CN103117135A - Preparation method for solar cell conductive mixed paste containing dioctyl phthalate (DOP) - Google Patents

Preparation method for solar cell conductive mixed paste containing dioctyl phthalate (DOP) Download PDF

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CN103117135A
CN103117135A CN2012105219891A CN201210521989A CN103117135A CN 103117135 A CN103117135 A CN 103117135A CN 2012105219891 A CN2012105219891 A CN 2012105219891A CN 201210521989 A CN201210521989 A CN 201210521989A CN 103117135 A CN103117135 A CN 103117135A
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organic carrier
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glass dust
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solar cell
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CN103117135B (en
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年福枭
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Chongqing Xinrui Technology Service Co.,Ltd.
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Bengbu City Zhifeng Science & Technology Co Ltd
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Abstract

The invention discloses solar cell conductive mixed paste containing dioctyl phthalate (DOP). The solar cell conductive mixed paste containing DOP is prepared by the following raw materials: by weight, A materials 52-56, B materials 18-20, C materials 22-25, silane coupling agents KH602 2-3, silicone oil 1-2, polyamide wax 1-2, and DOP 1-2. Due to the fact that lead is not contained, the solar cell conductive mixed paste containing DOP 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, gold powder and aluminum powder of different particle diameters are selected to increase contact areas among particles. Therefore, conductivity of silver paste is improved.

Description

A kind of preparation method who contains the solar cell conductive mixed slurry of dioctyl phthalate
Technical field
The present invention relates to the fine Electronic field of chemicals, is exactly a kind of preparation method who contains the solar cell conductive mixed slurry of dioctyl phthalate.
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 preparation method who contains the solar cell conductive mixed slurry of dioctyl phthalate.
Above-mentioned purpose realizes by following scheme:
A kind of preparation method who contains the solar cell conductive mixed slurry of dioctyl phthalate is characterized in that, 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 1200-1300 ℃ of sintering 2-3h, again the gained melting charge is poured in cold water and quenched, 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, the hydrochloric acid solution that is 5-7% with concentration respectively again soaked 3-5 hour, then cleaned to neutral with deionized water, dried to such an extent that the glass dust of different-grain diameter is standby;
Described glass dust is made by the raw material of following weight parts: Sb 2O 36.6-7.9, Na 2O 5-7, Bi 2O 315-18, B 2O 37.2-9.8, Al 2O 35.8-8, SiO 212.5-14.2, K 2O 7-9, CuO 8-10, AS 2O 39.2-11.7, Co 2O 35.8-8, trees ashes 6-7;
(2) will prepare by weight each raw material blending of organic carrier A after, in 75-80 ℃ of lower stirring and dissolving, cross 500-600 order filter cloth, namely get organic carrier A standby;
Described organic carrier A is made by the raw material of following weight parts: 145 abietic resin 7-10, polyvinylpyrrolidone 2-4, butyl carbitol 12-15, terpinol 6-11, diethylene glycol monobutyl ether acetate 2-4;
(3) will prepare by weight each raw material blending of organic carrier B after, in 65-70 ℃ of lower stirring and dissolving, cross 600-800 order filter cloth, namely get organic carrier B standby;
Described organic carrier B is made by the raw material of following weight parts: polyacrylate 7-9, dimethyl succinate 18-22, diethylene glycol ether acetate 10-12, dimethyl glutarate 6-8;
(4) will prepare by weight each raw material blending of organic carrier C after, in 75-80 ℃ of lower stirring and dissolving, cross 600-800 order filter cloth, namely get organic carrier C standby;
Described organic carrier C is made by the raw material of following weight parts: methylcellulose 8-10, isopropyl alcohol 10-15, ethyl acetate 16-18, propylene glycol monobutyl ether 10-12;
(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, stirs to mix, then adds all the other preparation A material needed raw materials, mixes 3-5 hour, obtains the A material;
Described A material is made by the raw material of following weight parts: 1-5 μ m silver powder 20-25,11-15 μ m silver powder 30-35,16-25 μ m silver powder 20-25,1-5 μ m glass dust 8-10, organic carrier A 18-20, n-butanol 1-2;
(6) the prepared 20-25 μ of step (1) m glass dust is added in the prepared organic carrier B of step (3), stirring is mixed, then adds all the other preparation B material needed raw materials, mixes 2-3 hour, obtains the B material;
Described B material is made by the raw material of following weight parts: 6-10 μ m bronze 35-38,16-25 μ m bronze 30-35,20-25 μ m glass dust 8-10, organic carrier B 18-20, organic silicone oil 0.5-1.2, dibutyl maleate 2-3;
(7) the prepared 10-15 μ of step (1) m glass dust is added in the prepared organic carrier C of step (4), stirring is mixed, then adds all the other preparation C material needed raw materials, mixes 2-3 hour, obtains the C material;
Described C material is made by the raw material of following weight parts: 11-15 μ m aluminium powder 30-35,30-60nm aluminium powder 25-30,10-15 μ m glass dust 8-10, organic carrier C 18-19, epoxy linseed oil 1-2;
(8) preparation is contained each raw material mixing by weight of the solar cell conductive mixed slurry of dioctyl phthalate, ball milling is ground to the slurry fineness less than 10 μ m, transfers viscosity, and viscosity is 120-200Pas, and get final product;
The solar cell conductive mixed slurry that contains dioctyl phthalate is that the raw material by following weight parts makes:
A expects 52-56, and B expects 18-20, and C expects 22-25, silane coupler KH602 2-3, organic silicone oil 1-2, polyamide wax 1-2, dioctyl phthalate 1-2.
Described a kind of preparation method who contains the solar cell conductive mixed slurry of dioctyl phthalate, it is characterized in that: described silver powder is flake silver powder.
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, the silver powder of different-grain diameter and bronze, aluminium powder have been selected simultaneously, increase interparticle contact area, thereby improved the conductive capability of silver-colored slurry;
2, the present invention has added aluminium powder and can help to reduce silver slurry production cost in electrocondution slurry, 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 preparation method who contains the solar cell conductive mixed slurry of dioctyl phthalate comprises the following steps:
(1) by weight (kg) takes required each raw material of preparation glass dust and puts into mixing in silica crucible, after put into electric furnace in 1200 ℃ of sintering 3h, again the gained melting charge is poured in cold water and quenched, 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, be that 5% hydrochloric acid solution soaked 3-5 hour with concentration respectively again, then clean to neutral with deionized water, dry to such an extent that the glass dust of different-grain diameter is standby;
Described glass dust is made by the raw material of following weight parts: Sb 2O 37.9, Na 2O 7, Bi 2O 318, B 2O 39.8, Al 2O 38, SiO 214.2, K 2O 9, and CuO 10, AS 2O 311.7, Co 2O 38, trees ashes 7;
(2) will prepare by weight each raw material blending of organic carrier A after, in 77 ℃ of lower stirring and dissolving, cross 500 order filter clothes, namely get organic carrier A standby;
Described organic carrier A is made by the raw material of following weight parts: 145 abietic resins 10, polyvinylpyrrolidone 2, butyl carbitol 15, terpinol 11, diethylene glycol monobutyl ether acetate 2;
(3) will prepare by weight each raw material blending of organic carrier B after, in 70 ℃ of lower stirring and dissolving, cross 800 order filter clothes, namely get organic carrier B standby;
Described organic carrier B is made by the raw material of following weight parts: polyacrylate 9, dimethyl succinate 18, diethylene glycol ether acetate 12, dimethyl glutarate 8;
(4) will prepare by weight each raw material blending of organic carrier C after, in 80 ℃ of lower stirring and dissolving, cross 800 order filter clothes, namely get organic carrier C standby;
Described organic carrier C is made by the raw material of following weight parts: methylcellulose 10, isopropyl alcohol 15, ethyl acetate 16, propylene glycol monobutyl ether 12;
(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, stirs to mix, then adds all the other preparation A material needed raw materials, mixes 5 hours, obtains the A material;
Described A material is made by the raw material of following weight parts: 1-5 μ m silver powder 25,11-15 μ m silver powder 35,16-25 μ m silver powder 20,1-5 μ m glass dust 10, organic carrier A 20, n-butanol 1;
(6) the prepared 20-25 μ of step (1) m glass dust is added in the prepared organic carrier B of step (3), stirring is mixed, then adds all the other preparation B material needed raw materials, mixes 3 hours, obtains the B material;
Described B material is made by the raw material of following weight parts: 6-10 μ m bronze 38,16-25 μ m bronze 30,20-25 μ m glass dust 8, organic carrier B 20, organic silicone oil 1.2, dibutyl maleate 3;
(7) the prepared 10-15 μ of step (1) m glass dust is added in the prepared organic carrier C of step (4), stirring is mixed, then adds all the other preparation C material needed raw materials, mixes 2 hours, obtains the C material;
Described C material is made by the raw material of following weight parts: 11-15 μ m aluminium powder 35,30-60nm aluminium powder 30,10-15 μ m glass dust 10, organic carrier C 19, epoxy linseed oil 2;
(8) preparation is contained each raw material mixing by weight of the solar cell conductive mixed slurry of dioctyl phthalate, ball milling is ground to the slurry fineness less than 10 μ m, transfers viscosity, and viscosity is 200Pas, and get final product;
The solar cell conductive mixed slurry that contains dioctyl phthalate is that the raw material by following weight parts makes:
A material 56, B material 20, C material 25, silane coupler KH602 3, organic silicone oil 2, polyamide wax 1, dioctyl phthalate 1.
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 15 N/cm, soldering is functional, sheet resistance<10 Siements/sq, the solar cell photoelectric transformation efficiency of preparation is 19.3%, the tensile test result is adhesive force〉13N/mm 2

Claims (2)

1. a preparation method who contains the solar cell conductive mixed slurry of dioctyl phthalate, is characterized in that, 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 1200-1300 ℃ of sintering 2-3h, again the gained melting charge is poured in cold water and quenched, 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, the hydrochloric acid solution that is 5-7% with concentration respectively again soaked 3-5 hour, then cleaned to neutral with deionized water, dried to such an extent that the glass dust of different-grain diameter is standby;
Described glass dust is made by the raw material of following weight parts: Sb 2O 36.6-7.9, Na 2O 5-7, Bi 2O 315-18, B 2O 37.2-9.8, Al 2O 35.8-8, SiO 212.5-14.2, K 2O 7-9, CuO 8-10, AS 2O 39.2-11.7, Co 2O 35.8-8, trees ashes 6-7;
(2) will prepare by weight each raw material blending of organic carrier A after, in 75-80 ℃ of lower stirring and dissolving, cross 500-600 order filter cloth, namely get organic carrier A standby;
Described organic carrier A is made by the raw material of following weight parts: 145 abietic resin 7-10, polyvinylpyrrolidone 2-4, butyl carbitol 12-15, terpinol 6-11, diethylene glycol monobutyl ether acetate 2-4;
(3) will prepare by weight each raw material blending of organic carrier B after, in 65-70 ℃ of lower stirring and dissolving, cross 600-800 order filter cloth, namely get organic carrier B standby;
Described organic carrier B is made by the raw material of following weight parts: polyacrylate 7-9, dimethyl succinate 18-22, diethylene glycol ether acetate 10-12, dimethyl glutarate 6-8;
(4) will prepare by weight each raw material blending of organic carrier C after, in 75-80 ℃ of lower stirring and dissolving, cross 600-800 order filter cloth, namely get organic carrier C standby;
Described organic carrier C is made by the raw material of following weight parts: methylcellulose 8-10, isopropyl alcohol 10-15, ethyl acetate 16-18, propylene glycol monobutyl ether 10-12;
(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, stirs to mix, then adds all the other preparation A material needed raw materials, mixes 3-5 hour, obtains the A material;
Described A material is made by the raw material of following weight parts: 1-5 μ m silver powder 20-25,11-15 μ m silver powder 30-35,16-25 μ m silver powder 20-25,1-5 μ m glass dust 8-10, organic carrier A 18-20, n-butanol 1-2;
(6) the prepared 20-25 μ of step (1) m glass dust is added in the prepared organic carrier B of step (3), stirring is mixed, then adds all the other preparation B material needed raw materials, mixes 2-3 hour, obtains the B material;
Described B material is made by the raw material of following weight parts: 6-10 μ m bronze 35-38,16-25 μ m bronze 30-35,20-25 μ m glass dust 8-10, organic carrier B 18-20, organic silicone oil 0.5-1.2, dibutyl maleate 2-3;
(7) the prepared 10-15 μ of step (1) m glass dust is added in the prepared organic carrier C of step (4), stirring is mixed, then adds all the other preparation C material needed raw materials, mixes 2-3 hour, obtains the C material;
Described C material is made by the raw material of following weight parts: 11-15 μ m aluminium powder 30-35,30-60nm aluminium powder 25-30,10-15 μ m glass dust 8-10, organic carrier C 18-19, epoxy linseed oil 1-2;
(8) preparation is contained each raw material mixing by weight of the solar cell conductive mixed slurry of dioctyl phthalate, ball milling is ground to the slurry fineness less than 10 μ m, transfers viscosity, and viscosity is 120-200Pas, and get final product;
The solar cell conductive mixed slurry that contains dioctyl phthalate is that the raw material by following weight parts makes:
A expects 52-56, and B expects 18-20, and C expects 22-25, silane coupler KH602 2-3, organic silicone oil 1-2, polyamide wax 1-2, dioctyl phthalate 1-2.
2. a kind of preparation method who contains the solar cell conductive mixed slurry of dioctyl phthalate according to claim 1, it is characterized in that: described silver powder is flake silver powder.
CN201210521989.1A 2012-12-07 2012-12-07 A kind of preparation method of the solar cell conductive mixed slurry containing dioctyl phthalate Active CN103117135B (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108492911A (en) * 2018-03-13 2018-09-04 合肥择浚电气设备有限公司 Low volatilization electrocondution slurry and preparation method thereof is stablized in a kind of battery environmental protection

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CN101615637A (en) * 2009-07-08 2009-12-30 西安交通大学苏州研究院 Electrode of solar battery forms with slurry and preparation method thereof
CN101950594A (en) * 2010-09-20 2011-01-19 浙江大学 Lead-free environment-friendly electronic Ag/Al (silver/aluminum) paste and preparation method thereof
CN102097154A (en) * 2010-11-25 2011-06-15 长沙族兴金属颜料有限公司 Back surface field aluminium paste for solar cells
US20120000523A1 (en) * 2008-06-04 2012-01-05 Lg Chem, Ltd. Metal paste composition for forming electrode and silver-carbon composite electrode and silicon solar cell using the same
CN102585125A (en) * 2012-02-17 2012-07-18 广州三则电子材料有限公司 Method for preparing thermoset phenolic resin and method for preparing conductive slurry

Patent Citations (5)

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Publication number Priority date Publication date Assignee Title
US20120000523A1 (en) * 2008-06-04 2012-01-05 Lg Chem, Ltd. Metal paste composition for forming electrode and silver-carbon composite electrode and silicon solar cell using the same
CN101615637A (en) * 2009-07-08 2009-12-30 西安交通大学苏州研究院 Electrode of solar battery forms with slurry and preparation method thereof
CN101950594A (en) * 2010-09-20 2011-01-19 浙江大学 Lead-free environment-friendly electronic Ag/Al (silver/aluminum) paste and preparation method thereof
CN102097154A (en) * 2010-11-25 2011-06-15 长沙族兴金属颜料有限公司 Back surface field aluminium paste for solar cells
CN102585125A (en) * 2012-02-17 2012-07-18 广州三则电子材料有限公司 Method for preparing thermoset phenolic resin and method for preparing conductive slurry

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108492911A (en) * 2018-03-13 2018-09-04 合肥择浚电气设备有限公司 Low volatilization electrocondution slurry and preparation method thereof is stablized in a kind of battery environmental protection

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