CN103117134B - A kind of preparation method of the solar cell conductive mixed slurry containing butyl stearate - Google Patents
A kind of preparation method of the solar cell conductive mixed slurry containing butyl stearate Download PDFInfo
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- CN103117134B CN103117134B CN201210521988.7A CN201210521988A CN103117134B CN 103117134 B CN103117134 B CN 103117134B CN 201210521988 A CN201210521988 A CN 201210521988A CN 103117134 B CN103117134 B CN 103117134B
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Abstract
The invention discloses a kind of solar cell conductive mixed slurry containing butyl stearate, it it is to be prepared by the raw material of following weight parts: A material 42 45, B material 28 30, C material 8 10, graphite powder 0.9 1.6, epoxyfuoic-oleic 0.3 0.4, organic silicone oil 0.7 1.2, silane coupler kh791 12, acetyl triethyl citrate 0.2 0.4, triacetin 0.2 0.5, Tissuemat E 0.5 0.7.The electrocondution slurry of gained of the present invention is the most leaded, comply fully with environmental requirement, it is applied to the production of solaode, can form in solar cell surface that adhesive force is strong, cell photoelectric conversion efficiency high, selected the argentum powder 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 fine Electronic field of chemicals, be exactly a kind of solaode containing butyl stearate
The preparation method of conduction mixed slurry.
Background technology
Electrocondution slurry is electronic devices and components encapsulation, electrode and the critical material of interconnection, mainly includes burning infiltration type electrocondution slurry
Class big with curing type conducting resinl (electrically conductive ink) two.
Burning infiltration type electrocondution slurry is used primarily in the industries such as solaode, makees electrode and use after sintering, curing type conductive oil
Ink is widely used in the industry such as printed circuit and Electronic Packaging.
Electrocondution slurry is different according to filler therein, and carbon can be divided into starch (graphite conductor), metal paste (bronze, argentum powder,
Copper powder, yellow gold), and the ceramic size of modification.
Performance comparision, the electric conductivity of noble metal filler is best, and carbon slurry is secondly.But the price of gold is the highest, the resistance to oxidation of copper powder
Property is bad, and argentum powder and silver-bearing copper powder more equalize in price and performance.Getting well of the wearability silver slurry of carbon slurry.
Solar cell conductive paste is made up of argentum powder, aluminium powder, inorganic bond material, organic carrier and related auxiliaries etc..?
In most electric slurry, inorganic bond material be mainly the lead bearing glass powder of low melting point, big for environment pollution and weldability
Difference is its major defect.Therefore, the unleaded of electrocondution slurry has become inexorable trend.
Summary of the invention
It is an object of the invention to provide the preparation of a kind of solar cell conductive mixed slurry containing butyl stearate
Method.
Above-mentioned purpose is realized by below scheme:
The preparation method of a kind of solar cell conductive mixed slurry containing butyl stearate, it is characterised in that include
Following steps:
(1) weigh by weight prepare glass dust needed for each raw material put in silica crucible mix, after put in electric furnace in
1200-1300 DEG C of sintering 2-3h, then gained melting charge is poured into cold quenching-in water, ball milling, cross the sieve of different meshes, collect respectively
Obtain 1-5 μm glass dust, 10-15 μm glass dust and 20-25 μm glass dust, more respectively with the hydrofluoric acid solution leaching that concentration is 3-4%
Steep 3-5 hour, be then washed with deionized water clean to neutral, dry the glass dust of different-grain diameter is standby；
Described glass dust is prepared by the raw material of following weight parts: V2O5 12-14, AS2O36-8, Bi2O3 7-9,
SnO2 5-7, Al2O3 5-8,SiO2 13-15, TiO27-10, MgO 6-8, SnO2 12-15, B2O37.3-8.9；
(2) after each raw material blending of organic carrier A being prepared by weight, stirring and dissolving at 75-80 DEG C, cross 500-
600 mesh filter clothes, obtain organic carrier A standby；
Described organic carrier A is prepared by the raw material of following weight parts: 138 rosin resin 9-11, polyvinylpyrrolidone
2-4, benzyl alcohol 15-18, isopropanol 18-20；
(3) after each raw material blending of organic carrier B being prepared by weight, stirring and dissolving at 65-70 DEG C, cross 600-
800 mesh filter clothes, obtain organic carrier B standby；
Described organic carrier B is prepared by the raw material of following weight parts: celluloid 6-8, diethylene glycol dimethyl ether 18-
20, diethylene glycol ether acetate 10-12, ethylene glycol phenyl ether 2-4；
(4) after each raw material blending of organic carrier C being prepared by weight, stirring and dissolving at 75-80 DEG C, cross 600-
800 mesh filter clothes, obtain organic carrier C standby；
Described organic carrier C is prepared by the raw material of following weight parts: C5 Petropols 8-10, glycol monoethyl ether 15-
18, ethyl acetate 18-21；
(5) glass dust of the 1-5 μm obtained by step (1) is added the organic carrier A obtained by step (2) by weight
In, stirring mixing, add remaining and prepare A material needed raw material, stirring mixing 3-5 hour, obtain A material；
Described A material is prepared by the raw material of following weight parts: 1-5 μm argentum powder 40-42,11-15 μm argentum powder 18-22,16-25
μm argentum powder 10-15,1-5 μm glass dust 8-12, organic carrier A 15-20, silane coupler KH580 1-1.5, tributyl phosphate
1-2；
(6) the 10-15 μm glass dust obtained by step (1) is added in the organic carrier B obtained by step (3), stirring
Mixing, adds remaining and prepares B material needed raw material, stirring mixing 2-3 hour, obtain B material；
Described B material is prepared by the raw material of following weight parts: 6-10 μm bronze 45-48,16-25 μm bronze 20-25,10-
15 μm glass dust 8-10, organic carrier B 18-22, butyl stearate 0.8-1.2, diethyl phthalate 1-2；
(7) the 20-25 μm glass dust obtained by step (1) is added in the organic carrier C obtained by step (4), stirring
Mixing, adds remaining and prepares C material needed raw material, stirring mixing 2-3 hour, obtain C material；
Described C material is prepared by the raw material of following weight parts: 11-15 μm copper powder 30-35,16-25 μm copper powder 30-35,30-
60nm bronze 15-20,20-25 μm glass dust 9-11, organic carrier C 18-20, organosilicon levelling agent 1-2；
(8) each raw material of the solar cell conductive mixed slurry that preparation is contained butyl stearate mixes by weight,
Ball milling, is ground to slurry fineness and is less than 10 μm, adjust viscosity, and viscosity is 120-200Pa s, to obtain final product；
Solar cell conductive mixed slurry containing butyl stearate is to be prepared by the raw material of following weight parts:
A expects that 42-45, B material 28-30, C expect 8-10, graphite powder 0.9-1.6, epoxyfuoic-oleic 0.3-0.4, organosilicon
Oil 0.7-1.2, silane coupler kh791 1-2, acetyl triethyl citrate 0.2-0.4, triacetin 0.2-0.5, poly-
Ethylene waxes 0.5-0.7.
The preparation method of described a kind of solar cell conductive mixed slurry containing butyl stearate, its feature exists
In: described argentum powder is flake silver powder.
The invention have the benefit that
1, the electrocondution slurry of gained of the present invention is the most leaded, complies fully with environmental requirement, is applied to the production of solaode,
Can form in solar cell surface that adhesive force is strong, cell photoelectric conversion efficiency high, selected simultaneously the argentum powder of different-grain diameter with
Bronze, copper powder, increase interparticle contact area, thus improve the conductive capability of silver slurry；
2, the present invention with the addition of copper powder in electrocondution slurry, it is possible to contributes to reducing silver slurry production cost, saves substantial amounts of
Noble silver, improves the electric conductivity of silver slurry simultaneously, thus has reached to reduce the purpose of solaode manufacturing cost, achieve
Good economic benefit.Present invention process is simple simultaneously, low cost, thus has broad application prospects.
Detailed description of the invention
The preparation method of a kind of solar cell conductive mixed slurry containing butyl stearate, comprises the following steps:
(1) weigh by weight prepare glass dust needed for each raw material put in silica crucible mix, after put in electric furnace in
1300 DEG C of sintering 3h, then gained melting charge is poured into cold quenching-in water, ball milling, cross the sieve of different meshes, collect respectively and obtain 1-5
μm glass dust, 10-15 μm glass dust and 20-25 μm glass dust, then soak 5 hours with the hydrofluoric acid solution that concentration is 4% respectively,
Then be washed with deionized water clean to neutral, dry the glass dust of different-grain diameter is standby；
Described glass dust is prepared by the raw material of following weight parts (kg): V2O5 14, AS2O38, Bi2O3 9, SnO2
7, Al2O3 5,SiO2 15, TiO210, MgO 8, SnO2 15, B2O38.9；
(2) after each raw material blending of organic carrier A being prepared by weight, stirring and dissolving at 80 DEG C, cross 500 mesh filters
Cloth, obtains organic carrier A standby；
Described organic carrier A is prepared by the raw material of following weight parts: 138 rosin resins 11, polyvinylpyrrolidone 2,
Benzyl alcohol 18, isopropanol 20；
(3) after each raw material blending of organic carrier B being prepared by weight, stirring and dissolving at 70 DEG C, cross 800 mesh filters
Cloth, obtains organic carrier B standby；
Described organic carrier B is prepared by the raw material of following weight parts: celluloid 8, diethylene glycol dimethyl ether 20, diethyl
Glycol ether acetate 12, ethylene glycol phenyl ether 3；
(4) after each raw material blending of organic carrier C being prepared by weight, stirring and dissolving at 80 DEG C, cross 600 mesh filters
Cloth, obtains organic carrier C standby；
Described organic carrier C is prepared by the raw material of following weight parts: C5 Petropols 10, glycol monoethyl ether 18, second
Acetoacetic ester 21；
(5) glass dust of the 1-5 μm obtained by step (1) is added the organic carrier A obtained by step (2) by weight
In, stirring mixing, add remaining and prepare A material needed raw material, stirring mixing 5 hours, obtain A material；
Described A material is prepared by the raw material of following weight parts: 1-5 μm argentum powder 42,11-15 μm argentum powder 22,16-25 μm argentum powder
15,1-5 μm glass dust 12, organic carrier A 20, silane coupler KH580 1.5, tributyl phosphate 2；
(6) the 10-15 μm glass dust obtained by step (1) is added in the organic carrier B obtained by step (3), stirring
Mixing, adds remaining and prepares B material needed raw material, stirring mixing 3 hours, obtain B material；
Described B material is prepared by the raw material of following weight parts: 6-10 μm bronze 48,16-25 μm bronze 25,10-15 μm glass
Glass powder 10, organic carrier B 22, butyl stearate 1.2, diethyl phthalate 2；
(7) the 20-25 μm glass dust obtained by step (1) is added in the organic carrier C obtained by step (4), stirring
Mixing, adds remaining and prepares C material needed raw material, stirring mixing 2 hours, obtain C material；
Described C material is prepared by the raw material of following weight parts: 11-15 μm copper powder 35,16-25 μm copper powder 35,30-60nm gold
Powder 20,20-25 μm glass dust 11, organic carrier C 20, organosilicon levelling agent 2；
(8) each raw material of the solar cell conductive mixed slurry that preparation is contained butyl stearate mixes by weight,
Ball milling, is ground to slurry fineness and is less than 10 μm, adjust viscosity, and viscosity is 170Pa s, to obtain final product；
Solar cell conductive mixed slurry containing butyl stearate is to be prepared by the raw material of following weight parts (kg):
A material 45, B material 30, C material 10, graphite powder 1.3, epoxyfuoic-oleic 0.4, organic silicone oil 1.2, silane coupler
Kh791 2, acetyl triethyl citrate 0.4, triacetin 0.5, Tissuemat E 0.5.
Use screen process press to be printed on 125mm × 125mm Si substrate by silver slurry, be then dried at 180 DEG C, then
880 DEG C carry out quick fired electrodes lead-in wire, the contact conductor surface silvery white made after high temperature sintering, and smooth zero defect is peeled off strong
Spending 15 N/cm, soldering is functional, sheet resistance ＜ 10 Siements/sq, and the solar cell photoelectric transformation efficiency of preparation is
18.7%, tensile test result is adhesive force > 13N/mm2。
Claims (2)
1. the preparation method of solar cell conductive mixed slurry containing butyl stearate, it is characterised in that include with
Lower step:
(1) weigh by weight prepare glass dust needed for each raw material put in silica crucible mix, after put in electric furnace in 1200-
1300 DEG C of sintering 2-3h, then gained melting charge is poured into cold quenching-in water, ball milling, cross the sieve of different meshes, collect respectively and obtain
1-5 μm glass dust, 10-15 μm glass dust and 20-25 μm glass dust, then soak 3-with the hydrofluoric acid solution that concentration is 3-4% respectively
5 hours, be then washed with deionized water clean to neutral, dry the glass dust of different-grain diameter is standby；Described glass dust is by following
The raw material of weight portion prepares: V2O5 12-14, As2O36-8, Bi2O3 7-9, SnO2 5-7, Al2O35-8, SiO213-15,
TiO27-10, MgO 6-8, B2O37.3-8.9；
(2) after each raw material blending of organic carrier A being prepared by weight, stirring and dissolving at 75-80 DEG C, cross 500-600 mesh
Filter cloth, obtains organic carrier A standby；Described organic carrier A is prepared by the raw material of following weight parts: 138 rosin resin 9-
11, polyvinylpyrrolidone 2-4, benzyl alcohol 15-18, isopropanol 18-20；
(3) after each raw material blending of organic carrier B being prepared by weight, stirring and dissolving at 65-70 DEG C, cross 600-800 mesh
Filter cloth, obtains organic carrier B standby；Described organic carrier B is prepared by the raw material of following weight parts: celluloid 6-8,
Diethylene glycol dimethyl ether 18-20, diethylene glycol ether acetate 10-12, ethylene glycol phenyl ether 2-4；
(4) after each raw material blending of organic carrier C being prepared by weight, stirring and dissolving at 75-80 DEG C, cross 600-800 mesh
Filter cloth, obtains organic carrier C standby；Described organic carrier C is prepared by the raw material of following weight parts: C5 Petropols 8-10,
Glycol monoethyl ether 15-18, ethyl acetate 18-21；
(5) glass dust of the 1-5 μm obtained by step (1) is added in the organic carrier A obtained by step (2) by weight,
Stirring mixing, adds remaining and prepares A material needed raw material, stirring mixing 3-5 hour, obtain A material；Described A expects by following heavy
The raw material of amount part prepares: 1-5 μm argentum powder 40-42,11-15 μm argentum powder 18-22,16-25 μm argentum powder 10-15,1-5 μm glass dust 8-
12, organic carrier A 15-20, silane coupler KH580 1-1.5, tributyl phosphate 1-2；
(6) the 10-15 μm glass dust obtained by step (1) is added in the organic carrier B obtained by step (3), stirring mixing,
Add remaining and prepare B material needed raw material, stirring mixing 2-3 hour, obtain B material；Former by following weight parts of described B material
Material prepares: 6-10 μm bronze 45-48,16-25 μm bronze 20-25,10-15 μm glass dust 8-10, organic carrier B 18-22, hard
Fat acid butyl ester 0.8-1.2, diethyl phthalate 1-2；
(7) the 20-25 μm glass dust obtained by step (1) is added in the organic carrier C obtained by step (4), stirring mixing,
Add remaining and prepare C material needed raw material, stirring mixing 2-3 hour, obtain C material；Former by following weight parts of described C material
Material prepares: 11-15 μm copper powder 30-35,16-25 μm copper powder 30-35,30-60nm bronze 15-20,20-25 μm glass dust 9-
11, organic carrier C 18-20, organosilicon levelling agent 1-2；
(8) each raw material of the solar cell conductive mixed slurry that preparation is contained butyl stearate mixes by weight, ball milling,
Being ground to slurry fineness and be less than 10 μm, adjust viscosity, viscosity is 120-200Pa s, to obtain final product；Solar energy containing butyl stearate
Battery conductive mixed slurry is to be prepared by the raw material of following weight parts: A expects that 42-45, B material 28-30, C expect 8-10, graphite powder
0.9-1.6, epoxyfuoic-oleic 0.3-0.4, organic silicone oil 0.7-1.2, silane coupler kh791 1-2, acetyl tributyl citrate
Triethyl 0.2-0.4, triacetin 0.2-0.5, Tissuemat E 0.5-0.7.
The preparation side of a kind of solar cell conductive mixed slurry containing butyl stearate the most according to claim 1
Method, it is characterised in that: described argentum powder is flake silver powder.
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| CN110510883B (en) * | 2019-08-16 | 2022-05-03 | 江苏聚盈新材料科技有限公司 | Vanadium-based lead-free glass powder and preparation method and application thereof |
| CN112358191A (en) * | 2020-11-11 | 2021-02-12 | 上海大洲电子材料有限公司 | Formula, preparation and surface modification methods of lead-free low-melting-point glass powder for conductive paste |
Citations (4)
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| CN1901234A (en) * | 2006-07-17 | 2007-01-24 | 谭富彬 | Synthesizing silicon solar energy cell back field aluminum conductive size |
| 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 |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2011034894A (en) * | 2009-08-05 | 2011-02-17 | Hitachi Chem Co Ltd | Cu-Al ALLOY POWDER, ALLOY PASTE USING IT, AND ELECTRONIC PARTS |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1901234A (en) * | 2006-07-17 | 2007-01-24 | 谭富彬 | Synthesizing silicon solar energy cell back field aluminum conductive size |
| 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 |
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Effective date of registration: 20201210 Address after: 402460 station 13, 10 / F, innovation and development center, 19 Lingfang Avenue, Changzhou street, Rongchang District, Chongqing Patentee after: Chongqing Xinrui Technology Service Co.,Ltd. Address before: 401120 Chongqing Yubei District Shuangfeng Bridge Street 3 East Road 7 buildings Patentee before: Chongqing Beijing Great Automotive Components Co.,Ltd. |