CN1901234A - Synthesizing silicon solar energy cell back field aluminum conductive size - Google Patents
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- CN1901234A CN1901234A CNA2006100110505A CN200610011050A CN1901234A CN 1901234 A CN1901234 A CN 1901234A CN A2006100110505 A CNA2006100110505 A CN A2006100110505A CN 200610011050 A CN200610011050 A CN 200610011050A CN 1901234 A CN1901234 A CN 1901234A
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Abstract
This invention relates to a method for preparing Al conductive sizing materials used in back field of silicon solar energy batteries synthesized chemically, in which, the sizing material includes(mass percentage) Al powder 78-80%, modified organic bond 30-20%, In powder 0.15-5.0% and glass 0.1-5.0% to be prepared to get the product. The inorganic bond glass raw material is got by adding B powder, dimethylsilicone and stearate when preparing the sizing material and sintering it to a film then to be oxidized and analyzed further to be synthesized to an inorganic bond glass, said sizing material has the advantages of high photoelectric transformation rate, good conductivity and stick adherence to silicon matrixes, the monocrystalline silicon of 125x125mm or 156x156mm with thickness smaller than 210 mumm is slightly curved and polycrystalline silicon of 156x156mm is not curved.
Description
One, technical field: the method with chemical synthesis prepares electronic information material-aluminum conductive electric slurry, belongs to the fine chemistry preparation field.
Two, background technology: aluminum conductive electric slurry belongs to one of electronic information material, and silicon solar cell is inexhaustible a kind of environmental protection regenerative resource.Research is very active in the world, purpose solves the photoelectric conversion efficiency of battery, the aluminium film adheres to the jail to silicon substrate before and after sintering, not crooked behind the thin silicon sheet sintering, do not play the pill of aluminium, do not blister after forming silicoaluminate, do not play " aluminium ash " during assembly and after EVA (the rare and rare copolymer of acetic acid second of the second) bonding.Also to solve not leaded or few leaded problem in the slurry composition in addition.
" the high efficiency, low cost monocrystaline silicon solar cell and the special-purpose electrocondution slurry thereof " of known Kunming Institute of Precious Metals research is with Ag powder, Al alloyed powder, glass dust, in the Ag powder, mix and have Gorgon euryale nurse contact functional element, add organic carrier and be rolled into slurry, machine test and application on the semiconductor of Yunnan, photoelectric conversion rate is greater than 13.20%.The solar module (number of patent application 200510056540.2) of Sanyo Electric Co., Ltd's invention, to improve the solar cell device electrode and to apply by the caking property between the jointing of lead-free solder, this electrode becomes with the thermosetting tree finger-type that contains silver paste, the electrode of solar cell device is made of the silver paste that comprises thermosetting resin and silver powder, and thermosetting resin contains volume ratio 70% or manyly records glass transition temperature at 80-200 ℃ epoxy resin by TMA (thermodynamic analysis) method.Application number is 00310113250.8, name is called a kind of preparation method of slurry and the invention of application thereof, the preparation method who relates to a kind of slurry, be about to slurry viscosity conditioning agent, slurry dispersant, surfactant dissolves in solvent, form liquid mixture, then this liquid mixture and pressed powder are mixed, thereby prepare the slurry of this pressed powder.This slurry is all good dispersion of a kind of stability of monodispersity, can be used for preparing the solid film of porous.
Inorganic binder in the slurry (glass) generally is to mix with oxide (metal or nonmetal), and melting at high temperature, shrend, broken back ball milling become borosilicate glass powder.Glass preparation is a very long course of processing, and the steam that produces in the process, dust pollute the environment and influence the healthy of workman.Crystalline silicon (monocrystalline or polycrystalline) battery electrode all is the old technology of high temperature melting with inorganic binder (glass), comprises the silver slurry of Kunming Institute of Precious Metals and Yunnan Semiconductor factory exploitation, silver-colored aluminium paste and aluminium paste, the silver slurry of Beijing Non-Ferrous Metal Research General Academy's development, aluminium paste.Patent application such as CN1744331, CN1694268, do not refer to the preparation method of inorganic binder glass yet, the Chinese patent CN1652354 of SANYO GS application, essence be thermosetting resin cured temperature (vitrifying) at 80-200 ℃, rather than the vitrification point of inorganic binder glass.The CN1606175 patent of Japanese Sharp company application is not referred to the manufacture method of glass yet.This shows, with oxidations at high temperature such as stearate (magnesium, calcium, lead, aluminium, zinc), dimethyl siloxane, element borons, resolve into MgO, CaO, PbO, Al
2O
3, ZnO, SiO
2, B
2O
3, the method that generates borosilicate glass is not then simultaneously appeared in the newspapers.
The present invention improves formula of size, intermediate composition, processing method exactly, to improve aluminium film before and after cell photoelectric conversion efficiency, the sintering slight curving less than the monocrystalline silicon of 125 * 125mm of 210 microns or 156 * 156mm to silicon substrate adhesion-tight, thickness to reach, and the polysilicon of 156 * 156mm is not crooked, aluminium film surface is smooth, do not play the pill of aluminium, do not blister, the EVA bonding can not peeled off not peeling of ash, lead content is controlled between the 0-500ppm, compliance with environmental protection requirements.
Three, summary of the invention
1, the purpose of this invention is to provide the preparation method of the synthetic silicon solar cell back surface field of a kind of chemical method with aluminum conductive electric slurry, this slurry comprises the aluminium powder of mass percent 70-80%, the modification organic bond of 30-20%, the indium powder of 0.1-5.0%, 0.1-5.0% glass, glass is by preparation during slurry, add the boron powder simultaneously, dimethyl siloxane, stearate, simultaneous oxidation in slurry sintering film forming, decompose and obtain frit, and a step synthesizing inorganic adhesive glass, it is simple that this slurry has preparation, and conductivity is good, to the characteristics of silicon substrate adhesion-tight, be low leaded or unleaded environment-friendly type slurry.
2, technical scheme
1) composition of slurry and prescription: by mass percent 70-80%, 15-30% modification organic bond, indium powder 0.1-5.0%, inorganic bond glass 0.1-5.0 forms, total amount 100%.
(1) aluminium powder is purity 99.9-99.99%, and its average grain diameter is 6.0-8.0 μ m, and surface coverage has the ball aluminum powder of the aln layer of 3-5 nanometer thickness, apparent density 0.60-0.85g/cc, specific area 0.70-1.00M
2/ g;
(2) the modification organic bond is ethyl cellulose 1-5% by mass percentage, phenolic resins or novolac epoxy resin 0.5-10.0%, rosin 0.1-2.0%, butyl stearate 1.0-10.0%, terpinol 30-60%, additive 30-50%, total amount 100%: wherein additive comprises one or more in ethylene glycol phenyl ether, diethyl phthalate, diethylene glycol monobutyl ether, diethylene glycol monobutyl ether acetate, the phenmethylol;
(3) the indium powder is selected commercially available purity 〉=99.99% for use, the ready-made article of particle mean size≤8.0 μ m.
(4) composition of inorganic bond glass
A, flint glass raw material are formed (mass percent)
B
2O
3 10-30％、PbO 40-70％、SiO
2 10-20％、Al
2O
3 10-15％、V
2O
5 3-5％。
More than these oxides remove V
2O
5All in the slurry sintering process, decompose acquisition outward, by the oxidation of boron powder, dimethyl siloxane, lead stearate, the aluminum stearate that adds in the slurry in advance.
B, crown glass are formed (mass percent)
B
2O
3 30-50％、MgO 10-15％、CaO 3-10％、Al
2O
3 10-15％、SiO
2 15-20％、ZnO 5-10％、V
2O
52-5％。
More than these oxides remove V
2O
5Outward, all by adding the oxidation of boron powder, dimethyl siloxane, dolomol, calcium stearate, aluminum stearate, the zinc stearate in the slurry in advance, oxidation Decomposition obtains in the slurry sintering process.
When two glass ingredients of a, b obtain, at high temperature also synthesized inorganic bond glass.
2) preparation of slurry each component
(1) by the prescription of above-mentioned organic bond, under 80-150 ℃ of temperature, dissolves, get the organic bond of transparent modification.
(2) preparation of glass component
A, add purity 〉=99.99% during slurry in preparation, granularity≤8.0 μ m boron powder, oxidation gets diboron trioxide (450 ℃ of fusing points) during the slurry sintering;
B, add dimethyl siloxane during slurry in preparation, the slurry sintering time-division solves silicon dioxide;
(n＝100-2000)
C, add lead stearate during slurry in preparation, slurry decomposes acquisition lead oxide in sintering process;
D, add aluminum stearate during slurry in preparation, slurry divides in sintering process and solves aluminium oxide;
E, add zinc stearate during slurry in preparation, slurry divides in sintering process and solves zinc oxide;
F, add dolomol during slurry in preparation, slurry divides in sintering process and solves magnesium oxide.
G, add calcium stearate during slurry in preparation, slurry divides in sintering process and solves calcium oxide.
H, commercially available vanadic oxide purity are AR, the commercially available vanadic oxide of granularity≤5.0 μ m.
3) preparation of aluminum conductive electric slurry
The aluminium powder 70-80 quality % that is wrapped up by aluminium nitride, modification organic bond 15-30 quality %, indium powder 0.1-5 quality %, glass 0.1-5 quality % (flint glass by chemical equation 1., 2., 3., the oxide that 4. produces and the V that adds
2O
5Form, crown glass by chemical equation 1., 2., 4., 5., 6., the oxide that 7. produces and the V that adds
2O
5Form, total amount 100%) mixing is back with the rolling fineness 15-18 μ m that is ground to of three-high mill, viscosity 25000-35000mPa fiber S, must grind the back aluminum conductive electric slurry, through the silk screen printing oven dry, get the aluminium conducting film behind the sintering, stearate, dimethyl siloxane, boron powder solve oxide at simultaneous oxidation, the branch of sintering film forming, and fusion becomes glass and participates in reaction, makes glass, one step of aluminium conducting film synthetic.
3, compare advantage and the good effect that has with known technology
(1) add phenolic resins, novolac epoxy resin in organic adhesion agent, make aluminium film oven dry back (before the sintering) that adhesion strength be arranged with the thermosetting resin modification, the aluminium film does not come off;
(2) add natural resin rosin, burn during sintering, produce reducing atmosphere, the not oxidation of protection aluminium improves the aluminium film conductivity;
(3) use butyl stearate to improve the net performance excessively of slurry as lubricant;
(4) in order to improve the photoelectric conversion efficiency of battery, add the In functional element in aluminium paste, making between aluminium electrode and the silicon has good Ohmic contact, thereby improves photoelectric conversion efficiency, and the silicoaluminate layer also can improve the aluminium film to the silicon substrate adhesive strength;
(5) aluminium powder is a slurry critical function phase, the aluminium powder that the present invention uses purity 99.9-99.99% aluminium ingot to make, surface coverage has the aln layer of 3-5 nanometer thickness, with the slurry of such aluminium powder preparation except that satisfying the electrical property, bending is little after can also making the silicon chip sintering, do not play the pill of aluminium, do not blister when forming silicoaluminate, the aluminium film is smooth;
(6) preparation frit of the present invention, be by preparation during slurry except that vanadic oxide, add boron powder, dimethyl siloxane, chemical pure stearate simultaneously, obtain frit in the simultaneous oxidation of sintering film forming, decomposition, an and step synthesizing inorganic adhesive glass, simplified traditional glass melting processing technology like this, saved time, economized energy, province's equipment, few factory building, reduced the pollution of dust, steam environment.Glass adheres to well matrix, side's resistance 8.0-12m Ω/25 μ m/ mouths.
(7), slurry can be made low leaded and lead-free two kinds of products according to the different formulations of glass.
(8) The present invention be directed to silicon solar cell designs less with the aluminium paste glass content.This method also can be starched with silver-colored aluminium paste, front grid silver as silicon solar cell.Also can be used as simultaneously its electronic component slurry, as platinum slurry, gold paste, silver-colored palladium slurry, silver slurry etc., but inapplicable to PTC themistor with aluminium paste.
Comprehensively above-mentioned, raw material sources of the present invention have been bought easily, and preparation technology is simple, and environmental protection is qualified, aluminium electrode pair matrix adhesion-tight behind the sintering, and resistance is between 8.0-12m Ω/25 μ m/ mouths, and conductivity is good.
Four, embodiment
Embodiment one
1, the preparation of modification organic bond (mass ratio): 6031-2 novolac epoxy resin 7.0%, ethyl cellulose 4.0%, rosin 1.0%, butyl stearate 5.0%, terpinol 40.0%, ethylene glycol phenyl ether 15.0%, diethyl phthalate 10.0%, diethylene glycol monobutyl ether 8.0%, diethylene glycol monobutyl ether acetate 6.0%, phenmethylol 4.0%, more than in container, mix, electromagnetic oven directly be heated to 100 ℃ melted till.
2, aluminum conductive electric slurry preparation (quantity 1000g)
Aluminium powder purity 〉=99.99%, the surface is by the thick aluminium nitride parcel of 3-5nm, average grain diameter 7.5 μ m, (apparent density 0.78g/cc, specific area 0.945M
2/ g) 740g, 74.0%
Indium powder (purity 〉=99.99%, granularity≤8.0 μ m) 10g, 1.0%
Glass 10g, 1.0%
Wherein:
B
2O
32.0g account for 20%[according to 1. formula calculating of chemical reaction, add boron powder (purity 〉=99.99% granularity≤5 μ m) 0.62g]
PbO 6.0g accounted for for 60% (according to 3. formula calculating of chemical reaction, adding lead stearate 19.9g)
SiO
2(according to 2. formula of chemical reaction, burning 100g gets SiO 1.0g account for 10%
2For 4.69g calculates, add dimethyl siloxane 21.3g)
Al
2O
30.7g accounted for for 7% (, containing aluminum stearate 8.5g) according to 4. formula calculating of chemical reaction
V
2O
50.3g account for 3% (purity is AR, granularity≤5.0 μ m)
Modification organic bond 240g 24.0%
By above mixed, with rolling fineness≤16.0 μ m, the viscosity 26000mPaS of being ground to of three-high mill.Be printed on the Al of mass percent 96% with 280 order silk screen labyrinth shape patterns
2O
3On the substrate, dried 10 minutes down at 200 ℃, again sintering in continuous tunnel furnace, 25 minutes time, 650 ± 5 ℃ of peak temperatures, time to peak 5 minutes, glass, one step of aluminium film are synthesized, and are 12m Ω/25 μ m/ mouths with the resistance of precision 0.1m Ω electric bridge survey side, and lead content is less than 550ppm.
Embodiment two
1, the preparation of modification organic bond is identical with example one;
2, aluminum conductive electric slurry preparation and electrical property (quantity 1000g)
Aluminium powder (with embodiment one aluminium powder specification) 740g accounts for 74.0%, and indium powder (purity 〉=99.99%, granularity≤8.0 μ m) 10g accounts for 1.0%, and glass 10g accounts for 1.0%, wherein:
B
2O
33.0g account for 30%[according to 1. formula calculating of chemical reaction, add boron powder (purity 〉=99.99%, granularity≤5 μ m) 0.93g]
MgO 1.5g accounted for for 15% (according to 5. formula calculating of chemical reaction, adding dolomol 22.0g)
CaO 1.0g accounted for for 10% (according to 6. formula calculating of chemical reaction, adding calcium stearate 10.8g)
Al
2O
31.0g accounted for for 10% (, containing aluminum stearate 12.1g) according to 4. formula calculating of chemical reaction
SiO
2(according to 2. formula of chemical reaction, burning 100g gets SiO 2.0g account for 20%
2For 4.69g calculates, add dimethyl siloxane 42.6g)
ZnO 1.0g accounted for for 10% (according to 7. formula calculating of chemical reaction, adding zinc stearate 7.8g)
V
2O
50.5g account for 5% (purity is AR, granularity≤5.0 μ m)
Modification organic bond 240g, 24.0%,
By above mixed, be rolled to fineness of grind≤18.0 μ m, viscosity 28000mPaS with three-high mill.Be printed on mass percent 96%Al with 280 order silk screen labyrinth shape patterns
2O
3On the substrate, dried 10 minutes sintering in continuous tunnel furnace, 25 minutes time, 650 ± 5 ℃ of peak temperatures, time to peak 5 minutes down at 200 ℃.Glass, one step of aluminium film are synthesized, and are 9m Ω/25 μ m/ mouths with the resistance of precision 0.1m Ω electric bridge survey side, and lead content is zero.
Claims (6)
1, a kind of synthesizing silicon solar energy cell back field aluminum electrocondution slurry, it is characterized in that: slurry is by mass percent 70-80% aluminium powder, 15-30% modification organic bond, the indium powder of 0.1-5.0%, the inorganic bond glass of 0.1-5.0% is formed, total amount 100%, described aluminium powder is that the aluminium ingot of purity 99.9-99.99% is made, its average grain diameter is 6.0-8.0 μ m, and surface coverage has the aln layer of 3-5 nanometer thickness, and the modification organic bond is ethyl cellulose 1-5% by mass percentage, phenolic resins or novolac epoxy resin 0.5-10.0%, rosin 0.1-2.0%, butyl stearate 1.0-10.0%, terpinol 30-60%, additive 30-50%, total amount 100%, indium powder are purity 〉=99.99%, the finished product of particle mean size≤8.0 μ m, inorganic bond glass is when the preparation slurry, add the boron powder simultaneously, dimethyl siloxane, stearate is in the simultaneous oxidation of slurry sintering film forming, decompose acquisition oxide glass raw material, and a step synthesizing inorganic adhesive glass.
2, synthesizing silicon solar energy cell back field aluminum electrocondution slurry according to claim 1 is characterized in that: described additive comprises one or more in ethylene glycol phenyl ether, diethyl phthalate, diethylene glycol monobutyl ether, diethylene glycol monobutyl ether acetate, the phenmethylol.
3, synthesizing silicon solar energy cell back field aluminum electrocondution slurry according to claim 1 and 2 is characterized in that: described inorganic bond frit is formed by two kinds, and first kind consists of mass percent B for the flint glass raw material
2O
310-30%, PbO 40-70%, SiO
210-20%, Al
2O
310-15%, V
2O
53-5%; Form B by mass percentage for crown glass for second kind
2O
330-50%, MgO 10-15%, CaO 3-10%, Al
2O
310-15%, SiO
215-20%, ZnO5-10%, V
2O
52-5%.
4, synthesizing silicon solar energy cell back field aluminum electrocondution slurry according to claim 3 is characterized in that: the oxide during described flint glass raw material is formed removes V
2O
5Outward, be when the preparation slurry, add the boron powder simultaneously, dimethyl siloxane, lead stearate and aluminum stearate decompose acquisition in the simultaneous oxidation of slurry sintering film forming; Oxide during described crown glass raw material is formed removes V
2O
5Outward, be when the preparation slurry, add the boron powder simultaneously, dimethyl siloxane, aluminum stearate, zinc stearate, dolomol, calcium stearate decomposes acquisition in the simultaneous oxidation of slurry sintering film forming; Directly adding purity when the preparation slurry is AR, the vanadic oxide of granularity≤5.0 μ m.
5, a kind of synthesizing silicon solar energy cell back field aluminum electrocondution slurry is characterized in that: by the method for described this aluminum conductive electric slurry of formulation of claim 1, finishes according to the following steps,
(1), with the above-mentioned organic bond for preparing, heating for dissolving under 80-150 ℃ of temperature, the organic bond of transparent modification,
(2) with aluminium powder, the modification organic bond, the indium powder, mix, add the boron powder again, dimethyl siloxane, after stearate and vanadic oxide mix again, with rolling fineness 15-18 μ m, the viscosity 25000-35000mPa fiber S of being ground to of three-high mill, must grind the back aluminum conductive electric slurry, through the silk screen printing oven dry, get the aluminium conducting film behind the sintering, stearate, dimethyl siloxane, boron powder solve oxide at simultaneous oxidation, the branch of sintering film forming, and fusion becomes glass and participates in reaction, makes glass, one step of aluminium conducting film synthetic.
6, synthesizing silicon solar energy cell back field aluminum electrocondution slurry according to claim 5 is characterized in that: oven dry is to dry 10 minutes down at 200 ℃, reenters sintering in the continuous tunnel furnace, 25 minutes time, 650 ± 5 ℃ of peak temperatures, time to peak 5 minutes.
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| CN102169739A (en) * | 2011-02-25 | 2011-08-31 | 乐山新天源太阳能电力有限公司 | Nanometer aluminum paste for solar battery and manufacturing method thereof |
| CN102169739B (en) * | 2011-02-25 | 2012-09-05 | 乐山新天源太阳能电力有限公司 | Nanometer aluminum paste for solar battery and manufacturing method thereof |
| CN102522156A (en) * | 2011-12-06 | 2012-06-27 | 南昌大学 | Preparation method of aluminum boron slurry for crystalline silicon solar battery |
| CN103117134A (en) * | 2012-12-07 | 2013-05-22 | 蚌埠市智峰科技有限公司 | Preparation method of solar cell conductive mixed slurry containing butyl stearate |
| CN103117134B (en) * | 2012-12-07 | 2016-08-31 | 蚌埠市智峰科技有限公司 | A kind of preparation method of the solar cell conductive mixed slurry containing butyl stearate |
| CN104464882A (en) * | 2014-12-05 | 2015-03-25 | 清华大学 | Photovoltaic cell silver paste and sintering method thereof |
| CN104464882B (en) * | 2014-12-05 | 2016-08-17 | 清华大学 | A kind of photovoltaic cell silver slurry and sintering method thereof |
| CN108463500A (en) * | 2016-01-12 | 2018-08-28 | 诺利塔克股份有限公司 | Conductive composition |
| CN109903884A (en) * | 2017-12-07 | 2019-06-18 | 三星Sdi株式会社 | It is used to form the composition of electrode of solar battery and the electrode using its manufacture |
| CN108877989A (en) * | 2018-07-05 | 2018-11-23 | 江西核工业兴中新材料有限公司 | A kind of anti-light PERC monocrystaline silicon solar cell aluminium paste and preparation method thereof to decline |
| CN111276280A (en) * | 2020-02-05 | 2020-06-12 | 营口理工学院 | Indium-containing back surface field aluminum paste for crystalline silicon solar cell and preparation method thereof |
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