CN102779566B - Lead-free conductive silver paste for front faces of crystalline silicon solar cells - Google Patents
Lead-free conductive silver paste for front faces of crystalline silicon solar cells Download PDFInfo
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- CN102779566B CN102779566B CN201210254073.4A CN201210254073A CN102779566B CN 102779566 B CN102779566 B CN 102779566B CN 201210254073 A CN201210254073 A CN 201210254073A CN 102779566 B CN102779566 B CN 102779566B
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Abstract
The invention discloses lead-free conductive silver paste for front faces of crystalline silicon solar cells. The lead-free conductive silver paste is composed of, by weight, 75-85% of silver powder, 0.5-2% of lead-free glass binder, 1-10% of metal alloy powder, 5-15% of organic binder and 1-5% of active oxide, wherein the average particle size of the silver powder ranges from 0.2 micrometer to 1 micrometer, the tap density is larger than 4.5g/cc, and the active oxide is nano gamma-Al2O3 powder. Oxidation of silver particles can be effectively reduced while high-temperature liquidity and wettability of glass materials are improved and stability and electrical performances of the glass materials are improved, and accordingly the open-circuit voltage of the cells can be increased, electrical performances of the cells can be improved, and high conversion efficiency of the solar cells is achieved.
Description
Technical field
The invention belongs to photovoltaic cell technical field, particularly the unleaded conductive silver paste in a kind of crystal silicon solar energy battery front.
Background technology
Solar cell 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 electric energy be exported by electrode.For by the output of electric energy maximum, electrode fabrication is a very important link.Silicon solar battery electrode comprises positive silver electrode and back surface field aluminium electrode, positive silver electrode is larger on the battery conversion efficiency impact of silicon solar cell, the performance of silver paste has directly determined the performance of solar battery sheet front electrode, is the critical material during crystal silicon solar energy battery is manufactured.
Application number is that 201010286804.4 Chinese patent application discloses a kind of leadless environment-friendly type electronic silver paste and preparation method thereof, and this electronic silver paste, by using crown glass binding agent, reaches the problem of leadless environment-friendly, for the front electrode of solar cell.But, due to Shortcomings also aspect its wettability at glass temperature flowing, glass and substrate and stability, cause the cell piece short circuit current after sintering on the low side, thereby affected the conversion efficiency of battery.
In addition, because solar battery front side need to be at sintering under hot conditions with silver-colored slurry, cause silver-colored particle that oxidation easily occurs under hot environment and generate silver oxide, cause the electric conductivity of electrode to decline, thereby also affect the conversion efficiency of solar cell.
Summary of the invention
Technical problem to be solved by this invention is: overcome above-mentioned prior art defect, provide that a kind of crystal silicon solar energy battery is positive uses unleaded conductive silver paste.
For solving the problems of the technologies described above, the technical solution used in the present invention is as follows:
A kind of crystal silicon solar energy battery is positive uses unleaded conductive silver paste, and its component and weight percentage are as follows: silver powder 75～85%; Crown glass binding agent 0.5～2%; Metal alloy powder 1～10%; Organic binder bond 5～15%; Activating oxide 1～5%; Wherein, 0.2～1 micron of described silver powder average grain diameter, tap density are greater than 4.5g/cc; Described activating oxide is nanometer γ-Al
2o
3powder.
Above-mentioned crystal silicon solar energy battery is positive uses unleaded conductive silver paste, and described conductive silver paste also comprises 0.1～2% IrO
2antioxidant.
It is the one of Sn-Ag alloyed powder, Sn-Ag-Cu alloyed powder, Sn-Sb alloyed powder that unleaded conductive silver paste, described metal alloy powder are used in above-mentioned crystal silicon solar energy battery front.
The positive unleaded conductive silver paste, described nanometer γ-Al used of above-mentioned crystal silicon solar energy battery
2o
3the particle diameter of powder is 15～25nm.
The unleaded conductive silver paste in above-mentioned crystal silicon solar energy battery front, described crown glass binding agent adopts the one in B-Zn-Sb glass system, Bi-B-Si glass system, Bi-Si-Zn glass system.
Above-mentioned crystal silicon solar energy battery is positive uses unleaded conductive silver paste, and the organic resin that described organic binder bond is 5～20% by percentage by weight and 80～95% organic solvent form; Described organic resin is one or more in ethyl cellulose, acrylic resin, rosin, NC Nitroncellulose; Described organic solvent is one or more in terpinol, butyl carbitol acetate, diethylene glycol butyl ether, dibutyl phthalate.
The beneficial effect that the present invention obtains is:
(1) the present invention is by adding appropriate activating oxide γ-Al
2o
3, and control the consumption of crown glass binding agent, in the time of high temperature sintering, the glassy phase mutual effect of this activating oxide and melting, has improved temperature flowing and the wettability of frit, has improved stability and the electrical property of frit, activating oxide γ-Al simultaneously
2o
3can also improve compactness and the smoothness of generated electrode film, thereby increase the short circuit current of battery, improve the conversion efficiency of cell piece.
(2) the present invention is also by adding appropriate antioxidant IrO
2, in improving the stability and electrical property of the temperature flowing of frit and wettability, improvement frit, can effectively reduce the oxidation of silver-colored particle, thereby improve the open circuit voltage of battery, improve the electrical property of battery.
Embodiment
Conductive silver paste is mainly made up of conductive phase, glassy phase and organic binder bond, and glassy phase is melting in the time of high temperature mainly, etching antireflective coating, and form and be connected between silicon chip and electrode.For meeting environmental requirement, glassy phase in the present invention adopts crown glass binding agent, select especially B-Zn-Sb glass system, Bi-B-Si glass system or Bi-Si-Zn 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.It is more even for crown glass binding agent is mixed, the particle diameter of glass binder is controlled at below 10 microns, and consumption is controlled at 0.5～2.0% of conductive silver paste total weight, because, if by quantity not sufficient 0.5%, can affect the adhesive force between etching and silicon substrate and the silver electrode of antireflective coating; If consumption exceedes 2.0%, can reduce the electrical property of cell piece.
The consumption of glass binder and kind are one of key factors affecting electrode adhesion and electrical property, for ensureing the adhesive force between silica-based and silver electrode, if use separately glass binder, need to increase its consumption, but a large amount of glass binders easily occurs softening and flows in sintering process, between silica-based and electrode, generate a layer insulating, cause contact resistance to increase, reduce the electrical property of cell piece.In order to keep the equilibrium relation between electrical property and adhesive force, the present invention has taked the method for adding appropriate metal alloy powder, having reduced glass binder consumption, has ensured adhesive force between silicon chip and silver electrode and the electrical property of cell piece.In the present invention, the consumption of metal alloy powder is controlled at 1.0～10% of conductive silver paste total weight, if consumption is less than 1.0%, the adhesive force between silica-based and silver electrode can not be guaranteed; If consumption is greater than 10%, too much alloyed powder is attached to above silicon nitride layer, has affected the etching process of glass dust to antireflective coating.
Be applicable to metal alloy powder of the present invention and there is lower density and fusing point, preferentially adopt Sn-Ag alloyed powder, Sn-Ag-Cu alloyed powder, Sn-Sb alloyed powder.Fusing in metal alloy powder sintering process, infiltration silicon chip and silver-colored particle, reduce the contact resistance between silver-silicon, after cooling, make silica-based and silver electrode formation bonding, strengthen the adhesive force between silica-based and silver electrode, between silver-colored particle and silver-colored particle, also closely link together by metal alloy powder simultaneously, improve electrical property.
Silver powder is as the conducting function phase in conductive silver paste, and general more options are spherical or class is spherical, and the silver powder in the present invention selects average grain diameter to be greater than 4.5g/cc at 0.2～1 micron, tap density.The particle diameter of silver powder is excessive or too small, all can affect sintering process, thereby affect electrical property.The dispersiveness of the tap density reaction silver powder of silver powder, if tap density is too small, the dispersiveness of silver powder is poor, the conductive network forming in sintering process is discontinuous, causes electric conductivity to reduce.In high-temperature sintering process, silver powder also can react with airborne oxygen and generate silver oxide, and the conductivity of silver oxide is poor, causes the electrical property of cell piece to decline.
Inventor finds after deliberation, adds activating oxide nanometer γ-Al in conductive silver paste
2o
3powder, can improve temperature flowing and the wettability of glass binder, improves stability and the electrical property of glass binder, can also improve compactness and the smoothness of generated electrode film simultaneously, raising electrical property.This be because, compared with known technology, activating oxide nanometer γ-Al
2o
3powder can be diffused in the glassy phase of melting in the time of high temperature sintering.γ-Al in the present invention
2o
3consumption be controlled at 1.0～5.0% of conductive silver paste total weight.If addition is less than 1.0%, do not have the effect that improves glass binder performance and electrode film; If addition is greater than 5.0%, the mobility of slurry is excessively strong, the depth-width ratio of impact printing grid line.
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 5～15% of conductive silver paste total weight, if the consumption of organic binder bond is less than 5%, slurry thixotropy reduces, and printing performance is influenced; If the consumption of organic binder bond is greater than 15%, slurry viscosity is too low, is unfavorable for the raising of conductivity.The organic resin that organic binder bond is 5～20% by percentage by weight and 80～95% organic solvent form; Described organic resin is one or more in ethyl cellulose, acrylic resin, rosin, NC Nitroncellulose; Described organic solvent is one or more in terpinol, butyl carbitol acetate, diethylene glycol butyl ether, dibutyl phthalate.
Inventor also finds after deliberation, if appropriate antioxidant IrO is added in invention again
2, in improving the stability and electrical property of the temperature flowing of glass binder and wettability, improvement frit, can effectively reduce the oxidation of silver-colored particle, thereby improve the open circuit voltage of battery, improve the electrical property of battery.In the present invention, antioxidant IrO
2consumption be controlled at 0.1～2.0% of conductive silver paste total weight.If consumption is less than 0.1%, do not have oxidation resistant function; If consumption is greater than 2.0%, affect the adhesive force of electrode.
Conductive silver paste provided by the invention can be prepared by following method:
By the organic solvent mixing and stirring of 5～20% organic resin and 80～95% and be heated to 60-90 DEG C, until polymer dissolves completely, obtain organic binder bond.
Activating oxide, crown glass binding agent and organic bond are mixed by formula rate, then add silver powder and metal alloy powder, stir, grind, obtain the unleaded conductive silver paste in crystal silicon solar batteries front.
200-400 order web plate for above-mentioned slurry, is printed on solar cell silicon chip front by the mode of silk screen printing, and under slurry drying after printing, high temperature, sintering forms positive silver electrode.
Below in conjunction with specific embodiment, the invention will be further described.
Embodiment 1
(1) preparation of organic binder bond
Take 2g ethyl cellulose, 1g acrylic resin, add 3g terpinol, 5g butyl carbitol acetate, 4g diethylene glycol butyl ether, mix and be heated to 60～90 DEG C, dissolve, obtain organic binder bond, for subsequent use.
(2) preparation of unleaded conductive silver paste
Take γ-Al of 1.0g
2o
3the B of (particle diameter is 20nm), 0.5g
2o
3-SiO
2-Bi
2o
3system crown glass binding agent (softening temperature is 500 DEG C), after mixing with 15 grams of above-mentioned organic binder bonds, add again the silver powder (particle diameter is that 0.2 micron, tap density are 4.7g/cc) of 75g, the Sn-Ag(96.5Sn of 10g, 3.5Ag) metal alloy powder, mix, after stirring, grind, obtain the unleaded conductive silver paste of required solar battery front side.
Embodiment 2
(1) preparation of organic binder bond
Take 0.5g rosin, add 4.0g dibutyl phthalate, 5.5g terpinol, mix and be heated to 60～90 DEG C, dissolve, obtain organic binder bond, for subsequent use.
(2) preparation of unleaded conductive silver paste
Take γ-Al of 3.0g
2o
3the Bi of (particle diameter is 15nm), 2.0g
2o
3-SiO
2-ZnO system crown glass binding agent (softening temperature is 550 DEG C), after mixing with 10 grams of above-mentioned organic binder bonds, add again 80g silver powder (particle diameter is that 1.0 microns, tap density are 4.9g/cc), 5.0gSn-Ag-Cu (95.5Sn3.5Ag0.7Cu) metal alloy powder, mix, after stirring, grind, obtain the unleaded conductive silver paste of required solar battery front side.
Embodiment 3
(1) preparation of organic binder bond
Take 0.75g ethyl cellulose, add 2.25g butyl carbitol acetate, 2.0g diethylene glycol butyl ether, mix and be heated to 60～90 DEG C, dissolve, obtain organic binder bond, for subsequent use.
(2) preparation of unleaded conductive silver paste
Take γ-Al of 5.0g
2o
3the B of (particle diameter is 25nm), 1.3g
2o
3-ZnO-Sb
2o
3system crown glass binding agent (softening temperature is 600 DEG C), after mixing with 5.0 grams of above-mentioned organic binder bonds, add again 85g silver powder (particle diameter is that 0.5 micron, tap density are 5.5g/cc), 1.0g metal alloy powder Sn-Sb((95Sn5Sb), mix, after stirring, grind, obtain the unleaded conductive silver paste of required solar battery front side.
Embodiment 4
Prepare when slurry weighs and add 2.0g antioxidant IrO2, addition sequence is not limit.All the other are with embodiment 3
Embodiment 5
(1) preparation of organic binder bond
Prepare when slurry weighs and add 0.1g antioxidant IrO2, addition sequence is not limit.All the other are example 2 simultaneously
Embodiment 6
Prepare when slurry weighs and add 1.0g antioxidant IrO2, addition sequence is not limit.All the other are example 1 simultaneously
Embodiment 7
(1) preparation of organic binder bond
Take 1.0g ethyl cellulose, 0.5g NC Nitroncellulose, add 5.5g butyl carbitol acetate, 3.0g terpinol, mix and be heated to 60～90 DEG C, dissolve, obtain organic binder bond, for subsequent use.
(2) preparation of unleaded conductive silver paste
Take γ-Al of 2.0g
2o
3the B of (particle diameter is 20nm), 1.3g
2o
3-SiO
2-Bi
2o
3system crown glass binding agent (softening temperature is 500 DEG C), after mixing with 10 grams of above-mentioned organic binder bonds, add again 80g silver powder (particle diameter is that 0.7 micron, tap density are 5.8g/cc), 1.0g antioxidant IrO2,5.0g metal alloy powder Sn-Ag(96.5Sn3.5Ag), mix, after stirring, grind, obtain the unleaded conductive silver paste of required solar battery front side.
Comparative example
(1) preparation of organic binder bond
Example 1 simultaneously
(2) preparation of unleaded conductive silver paste
Take the B of 3.0g
2o
3-SiO
2-Bi
2o
3system crown glass binding agent (softening temperature is 500 DEG C), after mixing with 15 grams of above-mentioned organic binder bonds, then add 82g silver powder (particle diameter is that 0.5 micron, tap density are 5.5g/cc), mix, after stirring, grind, obtain the unleaded conductive silver paste of required solar battery front side.
The silver slurry that above-described embodiment 1～7 and comparative example are obtained is applied to following formula:
By back surface field aluminum paste of solar battery by silk screen printing in the crystalline silicon substrate of 125*125mm two sides making herbs into wool, form electrode film, enter 200 DEG C of oven dry of continuous tunnel furnace.Then change another side and print above-mentioned gained front side silver paste, sintering after drying, 890 DEG C of peak temperatures, with silicon solar cell efficiency test measurement device electrical property, apparent with microscopic examination gate line electrode cross section after coming out of the stove.Measure respectively the adhesive force of silver compound layer according to BG1720-1979.
The properties mean value of measuring is as follows:
。
Note: Isc is short circuit current;
Voc is open circuit voltage;
FF is fill factor, curve factor.
Claims (6)
1. crystal silicon solar energy battery is positive uses a unleaded conductive silver paste, it is characterized in that, the component of described unleaded conductive silver paste by weight percentage composition meter comprises: silver powder 75～85%; Crown glass binding agent 0.5～2%; Metal alloy powder 1～10%; Organic binder bond 5～15%; Activating oxide 1～5%; Wherein, 0.2～1 micron of described silver powder average grain diameter, tap density are greater than 4.5g/cc; Described activating oxide is nanometer γ-Al
2o
3powder.
2. unleaded conductive silver paste according to claim 1, is characterized in that, also comprises 0.1～2% IrO
2antioxidant.
3. unleaded conductive silver paste according to claim 2, is characterized in that, described metal alloy powder is the one of Sn-Ag alloyed powder, Sn-Ag-Cu alloyed powder, Sn-Sb alloyed powder.
4. unleaded conductive silver paste according to claim 3, is characterized in that, described nanometer γ-Al
2o
3the particle diameter of powder is 15～25nm.
5. unleaded conductive silver paste according to claim 4, is characterized in that, described crown glass binding agent adopts the one in B-Zn-Sb glass system, Bi-B-Si glass system, Bi-Si-Zn glass system.
6. unleaded conductive silver paste according to claim 5, is characterized in that, the organic resin that described organic binder bond is 5～20% by percentage by weight and 80～95% organic solvent form; Described organic resin is one or more in ethyl cellulose, acrylic resin, rosin, NC Nitroncellulose; Described organic solvent is one or more in terpinol, butyl carbitol acetate, diethylene glycol butyl ether, dibutyl phthalate.
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| KR101716525B1 (en) * | 2012-12-21 | 2017-03-14 | 제일모직주식회사 | Electrode paste composition and electrode prepared using the same |
| KR101648242B1 (en) * | 2013-03-27 | 2016-08-12 | 제일모직주식회사 | Composition for forming solar cell electrode and electrode prepared using the same |
| CN103440900B (en) * | 2013-09-10 | 2016-06-15 | 乐凯胶片股份有限公司 | A kind of unleaded positive silver paste of crystal silicon solar energy battery |
| CN103559939A (en) * | 2013-09-22 | 2014-02-05 | 江苏瑞德新能源科技有限公司 | Solar cell positive silver paste suitable for high-temperature sintering |
| CN105565905A (en) * | 2014-10-08 | 2016-05-11 | 陈章椿 | Ceramic container antioxidant electric-conduction film composite silver material, preparation process and applications thereof |
| CN105761775B (en) * | 2014-12-18 | 2017-07-21 | 上海宝银电子材料有限公司 | A kind of chip inductor external electrode conductive silver paste and preparation method thereof |
| CN104575667B (en) * | 2014-12-24 | 2017-09-26 | 乐凯胶片股份有限公司 | Crystal silicon solar energy battery front conductive silver paste |
| CN109004043B (en) * | 2018-07-16 | 2021-03-16 | 南通天盛新能源股份有限公司 | Preparation method and application of back electrode of solar cell |
| CN109192811B (en) * | 2018-08-09 | 2020-06-09 | 江苏辉伦太阳能科技有限公司 | Preparation method of SE battery |
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| CN101609850A (en) * | 2009-07-14 | 2009-12-23 | 中南大学 | Lead-free silver conductive paste used for positive electrode of solar battery and preparation technology thereof |
| CN101937736A (en) * | 2010-09-20 | 2011-01-05 | 浙江大学 | Lead-free environment-friendly electronic silver paste and preparation method thereof |
| CN101964219A (en) * | 2010-08-10 | 2011-02-02 | 上海九晶电子材料股份有限公司 | Silver paste for positive of crystalline silicon solar cell and preparation method thereof |
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| CN101609724A (en) * | 2008-06-20 | 2009-12-23 | 北京有色金属研究总院 | A kind of electrode thick liquid without lead and silver and preparation method thereof |
| CN101613186A (en) * | 2008-06-27 | 2009-12-30 | 上海昌银电子材料科技有限公司 | Lead-free silver slurry for high-temperature sintered automobile glass heating wire and preparation method thereof |
| CN102280161B (en) * | 2011-08-18 | 2013-08-28 | 陈晓东 | Conductive paste for positive electrode of crystal silicon solar cell and preparation method of conductive paste |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101609850A (en) * | 2009-07-14 | 2009-12-23 | 中南大学 | Lead-free silver conductive paste used for positive electrode of solar battery and preparation technology thereof |
| CN101964219A (en) * | 2010-08-10 | 2011-02-02 | 上海九晶电子材料股份有限公司 | Silver paste for positive of crystalline silicon solar cell and preparation method thereof |
| CN101937736A (en) * | 2010-09-20 | 2011-01-05 | 浙江大学 | Lead-free environment-friendly electronic silver paste and preparation method thereof |
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