1.2, avocado oil 0.2-
0.3rd, polyurethane levelling thickener pu-8080 0.4-0.6, glass dust 10-14;
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, stirred,
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,
Centrifugation, is washed 3-5 times with deionized water and ethanol, drying, is obtained final product.
2nd, a kind of preparation method of the effectively conductive silver paste of thickening as claimed in claim 1, it is characterised in that including with
Lower step:
(1)Cellulose acetate is added in 3-5 times of acetone, polyurethane levelling thickener pu- is added after stirring and dissolving
8080, insulated and stirred 4-7 minutes at 50-60 DEG C, obtain thickener;
(2)Epoxy resin E51 is added in remaining acetone, diethyl phosphate, thickener is stirring evenly and then adding into,
Mixing 10-15 minutes is stirred at 60-70 DEG C, organic carrier is obtained;
(3)Diacetone alcohol, nickel sulfamic acid, leukotrienes are mixed, mixing 3-5 minutes is stirred at 40-50 DEG C, obtain active
Agent;
(4)High dispersive conductive silver powder is added in organic carrier, is well mixed, add activating agent and remaining each raw material,
Disperse at a high speed, mixed on feeding three-roll grinder, ground slurry granularity gets product to 8-15 microns.
It is an advantage of the invention that:
High dispersive conductive silver powder of the invention is the surface that nano-silver powder uniformly and is densely coated on 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;
Organic carrier of the invention, by adding thickener, can effectively improve slurry viscosity, and obtained slurry is more
Stabilization, prevented from caking, precipitation and layering, it is ensured that the figure of printing is fine and close, bubble-free stomata;
The activating agent of addition can effectively improve the electric conductivity of silver paste, improve the printing quality of silver paste.
Specific embodiment
Embodiment 1
A kind of conductive silver paste of effective thickening, it is characterised in that it is made up of the raw material of following weight parts:
High dispersive conductive silver powder 104, epoxy resin E51 17, acetone 25, leukotrienes 0.5, diethyl phosphate 1, acetic acid are fine
Dimension element 0.5, gelatin 0.5, diacetone alcohol 0.6, nickel sulfamic acid 1.2, avocado oil 0.3, polyurethane levelling thickener pu-8080
0.6th, glass dust 14;
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 4, APES 0.8,
Silane coupler KH560 1, ammonium persulfate 0.02, silver nitrate 140, polyvinylpyrrolidone 2, 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 mix 30 minutes,
Styrene, APES, the 35% of deionized water weight are added, magnetic agitation 50 minutes adds ammonium persulfate, surpasses
Sound wave shock 15h, obtains nanoemulsions;
Silver nitrate, polyvinylpyrrolidone are mixed, the 50% of remaining deionized water weight is added, stirred, 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 are added after completion of dropping, stirring reaction 30-50 minutes,
Centrifugation, is washed 3 times with deionized water and ethanol, drying, is obtained final product.
A kind of preparation method of the conductive silver paste of effective thickening, comprises the following steps:
(1)Cellulose acetate is added in 5 times of acetone, polyurethane levelling thickener pu- is added after stirring and dissolving
8080, insulated and stirred 7 minutes, obtain thickener at 60 DEG C;
(2)Epoxy resin E51 is added in remaining acetone, diethyl phosphate, thickener, 70 is stirring evenly and then adding into
Mixing 15 minutes is stirred at DEG C, organic carrier is obtained;
(3)Diacetone alcohol, nickel sulfamic acid, leukotrienes are mixed, mixing 3 minutes is stirred at 40 DEG C, obtain activating agent;
(4)High dispersive conductive silver powder is added in organic carrier, is well mixed, add activating agent and remaining each raw material,
Disperse at a high speed, mixed on feeding three-roll grinder, ground slurry granularity gets product to 8-15 microns.
Performance test:
After stirring without lump, in uniform state;
Fineness≤15 μm;
Adhesive force 5B;
Hardness 1.7H.
Claims (1)
1. a kind of conductive silver paste of effective thickening, it is characterised in that it is made up of the raw material of following weight parts:High dispersive is led
Electric silver powder 100-104, epoxy resin E51 14-17, acetone 20-25, leukotrienes 0.5-1, diethyl phosphate 1-2, acetate fiber
Plain 0.5-1, gelatin 0.3-0.5, diacetone alcohol 0.6-1, nickel sulfamic acid 1-1.2, avocado oil 0.2-0.3, polyurethane levelling increase
Thick dose of pu-8080 0.4-0.6, glass dust 10-14;Described high dispersive conductive silver powder is formed by the raw material of following weight parts
's:Nano aluminium oxide 5-10, di-n-octyl sebacate 0.1-0.2, deionized water 300-400, styrene 4-7, alkyl phenol polyoxy second
Alkene ether 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 (nonyl phenyl) phosphite 2-3;By nano aluminium oxide, di-n-octyl sebacate, silane coupler
KH560 mixes, and 500-700 revs/min of stirring mixes 20-30 minutes, adds styrene, APES, deionized water
The 30-35% of weight, magnetic agitation 40-50 minutes, adds ammonium persulfate, ultrasonic oscillation 10-15h to obtain nanoemulsions;By nitre
Sour silver, polyvinylpyrrolidone mixing, add the 40-50% of remaining deionized water weight, stir, and obtain oxidation solution;Will
Remaining each raw material mixing, is added dropwise ammoniacal liquor, and 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, centrifugation was washed 3-5 times with deionized water and ethanol,
Drying, obtains final product;
The preparation method of the conductive silver paste of described effective thickening, comprises the following steps:(1)Cellulose acetate is added to 3-5
In acetone again, polyurethane levelling thickener pu-8080 is added after stirring and dissolving, insulated and stirred 4-7 minutes at 50-60 DEG C,
Obtain thickener;(2)Epoxy resin E51 is added in remaining acetone, diethyl phosphate, thickener is stirring evenly and then adding into,
Mixing 10-15 minutes is stirred at 60-70 DEG C, organic carrier is obtained;(3)Diacetone alcohol, nickel sulfamic acid, leukotrienes are mixed,
Mixing 3-5 minutes is stirred at 40-50 DEG C, activating agent is obtained;(4)High dispersive conductive silver powder is added in organic carrier, mixing is equal
It is even, activating agent and remaining each raw material are added, disperse at a high speed, mixed on feeding three-roll grinder, ground slurry granularity to 8-
15 microns, get product.
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CN201410775486.6A CN104505140B (en) | 2014-12-16 | 2014-12-16 | A kind of conductive silver paste of effective thickening |
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CN201410775486.6A CN104505140B (en) | 2014-12-16 | 2014-12-16 | A kind of conductive silver paste of effective thickening |
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CN104505140B true CN104505140B (en) | 2017-06-23 |
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CN105006267A (en) * | 2015-08-10 | 2015-10-28 | 浙江凯盈新材料有限公司 | Silver powder based on processing of aminosilane coupling agent, preparation method and application thereof |
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CN103192074A (en) * | 2013-04-10 | 2013-07-10 | 张宇 | Highly dispersed sliver powder and conductive silver paste for film batteries |
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JP5032005B2 (en) * | 2005-07-05 | 2012-09-26 | 三井金属鉱業株式会社 | High crystal silver powder and method for producing the high crystal silver powder |
CN101972855B (en) * | 2010-11-11 | 2012-10-17 | 肇庆市羚光电子化学品材料科技有限公司 | Method for preparing silver micro-powder for high-temperature sintering silver pastes |
CN102103895B (en) * | 2010-11-23 | 2012-02-29 | 湖南威能新材料科技有限公司 | Silver paste used for positive electrodes of solar batteries and grid lines, preparation method thereof and solar battery containing same |
CN103258584B (en) * | 2013-01-09 | 2018-04-10 | 深圳市创智材料科技有限公司 | A kind of conductive silver paste and preparation method thereof |
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