CN103440901A - Low-cost leadless back silver paste for crystalline silica solar energy battery, and preparation method thereof - Google Patents
Low-cost leadless back silver paste for crystalline silica solar energy battery, and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a low-cost leadless back silver paste for a crystalline silica solar energy battery, and a preparation method thereof. The components of the leadless conductive silver paste and the mass percentage of the components are as follows: silver powder 40-55%, a leadless glass binder 5-15%, an organic binder 30-55%, and a decomposition auxiliary agent 0-1.0%, wherein the silver powder is micro-sheet silver powder with an average particle size of 2-10 [mu] m and a specific surface area of 1.8-2.4 m<2>/g, and the organic binder is composed of organic resins with different decomposition temperatures and organic solvents with different volatilization speeds. The back silver conductive paste prepared by the provided method has the advantages of moderate viscosity, a compact electrode film layer, excellent welding performance and high conversion efficiency.
Description
Technical field
The present invention relates to unleaded back of the body silver slurry and preparation method for a kind of crystal silicon solar energy battery.
Background technology
Solar cell is a kind of semiconductor device that solar energy is changed into to electric energy, and under illumination condition, inside solar energy battery produces photogenerated current, by electrode, can directly electric energy be exported.For the output by the electric energy maximum, electrode fabrication is a very important link.Silicon solar battery electrode comprises positive silver electrode and back silver electrode, aluminium electrode, and crystal silicon solar batteries back silver slurry is used as the back electrode of solar cell, mainly plays the effect of collected current.Back silver paste mainly is comprised of conducting function phase, organic carrier, inorganic binder three parts, because the back silver electrode needs and metal electrode welds together and is connected into assembly, therefore, the solderability of electrode has become the important performance characteristic of back silver paste with adhesive force.
Along with back of the body conductive silver slurry formula reaching its maturity on market, the silver content that constantly reduces slurry has become the inexorable trend of current back silver paste development and the competitive method of numerous slurry manufacturer.Along with the reduction of silver content, must have influence on printing performance and the welding performance of back silver paste.In order to guarantee the printing performance of slurry, need to increase the consumption of organic carrier in slurry, but under the sintering condition that a large amount of organic carriers burns in the high temperature sudden strain of a muscle, decompose not thorough, organic resin is charing fully not, cause surperficial yellowing, electrical property and the welding performance of the electrode of formation to descend, thereby affect the conversion efficiency of solar cell.
Summary of the invention
Technical problem to be solved by this invention is for the prior art above shortcomings, provides a kind of low-cost crystal silicon solar energy battery unleaded back silver paste.
Another technical problem to be solved by this invention is to provide the preparation method of a kind of low-cost crystal silicon solar energy battery with unleaded back silver paste.
For solving the problems of the technologies described above, the technical solution used in the present invention is as follows:
The unleaded back silver paste of a kind of low-cost crystal silicon solar energy battery, prepared by each component of following mass percent by described silver paste: silver powder 40～55%; Crown glass binding agent 5～15%; Organic binder bond 30～55%; Divide enzymolysis auxiliary agent 0～1.0%; Described silver powder is that 2～10 microns of average grain diameters, specific area are 1.8～2.4m
2the microplate shape silver powder of/g; Described organic binder bond is prepared from by the organic resin of mass percent 5～20%, 80～95% organic solvent, organic resin is selected from epoxy resin that decomposition temperature is 180～200 ℃, the cellulose of 200～220 ℃, phenolic resins, two or more in the acrylic resin more than 270 ℃ of 200～250 ℃, and organic solvent is selected from the dimethylbenzene of 140 ℃ of boiling points, the diethylene glycol ether of 200 ℃, the terpinol of 220 ℃, butyl carbitol acetate, two or more in the fine tributyl citrate of second of 340 ℃ of 250 ℃.
Above-mentioned unleaded back silver paste, described minute enzymolysis auxiliary agent is selected from slaine or the metal oxide of copper ions, iron ion and manganese ion.
Above-mentioned unleaded back silver paste, within described minute, enzymolysis auxiliary agent is one or more in copper nitrate, ferric nitrate, manganese dioxide, ferrocene.
The preparation method of unleaded back silver paste for a kind of low-cost crystal silicon solar energy battery, it comprises the following steps:
(1) preparation of organic binder bond
Take according to formula rate the organic solvent that mass percent is 80～95%, described organic solvent is comprised of two or more following substances: the dimethylbenzene that boiling point is 140 ℃, the diethylene glycol ether of 200 ℃, the terpinol of 220 ℃, the butyl carbitol acetate of 250 ℃, the fine tributyl citrate of second of 340 ℃; Under stirring, add the organic resin that mass percent is 5%～20%, described organic resin is comprised of two or more following substances: the epoxy resin that decomposition temperature is 180～200 ℃, the cellulose of 200～220 ℃, phenolic resins, the acrylic resin more than 270 ℃ of 200～250 ℃; Then dissolve 0.5～3 hour at 70～120 ℃ of temperature, obtain transparent organic binder bond;
(2) preparation of unleaded back silver paste
Formula rate according to the unleaded conductive silver paste in the above-mentioned back side, inorganic binder and minute enzymolysis auxiliary agent are joined in the organic binder bond that step (1) prepares, mix and roll 2～4 times with three-roll grinder afterwards, the silver powder that adds again required quality, being rolling to the slurry fineness with three-roller again after mixing, to be less than 10 microns, viscosity be 25～35Pa.s, obtains unleaded back silver paste.
Compared with prior art, beneficial effect of the present invention is embodied in:
(1) by the organic resin of two or more different decomposition temperature and the organic solvent of different boiling, be used in combination, make organic solvent, organic resin volatilize in gradient, decompose in drying, sintering process, the concentrated volatilization because of solvent, resin, the bulge of electrode rete and the cavitation that decomposition produces have been avoided, make the electrode rete of formation smooth, fine and close, improved conversion efficiency and the welding performance of cell piece.
(2) by adding appropriate minute enzymolysis auxiliary agent, be conducive to organic resin in sintering process evenly, stably gasification, while making to burn, the oxidation contact area increases, and then sufficient combustion, and organic system is decomposed fully, avoids electrode rete yellowing phenomenon; Reduce the content of ashes that burning forms, intensifier electrode electric conductivity and welding performance.
(3) this preparation method technique is simple, and what prepare unleadedly leads that back silver paste is uniformly dispersed, modest viscosity, when keeping low silver amount, has guaranteed the printing performance of back of the body silver slurry; Formed electrode film is fine and close evenly, good with the adhesive force of silicon chip, and the electric conductivity of electrode is high, welding performance is good.
Embodiment
Unleaded back silver paste provided by the invention is comprised of silver powder, inorganic binder, organic binder bond and a minute enzymolysis auxiliary agent.Inorganic binder melting when high temperature, and form and be connected between silicon chip and electrode.For meeting environmental requirement, inorganic binder in the present invention adopts the crown glass binding agent, select especially Ba-Zn-B glass system, Bi-B-Si glass system or diethylene glycol butyl ether glass system, these crown glass binding agents are conventionally known to one of skill in the art, and it can directly be bought and also can adopt method well known to those skilled in the art to prepare from market.More even for the crown glass binding agent is mixed, the particle diameter of glass binder is controlled at below 10 microns, and consumption is controlled at 5～15% of conductive silver paste total weight.Because, if, by quantity not sufficient 5%, can affect the adhesive force between silicon substrate and silver electrode; If consumption surpasses 15%, can affect electrical property and the welding performance of cell piece.
Silver powder is as the conducting function phase in conductive silver paste, can select spherical, sheet or microplate shape silver powder.The differences such as the particle diameter of silver powder, pattern, specific area, can cause the performance of gained slurry to have larger difference.The inventor finds after deliberation, under the same conditions, use the resulting slurry viscosity of spherical silver powder on the low side, and after sintering, silver-colored intergranular connection is not tight, easily forms cavity, and the welding performance of electrode is poor.Although the welding performance of flake silver powder is better than ball shape silver powder, if the sheet degree is excessive, during the preparation slurry, can cause the viscosity of slurry higher, and the sintering difficulty, cause electrical property to descend.Consider the relation between slurry viscosity and performance, it is 1.8～2.4m at 2～10 microns, specific area that the present invention selects average grain diameter
2the microplate shape silver powder of/g, if the particle diameter of silver powder is excessive or too small, all can affect sintering process, thereby affect electrical property; If the specific area of silver powder is excessive, will affect be mixed with slurry viscosity; If specific area is too small, can affect formed electrode welding performance.
The Main Function of organic binder bond is to give the certain viscosity of electrocondution slurry and thixotropy, makes it to be suitable for the requirement of typography.In the present invention, the consumption of organic binder bond is controlled at 30～55% of conductive silver paste total weight, if the consumption of organic binder bond is less than 30%, the slurry thixotropy reduces, and printing performance is influenced; If the consumption of organic binder bond is greater than 55%, slurry viscosity is too low, is unfavorable for the raising of conductivity.In the present invention, organic binder bond is comprised of from the organic solvent of different evaporation rates the organic resin of several different decomposition temperature.Particularly preferably be, the phenolic resins of the cellulose of the epoxy resin that organic resin is 180-200 ℃ by decomposition temperature, 200-220 ℃, 200-250 ℃, two or more in the acrylic resin more than 270 ℃ form; Two or more in the fine tributyl citrate of second of the dimethylbenzene of 140 ℃ of boiling points, the diethylene glycol ether of 200 ℃, the terpinol of 220 ℃, the butyl carbitol acetate of 250 ℃ and 340 ℃ of organic solvent forms.The inventor finds after deliberation, use organic binder bond provided by the invention during the preparation slurry, when the drying of cell piece, high-temperature sintering process, the shape volatilization in gradient of organic solvent, organic resin, decomposition, the concentrated volatilization because of solvent, resin, the bulge of electrode rete and the cavitation that decomposition produces have been avoided, make the electrode rete of formation smooth, fine and close, because interelectrode cavity easily causes electrode at the how empty area change of weld interface existence and in initiation crack, interface, cause that series resistance increases, and reduce the welding pulling force.
Reduction along with silver content, for guaranteeing the printing performance of slurry, the consumption of organic binder bond will increase, a large amount of organic binder bonds dodges at high temperature under the sintering condition burnt and decomposes not thorough, organic resin charing fully, cause the electrode surface yellowing formed, the electrical property of electrode and welding performance descend, thereby also affect the conversion efficiency of solar cell.The inventor finds after deliberation, the reaction that metal copper ion, iron ion at high temperature have the thermal oxidation of catalysis organic macromolecule to decompose.Can the oxy radical in resin be combined and form complex compound due to metal copper ion, iron ion, accelerate the fracture of c-c key by In frared spectra.Metal oxide with catalytic action also can promote the fracture of c-c key in long carbochain to decompose.Therefore, by adding appropriate minute enzymolysis auxiliary agent, can be when keeping low silver amount, guaranteed the printing performance of back silver paste, and be easy to resin in sintering process evenly, stably gasification, while making to burn, the oxidation contact area increases, and then sufficient combustion, organic system is decomposed fully, avoid electrode rete yellowing phenomenon; Reduce the content of ashes that burning forms, intensifier electrode electric conductivity and welding performance.In the present invention, the consumption of minute enzymolysis auxiliary agent is controlled at 0～1.0% of conductive silver paste total weight.If consumption is greater than 1.0%, affect the electrical property of electrode.
Can prepare by following method by unleaded back silver paste provided by the invention:
(1) preparation of organic binder bond
Take according to formula rate the organic solvent that mass percent is 80%～95%, described organic solvent is comprised of two or more following substances: the dimethylbenzene that boiling point is 140 ℃, the diethylene glycol ether of 200 ℃, the terpinol of 220 ℃, the butyl carbitol acetate of 250 ℃, the fine tributyl citrate of second of 340 ℃; Under stirring, add the organic resin that mass percent is 5%～20%, described organic resin is comprised of two or more following substances: the epoxy resin that decomposition temperature is 180～200 ℃, the cellulose of 200～220 ℃, phenolic resins, the acrylic resin more than 270 ℃ of 200～250 ℃; Then dissolve 0.5～3 hour at 70～120 ℃ of temperature, obtain transparent organic binder bond;
(2) preparation of unleaded back silver paste
Formula rate according to the unleaded conductive silver paste in the above-mentioned back side, inorganic binder and minute enzymolysis auxiliary agent are joined in the organic binder bond that step (1) prepares, mix and roll 2～4 times with three-roll grinder afterwards, the silver powder that adds again required quality, being rolling to the slurry fineness with three-roller again after mixing, to be less than 10 microns, viscosity be 25～35Pa.s, obtains unleaded back silver paste.
Below in conjunction with specific embodiment, the invention will be further described.
Embodiment 1
(1) preparation of organic binder bond
Take 16g terpinol, 10g butyl carbitol acetate, 12g diethylene glycol butyl ether, mix, add 1g ethyl cellulose, 1g acrylic resin under stirring and be heated to 90 ℃, dissolve 1.5 hours, obtain organic binder bond, standby.
(2) preparation of unleaded back silver paste
Take the Bi of 5g
2o
3--SiO
2-ZnO system crown glass binding agent (softening temperature is 500 ℃, Kunming Nuo Man Electron Material Co., Ltd produce) adds in above-mentioned organic binder bond, after mixing, with three-roll grinder, grind 2 times, then to add the 55g average grain diameter is that 5 μ m, specific area are 1.8m
2the microplate shape silver powder of/g, being ground to the slurry fineness after stirring, to be less than 10 microns, viscosity be 25～35Pa.s, obtains unleaded back silver paste.
Embodiment 2
(1) preparation of organic binder bond
Take 20g dimethylbenzene, 7g diethylene glycol butyl ether, mix, add 2g epoxy resin, 1g phenolic resins under stirring and be heated to 70 ℃, dissolve 3 hours, obtain organic binder bond, standby.
(2) preparation of unleaded back silver paste
(softening temperature is 550 ℃ to take the Ba-Zn-B system crown glass binding agent of 15g, Kunming Nuo Man Electron Material Co., Ltd produces) add in above-mentioned organic binder bond, after mixing, with three-roll grinder, grind 3 times, then to add the 55g average grain diameter be that 5 μ m, specific area are 1.8m
2the microplate shape silver powder of/g, being ground to the slurry fineness after stirring, to be less than 10 microns, viscosity be 25～35Pa.s, obtains unleaded back silver paste.
Embodiment 3
(1) preparation of organic binder bond
Take 20g dimethylbenzene, 14g tributyl 2-acetylcitrate, 10g terpinol, mix, add 5g epoxy resin, 2g acrylic resin, 4g ethyl cellulose resin under stirring and be heated to 120 ℃, dissolve 0.5 hour, obtain organic binder bond, standby.
(2) preparation of unleaded back silver paste
(softening temperature is 550 ℃ to take the Ba-Zn-B system crown glass binding agent of 5g, Kunming Nuo Man Electron Material Co., Ltd produces) add in above-mentioned organic binder bond, after mixing, with three-roll grinder, grind 3 times, then to add the 40g average grain diameter be that 2 μ m, specific area are 2.4m
2the microplate shape silver powder of/g, being ground to the slurry fineness after stirring, to be less than 10 microns, viscosity be 25～35Pa.s, obtains unleaded back silver paste.
Embodiment 4
(1) preparation of organic binder bond
Take 10g dimethylbenzene, 15g tributyl 2-acetylcitrate, 10g diethylene glycol butyl ether, mix, add 1g phenolic resins, 1g acrylic resin, 2g ethyl cellulose resin under stirring and be heated to 100 ℃, dissolve 2 hours, obtain organic binder bond, standby.
(2) preparation of unleaded back silver paste
(softening temperature is 490 ℃ to take the Bi-B-Si system crown glass binding agent of 10g, the production of Zhuhai Xuan Yang Co., Ltd), the 1g copper nitrate adds in above-mentioned organic binder bond, after mixing, with three-roll grinder, grind 4 times, then to add the 48g average grain diameter be that 10 μ m, specific area are 2.2m
2the microplate shape silver powder of/g, being ground to the slurry fineness after stirring, to be less than 10 microns, viscosity be 25～35Pa.s, obtains unleaded back silver paste.
Embodiment 5
(1) preparation of organic binder bond
With embodiment 4
(2) preparation of unleaded back silver paste
(softening temperature is 490 ℃ to take the Bi-B-Si system crown glass binding agent of 10g, the production of Zhuhai Xuan Yang Co., Ltd), the 0.5g ferric nitrate adds in above-mentioned organic binder bond, after mixing, with three-roll grinder, grind 4 times, then to add the 50g average grain diameter be that 6 μ m, specific area are 2.0m
2the microplate shape silver powder of/g, being ground to the slurry fineness after stirring, to be less than 10 microns, viscosity be 25～35Pa.s, obtains unleaded back silver paste.
Execute example 6
(1) preparation of organic binder bond
With embodiment 4
(2) preparation of unleaded back silver paste
Take the Bi of 10g
2o
3--SiO
2(softening temperature is 500 ℃ to-ZnO system crown glass binding agent, the production of Kunming Nuo Man Electron Material Co., Ltd), 0.2g manganese dioxide adds in above-mentioned organic binder bond, after mixing, with three-roll grinder, grind 4 times, then to add the 50g average grain diameter be that 4 μ m, specific area are 2.0m
2the microplate shape silver powder of/g, being ground to the slurry fineness after stirring, to be less than 10 microns, viscosity be 25～35Pa.s, obtains unleaded back silver paste.
Execute example 7
(1) preparation of organic binder bond
With embodiment 4
(2) preparation of unleaded back silver paste
Take the Bi of 10g
2o
3--SiO
2(softening temperature is 500 ℃ to-ZnO system crown glass binding agent, the production of Kunming Nuo Man Electron Material Co., Ltd), 0.2g ferrocene, 0.1g manganese dioxide add in above-mentioned organic binder bond, after mixing, with three-roll grinder, grind 4 times, then to add the 50g average grain diameter be that 4 μ m, specific area are 2.0m
2the microplate shape silver powder of/g, being ground to the slurry fineness after stirring, to be less than 10 microns, viscosity be 25～35Pa.s, obtains unleaded back silver paste.
Comparative Examples
(1) preparation of organic binder bond
Take under the stirring of 4g ethyl cellulose resin and add in the 36g diethylene glycol ether and be heated to 90 ℃, dissolve 1 hour, obtain organic binder bond, standby.
(2) preparation of unleaded back silver paste
Take the Bi of 10g
2o
3--SiO
2-ZnO system crown glass binding agent (softening temperature is 500 ℃, Kunming Nuo Man Electron Material Co., Ltd produce) adds in above-mentioned organic binder bond, after mixing, with three-roll grinder, grind 3 times, then to add the 50g average grain diameter is that 4 μ m, specific area are 2.0m
2the microplate shape silver powder of/g, being ground to the slurry fineness after stirring, to be less than 10 microns, viscosity be 25～35Pa.s, obtains unleaded back silver paste.
The back of the body silver slurry that above-described embodiment 1～7 and Comparative Examples are obtained is applied to following formula:
By back surface field aluminum paste of solar battery by silk screen printing on the polycrystalline silicon substrate of 156*156mm two sides making herbs into wool, form electrode film, advance 200 ℃ of oven dry of continuous tunnel furnace.Print above-mentioned gained back silver paste at the same face again, dry, then change another side printing front side silver paste, sintering after drying, 930 ℃ of peak temperatures, come out of the stove rear with silicon solar cell efficiency test measurement device electrical property, apparent with microscopic examination gate line electrode cross section.
With 180
0tensile test is estimated the welding pulling force of back electrode.The welding (1.8mm) that manually will be soaked with scolder with 325 ℃ of flatirons is welded on back of the body silver electrode, uses dynamometer 180
0direction is peeled off with the speed of 0.5cm/s, often carries out a numerical value of 2cm record, then averages.
The properties mean value of measuring is as follows:
| ? | Isc（A） | Voc(V) | Rs(m?) | Conversion efficiency (%) | Adhesive force | Electrode is apparent |
| Embodiment 1 | 8.5054 | 0.6228 | 2.502 | 17.23 | 4.6 N | Fine and close, smooth |
| Embodiment 2 | 8.5130 | 0.6230 | 2.478 | 17.22 | 4.7 N | Fine and close, smooth |
| Embodiment 3 | 8.5120 | 0.6231 | 2.326 | 17.23 | 4.2 N | Fine and close, smooth |
| Embodiment 4 | 8.5035 | 0.6229 | 2.330 | 17.11 | 4.5N | Fine and close, smooth |
| Embodiment 5 | 8.5139 | 0.6226 | 2.249 | 17.24 | 4.3 N | Fine and close, smooth |
| Embodiment 6 | 8.5046 | 0.6225 | 2.312 | 17.19 | 3.9 N | Fine and close, smooth |
| Embodiment 7 | 8.5190 | 0.6228 | 2.420 | 17.26 | 4.6N | Fine and close, smooth |
| Comparative Examples | 8.3419 | 0.6156 | 3.126 | 16.25 | 2.8N | Cavity is arranged |
Annotate: Isc is short circuit current, and Voc is open circuit voltage, and Rs is series resistance.
Claims (4)
1. the unleaded back silver paste of low-cost crystal silicon solar energy battery, is characterized in that, prepared by each component of following mass percent by described silver paste: silver powder 40～55%; Crown glass binding agent 5～15%; Organic binder bond 30～55%; Divide enzymolysis auxiliary agent 0～1.0%; Described silver powder is that 2～10 microns of average grain diameters, specific area are 1.8～2.4m
2the microplate shape silver powder of/g; Described organic binder bond is prepared from by the organic resin of mass percent 5%～20%, 80%～95% organic solvent, and organic resin is selected from epoxy resin that decomposition temperature is 180～200 ℃, the cellulose of 200～220 ℃, phenolic resins, two or more in the acrylic resin more than 270 ℃ of 200～250 ℃; Organic solvent is selected from the dimethylbenzene of 140 ℃ of boiling points, the diethylene glycol ether of 200 ℃, the terpinol of 220 ℃, butyl carbitol acetate, two or more in the fine tributyl citrate of second of 340 ℃ of 250 ℃.
2. unleaded back silver paste according to claim 1, is characterized in that, slaine or metal oxide that described minute enzymolysis auxiliary agent is copper ions, iron ion and manganese ion.
3. unleaded back of the body silver slurry according to claim 2, is characterized in that, within described minute, enzymolysis auxiliary agent is one or more in copper nitrate, ferric nitrate, manganese dioxide, ferrocene.
4. one kind prepares as claim 1, the 2 or 3 described low-cost crystal silicon solar energy batteries method with unleaded back silver paste, it is characterized in that, it comprises the following steps:
The preparation of A, organic binder bond
Take by described formula rate the organic solvent that mass percent is 80%～95%, described organic solvent is comprised of two or more following substances: the dimethylbenzene that boiling point is 140 ℃, the diethylene glycol ether of 200 ℃, the terpinol of 220 ℃, the butyl carbitol acetate of 250 ℃, the fine tributyl citrate of second of 340 ℃; Under stirring, add the organic resin that mass percent is 5%～20%, described organic resin is comprised of two or more following substances: the epoxy resin that decomposition temperature is 180～200 ℃, the cellulose of 200～220 ℃, phenolic resins, the acrylic resin more than 270 ℃ of 200～250 ℃; Then dissolve 0.5～3 hour at 70～120 ℃ of temperature, obtain transparent organic binder bond;
The preparation of B, unleaded back silver paste
Formula rate according to the unleaded conductive silver paste in the above-mentioned back side, inorganic binder and minute enzymolysis auxiliary agent are joined in the organic binder bond that step (1) prepares, mix and roll 2～4 times with three-roll grinder afterwards, the silver powder that adds again required quality, being rolling to the slurry fineness with three-roller again after mixing, to be less than 10 microns, viscosity be 25～35Pa.s, obtains unleaded back silver paste.
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