CN100446277C - Aluminum back-surface-field conductive paste composition in silicon solar cell and method for preparing same - Google Patents
Aluminum back-surface-field conductive paste composition in silicon solar cell and method for preparing same Download PDFInfo
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- CN100446277C CN100446277C CNB2006100110011A CN200610011001A CN100446277C CN 100446277 C CN100446277 C CN 100446277C CN B2006100110011 A CNB2006100110011 A CN B2006100110011A CN 200610011001 A CN200610011001 A CN 200610011001A CN 100446277 C CN100446277 C CN 100446277C
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Abstract
The present invention relates to back-field aluminum conductive slurry composition for a silicon solar battery and a preparation method thereof. The slurry composition comprises the components by mass percentage: 70 to 80% of aluminum powder, 15 to 30% of modified organic binding agent, 40 to 60% of inorganic binding agent containing indium, gallium or thallium, and 1 to 10% of glass metal powder. After the preparation of the slurry, aluminum conductive slurry can be obtained. The organic binding agent is modified by thermosetting resin, and thus, aluminum film has high binding strength after the aluminum film is dried. Rosin is added, the conductivity of the aluminum film can be improved; the net-passing performance of the slurry can be improved by the method that hard ester acid calcium (zinc) serves as a lubricant agent; functional elements of Ga, In and Ti are added to the aluminum slurry so that the photoelectric conversion efficiency can be improved; the surface of the aluminum powder made of high-purity aluminum ingots is coated with an aluminum nitride layer of which the thickness is from 3 to 5 nm, and glass of the inorganic binding agent is smelted and re-smelted for a long time so that the bending degree of the prepared silicon chip after the silicon chip is sintered can be low and aluminum balls can not be generated; furthermore, when silicoaluminate is formed, vesication can not happen, and the aluminum film is smooth; the photoelectric conversion efficiency of monocrystal silicon is more than 17.0 percent.nt.
Description
One, technical field:
A kind ofly prepare the method for electronic information material-electrocondution slurry, belong to the chemical preparation field with chemical method.
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 patented technology of seeing at present or the product of internationally famous major company (as E.I.Du Pont Company and FERRO company) still have certain gap.The present invention is exactly at above-mentioned existing problems, carrying out formula of size, intermediate composition, processing method improves, 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 grey peeling.The lead content control between 0-500ppm, compliance with environmental protection requirements.
Known correlation technique has multiple, Kunming Institute of Precious Metals and Yunnan Semiconductor factory, the production domesticization research and development of single crystal silicon solar cell and conductors dedicated slurry thereof are carried out in cooperation, belong to the self-control Ag of research institute powder, Al alloyed powder, self-control glass dust, in the Ag powder, mix and have the ohmic contact functional element, add the rolling pulping of organic carrier, machine test and application on the semiconductor of Yunnan, photoelectric conversion rate is greater than 13.20%.The solid-state dye sensitized thin-film solar cells of soft base of Southeast China University's development, be that a kind of cost is low, manufacturing process is simple, stable performance, the life-span can reach the soft based solar battery more than 20 years in theory, the structure of this solar cell is layer structure (solid-state dye sensitized thin-film solar cells of soft base and preparation method CN1564326).A kind of slurry of Inst. of Physics, CAS's development, its method be with slurry viscosity conditioning agent, slurry dispersant, surfactant dissolves in solvent, be split into liquid mixture, then this liquid mixture and pressed powder mixed, thereby prepare the slurry of this pressed powder.This slurry can be used for preparing the solid film of porous, and made film has that surface area is big, surfacing, hole are evenly distributed, combine characteristics such as firm with substrate; The film that this slurry makes with the slurry of wide bandgap semiconductor powder simultaneously can be used for the aspects such as pollutant (a kind of preparation method of slurry and use CN1616142) of DSSC, photolysis water device, degradation of sewage.In addition, electrical machinery of Japanese sanyo Co., Ltd. has obtained the solar module patent in China's application, the electrode of solar cell device is separated slurry and is made by containing conduction that thermosetting resin and conduction separate powder, thermosetting resin contain 70% or more glass transition temperature at 80 ℃～200 ℃ resin (solar module CN 1652354).The solar cell that Sharp Co., Ltd. obtains is made patent, by the sintering metal grout material, forms little width grid electricity level on the sensitive surface of the substrate with pn knot; Be electrically connected to grid electricity grade (the solar cell CN 1606175 that makes the method for solar cell and make thus) with the bar-shaped main electricity level of formation.
Three, summary of the invention
1, the purpose of this invention is to provide a kind of silicon solar cell back surface field aluminum conductive electric slurry forms and the preparation method, the composition of this slurry comprise mass percent 70-80% aluminium powder, 30-20% modification organic bond, contain the inorganic bond glass metal powder 1-10% of Indium, gallium or thallium 40～60%, this slurry that after preparation, obtains, have and conduct electricity very well, the photoelectric conversion efficiency height, crooked little behind the silicon chip sintering, beading up not, advantage such as do not blister.
2, technical scheme
1), the composition and the prescription of slurry: by aluminium powder, the 15-30% modification organic bond of mass percent 70-80%, contain Indium, gallium or thallium 40～60% inorganic bond glass metal powder 1-10% and form total amount 100%.
(1), 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, surface coverage has the aln layer of 3-5 nanometer thickness, apparent density 0.60-0.85g/cc, specific area 0.70-1.00M
2The ball aluminum powder of/g;
(2), the modification organic bond is for pressing quality than ethyl cellulose 1-5%, phenolic resins or novolac epoxy resin 0.5-10.0%, rosin 0.1-2.0%, calcium stearate or zinc 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), inorganic bond glass metal powder is by containing Indium, gallium or thallium 40～60 quality %, surplus is the glass dust prescription, granularity less than
μ m, glass dust elder generation is diboron trioxide (B by mass percentage
2O
3) 15～25%, lead oxide (Pb0) 40～50%, vanadium pentoxide (V
2O
5) 1～2%, silicon dioxide (SiO
2) 15～28%, alundum (Al (Al
2O
3) 3～6% be mixed with the glass oxidate powder.
2), the preparation of each composition branch of slurry
(1), by the prescription of above-mentioned organic bond, under 80-150 ℃ of temperature, dissolve, the organic bond of transparent modification;
(2), glass dust preparation
The glass oxidate powder that prescription is good mixes, and in the porcelain crucible of packing into, puts into silicon carbide rod furnace, intensification is preheated to 500～600 ℃ of insulation 0.5h, rises to 1100～1250 ℃ again, melting 3h, shrend, oven dry reinstalls in 1100～1250 ℃ of stoves to moisture less than 8%, and melting is 3 hours again, shrend, after being crushed to 150～74 μ m, refill people's ball grinder, control ZrO
2Ball: material: deionized water=2: 1: 0.5, jar fast 80-120/ branch, ball milling obtained granularity≤10 μ m glass dust, dry for standby after 24 hours.Its coefficient of linear expansion 4.5 * 10
-6/ ℃ (silicon 4.2 * 10
-6/ ℃);
(3), contain the dispersion preparation of the inorganic bond glass dust of Indium, gallium or thallium 40～60 quality %: it is after 20～35 seconds of pulverizer commentaries on classics of 1000-1500 rev/min with speed that glass dust and indium powder or thallium powder mix the back, get the inorganic bond glass metal powder of granularity 2-5 μ m, indium powder, thallium powder with metal melting after atomizing obtain, and only 29.75 ℃ of the fusing points of gallium often exist with liquid state at normal temperatures.The present invention after quantitative liquid gallium is arranged in pairs or groups with quantitative glass dust, carries out mechanical lapping, and the gallium disperse makes granularity 2-5 μ m inorganic bond glass metal gallium powder in glass dust;
3), aluminum conductive electric slurry preparation: the aluminium powder 70-80 quality % that is wrapped up by aluminium nitride, modification organic bond 15～30 quality %, the inorganic bond glass metal powder 1-10 quality % of the Indium that contains, gallium or thallium 40～60 quality %, after (total amount 100%) mixes, reach 15.0-25.0 μ m with the rolling granularity that is ground to of three-high mill again, viscosity is the product aluminum conductive electric slurry of 20000-35000mpas.
3), compare advantage and the good effect that has with known technology
(1), in organic adhesion agent, add phenolic resins, novolac epoxy resin, 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 calcium stearate or zinc stearate to improve the net performance excessively of slurry as lubricant;
(4) the long-time melting of inorganic bond glass and heavily refining, and carry out slaking and make the coefficient of linear expansion of glass close with the silicon coefficient of linear expansion.Solve not buckling problem of silicon chip sintering;
(5) in order to improve the photoelectric conversion efficiency of battery.Add functional elements such as Ga, In, Tl in aluminium paste, making has good Ohmic contact between aluminium electrode and the silicon, thereby improves photoelectric conversion efficiency, and the silicoaluminate layer also can improve the aluminium film to the silicon substrate adhesive strength;
(6) aluminium powder is a slurry critical function phase, the aluminium powder that the present invention selects for use purity 99.9-99.99% aluminium ingot to make, surface coverage has the aln layer of 3-5 nanometer thickness, with the material 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;
(7) glass is that aluminium also is to influence the crooked major reason of silicon chip to the bonding composition that silicon adheres to behind the sintering.The present invention reduces the glass composition in slurry except that improving glass preparation technology, make it and the silicon chip adhesion-tight, and lead content can be controlled between the 0-500ppm, is environmentally friendly machine.
The photoelectric conversion efficiency of monocrystalline silicon＞17.0%, polysilicon＞16.0%, 125 * 125mm wafer warpage＜0.80mm of the thick 210 μ m of monocrystalline silicon, the 210 μ m thin slices of polysilicon 156 * 156mm are not crooked, do not play the pill of aluminium, do not blister, do not have the fragment phenomenon when electric performance test and assembly, assembly bonds with EVA, does not play ash, no aluminium is peeled off phenomenon, lead content 0-500ppm.
Four, embodiment
Embodiment one:
1, the preparation of modification organic bond (pressing mass ratio)
Ethyl cellulose 4.0%, 6031-2 novolac epoxy resin 7.0%, rosin 1.0%, calcium stearate 1.0%, terpinol 40%, ethylene glycol phenyl ether 19%, diethyl phthalate 10%, diethylene glycol monobutyl ether 8%, diethylene glycol monobutyl ether acetate 6%, phenmethylol 4%, more than each thing be heated to 80-100 ℃ after mixing, to rosin, till ethyl cellulose has dissolved, transparent have a good lubricity printing glue;
2, glass dust founds
By mass percentage with diboron trioxide (B
2O
3) 20%, lead oxide (PbO) 50%, vanadium pentoxide (V
2O
5) 2%, silicon dioxide (SiO
2) 23%, alundum (Al (Al
2O
3) 5% be mixed with the glass oxidate powder, mix with the V-type batch mixer, place the porcelain crucible of glazing, under 500 ℃, preheating 30 minutes, 1200 ℃ of melting 3h, (beginning is B
2O
3, PbO, V
2O
5SiO fluxes
2, Al
2O
3, fully melt back B
2O
3, PbO, V
2O
5Part evaporation), the shrend oven dry is to moisture less than 8 quality %,, repeat top process again, shrend after 3 hours, oven dry, be crushed to granularity 150～74 μ m after, put into the polyurethane ball grinder, ratio: ZrO
2Ball: material: deionized water=2: 1: 0.5,80 rev/mins on ball mill grinds 24 hours to granularity≤10 μ m, and 150 ℃ of oven dry, getting coefficient of linear expansion is 4.5 * 10
-6/ ℃ (the coefficient of linear expansion 4.2 * 10 of silicon
-6/ ℃) glass dust, the two coefficient of linear expansion is approaching.The bending of silicon is relevant with the coefficient of linear expansion of glass;
3, obtain the indium powder with atomizing after the indium metal fusion, again by 50% indium powder, 50% glass dust mixing is after 1000-1500 rev/min pulverizer rotated for 30 seconds, to get the glass metal powder, granularity 2-5 μ m with speed;
4, aluminum conductive electric slurry preparation
The ball aluminum powder 74.0 quality % of the existing 2-5nm aluminium nitride passivation of particle surface, glass metal powder 2.0 quality %, modification organic bond 24 quality %, behind the mixing, being rolling to fineness of grind with three-high mill is 17-19 μ m, and viscosity 27000mpas gets the product aluminum conductive electric slurry.
Above-mentioned gained aluminum conductive electric slurry is on probation at production line: monocrystalline silicon specification 125 * 125mm, and thickness 200 μ m (before the corrosion), thickness is 180 μ m before the printing, printing screen 280 orders, the automatic press printing, print thickness be every with the slurry 0.79g, about 3 minutes of 250 ℃ of bake out temperatures, oven dry aluminium film does not have obscission, changes another side printing front side silver paste, after the oven dry, send the continuous tunnel furnace sintering, 860 ± 2 ℃ of sintering temperatures, 1.9 minutes cycles, about 18 seconds of peak temperature time, battery performance (mean value) is surveyed in the back of coming out of the stove
Power open circuit voltage short circuit current fill factor, curve factor parallel resistance series resistance conversion efficiency
(W) (mV) (mA) (％) (Ω) (Ω) (％)
2.538?620 5270 77.739 56.158 0.0064 17.08
Measure between the crooked 0.50-0.80mm with the vernier caliper sheet.Aluminium film grey, smooth, the no pill of aluminium, do not blister, do not fall ash, assembly does not have the phenomenon of peeling off with EVA bonding aluminium film, and lead tolerance is less than 500ppm.
Embodiment two:
1, founding of glass dust: diboron trioxide (B by mass percentage
2O
3) 30%, lead oxide (PbO) 30%, vanadium pentoxide (V
2O
5) 5%, silicon dioxide (SiO
2) 28%, alundum (Al (Al
2O
3) 7% preparation, melting method is undertaken by example one, and must get coefficient of linear expansion is 4.5 * 10
-6/ ℃, the glass dust 4.0% of granularity≤10 μ m;
2, aluminum conductive electric slurry preparation: the ball aluminum powder 74.0 quality % of the existing 2-5nm aluminium nitride passivation of particle surface, purity is greater than 99.99% thallium 1%, glass dust 1%, modification organic bond 24%, by example one preparation method preparation, after the aluminum conductive electric slurry utilization that makes, the battery performance result is as follows after tested:
Power open circuit voltage short circuit current fill factor, curve factor parallel resistance series resistance conversion efficiency
(W) (mV) (mA) (％) (Ω) (Ω) (％)
2.523?619 5269 77.22 50.622 0.0066 17.04
Measure between the crooked 0.50-0.80mm with the vernier caliper sheet.Aluminium film grey, smooth, the no pill of aluminium, do not blister, do not fall ash, assembly does not have the phenomenon of peeling off with EVA bonding aluminium film, and lead tolerance is less than 250ppm.
Claims (4)
1, a kind of silicon solar cell back surface field aluminum conductive electric slurry is formed and the preparation method, it is characterized in that: slurry is by the aluminium powder of mass percent 70-80%, 15-30% modification organic bond, contain Indium, the inorganic bond glass metal powder 1-10% of gallium or thallium 40～60% forms, 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, surface coverage has the aln layer of 3-5 nanometer thickness, the modification organic bond is for pressing quality than ethyl cellulose 1-5%, phenolic resins or novolac epoxy resin 0.5-10.0%, rosin 0.1-2.0%, calcium stearate or zinc stearate 1.0-10.0%, terpinol 30-60%, additive 30-50%, total amount 100%.
2, silicon solar cell back surface field aluminum conductive electric slurry according to claim 1 is formed and the preparation method, and it is characterized in that: described additive is one or more in ethylene glycol phenyl ether, diethyl phthalate, diethylene glycol monobutyl ether, diethylene glycol monobutyl ether acetate, the phenmethylol.
3, silicon solar cell back surface field aluminum conductive electric slurry according to claim 1 and 2 is formed and the preparation method, it is characterized in that: the first diboron trioxide 15～25% by mass percentage of described glass dust, lead oxide 40～50%, vanadium pentoxide 1～2%, silica 1 5～28%, alundum (Al 3～6% is mixed with the glass oxidate powder.
4, a kind of preparation method of silicon solar cell back surface field aluminum conductive electric slurry is characterized in that: prepares the method for this aluminum conductive electric slurry by the described composition 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, to rosin, ethyl cellulose molten intact till, the organic bond of transparent modification,
(2), the glass oxidate powder for preparing is mixed, in the porcelain crucible of packing into, put into silicon carbide rod furnace, intensification is preheated to 500～600 ℃ of insulation 0.5h, rises to 1100～1250 ℃ again, melting 3h, shrend, oven dry reinstalls in 1100～1250 ℃ of stoves to moisture less than 8%, and melting is 3 hours again, shrend, after being crushed to 150～74 μ m, refill people's ball grinder, control ZrO
2Ball: material: deionized water=2: 1: 0.5, jar fast 80-120/ branch, ball milling obtained granularity≤10 μ m glass dust after 24 hours, dry for standby,
(3), to mix the back be after 20～35 seconds of pulverizer commentaries on classics of 1000-1500 rev/min with speed for glass dust and indium Fen Huo powder, get the inorganic bond glass metal powder of granularity 2-5 μ m, indium powder, thallium powder with metal melting after atomizing obtain, the gallium powder is with quantitative liquid gallium and quantitatively glass dust collocation back mechanical lapping, the gallium disperse makes the glass metal thallium powder of granularity 2-5 μ m in glass dust
(4) aluminum conductive electric slurry preparation: the aluminium powder 70-80 quality % that is wrapped up by aluminium nitride, modification organic bond 15～30 quality %, the inorganic bond glass dust 1-10 quality % of the Indium that contains, gallium or thallium 40～60 quality %, after the mixing, reach 15.0-25.0 μ m with the rolling granularity that is ground to of three-high mill again, viscosity is 20000-35000mpas, gets the product aluminum conductive electric slurry.
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| CN100446277C true CN100446277C (en) | 2008-12-24 |
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Assignee: Fu Bang new energy technology Co., Ltd of Shenzhen Assignor: Tan Fubin Contract record no.: 2010440020226 Denomination of invention: Aluminum back-surface-field conductive paste composition in silicon solar cell and method for preparing same Granted publication date: 20081224 License type: Exclusive License Open date: 20061213 Record date: 20101201 |
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