CN104157332A - Silicon solar cell front face electrode lead-free silver paste and preparing method thereof - Google Patents
Silicon solar cell front face electrode lead-free silver paste and preparing method thereof Download PDFInfo
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Abstract
The invention discloses silicon solar cell front face electrode lead-free silver paste and a preparing method thereof. The silicon solar cell front face electrode lead-free silver paste is characterized in that inorganic glass powder is not contained in the silver paste, and the silver paste comprises, by mass, 75-85 percent of conductive silver powder, 1-5 percent of antireflective film corrosive, 10-20 percent of organic vehicle and 1-5 percent of additive; the conductive silver powder is formed by mixing micro silver powder and nano silver powder with the mass ratio of 10:1-2; the antireflective film corrosive comprises one or more of potassium fluotitanate, potassium fluoroaluminate, potassium fluosilicate and potassium fluoborate; the additive comprises one or more of ethanol amine, diethanol amine, triethanol amine, tetramethylammonium hydroxide, tetraethylammonium hydroxide and tetramethylammonium hydroxide. According to the silicon solar cell front face electrode lead-free silver paste and the preparing method thereof, lead-free silver paste printing and antireflective film removing are conducted in one step, sintering can be conducted at a low temperature, the compactness and the smoothness of a silver electrode film are improved, and the photoelectric conversion efficiency of a silicon cell piece is improved.
Description
Technical field
The present invention relates to a kind of silicon solar cell front electrode lead-free silver slurry and preparation method thereof, particularly a kind of silicon solar cell front electrode lead-free silver slurry that does not contain glass dust and preparation method thereof, the silicon solar cell system that is applicable to high electricity conversion, high printing precision requirement, belongs to new material and area of solar cell.
Background technology
Solar cell is a kind of semiconductor device that solar energy can be converted to electric energy, and under the condition of illumination, solar cell meeting generation current, is got up electric collecting and transferred out by grid line and electrode.Suitability for industrialized production crystal silicon cell is by p-type crystal silicon material is cut into slices, through cleaning, chemical corrosion making herbs into wool; Make p-n junction in the diffusion of sensitive surface phosphorus; Be coated with silicon nitride antireflection layer; Aluminium paste is imprinted on to silicon chip back side by silk screen print method, silver slurry is imprinted on to silicon chip positive and negative; Be dried, be sintered into several link compositions such as cell piece.Front electrode divides gate line and main electrode line, and grid is mainly to accept the majority carrier that light conversion produces; And main electrode is mainly that cell piece is connected with outside line.The electrical property of the performance impact solar cell of front electrode, as technical indicators such as open circuit voltage, short circuit current, parallel resistance, series resistance, conversion efficiencies.
Solar cell conductive silver slurry is mainly made up of silver powder, unorganic glass powder adhesive, organic carrier and additive four parts.Silver powder is as conducting medium; Glass glue melts in the time of high temperature sintering, between silver powder and silicon base, forms ohmic contact; Organic carrier mainly plays a part to disperse and parcel silver powder particles, makes the silver powder in conductive silver paste be not easy precipitation and oxidation.Additive is processing performance and the combination property that promotes silver powder slurry, further improves conductive silver paste electric conductivity.
The key technical index of conductive silver paste is mainly determined by the performance of silver powder, and silver powder performance depends primarily on its appearance structure feature, granularity and particle size distribution.Silver powder accounts for the 70%-90% of its quality in solar cell conductive silver slurry, is the key factor that determines silver slurry and form performance of silver electrode.Silver powder structure and morphology can be spherical, class is spherical, bar-shaped, sheet, dendroid etc., it between flake silver powder particulate, is face contact, conductivity can be more better in theory, but front electrode of solar battery requires depth-width ratio as far as possible large, to reduce silver electrode line, the light of silicon chip is blocked, so the spherical or class ball shape silver powder of the general employing of solar cell conductive silver slurry.If silver powder granularity is excessive, when printing in silver slurry, just can not be passed through silk screen completely, also cannot densified sintering product in the short time, and easily there is hole in sintered membrane, thereby affects conductivity.If silver powder undersized, silver powder slurry is difficult for by organic carrier complete wetting, causes printing effect bad, after sintering large, the hole of silverskin shrinkage many be connected not fine and close.Experimental results show that and adopt particle diameter can obtain good electrical property at the ball shape silver powder of 1-3 μ m, and the good silver powder of uniform particles can reduce the reverse leakage current of battery, thereby improve open circuit voltage and short circuit current, and effectively promote the unit for electrical property parameters such as parallel resistance and conversion efficiency.
Unorganic glass powder melting in the time of high temperature in front electrode conductive silver paste, etching antireflective coating, and form and be connected between silicon chip and silver electrode.In order to obtain better ohmic contact, in front electrode silver slurry, glass dust must have good eating thrown to silicon nitride anti-reflecting film.In traditional front electrode conductive silver paste, the general glass dust that contains lead oxide that adopts, because flint glass powder has lower fusing point, has good eating thrown to silicon nitride anti-reflecting film, makes silver electrode have good adhesive force and good battery performance simultaneously.But traditional front electrode silver slurry medium lead crystal glass easily causes the excessive eating thrown of silicon nitride anti-reflecting film in electrode sintering process.In addition, there is environment and potential safety hazard in leaded solar cell conductive silver slurry, and it uses oneself to be restricted, and will eliminate gradually, and leadless environment-friendly type conductive silver paste could meet large solar battery production demand.
The lead-free low-melting-point glass systems such as borate glass, phosphate glass, vanadate glass and bismuthate glass are studied both at home and abroad.The vanadate glass cost of raw material is higher, phosphate glass facile hydrolysis and unstable chemcial property, and borate glass fusing point can only drop to 600 DEG C of left and right.Because bismuth is similar to plumbous character, therefore, the research and development of bismuthate glass powder are in widespread attention, expect to replace lead oxide to prepare lead-free glass powder with bismuth oxide.
Organic carrier is made up of organic solvent, thickener, thixotropic agent, surfactant and curtain coating controlling agent, and the simplest carrier also should comprise organic solvent and two kinds of compositions of thickener.Organic solvent content is about the 65%-90% of organic carrier gross mass, more sticky liquid, there is higher boiling point, under normal temperature, volatility is low, the thickener of energy dissolving cellulos and so on, the most frequently used organic solvent is diethylene glycol ethers acetate (butyl carbitol acetate), tributyl citrate, dibutyl phthalate etc.Thickener effect is viscosity and the plasticity that improves slurry, conventionally adopt high molecular polymer to make thickener, they have netted or chain structure, there is the more intense group of polarity, be pressed powder state or cohesion shape liquid at normal temperatures, can be by organic solvent dissolution, more than 300 DEG C, can be divided completely and take off and do not stay ash content, conventional thickener has ethyl cellulose, nitrocellulose, polyisobutene and various synthetic resin etc.Action of Surfactant is to make organic carrier fully soak solia particle, and conventional surfactant has toluene and ethanol etc.The effect of curtain coating controlling agent is to stop slurry Yin Wendu in drying course raise and produce secondary flow, and conventional curtain coating controlling agent has terephthalic acid (TPA) and furancarboxylic acid etc.Thixotropic agent effect is to make thick film ink obtain necessary thixotropy, and conventional thixotropic agent has bentonite, calcium silicates, aluminium oxide or silica etc.
Unleaded conductive silver paste used for solar batteries has many disclosed technology.Chinese patent CN103943168 (2014-07-23) discloses a kind of Ag (Ti, Zr)/rare earth crystal-silicon solar cell composite mortar and preparation method thereof, and the average grain diameter of the super fine silver powder of employing is 0. 2-2 μ m; Glass dust binding agent is Bi-Zn-Al-B-Si glass system; Add the superfine Ti O that particle diameter is less than 5 μ m
2and ZrO
2powder; Add Rare-Earth Ce, Eu or Gd powder, so that make silver-colored silicon contact finer and close in sintering process, further reduce contact resistance and the adhesive force that has strengthened electrode, reduced the consumption of argent simultaneously, improved crystal-silicon solar cell efficiency and reduced battery cost.
Chinese patent CN103559939 (2014-02-05) discloses a kind of solar cell positive silver paste that adapts to high temperature sintering, the silver powder particle diameter adopting is 1-3 μ m, and the composition of lead-free glass powder and percetage by weight thereof are: bismuth oxide 50-60%, zinc oxide 10-30%, boric acid 3-5%, silica 5-9%, antimony oxide 0-15% and strontium oxide strontia 0-5%; Add simple substance or the compound of sintering aids rhodium, ruthenium or iridium; Solvent is one or more the mixture in terpinol, butyl carbitol, butyl carbitol acetate, tributyl citrate and tributyl phosphate; Thickener is one or more the mixture in ethyl cellulose, CMC, nitrocellulose.
Chinese patent CN103440900 (2013-12-11) discloses the unleaded positive silver paste of a kind of crystal silicon solar energy battery, and the silver powder of employing is the silver powder that average grain diameter 0.2-2 μ m, tap density are greater than 4. 5g/ml; Lead-free glass powder is the crown glass system being made up of Bi-Zn-Al-B-Si, and softening temperature is 350 DEG C～600 DEG C; Add one or more in acid additive diboron trioxide, phosphorus pentoxide, selenium dioxide, vanadic oxide, tellurium dioxide.
Ying Li group company discloses a kind of preparation method of front electrode of solar battery at Chinese patent CN102800755 (2012-08-27), adopt corrosive agent to remove the locational silicon nitride film of pre-formed front gate line before printed silver slurry, thereby in silver slurry, do not need to mix leaded borate glass powder and carry out corroding silicon nitride film, follow-uply do not need to adopt high-sintering process yet.Owing to not comprising glass dust in silver slurry, can improve the silver content in silver slurry, and then improve the electric conductivity of silver slurry.When concrete enforcement, print corrosive reagents by the mode of silk screen printing on described silicon nitride film on the position corresponding to described pre-formed front gate line, corrosive reagents is the corrosive slurry of BES series paste fluid.This BES series chemical sizwe is produced by German Merck company, has advantages of that corrosion rate is fast, can realize at normal temperatures efficient selective corrosion to silicon nitride film.The chemical slurry thickness of silk screen printing BES series is 2-20um, and corrosion reaction can complete in 10 seconds.Printed silver slurry is made up of argent particulate and organic solvent, the argent particulate that comprises 80%-90% in described silver slurry and the organic solvent of 10%-20%, and described organic solvent is phenolic resins or epoxy resin.
Existing unleaded conductive silver paste sintering range is narrow, volume resistance is large, the adhesive force of silver layer on silicon chip general, have gap with traditional leaded conductive silver paste aspect electrode solderability and oxidative resistance, and product cost is also higher.Although the disclosed electrocondution slurry of Ying Li group company patent is not containing unorganic glass powder and improved the silver content in silver-colored slurry, increase the operation of printing corrosive agent, corrosion operating procedure technical requirement is high, needs special equipment, is difficult for commercial application.
Summary of the invention
The object of the invention is for silicon solar cell front electrode silver slurry the deficiencies in the prior art, a kind of silicon solar cell front electrode lead-free silver slurry is provided, particularly, not containing a silicon solar cell front electrode lead-free silver slurry for glass dust, its composition comprises conductive silver powder, antireflective coating corrosive agent, organic carrier and additive.
In lead-free silver slurry of the present invention, the mass percentage content of conductive silver powder is 75%-85%, and the mass percentage content of antireflective coating corrosive agent is 1%-5%, and the quality percentage composition of organic carrier is 10%-20%, and the mass percentage content of additive is 1%-5%.
In the present invention's silver slurry, conductive silver powder is mixed and forms with mass ratio 10:1-2 by micro aluminum powder and nano-silver powder, wherein, and the average grain diameter 1-2 μ m of micro aluminum powder, tap density 4.5-5.0g/ml, specific area 0.4-1.0m
2/ g; Nano-silver powder average grain diameter 50-150nm, tap density 0.8-2.5g/ml, specific area 10-50m
2/ g.Micro aluminum powder and nano-silver powder are prepared by electronation silver nitrate method.When conductive silver paste printing, nano-silver powder can be filled in the space of micro aluminum powder formation, improves the compactness of printed silver electrode.
Antireflective coating corrosive agent of the present invention comprises one or more of potassium fluotitanate, potassium fluoroaluminate, potassium fluosilicate, potassium fluoborate; stable chemical nature under their normal temperature; under the hot conditions of silver slurry sintering as silver-colored silicon welding protecting agent; the fluoride that decomposed produces is eating thrown silicon nitride anti-reflecting film and alligatoring silicon chip surface completely; reduce the contact resistance of silver layer and silicon chip; improve the adhesive force of silver electrode on silicon chip; can adjust corrosive agent content in formula according to sintering temperature and time, to prevent excessive erosion.
Organic carrier of the present invention is made up of solvent and thickener, and its component and percentage by weight are: butyl carbitol 50%-60%, terpinol 15%-20%, dihydroxy ethyl coco amine 15%-20%, ethyl cellulose 5%-10%.Dihydroxy ethyl coco amine boiling point more than 350 DEG C, is not only good organic solvent, is also good surfactant simultaneously, can make the wetting silicon chip surface of silver slurry, improves silver electrode printing quality, reaches the depth-width ratio of silver grating line design.
Additive of the present invention be monoethanolamine, diethanol amine, triethanolamine, Tetramethylammonium hydroxide, tetraethyl ammonium hydroxide or TBAH any one or more, under their normal temperature, there is corrosivity and strong basicity, can eating thrown silicon nitride anti-reflecting film, can regulate its corrosion rate according to addition.
Another object of the present invention is to provide a kind of preparation method who does not contain the silicon solar cell front electrode lead-free silver slurry of glass dust, and the technical scheme of taking is.
1. conductive silver powder is prepared
In container by average grain diameter 1-2 μ m, tap density 4.5-5.0g/ml, specific area 0.4-1.0m
2the micro aluminum powder of/g and average grain diameter 50-150nm, tap density 0.8-2.5g/ml, specific area 10-50m
2the nano-silver powder of/g mixes and obtains conductive silver powder with mass ratio 10:1-2.
2. organic carrier preparation
(1) press formulation ratio butyl carbitol 50%-60% and terpinol 15%-20%, butyl carbitol, terpinol are mixed;
(2) press formulation ratio dihydroxy ethyl coco amine 15%-20% and ethyl cellulose 5%-10%, add successively dihydroxy ethyl coco amine and ethyl cellulose to dissolve, stir and make transparent organic carrier.
3. silicon solar battery electrode lead-free silver slurry preparation
(1) mass percentage content of conductive silver powder is 75%-85%, and the mass percentage content of antireflective coating corrosive agent is 1%-5%, and the quality percentage composition of organic carrier is 10%-20%, and the mass percentage content of additive is 1%-5%;
(2) in container, above mixture is stirred, mixture is ground 10-20 time on three-roll grinder, finely tuned silver slurry fineness is reached below 8 μ m by solvent, viscosity is 200-300PaS, obtains silicon solar battery electrode lead-free silver slurry.
The beneficial effect that the present invention obtains is:
(1) in lead-free silver slurry of the present invention, do not contain glass dust, sintering at a lower temperature, has improved compactness and the smoothness of electrode film, thereby has increased the short circuit current of battery, has improved the photoelectric conversion efficiency of cell piece;
(2) additive chemical corrosion silicon nitride anti-reflecting film at normal temperatures in lead-free silver slurry of the present invention, improves slurry wets and flow leveling, makes the printing of silver slurry and goes antireflective coating one step to complete, and has simplified silicon cell production technology;
(3) the at high temperature chemical corrosion of antireflective coating corrosive agent and alligatoring silicon chip surface in lead-free silver slurry of the present invention, remove silicon nitride anti-reflecting film completely, reduces silver electrode and silicon chip contact resistance and improve silver electrode peel strength.
Embodiment
Embodiment 1
In container by average grain diameter 1-2 μ m, tap density 4.5-5.0g/ml, specific area 0.4-1.0m
2the micro aluminum powder 100g of/g and average grain diameter 50-150nm, tap density 0.8-2.5g/ml, specific area 10-50m
2the nano-silver powder 10g of/g mixes and obtains conductive silver powder 110g.
Butyl carbitol 50g and terpinol 20g are mixed; Add successively dihydroxy ethyl coco amine 20g and ethyl cellulose 10g to dissolve, stir and make transparent organic carrier 100g.
By the conductive silver powder 85g preparing above, antireflective coating corrosive agent potassium fluotitanate 3g, the more than organic carrier 10g of preparation, additive triethanolamine 2g, in container, above mixture is stirred, this mixture is ground 10 times on three-roll grinder, by the fine setting of solvent, silver slurry fineness is reached below 8 μ m, viscosity is 200-300PaS, obtains silicon solar battery electrode lead-free silver slurry.
Silver slurry is printed on 125mm × 125mm silicon substrate with screen printing mode, then dry at 200 DEG C, heat up with the speed of 150 DEG C/min, carry out quick fired electrodes lead-in wire at 700-800 DEG C, the contact conductor surface silvery white of making after high temperature sintering, microscopic examination smooth surface zero defect, peel strength 8N/cm, soldering is functional, and solar cell photoelectric transformation efficiency is 19. 6%.
Embodiment 2
In container by average grain diameter 1-2 μ m, tap density 4.5-5.0g/ml, specific area 0.4-1.0m
2the micro aluminum powder 100g of/g and average grain diameter 50-150nm, tap density 0.8-2.5g/ml, specific area 10-50m
2the nano-silver powder 20g of/g mixes and obtains conductive silver powder 120g.
Butyl carbitol 60g and terpinol 15g are mixed; Add successively dihydroxy ethyl coco amine 20g and ethyl cellulose 5g to dissolve, stir and make transparent organic carrier 100g.
By the conductive silver powder 75g preparing above, antireflective coating corrosive agent potassium fluoroaluminate 3g, the more than organic carrier 20g of preparation, additive Tetramethylammonium hydroxide 2g, mixing and stirring in container is ground this mixture 10 times on three-roll grinder, by the fine setting of solvent, silver slurry fineness is reached below 8 μ m, viscosity is 200-300PaS, obtains silicon solar battery electrode lead-free silver slurry.
Silver slurry is printed on 125mm × 125mm silicon substrate with screen printing mode, then dry at 200 DEG C, heat up with the speed of 150 DEG C/min, carry out quick fired electrodes lead-in wire at 700-800 DEG C, the contact conductor surface silvery white of making after high temperature sintering, microscopic examination smooth surface zero defect, peel strength 9N/cm, soldering is functional, and solar cell photoelectric transformation efficiency is 19. 3%.
Claims (5)
1. a silicon solar cell front electrode lead-free silver slurry, it is characterized in that not containing unorganic glass powder, its component and mass percent are: conductive silver powder 75%-85%, antireflective coating corrosive agent 1%-5%, organic carrier 10%-20%, additive 1%-5%, described conductive silver powder is mixed and forms with mass ratio 10:1-2 by micro aluminum powder and nano-silver powder, wherein, the average grain diameter 1-2 μ m of micro aluminum powder, tap density 4.5-5.0g/ml, specific area 0.4-1.0m
2/ g; Nano-silver powder average grain diameter 50-150nm, tap density 0.8-2.5g/ml, specific area 10-50m
2/ g.
2. silicon solar cell front electrode lead-free silver slurry according to claim 1, is characterized in that antireflective coating corrosive agent comprises one or more of potassium fluotitanate, potassium fluoroaluminate, potassium fluosilicate or potassium fluoborate.
3. silicon solar cell front electrode lead-free silver slurry according to claim 1, it is characterized in that organic carrier is made up of solvent and thickener, its component and percentage by weight are: butyl carbitol 50%-60%, terpinol 15%-20%, dihydroxy ethyl coco amine 15%-20%, ethyl cellulose 5%-10%.
4. silicon solar cell front electrode lead-free silver slurry according to claim 1, is characterized in that additive is one or more of monoethanolamine, diethanol amine, triethanolamine, Tetramethylammonium hydroxide, tetraethyl ammonium hydroxide or TBAH.
5. a preparation method for silicon solar cell front electrode lead-free silver slurry described in claim 1, is characterized in that technical scheme and preparation process are:
(1) in container, micro aluminum powder and nano-silver powder are mixed with mass ratio 10:1-2, obtain conductive silver powder;
(2) first butyl carbitol 50%-60% and terpinol 15%-20% are mixed by formula, then by formula, dihydroxy ethyl coco amine 15%-20% and ethyl cellulose 5%-10% are added to dissolving successively, stir and make transparent organic carrier;
(3) be 75%-85% by the mass percentage content of formula conductive silver powder, the mass percentage content of antireflective coating corrosive agent is 1%-5%, the quality percentage composition of organic carrier is 10%-20%, and the mass percentage content of additive is 1%-5%, in container by above component mixing and stirring;
(4) above mixture is ground 10-20 time on three-roll grinder, by the fine setting of solvent, silver slurry fineness is reached below 8 μ m, viscosity is 200-300PaS, obtains silicon solar battery electrode lead-free silver slurry.
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Application publication date: 20141119 |