CN103117111A - Conductive paste containing trioctyl trimellitate (TOTM) - Google Patents
Conductive paste containing trioctyl trimellitate (TOTM) Download PDFInfo
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- CN103117111A CN103117111A CN2012105220545A CN201210522054A CN103117111A CN 103117111 A CN103117111 A CN 103117111A CN 2012105220545 A CN2012105220545 A CN 2012105220545A CN 201210522054 A CN201210522054 A CN 201210522054A CN 103117111 A CN103117111 A CN 103117111A
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Abstract
The invention discloses conductive paste containing trioctyl trimellitate (TOTM). The conductive paste containing the TOTM is prepared by the following raw materials: by weight, A materials 52-56, B materials 13.6-15.7, C materials 22-25, TOTM 0.7-1.6, silicone oil 1.2-1.6, and polyamide wax 1-2. Due to the fact that lead is not contained, the conductive paste containing the TOTM completely conforms to the requirements of environmental protection, can be applied to the production of solar cells, and can form strong adhesion on the surfaces of solar cells, cell photoelectric conversion efficiency is high, and meanwhile silver powder, aluminum powder and copper powder of different particle diameters are selected to increase contact areas among particles. Therefore, conductivity of silver paste is improved.
Description
Technical field
The present invention relates to the fine Electronic field of chemicals, is exactly a kind of electrocondution slurry that contains trioctyl trimellitate (TOTM).
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.
Burning infiltration type electrocondution slurry mainly is used in the industries such as solar cell, makes electrode after sintering and uses, and the curing type electrically conductive ink is widely used in the industries such as printed circuit and Electronic Packaging.
Electrocondution slurry is different according to filler wherein, can be divided into carbon slurry (graphite conductor), metal paste (bronze, silver powder, copper powder, yellow gold), and the ceramic size of modification.
Performance Ratio, the conductivity of noble metal filler is best, carbon slurry secondly.But the price of gold is too high, and the oxidative resistance of copper powder is bad, and silver powder and silver-bearing copper powder are comparatively balanced on price and performance.Will getting well of the resistance to wear silver slurry of carbon slurry.
Solar cell conductive paste is comprised of silver powder, aluminium powder, inorganic bond material, organic carrier and relevant auxiliary agent etc.In most electric slurry, the inorganic bond material is mainly the flint glass powder of low melting point, big for environment pollution and weldability is poor is its major defect.Therefore, the unleaded inexorable trend that become of electrocondution slurry.
Summary of the invention
The object of the present invention is to provide a kind of efficient, environmental protection, the unleaded electrocondution slurry that contains trioctyl trimellitate (TOTM).
Above-mentioned purpose realizes by following scheme:
A kind of electrocondution slurry that contains trioctyl trimellitate (TOTM) is characterized in that, it is that raw material by following weight parts makes:
A expects 52-56, and B expects 13.6-15.7, and C expects 22-25, trioctyl trimellitate (TOTM) 0.7-1.6, organic silicone oil: 1.2-1.6, polyamide wax 1-2;
Described A material is made by the raw material of following weight parts: 1-5 μ m silver powder 45-48,11-15 μ m silver powder 10-15,16-25 μ m silver powder 10-15,10-15 μ m glass dust 8-12, organic carrier A 15-20, silane coupler KH570 1-1.5, DMIP 0.7-1.2;
Described B material is made by the raw material of following weight parts: 6-10 μ m bronze 48-51,16-25 μ m bronze 20-25,20-25 μ m glass dust 9-11, organic carrier B 25-30, organic silicone oil 0.5-1.2, dibutyl maleate 2-3;
Described C material is made by the raw material of following weight parts: 11-15 μ m aluminium powder 20-25,30-60nm aluminium powder 35-40,10-15 μ m glass dust 8-11, organic carrier C 28-30;
Described glass dust is made by the raw material of following weight parts: NA
3ALF
66-8, Bi
2O
311-13, B
2O
34-6, Al
2O
34.8-5.8, SiO
218-20, Sb
2O
37-9, Na
2O 8-10, K
2O 6-8, CuO 4-6, AS
2O
35.8-6.7, Co
2O
311-13, trees ashes 11-13;
Described organic carrier A is made by the raw material of following weight parts: abietic resin 11-12, polyvinylpyrrolidone 9-11, butyl carbitol 32-34, benzinum 0.8-1.3;
Described organic carrier B is made by the raw material of following weight parts: celluloid 6-8, methyl alcohol 8-12, diethylene glycol ether acetate 10-12, di-2-ethylhexyl maleate 0.5-1;
Described organic carrier C is made by the raw material of following weight parts: ethyl cellulose 8-10, graphite powder 1-2, polyethylene glycol 10-15, ethyl acetate 16-18.
Described a kind of electrocondution slurry that contains trioctyl trimellitate (TOTM) is characterized in that:
The preparation method comprises the following steps:
(1) take by weight required each raw material of preparation glass dust and put into mixing in silica crucible, after put into electric furnace in 1100-1300 ℃ of sintering 2-3h, again the glass metal after the gained fusing is poured in cold water, then ball milling, cross the 200-300 mesh sieve, cooling, again at 500-600 ℃ of insulation 4-5h, then, quench with deionized water again, ball milling, cross the sieve of different meshes, collect respectively and obtain 1-5 μ m glass dust, 10-15 μ m glass dust and 20-25 μ m glass dust, use respectively again 10-15% salt acid soak 1-2 hour, then clean to neutral with deionized water, dry to such an extent that the glass dust of different-grain diameter is standby,
(2) will prepare by weight each raw material blending of organic carrier A, and be stirred to dissolving under 70-80 ℃, the rear 100-200 order filter cloth of crossing namely gets the standby of organic carrier A;
(3) will prepare by weight each raw material blending of organic carrier B, be stirred to the rear 100-200 of mistake of dissolving order filter cloth under 65-70 ℃, namely get organic carrier B standby;
(4) will prepare by weight each raw material blending of organic carrier C, be stirred to the rear 100-200 of mistake of dissolving order filter cloth under 65-70 ℃, namely get organic carrier C standby;
(5) glass dust with the prepared 1-5 μ of step (1) m adds in the prepared organic carrier A of step (2) by weight, stir mixed, added by weight successively again 1-5 μ m silver powder, 16-25 μ m silver powder, 61-90nm silver powder every 25-35 minute, mix 2-3 hour, obtain the A material;
(6) the prepared 10-15 μ of step (1) m glass dust is added in the prepared organic carrier B of step (3), stir mixedly, then added successively 1-5 μ m aluminium powder, 16-25 μ m aluminium powder in every minor tick 30-40 minute, mix 2-3 hour, obtain the B material;
(7) the prepared 20-25 μ of step (1) m glass dust is added in the prepared organic carrier C of step (4), stirring is mixed, then adds successively 1-5 μ m copper powder in every minor tick 30-40 minute, and the 30-60nm copper powder mixes 2-3 hour, obtains the C material;
(8) A material, B material, C material and all the other preparations are contained the raw material mixing by weight of the electrocondution slurry of trioctyl trimellitate (TOTM), ball milling 7-9 hour, after crossing the 400-500 mesh sieve and get 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 fully, be applied to the production of solar cell, can form strong adhesion in solar cell surface, the cell photoelectric conversion efficiency is high, silver powder and the aluminium of different-grain diameter have been selected simultaneously, the copper powder powder increases interparticle contact area, thereby has improved the conductive capability of silver-colored slurry;
2, the present invention has added copper powder in electrocondution slurry, aluminium powder can help to reduce silver slurry production cost, save a large amount of noble silvers, improve simultaneously the electric conductivity of silver slurry, thereby reached the purpose that reduces the solar cell manufacturing cost, obtained good economic benefit.Technique of the present invention is simple simultaneously, and cost is low, thereby has broad application prospects.
Embodiment
A kind of electrocondution slurry that contains trioctyl trimellitate (TOTM), it is that raw material by following weight parts (kg) makes:
A material 56, B material 15.7, C material 25, trioctyl trimellitate (TOTM) 1.6, organic silicone oil: 1.6, polyamide wax 2;
Described A material is made by the raw material of following weight parts: 1-5 μ m silver powder 48,11-15 μ m silver powder 15,16-25 μ m silver powder 10,10-15 μ m glass dust 12, organic carrier A 20, silane coupler KH570 1.2, DMIP 0.9;
Described B material is made by the raw material of following weight parts: 6-10 μ m bronze 51,16-25 μ m bronze 25,20-25 μ m glass dust 11, organic carrier B 30, organic silicone oil 0.7, dibutyl maleate 3;
Described C material is made by the raw material of following weight parts: 11-15 μ m aluminium powder 25,30-60nm aluminium powder 40,10-15 μ m glass dust 11, organic carrier C 30;
Described glass dust is made by the raw material of following weight parts: NA
3ALF
68, Bi
2O
313, B
2O
34, Al
2O
35.8, SiO
220, Sb
2O
39, Na
2O 10, K
2O 8, and CuO 6, AS
2O
36.7, Co
2O
313, trees ashes 11;
Described organic carrier A is made by the raw material of following weight parts: abietic resin 12, polyvinylpyrrolidone 11, butyl carbitol 34, benzinum 1.3;
Described organic carrier B is made by the raw material of following weight parts: celluloid 8, methyl alcohol 12, diethylene glycol ether acetate 12, di-2-ethylhexyl maleate 0.5;
Described organic carrier C is made by the raw material of following weight parts: ethyl cellulose 10, graphite powder 2, polyethylene glycol 15, ethyl acetate 18.
Described a kind of electrocondution slurry that contains trioctyl trimellitate (TOTM), the preparation method comprises the following steps:
(1) take by weight required each raw material of preparation glass dust and put into mixing in silica crucible, after put into electric furnace in 1300 ℃ of sintering 3h, again the glass metal after the gained fusing is poured in cold water, then ball milling, cross 300 mesh sieves, cooling, then at 600 ℃ of insulation 5h, then, quench with deionized water again, ball milling, the sieve of different meshes, collect respectively and obtain 1-5 μ m glass dust excessively, 10-15 μ m glass dust and 20-25 μ m glass dust, use respectively again 10% salt acid soak 2 hours, then clean to neutral with deionized water, dry to such an extent that the glass dust of different-grain diameter is standby;
(2) will prepare by weight each raw material blending of organic carrier A, and be stirred to dissolving under 80 ℃, rear mistake 200 order filter clothes namely get the standby of organic carrier A;
(3) will prepare by weight each raw material blending of organic carrier B, be stirred to the rear 100 order filter clothes of crossing of dissolving under 65 ℃, namely get organic carrier B standby;
(4) will prepare by weight each raw material blending of organic carrier C, be stirred to the rear 100 order filter clothes of crossing of dissolving under 65 ℃, namely get organic carrier C standby;
(5) glass dust with the prepared 1-5 μ of step (1) m adds in the prepared organic carrier A of step (2) by weight, stir mixed, add by weight successively again 1-5 μ m silver powder, 16-25 μ m silver powder, 61-90nm silver powder every 35 minutes, mix 3 hours, obtain the A material;
(6) the prepared 10-15 μ of step (1) m glass dust is added in the prepared organic carrier B of step (3), stir mixedly, more every minor tick added successively 1-5 μ m aluminium powder, 16-25 μ m aluminium powder in 40 minutes, mixes 2 hours, obtained the B material;
(7) the prepared 20-25 μ of step (1) m glass dust is added in the prepared organic carrier C of step (4), stir mixedly, more every minor tick added 1-5 μ m copper powder in 40 minutes successively, and the 30-60nm copper powder mixes 2.5 hours, obtains the C material;
(8) A material, B material, C material and all the other preparations are contained the raw material mixing by weight of the electrocondution slurry of trioctyl trimellitate (TOTM), ball milling 7 hours is after crossing 400 mesh sieves and get final product.
Adopt screen process press that the silver slurry is printed on 125mm * 125mm Si substrate, then 180 ℃ of dryings, carry out quick fired electrodes lead-in wire at 880 ℃ again, the surperficial silvery white of the contact conductor of making after high temperature sintering, smooth zero defect, peel strength 14 N/cm, soldering is functional, sheet resistance＜10 Siements/sq, the solar cell photoelectric transformation efficiency of preparation is 18.9%, the tensile test result is adhesive force〉12N/mm
2
Claims (2)
1. an electrocondution slurry that contains trioctyl trimellitate (TOTM), is characterized in that, it is that raw material by following weight parts makes:
A expects 52-56, and B expects 13.6-15.7, and C expects 22-25, trioctyl trimellitate (TOTM) 0.7-1.6, organic silicone oil: 1.2-1.6, polyamide wax 1-2;
Described A material is made by the raw material of following weight parts: 1-5 μ m silver powder 45-48,11-15 μ m silver powder 10-15,16-25 μ m silver powder 10-15,10-15 μ m glass dust 8-12, organic carrier A 15-20, silane coupler KH570 1-1.5, DMIP 0.7-1.2;
Described B material is made by the raw material of following weight parts: 6-10 μ m bronze 48-51,16-25 μ m bronze 20-25,20-25 μ m glass dust 9-11, organic carrier B 25-30, organic silicone oil 0.5-1.2, dibutyl maleate 2-3;
Described C material is made by the raw material of following weight parts: 11-15 μ m aluminium powder 20-25,30-60nm aluminium powder 35-40,10-15 μ m glass dust 8-11, organic carrier C 28-30;
Described glass dust is made by the raw material of following weight parts: NA
3ALF
66-8, Bi
2O
311-13, B
2O
34-6, Al
2O
34.8-5.8, SiO
218-20, Sb
2O
37-9, Na
2O 8-10, K
2O 6-8, CuO 4-6, AS
2O
35.8-6.7, Co
2O
311-13, trees ashes 11-13;
Described organic carrier A is made by the raw material of following weight parts: abietic resin 11-12, polyvinylpyrrolidone 9-11, butyl carbitol 32-34, benzinum 0.8-1.3;
Described organic carrier B is made by the raw material of following weight parts: celluloid 6-8, methyl alcohol 8-12, diethylene glycol ether acetate 10-12, di-2-ethylhexyl maleate 0.5-1;
Described organic carrier C is made by the raw material of following weight parts: ethyl cellulose 8-10, graphite powder 1-2, polyethylene glycol 10-15, ethyl acetate 16-18.
2. a kind of electrocondution slurry that contains trioctyl trimellitate (TOTM) according to claim 1 is characterized in that:
The preparation method comprises the following steps:
(1) take by weight required each raw material of preparation glass dust and put into mixing in silica crucible, after put into electric furnace in 1100-1300 ℃ of sintering 2-3h, again the glass metal after the gained fusing is poured in cold water, then ball milling, cross the 200-300 mesh sieve, cooling, again at 500-600 ℃ of insulation 4-5h, then, quench with deionized water again, ball milling, cross the sieve of different meshes, collect respectively and obtain 1-5 μ m glass dust, 10-15 μ m glass dust and 20-25 μ m glass dust, use respectively again 10-15% salt acid soak 1-2 hour, then clean to neutral with deionized water, dry to such an extent that the glass dust of different-grain diameter is standby,
(2) will prepare by weight each raw material blending of organic carrier A, and be stirred to dissolving under 70-80 ℃, the rear 100-200 order filter cloth of crossing namely gets the standby of organic carrier A;
(3) will prepare by weight each raw material blending of organic carrier B, be stirred to the rear 100-200 of mistake of dissolving order filter cloth under 65-70 ℃, namely get organic carrier B standby;
(4) will prepare by weight each raw material blending of organic carrier C, be stirred to the rear 100-200 of mistake of dissolving order filter cloth under 65-70 ℃, namely get organic carrier C standby;
(5) glass dust with the prepared 1-5 μ of step (1) m adds in the prepared organic carrier A of step (2) by weight, stir mixed, added by weight successively again 1-5 μ m silver powder, 16-25 μ m silver powder, 61-90nm silver powder every 25-35 minute, mix 2-3 hour, obtain the A material;
(6) the prepared 10-15 μ of step (1) m glass dust is added in the prepared organic carrier B of step (3), stir mixedly, then added successively 1-5 μ m aluminium powder, 16-25 μ m aluminium powder in every minor tick 30-40 minute, mix 2-3 hour, obtain the B material;
(7) the prepared 20-25 μ of step (1) m glass dust is added in the prepared organic carrier C of step (4), stirring is mixed, then adds successively 1-5 μ m copper powder in every minor tick 30-40 minute, and the 30-60nm copper powder mixes 2-3 hour, obtains the C material;
(8) A material, B material, C material and all the other preparations are contained the raw material mixing by weight of the electrocondution slurry of trioctyl trimellitate (TOTM), ball milling 7-9 hour, after crossing the 400-500 mesh sieve and get final product.
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| CN201210522054.5A CN103117111B (en) | 2012-12-07 | 2012-12-07 | A kind of electrocondution slurry containing trioctyl trimellitate (TOTM) |
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| CN103117111B CN103117111B (en) | 2016-08-10 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR101907500B1 (en) * | 2016-03-10 | 2018-10-12 | 삼성에스디아이 주식회사 | Composition for forming electrode, electrode manufactured using the same and solar cell |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101345263A (en) * | 2008-09-09 | 2009-01-14 | 季福根 | Leadless electronic slurry composition for solar silicon photovoltaic cell and preparation method thereof |
| CN101794639A (en) * | 2010-03-16 | 2010-08-04 | 彩虹集团公司 | Environment-friendly glass frit and preparation method thereof |
| US20110073178A1 (en) * | 2009-09-30 | 2011-03-31 | BYD Co. Ltd | Electrically conductive paste, solar cell containing same and method |
| CN102360585A (en) * | 2011-06-28 | 2012-02-22 | 陕西天盛新材料科技有限公司 | Aluminum paste for improving conversion efficiency of solar cells and preparation method for aluminum paste |
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2012
- 2012-12-07 CN CN201210522054.5A patent/CN103117111B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101345263A (en) * | 2008-09-09 | 2009-01-14 | 季福根 | Leadless electronic slurry composition for solar silicon photovoltaic cell and preparation method thereof |
| US20110073178A1 (en) * | 2009-09-30 | 2011-03-31 | BYD Co. Ltd | Electrically conductive paste, solar cell containing same and method |
| CN101794639A (en) * | 2010-03-16 | 2010-08-04 | 彩虹集团公司 | Environment-friendly glass frit and preparation method thereof |
| CN102360585A (en) * | 2011-06-28 | 2012-02-22 | 陕西天盛新材料科技有限公司 | Aluminum paste for improving conversion efficiency of solar cells and preparation method for aluminum paste |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR101907500B1 (en) * | 2016-03-10 | 2018-10-12 | 삼성에스디아이 주식회사 | Composition for forming electrode, electrode manufactured using the same and solar cell |
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| Publication number | Publication date |
|---|---|
| CN103117111B (en) | 2016-08-10 |
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