CN103021514B - A kind of conductive silver aluminium paste containing adipate ester - Google Patents
A kind of conductive silver aluminium paste containing adipate ester Download PDFInfo
- Publication number
- CN103021514B CN103021514B CN201210527080.7A CN201210527080A CN103021514B CN 103021514 B CN103021514 B CN 103021514B CN 201210527080 A CN201210527080 A CN 201210527080A CN 103021514 B CN103021514 B CN 103021514B
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- CN
- China
- Prior art keywords
- raw material
- organic carrier
- glass dust
- weight parts
- adipate ester
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- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 title claims abstract description 28
- 239000004411 aluminium Substances 0.000 title claims abstract description 25
- 229910052782 aluminium Inorganic materials 0.000 title claims abstract description 25
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 title claims abstract description 25
- 229910052709 silver Inorganic materials 0.000 title claims abstract description 19
- 239000004332 silver Substances 0.000 title claims abstract description 19
- -1 adipate ester Chemical class 0.000 title claims abstract description 18
- 239000002994 raw material Substances 0.000 claims abstract description 37
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims abstract description 4
- 229910000077 silane Inorganic materials 0.000 claims abstract description 4
- 239000011521 glass Substances 0.000 claims description 24
- 239000000428 dust Substances 0.000 claims description 21
- 239000000463 material Substances 0.000 claims description 18
- 238000002360 preparation method Methods 0.000 claims description 16
- 239000000843 powder Substances 0.000 claims description 12
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 9
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 6
- 238000000498 ball milling Methods 0.000 claims description 6
- 239000008367 deionised water Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- 239000004744 fabric Substances 0.000 claims description 5
- 238000005245 sintering Methods 0.000 claims description 4
- POAOYUHQDCAZBD-UHFFFAOYSA-N 2-butoxyethanol Chemical compound CCCCOCCO POAOYUHQDCAZBD-UHFFFAOYSA-N 0.000 claims description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 3
- QWDBCIAVABMJPP-UHFFFAOYSA-N Diisopropyl phthalate Chemical compound CC(C)OC(=O)C1=CC=CC=C1C(=O)OC(C)C QWDBCIAVABMJPP-UHFFFAOYSA-N 0.000 claims description 3
- MUXOBHXGJLMRAB-UHFFFAOYSA-N Dimethyl succinate Chemical compound COC(=O)CCC(=O)OC MUXOBHXGJLMRAB-UHFFFAOYSA-N 0.000 claims description 3
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 3
- 229910052799 carbon Inorganic materials 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 3
- SBZXBUIDTXKZTM-UHFFFAOYSA-N diglyme Chemical compound COCCOCCOC SBZXBUIDTXKZTM-UHFFFAOYSA-N 0.000 claims description 3
- XTDYIOOONNVFMA-UHFFFAOYSA-N dimethyl pentanedioate Chemical compound COC(=O)CCCC(=O)OC XTDYIOOONNVFMA-UHFFFAOYSA-N 0.000 claims description 3
- 239000012467 final product Substances 0.000 claims description 3
- 238000009413 insulation Methods 0.000 claims description 3
- 229910052751 metal Inorganic materials 0.000 claims description 3
- 239000002184 metal Substances 0.000 claims description 3
- 229920000609 methyl cellulose Polymers 0.000 claims description 3
- 239000001923 methylcellulose Substances 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- MQHNKCZKNAJROC-UHFFFAOYSA-N phthalic acid dipropyl ester Natural products CCCOC(=O)C1=CC=CC=C1C(=O)OCCC MQHNKCZKNAJROC-UHFFFAOYSA-N 0.000 claims description 3
- 238000010791 quenching Methods 0.000 claims description 3
- 239000011347 resin Substances 0.000 claims description 3
- 229920005989 resin Polymers 0.000 claims description 3
- 238000005096 rolling process Methods 0.000 claims description 3
- 239000000377 silicon dioxide Substances 0.000 claims description 3
- 239000002002 slurry Substances 0.000 abstract description 13
- 210000004027 cell Anatomy 0.000 abstract description 9
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 230000007613 environmental effect Effects 0.000 abstract description 3
- 238000006243 chemical reaction Methods 0.000 abstract description 2
- 230000007547 defect Effects 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 206010013786 Dry skin Diseases 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000005538 encapsulation Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000005308 flint glass Substances 0.000 description 1
- 230000008595 infiltration Effects 0.000 description 1
- 238000001764 infiltration Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000005476 soldering Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 238000009864 tensile test Methods 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
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- Conductive Materials (AREA)
Abstract
The invention discloses a kind of conductive silver aluminium paste containing adipate ester, it is obtained by the raw material of following weight parts: A expects that 54-56, B expect 13-15, silane coupler KH602? 1-2, repefral 1-2, adipate ester 0.6-0.8.The electrocondution slurry of gained of the present invention is not leaded, meet environmental requirement completely, be applied to the production of solar cell, strong adhesion can be formed in solar cell surface, cell photoelectric conversion efficiency is high, selected the silver powder etc. of different-grain diameter simultaneously, increase interparticle contact area, thus improve the conductive capability of silver slurry.
Description
Technical field
The present invention relates to electrocondution slurry field, is exactly a kind of conductive silver aluminium paste containing adipate ester.
Background technology
Electrocondution slurry is electronic devices and components encapsulation, electrode and interconnected critical material, mainly comprises burning infiltration type electrocondution slurry and the large class of curing type conducting resinl (electrically conductive ink) two.
Solar cell conductive paste is made up of silver powder, aluminium powder etc., inorganic bond material, organic carrier and related auxiliaries etc.In most electric slurry, the flint glass powder of inorganic bond material mainly low melting point, big for environment pollution and weldability difference is its major defect.Therefore, electrocondution slurry efficient, environmental protection, unleadedly become inexorable trend.
Summary of the invention
The object of the present invention is to provide a kind of conductive silver aluminium paste containing adipate ester.
Above-mentioned purpose is realized by following scheme:
A conductive silver aluminium paste containing adipate ester, it is characterized in that, it is obtained by the raw material of following weight parts: A expects that 54-56, B expect 13-15, silane coupler KH6021-2, repefral 1-2, adipate ester 0.6-0.8;
Described A material is obtained by the raw material of following weight parts: 1-5 μm silver powder 42-44,16-25 μm silver powder 35-37,1-5 μm of glass dust 8-12, organic carrier A23-24, diisopropyl phthalate 0.5-0.8;
Described B material is obtained by the raw material of following weight parts: 11-15 μm of aluminium powder 25-28,30-60nm aluminium powder 22-25,61-90nm aluminium powder 8-10,10-15 μm of glass dust 8-10, organic carrier B18-20, graphite powder 1-2;
Described glass dust is obtained by the raw material of following weight parts: K
2o2.8-4.7, CuO6-8, AS
2o
35-7, Bi
2o
36-8, B
2o
316-18, Al
2o
35-7, SiO
26.2-8.6, V
2o
59-11, Sb
2o
38-9, AgO
211-12, Co
2o
38-9.7, ZnO6.5-7.9;
Described organic carrier A is obtained by the raw material of following weight parts: methylcellulose 10-12, dimethyl succinate 16-18, dimethyl glutarate 18-20;
Described organic carrier B is obtained by the raw material of following weight parts: 145 abietic resin 9-11,2-methyl-4-ethyl imidazol(e) 1-2, butyl glycol ether 18-20, diethylene glycol dimethyl ether 16-18.
Described a kind of conductive silver aluminium paste containing adipate ester, is characterized in that:
Preparation method comprises the following steps:
(1) take by weight and prepare each raw material needed for glass dust and put in silica crucible and mix, after put into electric furnace in 1000-1200 DEG C sintering 3-4h, glass metal after being melted by gained is again poured in cold water, then ball milling, cross 200-300 mesh sieve, cooling, again at 600-700 DEG C of insulation 2-3h, then, quench with deionized water again, ball milling, cross the sieve of different meshes, collect respectively and obtain 1-5 μm of glass dust and 10-15 μm of glass dust, 2-3 hour is soaked respectively again with the acetic acid solution that concentration is 9-12%, then clean to neutrality with deionized water, dry the glass dust of different-grain diameter is for subsequent use,
(2) will prepare each raw material blending of organic carrier A by weight, at 70-80 DEG C, be stirred to dissolving, the rear filter cloth of 300-500 order excessively, obtains for subsequent use of organic carrier A;
(3) will each raw material blending of organic carrier B be prepared by weight, and be stirred at 75-80 DEG C after dissolving and cross 200-400 order filter cloth, obtain organic carrier B for subsequent use;
(4) preparation A is expected that needed raw material stirs, obtain A material;
(5) preparation B is expected that needed raw material stirs, obtain B material;
(6) A is expected, B material and the raw material of conductive silver aluminium paste of all the other preparations containing adipate ester mixes by weight, then on three-roll grinder according to blank preparation technics rolling more than 10 times, adjust viscosity, viscosity is 150-200Pas, to obtain final product.
Beneficial effect of the present invention is:
1, the electrocondution slurry of gained of the present invention is not leaded, meet environmental requirement completely, be applied to the production of solar cell, strong adhesion can be formed in solar cell surface, cell photoelectric conversion efficiency is high, selected the silver powder etc. of different-grain diameter simultaneously, increase interparticle contact area, thus improve the conductive capability of silver slurry;
2, the present invention with the addition of aluminium powder in electrocondution slurry, can contribute to reducing silver slurry production cost, save a large amount of noble silvers, improve the electric conductivity of silver slurry simultaneously, thus reach the object reducing solar cell manufacturing cost, achieve good economic benefit.Present invention process is simple simultaneously, and cost is low, thus has broad application prospects.
Embodiment
A conductive silver aluminium paste containing adipate ester, it is obtained by the raw material of following weight parts (kg): A expects that 56, B expects 15, silane coupler KH6021.2, repefral 1.8, adipate ester 0.8;
Described A material is obtained by the raw material of following weight parts: 1-5 μm of silver powder 44,16-25 μm silver powder 37,1-5 μm glass dust 12, organic carrier A24, diisopropyl phthalate 0.8;
Described B material is obtained by the raw material of following weight parts: 11-15 μm of aluminium powder 28,30-60nm aluminium powder 25,61-90nm aluminium powder 10,10-15 μm of glass dust 10, organic carrier B20, graphite powder 1.4;
Described glass dust is obtained by the raw material of following weight parts: K
2o4.2, CuO8, AS
2o
37, Bi
2o
38, B
2o
318, Al
2o
37, SiO
28.6, V
2o
511, Sb
2o
39, AgO
212, Co
2o
39.4, ZnO7.9;
Described organic carrier A is obtained by the raw material of following weight parts: methylcellulose 12, dimethyl succinate 18, dimethyl glutarate 20;
Described organic carrier B is obtained by the raw material of following weight parts: 145 abietic resins 11,2-methyl-4-ethyl imidazol(e) 2, butyl glycol ether 20, diethylene glycol dimethyl ether 18.
Described a kind of conductive silver aluminium paste containing adipate ester,
Preparation method comprises the following steps:
(1) take by weight and prepare each raw material needed for glass dust and put in silica crucible and mix, after put into electric furnace in 1200 DEG C sintering 3h, glass metal after being melted by gained is again poured in cold water, then ball milling, cross 300 mesh sieves, cooling, again at 700 DEG C of insulation 2h, then, then quench with deionized water, ball milling, cross the sieve of different meshes, collect respectively and obtain 1-5 μm of glass dust and 10-15 μm of glass dust, then soak 2 hours with the acetic acid solution that concentration is 12% respectively, then clean to neutrality with deionized water, dry the glass dust of different-grain diameter is for subsequent use;
(2) will prepare each raw material blending of organic carrier A by weight, at 80 DEG C, be stirred to dissolving, rear mistake 500 order filter cloth, obtains for subsequent use of organic carrier A;
(3) will each raw material blending of organic carrier B be prepared by weight, and be stirred at 75 DEG C after dissolving and cross 400 order filter clothes, obtain organic carrier B for subsequent use;
(4) preparation A is expected that needed raw material stirs, obtain A material;
(5) preparation B is expected that needed raw material stirs, obtain B material;
(6) A is expected, B material and the raw material of conductive silver aluminium paste of all the other preparations containing adipate ester mixes by weight, then on three-roll grinder according to blank preparation technics rolling 11 times, adjust viscosity, viscosity is 150Pas, to obtain final product.
Screen process press is adopted to be printed on 125mm × 125mmSi 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 14N/cm, soldering is functional, sheet resistance < 10Siements/sq, the solar cell photoelectric transformation efficiency of preparation is 18.1%, and tensile test result is adhesive force >15N/mm
2.。
Claims (2)
1. the conductive silver aluminium paste containing adipate ester, it is characterized in that, it is obtained by the raw material of following weight parts: A expects that 54-56, B expect 13-15, silane coupler KH6021-2, repefral 1-2, adipate ester 0.6-0.8; Described A material is obtained by the raw material of following weight parts: 1-5 μm silver powder 42-44,16-25 μm silver powder 35-37,1-5 μm of glass dust 8-12, organic carrier A23-24, diisopropyl phthalate 0.5-0.8; Described B material is obtained by the raw material of following weight parts: 11-15 μm of aluminium powder 25-28,30-60nm aluminium powder 22-25,61-90nm aluminium powder 8-10,10-15 μm of glass dust 8-10, organic carrier B18-20, graphite powder 1-2; Described glass dust is obtained by the raw material of following weight parts: K
2o2.8-4.7, CuO6-8, As
2o
35-7, Bi
2o
36-8, B
2o
316-18, Al
2o
35-7, SiO
26.2-8.6, V
2o
59-11, Sb
2o
38-9, Ag
2o11-12, Co
2o
38-9.7, ZnO6.5-7.9; Described organic carrier A is obtained by the raw material of following weight parts: methylcellulose 10-12, dimethyl succinate 16-18, dimethyl glutarate 18-20; Described organic carrier B is obtained by the raw material of following weight parts: 145 abietic resin 9-11,2-methyl-4-ethyl imidazol(e) 1-2, butyl glycol ether 18-20, diethylene glycol dimethyl ether 16-18.
2. a kind of conductive silver aluminium paste containing adipate ester according to claim 1, is characterized in that: preparation method comprises the following steps:
(1) take by weight and prepare each raw material needed for glass dust and put in silica crucible and mix, after put into electric furnace in 1000-1200 DEG C sintering 3-4h, glass metal after being melted by gained is again poured in cold water, then ball milling, cross 200-300 mesh sieve, cooling, again at 600-700 DEG C of insulation 2-3h, then, quench with deionized water again, ball milling, cross the sieve of different meshes, collect respectively and obtain 1-5 μm of glass dust and 10-15 μm of glass dust, 2-3 hour is soaked respectively again with the acetic acid solution that concentration is 9-12%, then clean to neutrality with deionized water, dry the glass dust of different-grain diameter is for subsequent use,
(2) will prepare each raw material blending of organic carrier A by weight, at 70-80 DEG C, be stirred to dissolving, the rear filter cloth of 300-500 order excessively, obtains for subsequent use of organic carrier A;
(3) will each raw material blending of organic carrier B be prepared by weight, and be stirred at 75-80 DEG C after dissolving and cross 200-400 order filter cloth, obtain organic carrier B for subsequent use;
(4) preparation A is expected that needed raw material stirs, obtain A material;
(5) preparation B is expected that needed raw material stirs, obtain B material;
(6) A is expected, B material and the raw material of conductive silver aluminium paste of all the other preparations containing adipate ester mixes by weight, then on three-roll grinder according to blank preparation technics rolling more than 10 times, adjust viscosity, viscosity is 150-200Pas, to obtain final product.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210527080.7A CN103021514B (en) | 2012-12-10 | 2012-12-10 | A kind of conductive silver aluminium paste containing adipate ester |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210527080.7A CN103021514B (en) | 2012-12-10 | 2012-12-10 | A kind of conductive silver aluminium paste containing adipate ester |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN103021514A CN103021514A (en) | 2013-04-03 |
| CN103021514B true CN103021514B (en) | 2016-02-17 |
Family
ID=47970018
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201210527080.7A Active CN103021514B (en) | 2012-12-10 | 2012-12-10 | A kind of conductive silver aluminium paste containing adipate ester |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100524835C (en) * | 2005-10-18 | 2009-08-05 | 东洋铝株式会社 | Aluminum paste composition and solar cell device making use of the same |
| CN101609849A (en) * | 2009-07-13 | 2009-12-23 | 中南大学 | Silver conductive paste used for positive electrode of solar battery and preparation technology thereof |
| CN102426873A (en) * | 2011-12-28 | 2012-04-25 | 彩虹集团公司 | Silicon solar battery positive silver paste and preparation method thereof |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP5853541B2 (en) * | 2011-04-25 | 2016-02-09 | 横浜ゴム株式会社 | Conductive composition for forming solar battery collecting electrode and solar battery cell |
| TW201308630A (en) * | 2011-05-17 | 2013-02-16 | Du Pont | Thick film paste containing bismuth-tellurium-oxide and its use in the manufacture of semiconductor devices |
-
2012
- 2012-12-10 CN CN201210527080.7A patent/CN103021514B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100524835C (en) * | 2005-10-18 | 2009-08-05 | 东洋铝株式会社 | Aluminum paste composition and solar cell device making use of the same |
| CN101609849A (en) * | 2009-07-13 | 2009-12-23 | 中南大学 | Silver conductive paste used for positive electrode of solar battery and preparation technology thereof |
| CN102426873A (en) * | 2011-12-28 | 2012-04-25 | 彩虹集团公司 | Silicon solar battery positive silver paste and preparation method thereof |
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| Publication number | Publication date |
|---|---|
| CN103021514A (en) | 2013-04-03 |
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