CN103310870A - Lead-free copper slurry applied to silicon solar battery electrode and preparation method thereof - Google Patents
Lead-free copper slurry applied to silicon solar battery electrode and preparation method thereof Download PDFInfo
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- CN103310870A CN103310870A CN2012100631476A CN201210063147A CN103310870A CN 103310870 A CN103310870 A CN 103310870A CN 2012100631476 A CN2012100631476 A CN 2012100631476A CN 201210063147 A CN201210063147 A CN 201210063147A CN 103310870 A CN103310870 A CN 103310870A
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Abstract
The present invention provides lead-free copper slurry applied to a silicon solar battery electrode and a preparation method thereof. The lead-free copper slurry is prepared from, by mass, 60% to 85% of mixed copper powder, 1% to 10% of inorganic binder, 10% to 30% of organic binder, 1% to 30% of mixed additive and 5% to 20% of organic solvent. The mixed copper powder comprises copper powder A whose particle diameter distribution is 0.5 to 2 microns, copper powder B whose particle size distribution is 1 to 3 microns and copper powder C whose particle diameter distribution is 4 to 7 microns, wherein the mass ratio of the three kinds of copper powder is 5 to 8:1 to 4:1. The mixed additive is composed of a first additive and a second additive. The first additive is the mixture of one or more than two of a defoaming agent, a silane coupling agent KH-550 and lecithin or span. The second additive is one or more of elements or compounds of transition family or III, IV and V family elements. Ratio restriction on the additive amount of the first additive and the second additive does not exist, and adding is carried out according to the actual situation. The lead-free copper slurry has the advantages of low cost and excellent conductivity, weldability and ohmic contact property, and can be used as universal electrode slurry of electrodes on front and back of a solar battery.
Description
Technical field
The present patent application relates to a kind of silicon solar battery electrode to be used without lead bronze slurry and preparation method thereof, belongs to technical field of solar batteries.
Background technology
Solar energy back electrode conductive silver paste is the important materials of solar cell, plays the effects such as conduction, welding in electrode of solar battery.At present, the solar energy back electrode mainly contains front electrode silver slurry, back electrode aluminium paste, silver-colored aluminium paste and silver-colored the slurry with electrocondution slurry.Because silver-colored aluminium paste all is worse than the silver slurry at aspects such as conductivity, solderabilities, so present silver-colored aluminium paste is replaced gradually.
Although the silver slurry is at aspect excellent performances such as conductivity, solderability, adhesive force, because the ore reserve of whole world silver are limited, again excessively exploitation in these several years has caused the surge of this several years prices of noble silver, makes the increase of enterprise's production cost.Since manufacturing enterprise increasing rapidly in recent years, Market competition, and producer constantly forces down the price of silver slurry, and overseas-funded enterprise utilizes technical advantage, captures high-end market, further causes the reduction of profit.And migration easily occurs and causes short circuit under the Dc bias effect in silver, greatly reduces the coefficient of safety of using.So the metal that needs to seek a kind of low price and good conductivity replaces argent, is applied to this metal paste on the electrode of silicon solar cell.
According to the electrical conduction mechanism of metal simple-substance, metallic copper has good conductivity, and the specific insulation of copper is 1.70 * 10
-6Ω cm is only second to silver (1.62 * 10
-6Ω cm), and the metallic copper wide material sources, low price fully can alternative metals silver, and as the silicon solar battery electrode slurry, and metallic copper has excellent weldability energy, and metal level has weldability after being prepared into copper and starching sintering.
Summary of the invention
The present patent application namely is the problems referred to above that exist in the present electrode paste of silicon solar cell, provide a kind of silicon solar battery electrode to use without lead bronze slurry and preparation method thereof, described with low cost without lead bronze slurry, have superior electrical conductivity and weldability, can replace the silver slurry as the used for solar batteries electrode slurry.
A purpose of the present patent application provides a kind of silicon solar battery electrode and uses without the lead bronze slurry, adopts following technical scheme:
A kind of silicon solar battery electrode is used without the lead bronze slurry, and described various components of starching by following quality percentage composition without lead bronze are prepared from:
Mix copper powder: 60%～85%; Inorganic bond: 1%～10%;
Organic bond: 10%～30%; Additive package: 1%～30%;
Organic solvent: 5%～20%;
Wherein, mix copper powder and comprise that particle diameter is distributed as the copper powder A of 0.5～2 μ m, particle size distribution is the copper powder B of 1～3 μ m and the copper powder C that particle diameter is distributed as 4～7 μ m, the mass ratio of three kinds of copper powders is: copper powder A: copper powder B: copper powder C=5～8: 1～4: 1; Described additive package is comprised of additive one and additive two, additive one is one or more mixture of defoamer, silane resin acceptor kh-550, lecithin or class of department, additive two is transition group or III, IV, the simple substance of V group element or one or more of compound, the addition Non-scale restriction of additive one and additive two is added according to actual conditions.
Further, in the described mixing copper powder, copper powder A is ultra-fine spherical copper powder, and its purity is 99.90%; Copper powder B is the superfine sheet copper powder, and its purity is 99.90%; Copper powder C is spherical copper powder, and its purity is 99.90%.
Further, described inorganic bond is the lead free and cadmium free glasses powder, and softening point temperature is 450 ℃～650 ℃, and its particle diameter is distributed as: 1～5 μ m.
Further, described organic bond consist of organic resin and organic solvent, wherein to occupy the quality percentage composition of machine adhesive be 5～30% to organic resin.
Further, described organic resin is one or more mixture of ethyl cellulose, acrylic resin.
Further, described organic solvent is one or more mixture of terpinol, diethylene glycol butyl ether, diethylene glycol monobutyl ether acetate.
Further, described organic solvent is one or more mixture of terpinol, butyl glycol ether, diethylene glycol butyl ether, diethylene glycol monobutyl ether acetate.
Another purpose of the present patent application provides the above-mentioned silicon solar battery electrode preparation method who starches without lead bronze, comprises following basic step:
1) preparation of mixing copper powder: take by weighing in proportion copper powder A, copper powder B and copper powder C, in batch mixer, mix 20～40min, form and mix copper powder, for subsequent use
2) preparation of organic bond:
The organic resin that will occupy machine adhesive total amount 5%～30% joins in the heating stirred tank, and then adding occupies the organic solvent of machine adhesive total amount 70%～95%, to heat stirred tank and be warmed up to 80 ℃～100 ℃ insulations, with 100～300r/min rotating speed insulated and stirred, 20～40min, stir complete be cooled to 25 ℃ after, obtain organic bond for subsequent use.
3) preparation of slurry:
Mixing copper powder 60%～85%, 1%～10% inorganic bond, 10%～30% organic bond and 1%～30% additive package are mixed to join in the three-high mill, rolling slurry adds organic solvent on one side on one side, adjusting viscosity, after grinding 20～40min, be dispersed into and have the homodisperse slurry of certain fineness, it is 300～700pas that slurry satisfies viscosity, and fineness is 10～20 μ m, and copper content is 70%～85%.
The described silicon solar battery electrode of the present patent application is used without the lead bronze slurry, has advantages of following:
1. used metal is copper, has wide material sources, the advantage that the argents such as low price can not be compared;
2. the high pure and ultra-fine copper powder that consists of three kinds of different-grain diameters and shape of used mixing copper powder, the copper powder of different-grain diameter and shape is combined the warpage that can alleviate silicon chip behind the sintering, reduce series resistance, suppress the increase of contact resistance, improve electricity conversion, reduce the generation of micro-crack, have good sintering character;
3. by adding simple substance or the compound of transition group or III, IV, V group element, by mixing or forming alloying with copper, overcome the Schottky barrier of metal electrode and surface silicon, make copper electrode and silicon form good ohmic contact;
4. described have excellent conductivity, weldability and ohm contact performance without the lead bronze slurry, can be used as the general electrode slurry of the positive backplate of solar cell;
5. used inorganic bond does not contain the poisonous metals such as Pb, Hg, and the slurry of preparation meets the RoHs standard, and organic solvent is the environmental protection organic solvent, meets the VOC discharge standard.
Embodiment
Below in conjunction with concrete execution mode; the described silicon solar battery electrode of the present patent application used without lead bronze slurry and preparation method thereof be described; purpose is better to understand described technology contents for the public; rather than to the restriction of described technology contents; in fact; with identical or approximate principle; to the described improvement of carrying out without lead bronze slurry and preparation method thereof; comprise the replacement of its component, the increase and decrease of content; and the improvement of process conditions; all to realize that same effect is as purpose, then all within the present patent application technical scheme required for protection.
Embodiment one
Mixing copper powder is to use following three kinds of copper powders preparation:
Spherical copper powder A particle size distribution is 0.5～2 μ m, and the particle size distribution of flake copper B is that the particle size distribution of 1～3 μ m, spherical copper powder C is 4～7 μ m, mixes copper powder and adopts multiple mixed proportion, and concrete mixing ratio sees Table-1.
The mixed proportion that table-1 mixes copper powder
| Mix the copper powder numbering | Cu1# | Cu2# | Cu3# | Cu4# |
| Copper powder A (wt%) | 63.6 | 61.5 | 66.7 | 58.3 |
| Copper powder B (wt%) | 27.3 | 30.8 | 25.0 | 33.3 |
| Copper powder C (wt%) | 9.1 | 7.7 | 8.3 | 8.4 |
| A: B: C mixing ratio | 7∶3∶1 | 8∶4∶1 | 8∶3∶1 | 7∶4∶1 |
Ratio in table-1 accurately takes by weighing copper powder A, copper powder B and copper powder C, mixes 30min in batch mixer, forms to mix copper powder, and is for subsequent use.
The softening temperature of glass dust is 450 ℃～650 ℃, and its particle size distribution is 1～5 μ m.
Embodiment two
The high thixotropic organic carrier is according to the difference of its material proportion, can produce multiple viscosity, different viscosity is useful in the different environment, the viscosity of the organic carrier that ethyl cellulose and acrylic resin ratio are large is large, be adapted at using summer, otherwise viscosity is just little, is adapted at use in winter, and the ratio of relevant each component of high thixotropic organic carrier of the present invention sees Table-2.
The ratio of table-2 relevant each component of high thixotropic organic carrier
The preparation technology of organic carrier: accurately take by weighing according to the above ratio various materials, place rustless steel container, carry out thermosol with the oil bath firing equipment, heating-up temperature is 80 ℃～100 ℃ insulated and stirred, until insulated and stirred dissolving is complete, obtain organic carrier after being cooled to room temperature, for subsequent use.
Embodiment three
Silicon solar battery electrode is used without lead bronze slurry Preparation Example, and its proportioning sees Table-3, shows-4.
Table-3 silicon solar battery electrodes are used without lead bronze slurry Preparation Example
Table-4 silicon solar battery electrodes are used without lead bronze slurry Preparation Example (continued)
Accurately take by weighing above-mentioned various material, carry out strictly mixing grinding and disperse thoroughly rolling, generate at last the paste liquid of even color and luster, produce namely to accuse and finish.
Complete being printed on the silicon solar cell substrate with 200～325 order stainless steel cloths without the lead bronze slurry will be made; at room temperature keep flat 10～15min; at 130～160 ℃ of drying 10～15min; then sintering in tunnel type nitrogen protection conveyer belt stove; 800 ℃ of peak temperatures, peak value temperature retention time 5～10s; sintering period 2～5min; can produce the rete that burns till of general copper luster, measure the indexs such as its thickness, sheet resistance, adhesive force, solderability and ageing properties and all reach the silicon solar cell performance need.The performance comparison of embodiment and Comparative Examples sees Table-5.
The performance comparison of table-5 embodiment and Comparative Examples
Economic and Efficiency Analysis:
Because the conductance of silver is better than copper, reaching under the prerequisite of same conductivity, the usage ratio of silver can lack 2% than copper, if use copper electrode paste, copper content is 75% performance that can be achieved requirement, if use silver electrode paste, silver content is 73% performance that can be achieved requirement.
At present, the silver ingot price is 6200 yuan/kg, and the rear price of solar energy silver slurry that is prepared into silver content 73% is 7500 yuan/Kg.The price of copper ingot is 60 yuan/kg, and the rear price of solar energy copper slurry that is prepared into copper content 75% is 2400 yuan/Kg.But because copper slurry need to use nitrogen protection in sintering, and the silver slurry just can sintering in air, is therefore using copper to starch the expenditure that need to pay more purchase nitrogen.Comprehensive these factors, Calculation Comparison once with the application cost of silver slurry.Now take solar silicon wafers as example, by the actual production norm quota of consumption, with above-mentioned two kinds of each 1Kg of slurry, with identical technique printing, the product quantity of printing is more or less the same.Replace silver-colored slurry with the copper slurry and can save 5600 yuan, sintering needs the about 80M of nitrogen
3(the refreshing good ceramic industry nitrogen sintering furnace quota in Luoyang, the nitrogen consumption of other sintering furnace is difference to some extent), calculate by every cubic metre of price 5 yuan, need 400 yuan of many parts, COMPREHENSIVE CALCULATING, 5100 yuan of escapable costs, be close to the solar energy market of white heat in price competition, the cost decline of this amplitude is highly significant.
Claims (8)
1. a silicon solar battery electrode is used without the lead bronze slurry, it is characterized in that: described various components of starching by following quality percentage composition without lead bronze are prepared from:
Mix copper powder: 60%～85%; Inorganic bond: 1%～10%;
Organic bond: 10%～30%; Additive package: 1%～30%;
Organic solvent: 5%～20%;
Wherein, mix copper powder and comprise that particle diameter is distributed as the copper powder A of 0.5～2 μ m, particle size distribution is the copper powder B of 1～3 μ m and the copper powder C that particle diameter is distributed as 4～7 μ m, the mass ratio of three kinds of copper powders is: copper powder A: copper powder B: copper powder C=5～8: 1～4: 1; Described additive package is comprised of additive one and additive two, additive one is one or more mixture of defoamer, silane resin acceptor kh-550, lecithin or class of department, additive two is transition group or III, IV, the simple substance of V group element or one or more of compound, the addition Non-scale restriction of additive one and additive two is added according to actual conditions.
2. according to claim 1 without the lead bronze slurry, it is characterized in that: in the described mixing copper powder, copper powder A is ultra-fine spherical copper powder, and its purity is 99.90%; Copper powder B is the superfine sheet copper powder, and its purity is 99.90%; Copper powder C is spherical copper powder, and its purity is 99.90%.
3. according to claim 1 it is characterized in that: described inorganic bond is the lead free and cadmium free glasses powder without the lead bronze slurry, and softening point temperature is 450 ℃～650 ℃, and its particle diameter is distributed as: 1～5 μ m.
4. according to claim 1 without lead bronze slurry, it is characterized in that: described organic bond consist of organic resin and organic solvent, wherein to occupy the quality percentage composition of machine adhesive be 5～30% to organic resin.
5. according to claim 1 without lead bronze slurry, it is characterized in that: described organic resin is one or more mixture of ethyl cellulose, acrylic resin.
6. according to claim 1 without lead bronze slurry, it is characterized in that: described organic solvent is one or more mixture of terpinol, diethylene glycol butyl ether, diethylene glycol monobutyl ether acetate.
7. according to claim 1 without lead bronze slurry, it is characterized in that: described organic solvent is one or more mixture of terpinol, butyl glycol ether, diethylene glycol butyl ether, diethylene glycol monobutyl ether acetate.
8. the preparation method of the described silicon solar battery electrode of claim 1-7 without the lead bronze slurry is characterized in that, comprises following basic step:
1) preparation of mixing copper powder: take by weighing in proportion copper powder A, copper powder B and copper powder C, in batch mixer, mix 20～40min, form and mix copper powder, for subsequent use
2) preparation of organic bond:
The organic resin that will occupy machine adhesive total amount 5%～30% joins in the heating stirred tank, and then adding occupies the organic solvent of machine adhesive total amount 70%～95%, to heat stirred tank and be warmed up to 80 ℃～100 ℃ insulations, with 100～300r/min rotating speed insulated and stirred, 20～40min, stir complete be cooled to 25 ℃ after, obtain organic bond for subsequent use.
3) preparation of slurry:
Mixing copper powder 60%～85%, 1%～10% inorganic bond, 10%～30% organic bond and 1%～30% additive package are mixed to join in the three-high mill, rolling slurry adds organic solvent on one side on one side, adjusting viscosity, after grinding 20～40min, be dispersed into and have the homodisperse slurry of certain fineness, it is 300～700pas that slurry satisfies viscosity, and fineness is 10～20 μ m, and copper content is 70%～85%.
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Cited By (9)
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|---|---|---|---|---|
| CN103778992A (en) * | 2014-01-10 | 2014-05-07 | 浙江大学 | Copper slurry based on copper ammonia complex and preparation method and application thereof |
| WO2016029398A1 (en) * | 2014-08-28 | 2016-03-03 | E.I. Du Pont De Nemours And Company | Solar cells with copper electrodes |
| CN105810293A (en) * | 2016-05-13 | 2016-07-27 | 浙江光达电子科技有限公司 | Silver paste for back electrode of crystalline silicon solar cell and preparation method of silver paste |
| CN106205771A (en) * | 2016-06-30 | 2016-12-07 | 金陵科技学院 | A kind of preparation method of oxidation resistant copper conductor slurry |
| US9951231B2 (en) | 2014-08-28 | 2018-04-24 | E I Du Pont De Nemours And Company | Copper-containing conductive pastes and electrodes made therefrom |
| CN109215838A (en) * | 2018-11-22 | 2019-01-15 | 河北晶乐光电科技有限公司 | Crystal silicon solar energy battery back electrode slurry, preparation method and battery |
| US10325693B2 (en) | 2014-08-28 | 2019-06-18 | E I Du Pont De Nemours And Company | Copper-containing conductive pastes and electrodes made therefrom |
| CN114242300A (en) * | 2021-12-14 | 2022-03-25 | 上海正银电子材料有限公司 | Conductive copper paste for ferrite core inductance and preparation method thereof |
| CN114464346A (en) * | 2022-03-24 | 2022-05-10 | 浙江晶科新材料有限公司 | Copper paste applied to grid line electrode of crystalline silicon solar cell and preparation method thereof |
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Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103778992A (en) * | 2014-01-10 | 2014-05-07 | 浙江大学 | Copper slurry based on copper ammonia complex and preparation method and application thereof |
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| CN106575537A (en) * | 2014-08-28 | 2017-04-19 | E.I.内穆尔杜邦公司 | Solar cells with copper electrodes |
| US9951231B2 (en) | 2014-08-28 | 2018-04-24 | E I Du Pont De Nemours And Company | Copper-containing conductive pastes and electrodes made therefrom |
| WO2016029398A1 (en) * | 2014-08-28 | 2016-03-03 | E.I. Du Pont De Nemours And Company | Solar cells with copper electrodes |
| US10672922B2 (en) | 2014-08-28 | 2020-06-02 | Dupont Electronics, Inc. | Solar cells with copper electrodes |
| CN105810293A (en) * | 2016-05-13 | 2016-07-27 | 浙江光达电子科技有限公司 | Silver paste for back electrode of crystalline silicon solar cell and preparation method of silver paste |
| CN105810293B (en) * | 2016-05-13 | 2017-07-25 | 浙江光达电子科技有限公司 | A kind of rear electrode for crystal silicon solar battery silver paste and preparation method thereof |
| CN106205771A (en) * | 2016-06-30 | 2016-12-07 | 金陵科技学院 | A kind of preparation method of oxidation resistant copper conductor slurry |
| CN106205771B (en) * | 2016-06-30 | 2018-05-15 | 金陵科技学院 | A kind of preparation method of oxidation resistant copper conductor slurry |
| CN109215838A (en) * | 2018-11-22 | 2019-01-15 | 河北晶乐光电科技有限公司 | Crystal silicon solar energy battery back electrode slurry, preparation method and battery |
| CN114242300A (en) * | 2021-12-14 | 2022-03-25 | 上海正银电子材料有限公司 | Conductive copper paste for ferrite core inductance and preparation method thereof |
| CN114464346A (en) * | 2022-03-24 | 2022-05-10 | 浙江晶科新材料有限公司 | Copper paste applied to grid line electrode of crystalline silicon solar cell and preparation method thereof |
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Application publication date: 20130918 |