CN103440901B - Low cost crystal silicon solar energy battery unleaded back silver paste and preparation method - Google Patents
Low cost crystal silicon solar energy battery unleaded back silver paste and preparation method Download PDFInfo
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Abstract
A kind of low cost crystal silicon solar energy battery unleaded back silver paste and preparation method.Component and the mass percent of described unleaded conductive silver paste are as follows: argentum powder 40～55%；Crown glass binding agent 5～15%；Organic binder bond 30～55%；Precipitation additive 0～1.0%；Wherein, described argentum powder be mean diameter 2～10 microns, specific surface area be 1.8～2.4m2Micro-flake silver powder of/g；Described organic binder bond is that the organic resin by several different decomposition temperature forms from the organic solvent of different evaporation rates.The back of the body conductive silver slurry that the present invention prepares, modest viscosity, the electrode film layer formed is fine and close, and welding performance is excellent, and conversion efficiency is high.
Description
Technical field
The present invention relates to a kind of crystal silicon solar energy battery unleaded back silver paste and preparation method.
Background technology
Solaode is a kind of semiconductor device that solar energy is changed into electric energy, and under illumination condition, inside solar energy battery produces photogenerated current, can directly be exported by electric energy by electrode.In order to by the maximum amount of for electric energy output, electrode fabrication is a very important link.Silicon solar battery electrode includes that front silver electrode and back silver electrode, aluminum electrode, crystal silicon solar batteries back silver slurry use as the back electrode of solaode, primarily serve the effect of collected current.Back silver paste is mainly made up of conducting function phase, organic carrier, inorganic binder three parts, and owing to back silver electrode needs to weld together with metal electrode to be 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 commercially, the silver content constantly reducing slurry has become inexorable trend and the competitive method of numerous slurry manufacturer of current back silver paste development.Along with the reduction of silver content, necessarily affect printing performance and the welding performance of back silver paste.In order to ensure the printing performance of slurry, need to increase the consumption of organic carrier in slurry, but substantial amounts of organic carrier decomposes the most thorough under the sintering condition of high temperature flash burning, organic resin not carbonization completely, the surface yellowing of the electrode resulted in, electrical property and welding performance decline, thus affect the conversion efficiency of solaode.
Summary of the invention
The technical problem to be solved is for deficiencies of the prior art, it is provided that a kind of unleaded back silver paste of low cost crystal silicon solar energy battery.
Another technical problem to be solved by this invention is to provide the preparation method of the unleaded back silver paste of a kind of low cost crystal silicon solar energy battery.
For solving above-mentioned technical problem, the technical solution used in the present invention is as follows:
A kind of unleaded back silver paste of low cost crystal silicon solar energy battery, silver paste material prepared by each component of following mass percent: argentum powder 40～55%；Crown glass binding agent 5～15%；Organic binder bond 30～55%；Precipitation additive 0～1.0%；Described argentum powder be mean diameter 2～10 microns, specific surface area be 1.8～2.4m2Micro-flake silver powder of/g；Described organic binder bond is prepared from by the organic solvent of mass percent 5～the organic resin of 20%, 80～95%, organic resin selected from decomposition temperature is in the epoxy resin of 180～200 DEG C, the cellulose of 200～220 DEG C, the phenolic resin of 200～250 DEG C, the acrylic resin of more than 270 DEG C two or more, organic solvent is selected from two or more in the dimethylbenzene of boiling point 140 DEG C, the diethylene glycol ether of 200 DEG C, the terpineol of 220 DEG C, the butyl carbitol acetate of 250 DEG C, the second fibre tributyl citrate of 340 DEG C.
Above-mentioned unleaded back silver paste, described precipitation additive is selected from copper ions, iron ion and the slaine of manganese ion or metal-oxide.
Above-mentioned unleaded back silver paste, described precipitation additive is one or more in copper nitrate, ferric nitrate, manganese dioxide, ferrocene.
A kind of low cost crystal silicon solar energy battery preparation method of unleaded back silver paste, it comprises the following steps:
(1) preparation of organic binder bond
Weighing, according to formula proportion, the organic solvent that mass percent is 80～95%, described organic solvent is made up of two or more following substances: the dimethylbenzene that boiling point is 140 DEG C, the diethylene glycol ether of 200 DEG C, the terpineol of 220 DEG C, the butyl carbitol acetate of 250 DEG C, the second fibre tributyl citrate of 340 DEG C；Under stirring, adding the organic resin that mass percent is 5%～20%, described organic resin is made up of two or more following substances: decomposition temperature is the epoxy resin of 180～200 DEG C, the cellulose of 200～220 DEG C, the phenolic resin of 200～250 DEG C, the acrylic resin of more than 270 DEG C；Then dissolve 0.5～3 hour at a temperature of 70～120 DEG C, obtain transparent with machine binding agent；
(2) preparation of unleaded back silver paste
Formula proportion according to the unleaded conductive silver paste in the above-mentioned back side, inorganic binder and precipitation additive are joined in the organic binder bond that step (1) prepares, 2～4 times are rolled with three-roll grinder after mix homogeneously, add the argentum powder of required quality, after mix homogeneously again with three-roller be rolling to slurry fineness less than 10 microns, viscosity be 25～35Pa.s, obtain unleaded back silver paste.
Compared with prior art, beneficial effects of the present invention is embodied in:
(1) used by the organic solvent combination of the organic resin of two or more different decomposition temperature with different boiling, organic solvent, organic resin is made to be dried, sintering process is volatilized in gradient, decompose, avoid the electrode film layer bulge and cavitation produced because of solvent, the concentration volatilization of resin, decomposition, the electrode film layer making formation is smooth, fine and close, improves conversion efficiency and the welding performance of cell piece.
(2) by adding appropriate precipitation additive, beneficially organic resin in sintering process uniformly, stably gasify, when making burning, oxidation contact area increases, and then burning is fully, makes organic system decompose completely, it is to avoid electrode film layer yellowing phenomenon；Reduce the content of ashes that burning is formed, strengthen electrodes conduct performance and welding performance.
(3) this preparation method technique is simple, prepare unleaded lead back silver paste be uniformly dispersed, modest viscosity, while keeping low silver amount, it is ensured that the printing performance of back silver paste；The electrode film dense uniform formed is good with the adhesive force of silicon chip, and the electric conductivity of electrode is high, welding performance is excellent.
Detailed description of the invention
The unleaded back silver paste that the present invention provides is made up of argentum powder, inorganic binder, organic binder bond and precipitation additive.Inorganic binder is at elevated temperature melts, and forms connection between silicon chip and electrode.For meeting environmental requirement, inorganic binder in the present invention uses crown glass binding agent, select Ba-Zn-B glass system, Bi-B-Si glass system or butyl glass system especially, these crown glass binding agents are known to those skilled in the art, and it directly can be bought from market and method well known to those skilled in the art can also be used to prepare.In order to make the mixing of crown glass binding agent more uniform, the size controlling of glass binder is below 10 microns, and consumption controls in the 5～15% of conductive silver paste gross weight.Because if consumption is less than 5%, then the adhesive force between silicon substrate and silver electrode can be affected；If consumption is more than 15%, then can affect electrical property and the welding performance of cell piece.
Argentum powder, as the conducting function phase in conductive silver paste, may select spherical, lamellar or micro-flake silver powder.The differences such as the particle diameter of argentum powder, pattern, specific surface area, can cause the performance of gained slurry to there is larger difference.Inventor it has been investigated that, under the same conditions, use obtained by spherical argentum powder slurry viscosity on the low side, and connection between Argent grain is tight after sintering, and 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 but flaking degree is excessive, and the viscosity that can cause slurry during preparation slurry is higher, and sinters difficulty, causes electrical property to decline.Consider the relation between slurry viscosity and performance, the present invention select mean diameter 2～10 microns, specific surface area be 1.8～2.4m2Micro-flake silver powder of/g, if the particle diameter of argentum powder is excessive or too small, all can affect sintering process, thus affect electrical property；If the specific surface area of argentum powder is excessive, it will the slurry viscosity that impact is configured to；If specific surface area is too small, then can affect formed electrode welding performance.
The Main Function of organic binder bond is to confer to the certain viscosity of electrocondution slurry and thixotropy, is allowed to be suitable to the requirement of typography.In the present invention, the consumption of organic binder bond controls in the 30～55% of conductive silver paste gross weight, if the consumption of organic binder bond is less than 30%, then slurry thixotropy reduces, and printing performance is impacted；If the consumption of organic binder bond is more than 55%, then slurry viscosity is too low, is unfavorable for the raising of electric conductivity.In the present invention, organic binder bond is made up of from the organic solvent of different evaporation rates the organic resin of several different decomposition temperature.It is particularly preferred that organic resin is made up of two or more in the epoxy resin that decomposition temperature is 180-200 DEG C, the cellulose of 200-220 DEG C, the phenolic resin of 200-250 DEG C, the acrylic resin of more than 270 DEG C；Organic solvent is made up of two or more in the second fibre tributyl citrate of the dimethylbenzene of boiling point 140 DEG C, the diethylene glycol ether of 200 DEG C, the terpineol of 220 DEG C, the butyl carbitol acetate of 250 DEG C and 340 DEG C.Inventor it has been investigated that, the organic binder bond that the present invention provides is used during preparation slurry, cell piece be dried, high-temperature sintering process time, the volatilization of organic solvent, organic resin shape in gradient, decomposition, avoid the electrode film layer bulge and cavitation produced because of solvent, the concentration volatilization of resin, decomposition, the electrode film layer making formation is smooth, fine and close, increase and in interfacial initiation crack because interelectrode cavity is easily caused the how empty areas that electrode exists at weld interface, cause series resistance to increase, and reduce welding pulling force.
Reduction along with silver content, for ensureing the printing performance of slurry, the consumption of organic binder bond will increase, substantial amounts of organic binder bond decomposes thoroughly under the sintering condition of high temperature flash burning, organic resin can not carbonization completely, the electrode surface yellowing resulted in, the electrical property of electrode and welding performance decline, thus also affect the conversion efficiency of solaode.Inventor it has been investigated that, metal copper ion, iron ion at high temperature have catalysis organic macromolecule thermal oxide decompose reaction.Owing to metal copper ion, iron ion can be combined formation complex with the oxy radical in resin, accelerated the fracture of c-c key by In frared spectra.The metal-oxide with catalytic action also can promote that the fracture of c-c key in Long carbon chain is decomposed.Therefore, by adding appropriate precipitation additive, can be while keeping low silver amount, ensure that the printing performance of back silver paste, and have and be prone to resin in sintering process uniformly, stably gasify, when making burning, oxidation contact area increases, and then burning is fully, organic system is made to decompose completely, it is to avoid electrode film layer yellowing phenomenon；Reduce the content of ashes that burning is formed, strengthen electrodes conduct performance and welding performance.In the present invention, the consumption of precipitation additive controls in the 0～1.0% of conductive silver paste gross weight.If consumption is more than 1.0%, then affect the electrical property of electrode.
The unleaded back silver paste that the present invention provides can be prepared by following method:
(1) preparation of organic binder bond
Weighing, according to formula proportion, the organic solvent that mass percent is 80%～95%, described organic solvent is made up of two or more following substances: the dimethylbenzene that boiling point is 140 DEG C, the diethylene glycol ether of 200 DEG C, the terpineol of 220 DEG C, the butyl carbitol acetate of 250 DEG C, the second fibre tributyl citrate of 340 DEG C；Under stirring, adding the organic resin that mass percent is 5%～20%, described organic resin is made up of two or more following substances: decomposition temperature is the epoxy resin of 180～200 DEG C, the cellulose of 200～220 DEG C, the phenolic resin of 200～250 DEG C, the acrylic resin of more than 270 DEG C；Then dissolve 0.5～3 hour at a temperature of 70～120 DEG C, obtain transparent with machine binding agent；
(2) preparation of unleaded back silver paste
Formula proportion according to the unleaded conductive silver paste in the above-mentioned back side, inorganic binder and precipitation additive are joined in the organic binder bond that step (1) prepares, 2～4 times are rolled with three-roll grinder after mix homogeneously, add the argentum powder of required quality, after mix homogeneously again with three-roller be rolling to slurry fineness less than 10 microns, viscosity be 25～35Pa.s, obtain unleaded back silver paste.
Below in conjunction with specific embodiment, the invention will be further described.
Embodiment 1
(1) preparation of organic binder bond
Weighing 16g terpineol, 10g butyl carbitol acetate, 12g butyl, mixing, stirring is lower to add 1g ethyl cellulose, 1g acrylic resin and is heated to 90 DEG C, dissolves 1.5 hours, obtains organic binder bond, standby.
(2) preparation of unleaded back silver paste
Weigh the Bi of 5g2O3--SiO2-ZnO system crown glass binding agent (softening temperature is 500 DEG C, Kunming Nuo Man Electron Material Co., Ltd produce) adds in above-mentioned organic binder bond, grinds 2 times with three-roll grinder after mixing, add 55g mean diameter be 5 μm, specific surface area be 1.8m2Micro-flake silver powder of/g, be ground to after stirring slurry fineness less than 10 microns, viscosity be 25～35Pa.s, obtain unleaded back silver paste.
Embodiment 2
(1) preparation of organic binder bond
Weighing 20g dimethylbenzene, 7g butyl, mixing, stirring is lower to add 2g epoxy resin, 1g phenolic resin and is heated to 70 DEG C, dissolves 3 hours, obtains organic binder bond, standby.
(2) preparation of unleaded back silver paste
(softening temperature is 550 DEG C to weigh 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, grind 3 times with three-roll grinder after mixing, add 55g mean diameter be 5 μm, specific surface area be 1.8m2Micro-flake silver powder of/g, be ground to after stirring slurry fineness less than 10 microns, viscosity be 25～35Pa.s, obtain unleaded back silver paste.
Embodiment 3
(1) preparation of organic binder bond
Weighing 20g dimethylbenzene, 14g tributyl 2-acetylcitrate, 10g terpineol, mixing, stirring is lower to add 5g epoxy resin, 2g acrylic resin, 4g ethyl cellulose resin and is heated to 120 DEG C, dissolves 0.5 hour, obtains organic binder bond, standby.
(2) preparation of unleaded back silver paste
(softening temperature is 550 DEG C to weigh 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, grind 3 times with three-roll grinder after mixing, add 40g mean diameter be 2 μm, specific surface area be 2.4m2Micro-flake silver powder of/g, be ground to after stirring slurry fineness less than 10 microns, viscosity be 25～35Pa.s, obtain unleaded back silver paste.
Embodiment 4
(1) preparation of organic binder bond
Weighing 10g dimethylbenzene, 15g tributyl 2-acetylcitrate, 10g butyl, mixing, stirring is lower to add 1g phenolic resin, 1g acrylic resin, 2g ethyl cellulose resin and is heated to 100 DEG C, dissolves 2 hours, obtains organic binder bond, standby.
(2) preparation of unleaded back silver paste
(softening temperature is 490 DEG C to weigh the Bi-B-Si system crown glass binding agent of 10g, Zhuhai Xuan Yang company limited produces), 1g copper nitrate adds in above-mentioned organic binder bond, grind 4 times with three-roll grinder after mixing, add 48g mean diameter be 10 μm, specific surface area be 2.2m2Micro-flake silver powder of/g, be ground to after stirring slurry fineness less than 10 microns, viscosity be 25～35Pa.s, obtain 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 DEG C to weigh the Bi-B-Si system crown glass binding agent of 10g, Zhuhai Xuan Yang company limited produces), 0.5g ferric nitrate adds in above-mentioned organic binder bond, grind 4 times with three-roll grinder after mixing, add 50g mean diameter be 6 μm, specific surface area be 2.0m2Micro-flake silver powder of/g, be ground to after stirring slurry fineness less than 10 microns, viscosity be 25～35Pa.s, obtain unleaded back silver paste.
Execute example 6
(1) preparation of organic binder bond
With embodiment 4
(2) preparation of unleaded back silver paste
Weigh the Bi of 10g2O3--SiO2(softening temperature is 500 DEG C to-ZnO system crown glass binding agent, Kunming Nuo Man Electron Material Co., Ltd produces), 0.2g manganese dioxide adds in above-mentioned organic binder bond, grind 4 times with three-roll grinder after mixing, add 50g mean diameter be 4 μm, specific surface area be 2.0m2Micro-flake silver powder of/g, be ground to after stirring slurry fineness less than 10 microns, viscosity be 25～35Pa.s, obtain unleaded back silver paste.
Execute example 7
(1) preparation of organic binder bond
With embodiment 4
(2) preparation of unleaded back silver paste
Weigh the Bi of 10g2O3--SiO2(softening temperature is 500 DEG C to-ZnO system crown glass binding agent, Kunming Nuo Man Electron Material Co., Ltd produces), 0.2g ferrocene, 0.1g manganese dioxide adds in above-mentioned organic binder bond, grind 4 times with three-roll grinder after mixing, add 50g mean diameter be 4 μm, specific surface area be 2.0m2Micro-flake silver powder of/g, be ground to after stirring slurry fineness less than 10 microns, viscosity be 25～35Pa.s, obtain unleaded back silver paste.
Comparative example
(1) preparation of organic binder bond
Weigh in 4g ethyl cellulose resin stirring lower addition 36g diethylene glycol ether and be heated to 90 DEG C, dissolving 1 hour, obtain organic binder bond, standby.
(2) preparation of unleaded back silver paste
Weigh the Bi of 10g2O3--SiO2-ZnO system crown glass binding agent (softening temperature is 500 DEG C, Kunming Nuo Man Electron Material Co., Ltd produce) adds in above-mentioned organic binder bond, grinds 3 times with three-roll grinder after mixing, add 50g mean diameter be 4 μm, specific surface area be 2.0m2Micro-flake silver powder of/g, be ground to after stirring slurry fineness less than 10 microns, viscosity be 25～35Pa.s, obtain unleaded back silver paste.
By above-described embodiment 1～7 and the back silver paste that obtains of comparative example be applied to following formula:
By back surface field aluminum paste of solar battery by being screen printed onto on the polycrystalline silicon substrate of 156*156mm two sides making herbs into wool, form electrode film, enter continuous tunnel furnace 200 DEG C drying.Print above-mentioned gained back silver paste at the same face again, dry, then change another side printing front side silver paste, sinter after drying, peak temperature 930 DEG C, with silicon solar cell efficiency test measurement device electrical property after coming out of the stove, observe gate line electrode transverse section with microscope apparent.
With 1800Tensile test evaluates the welding pulling force of back electrode.Manually the welding (1.8mm) being soaked with solder is welded on back of the body silver electrode with 325 DEG C of flatirons, with ergometer 1800Direction is peeled off with the speed of 0.5cm/s, often carries out 2cm and records a numerical value, then averages.
The properties meansigma methods measured is as follows:
| Isc(A) | Voc(V) | Rs(mΩ) | 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 example | 8.3419 | 0.6156 | 3.126 | 16.25 | 2.8N | There is cavity |
Note: Isc is short circuit current, and Voc is open-circuit voltage, and Rs is series resistance.
Claims (3)
1. the unleaded back silver paste of low cost crystal silicon solar energy battery, it is characterised in that silver paste material is prepared by each component of following mass percent: argentum powder 40～55%；Crown glass binding agent 5～15%；Organic binder bond 30～55%；Precipitation additive 0～1.0%；Described argentum powder be mean diameter 2～10 microns, specific surface area be 1.8～2.4m2Micro-flake silver powder of/g；Described organic binder bond is prepared from by the organic solvent of organic resin, 80%～95% of mass percent 5%～20%, and it is two or more that organic resin is selected from the acrylic resin that decomposition temperature is the epoxy resin of 180～200 DEG C, the cellulose of 200～220 DEG C, the phenolic resin of 200～250 DEG C or more than 270 DEG C；It is two or more that organic solvent is selected from the second fibre tributyl citrate of the dimethylbenzene of boiling point 140 DEG C, the diethylene glycol ether of 200 DEG C, the terpineol of 220 DEG C, the butyl carbitol acetate of 250 DEG C or 340 DEG C；
Described precipitation additive is slaine or the metal-oxide of copper ions, iron ion and manganese ion.
The unleaded back silver paste of low cost crystal silicon solar energy battery the most according to claim 1, it is characterised in that described precipitation additive is one or more in copper nitrate, ferric nitrate, manganese dioxide, ferrocene.
3. the method preparing the unleaded back silver paste of low cost crystal silicon solar energy battery as claimed in claim 1 or 2, it is characterised in that comprise the following steps:
A, the preparation of organic binder bond
Weighing, by formula proportion, the organic solvent that mass percent is 80%～95%, described organic solvent is made up of two or more following substances: the dimethylbenzene that boiling point is 140 DEG C, the diethylene glycol ether of 200 DEG C, the terpineol of 220 DEG C, the butyl carbitol acetate of 250 DEG C, the second fibre tributyl citrate of 340 DEG C；Under stirring, adding the organic resin that mass percent is 5%～20%, described organic resin is made up of two or more following substances: decomposition temperature is the epoxy resin of 180～200 DEG C, the cellulose of 200～220 DEG C, the phenolic resin of 200～250 DEG C, the acrylic resin of more than 270 DEG C；Then dissolve 0.5～3 hour at a temperature of 70～120 DEG C, obtain transparent with machine binding agent；
B, the preparation of unleaded back silver paste
Formula proportion according to silver paste, crown glass binding agent and precipitation additive are joined in the organic binder bond that step A prepares, 2～4 times are rolled with three-roll grinder after mix homogeneously, add the argentum powder of required quality, after mix homogeneously again with three-roller be rolling to slurry fineness less than 10 microns, viscosity be 25～35Pa.s, obtain unleaded back silver paste.
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| CN103093861A (en) * | 2013-02-17 | 2013-05-08 | 上海大洲电子材料有限公司 | Low-cost unleaded environmental protection silver paste for back electrode of silicon solar cell and application thereof |
| CN103219064A (en) * | 2013-04-16 | 2013-07-24 | 江苏太阳新材料科技有限公司 | Unleaded back silver paste used for crystalline silicon solar cell and preparation method thereof |
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