CN103137239A - Front electrode silver paste for solar battery and preparation method thereof and solar battery piece - Google Patents
Front electrode silver paste for solar battery and preparation method thereof and solar battery piece Download PDFInfo
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- CN103137239A CN103137239A CN2011103801012A CN201110380101A CN103137239A CN 103137239 A CN103137239 A CN 103137239A CN 2011103801012 A CN2011103801012 A CN 2011103801012A CN 201110380101 A CN201110380101 A CN 201110380101A CN 103137239 A CN103137239 A CN 103137239A
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Abstract
The invention belongs to the technical field of solar batteries, and particularly discloses front electrode silver paste for a solar battery. The front electrode silver paste comprises an organic carrier and silver powder and glass powder which are dispersed in the organic carrier, wherein the organic carrier contains an organic solvent and high-temperature resistant lubricating grease or a high-temperature resistant thickening agent. The invention also relates to a method for preparing the front electrode silver paste for the solar battery and a solar battery piece which is manufactured by using the front electrode silver paste for the solar battery. The front electrode silver paste for the crystalline silicon solar battery is manufactured by adding the high-temperature resistant lubricating grease or the high-temperature resistant thickening agent which serves as the main component of the organic carrier, so that the front electrode silver paste has the advantages of high thixotropic property, low viscosity, uniform powder dispersion and easiness in net penetration and is used for manufacturing an electrode grid line, collapse is avoided at high temperature, and the final depth-width ratio of the electrode grid line can be improved obviously, so that the electrode grid line is attractive in appearance, and the photoelectric conversion rate and production yield of the solar battery are improved.
Description
Technical field
The invention belongs to technical field of solar batteries, relate in particular to a kind of front electrode of solar battery silver slurry and preparation method thereof and a kind of solar battery sheet.
Background technology
Solar cell is as a kind of green energy resource, inexhaustible, pollution-free with it, not more and more be subject to people's attention by the advantages such as region resource limitation, thereby, in recent years, crystal silicon solar energy battery is developed rapidly as main solar energy power generating unit, and wherein, solar battery front side is the important component part of crystal silicon solar energy battery, it is as the one side that directly receives solar energy, by sandwich construction in the hope of reaching the widest reception spectral line and minimum light reflection consumption.Conventional commercial crystal silicon solar energy battery front comprises silver electrode grid line, antireflection layer, N-shaped diffusion layer, p-n junction district four floor primary structure.
At present, the manufacture method of commercial crystal silicon solar energy battery front electrode, usually adopt printing and inkjet printing conductive silver paste to form the large as far as possible grid line structure of depth-width ratio, pass through subsequently the Fast Sintering process, the conductive electrode of formation and N-shaped diffusion layer close contact generally contains silver powder, glass dust and organic carrier in described conductive silver paste.Those skilled in the art will appreciate that in order to guarantee the photogenerated current amount, should increase light-receiving area, this area that just requires the front electrode grid line to hide is little, and gate electrode line is more thin better; Yet according to metallic conductor resistance basic principle, the cross section of wire is larger, and the resistance of unit length is less, and it is also just less that conductor resistance produces power loss, and this just requires gate electrode line more thick better.Thereby, in order to reach optimum electricity conversion, require in theory the ratio of the height and the width of silver electrode grid line after sintering to be the bigger the better.And to reach optimum depth-width ratio, at first need conductive silver paste that good thixotropic property is arranged in printing process.The basic conception of thixotropic property is that pseudoplastic fluid is subject to shearing rear viscosity and descends, and the shear rate that applies is higher, and it is more serious that viscosity descends, until a minimum, but shear stop after, the phenomenon that viscosity progressively recovers again.Thixotropic property is stronger, and the shear thinning effect is more obvious, and after removing shearing, the time that viscosity recovers is shorter.
A kind of existing method is ethyl cellulose to be coordinated with organic solvent in certain ratio make organic carrier.When ethyl cellulose is static in organic solvent, due to the winding of strand, viscosity is larger, and after applying shearing force in a certain direction, winding is untied, and molecule is stretching along shear direction, and viscosity descends; After shearing removes, be intertwined again, viscosity rises; So ethyl cellulose itself has certain thixotropic property, but because its thixotropic property mainly relies on physical process, so after removing shearing, the viscosity uphill process is slow, thereby thixotropic property is relatively poor.Another kind of Innovative method is to add industrial thixotropic agent in conductive silver paste, for example: and rilanit special, polyamide wax or other wax class thixotropic agent, add the thixotropic property that above-mentioned thixotropic agent can significantly improve conductive silver paste.But the fusing point of such thixotropic agent easily occurs melting in the low temperature drying process generally below 150 ℃, causes the conduction grid line that prints to subside.
Summary of the invention
The present invention is poor for the thixotropic property that solves existing conductive silver paste, perhaps be used for to make the conduction grid line, and in drying course, the technical problem of subsiding easily appears in the conduction grid line.
Accordingly, the invention provides a kind of front electrode of solar battery silver slurry, described silver slurry comprises organic carrier and is dispersed in silver powder and glass dust in organic carrier; Described organic carrier comprises organic solvent and high temperature resistant lubricating grease or high temperature resistant thickening agent.
In described front electrode of solar battery silver slurry, preferably, take the total weight of silver slurry as benchmark, the content of described silver powder is the 70-90 % by weight, and the content of described glass dust is the 1-8 % by weight, and the content of described organic carrier is the 6-25 % by weight.
In described front electrode of solar battery silver slurry, preferably, the specific area of described silver powder is 0.2-2.5m
2/ g; The particle diameter of described glass dust is 0.1-5 μ m; Described glass dust contains the compound of Pb or Bi, and the content of the compound of described Pb or Bi is 65-90wt%.
In described front electrode of solar battery silver slurry, preferably, described organic carrier also comprises additive, take the total weight of organic carrier as benchmark, the content of described organic solvent is the 60-90 % by weight, the content of described high temperature resistant lubricating grease or high temperature resistant thickening agent is the 5-30 % by weight, and the content of described additive is the 0.5-15 % by weight.
In described front electrode of solar battery silver slurry, preferably, the boiling point of described organic solvent is 180-340 ℃, is selected from one or more in fourth card, fourth card ester, terpinol, tributyl phosphate, lauryl alcohol ester.
In described front electrode of solar battery silver slurry, preferably, the dropping point of described high temperature resistant lubricating grease is selected from one or more in lithium base grease, urea-base grease, complex calcium lubricating grease, complex lithium grease, composite barium-base grease higher than 180 ℃-220 ℃.
In described front electrode of solar battery silver slurry, preferably, described high temperature resistant thickening agent is selected from one or more in lithium soap thickening agent, polyurea thickening agent, compound lithium soap thickening agent, compound barium soap thickening agent, calcium complex soap thickening agent.
In described front electrode of solar battery silver slurry, preferably, described additive comprises one or more in cellulose, thixotropic agent, wetting dispersing agent, essence.
The present invention also provides the preparation method of above-mentioned front electrode of solar battery silver slurry, comprises the following steps:
Step 1, add high temperature resistant lubricating grease or high temperature resistant thickening agent in organic solvent, stir, obtain organic carrier;
Step 2, with above-mentioned organic carrier with after silver powder, glass dust mix, grind, obtain described front electrode of solar battery silver slurry.
In described preparation method, preferably, in step 1, organic solvent is heated to 50-80 ℃, add high temperature resistant lubricating grease, stir 5-30min, then add additive, continue to stir 5-30min, be cooled to room temperature and obtain organic carrier.
In described preparation method, preferably, in step 1, organic solvent is heated to 80-120 ℃, adds high temperature resistant thickening agent, stir and be warming up to 150-200 ℃, continue to stir 1-5min, then add additive, continue to be stirred to cool to room temperature and obtain organic carrier.
The present invention further provides solar battery sheet, described solar battery sheet comprises silicon chip and the silver electrode grid line of being located on silicon chip, and described conduction grid line obtains after oven dry, sintering by silk screen printing conductive silver paste as above on silicon chip.
Crystal silicon solar energy battery front electrode silver slurry of the present invention, make front electrode silver slurry by adding Hmp grease or high temperature resistant thickening agent as the key component of organic carrier, thixotropic property is good, and have advantages of that viscosity is low, powder is uniformly dispersed, the easy net of crossing, be used for making gate electrode line, at high temperature can not subside, can significantly improve the final depth-width ratio of gate electrode line, obtain good pattern, and then improve the optoelectronic transformation efficiency of solar cell and produce yield.
Embodiment
In order to make technical problem solved by the invention, technical scheme and beneficial effect clearer, below in conjunction with embodiment, the present invention is further elaborated.Should be appreciated that specific embodiment described herein only in order to explain the present invention, is not intended to limit the present invention.
The invention provides a kind of front electrode of solar battery silver slurry, described silver slurry comprises organic carrier and is dispersed in silver powder and glass dust in organic carrier; Described organic carrier comprises organic solvent and high temperature resistant lubricating grease or high temperature resistant thickening agent.
The present inventor is in the research process to front electrode of solar battery silver slurry, once attempted the consumption by strict control thixotropic agent, and add the pattern that the difficult resin that softens of high temperature or fiber are usually kept gate electrode line in organic carrier, improve by this method the thixotropic property of front electrode of solar battery silver slurry, and the grid line of avoiding conducting electricity subsides, and keeps the pattern of conduction grid line.Yet, adding thixotropic agent over after certain ratio, high temperature subsides seriously; After ethyl cellulose surpassed certain proportion, viscosity was larger; Even under the ratio state of the best, still viscosity is high, silk thread is long to be added with above-mentioned resin or cellulosic carrier, cause printing the net performance not good, be prone to empty seal, bite, the burr at grid line edge is many, and inorganic particle (silver powder and glass dust) is difficult to effective dispersion in the process of lapping of preparation slurry.In the process that the present inventor continues to study, find unexpectedly to add high temperature resistant lubricating grease or high temperature resistant thickening agent in organic carrier, not only can make electrode silver plasm possess good thixotropic property, and have advantages of that viscosity is low, powder is uniformly dispersed, the easy net of crossing, be used for making gate electrode line, at high temperature can not subside, can significantly improve the final depth-width ratio of gate electrode line, obtain good pattern.
Specifically, described silver powder and glass dust can adopt silver powder and glass dust commonly used in this area.Take the total weight of silver slurry as benchmark, the content of described silver powder is the 70-90 % by weight, and the content of described glass dust is the 1-8 % by weight, and the content of described organic carrier is the 6-25 % by weight.
Wherein, the content of described silver powder should be less than 70wt%, otherwise can't pass through the densification of high temperature Fast Sintering between silver powder, and the conductivity of silver electrode grid line obviously reduces; Should be higher than 90wt% yet, otherwise the corresponding minimizing of organic carrier in the silver slurry, the viscosity of silver slurry is obviously too high, and inorganic particle is difficult to grinding distribution, and crosses net performance extreme difference, and in the preferred case, the content of silver powder is the 81-86 weight portion.The specific area of described silver powder is 0.2-2.5m
2/ g is if the specific area of described silver powder is less than 0.2 m
2/ g, powder diameter is large, and sintering character is poor, can't pass through the densification of high temperature Fast Sintering, and the conductivity of silver electrode grid line obviously reduces; And if the specific area of silver powder is greater than 2.5m
2During/g, the oil absorption of powder is large, and the viscosity of silver slurry is obviously too high, and inorganic particle is difficult to grinding distribution, and crosses net performance extreme difference; In the preferred case, the specific area of silver powder is 0.4-1.2 m
2/ g.
The content of described glass dust should be less than 1wt%, otherwise can not be scattered in effectively equably between silver powder, and the consumption of glass dust should be greater than 8wt% yet, otherwise frit will form connection, isolate the Ag crystal in the Ag electrode, seriously reduce the conductivity of Ag electrode.Under preferable case, the consumption of glass dust is 2-5wt%.
Glass dust is the known class material of ability technical staff, and the mixture that generally is comprised of various metal oxides or other oxides makes powder by melting, shrend, ball milling, oven dry.Preferably, described glass dust contains the Pb of 65-90wt% or the compound of Bi, or the combination of Pb, Bi compound.The lead borosilicate glass that more preferably contains 70-85wt% PbO.Wherein, the compound of Pb or Bi is the main matter for corrosion ARC film (antireflection layer).For example, the PbO in glass dust is by generating SiO with ARC film generation redox reaction
2And Pb, wherein SiO
2Dissolving enters in glass dust.Bi in glass dust
3+Same effect is also arranged.The content ratio of the Pb in glass dust or the compound of Bi needs to surpass more than 65wt%, the guarantee reaction density, and constantly corrosion thickness is the ARC film of 70-80nm effectively.Surpass simultaneously the above Pb of 65wt% or the compound of Bi and also play the effect of strong reduction glass softening point in glass.
The particle diameter of described glass dust is 0.1-5 μ m, because less than the glass dust of 0.1 μ m particle diameter, specific area is large, the powder oil absorption is large, easily reunites, and can make the viscosity of silver slurry obviously too high, is difficult to grinding distribution even; And greater than the glass dust of 5 μ m particle diameters, the individual amount in the silver slurry reduces, and specific area is little, reduces with the contact area of silver powder, to the wetting and solubility property decline of silver powder.
Organic carrier of the present invention comprises organic solvent, high temperature resistant lubricating grease or high temperature resistant thickening agent, preferably also comprises additive.Take the total weight of organic carrier as benchmark, the content of described organic solvent is the 60-90 % by weight, and the content of described high temperature resistant lubricating grease or high temperature resistant thickening agent is the 5-30 % by weight, and the content of described additive is the 0.5-15 % by weight.The content of a described organic carrier component can be according to the viscosity adjustment of organic carrier or last made silver slurry.Under optimum condition, the content of organic solvent is the 75-85 % by weight, and the content of described high temperature resistant lubricating grease or high temperature resistant thickening agent is the 10-24 % by weight, and the content of described additive is the 0.5-5 % by weight.
Wherein, organic solvent of the present invention can be selected from one or more in butyl carbitol, butyl carbitol acetate, terpinol, tributyl phosphate, phenmethylol, castor oil, tributyl citrate, dibutyl phthalate.In the preferred case, high boiling organic solvent during described organic solvent is selected, boiling point is 180-340 ℃, for example: can be selected from one or more in fourth card, fourth card ester, terpinol, tributyl phosphate, lauryl alcohol ester.During lower than 180 ℃, in slurrying, technological operation and preservation process, the speed that organic solvent volatilizees voluntarily is difficult to guarantee the stable of silver slurry rheological property when the boiling point of organic solvent.And when the boiling point of organic solvent during higher than 340 ℃, in sintering process, organic solvent is difficult to volatilization, affect follow-up sintering, and easily at the inner hole that forms of grid line, causes conductivity decline.Under optimum condition, the boiling point of organic solvent is 200-270 ℃.
Improvements of the present invention are, contain high temperature resistant lubricating grease or high temperature resistant thickening agent in described organic carrier.Described high temperature resistant lubricating grease or high temperature resistant thickening agent refer to can anti-lubricating grease or thickening agent higher than the temperature more than 100 ℃, but require its can be under the high temperature of 550 ℃ burn off.Wherein, described high temperature resistant lubricating grease need to possess following performance: 1, the dropping point of dropping point and organic solvent is close; 2, burn off is interval: under air ambient, and can the 95wt% burn off below 550 ℃, and burn off fully.3, viscosity: after making slurry fully, viscosity is at 120-280Pa.s(test condition Brookfield rotation viscometer 20rpm); 4, thixotropy: make thixotropy index S.V.I after slurry fully〉8(test condition Brookfield rotation viscometer 1rpm/20rpm, the viscosity that records under two kinds of speed conditions is divided by); 5, chemical property: do not corrode silver powder and glass dust; The high temperature resistant lubricating grease that satisfies above-mentioned performance requirement is used for system of the present invention and not only can makes electrode silver plasm possess good thixotropic property, and has advantages of that viscosity is low, powder is uniformly dispersed, the easy net of crossing.
Described high temperature resistant lubricating grease can adopt commercially available high temperature resistant lubricating grease, for example: the lithium base grease of General Corporation, complex lithium grease; Good degree (GADUS) series of shell (SHELL): the T100(urea-base grease), the V100(lithium base grease).Require the dropping point of described high temperature resistant lubricating grease higher than 180 ℃, for example: described high temperature resistant lubricating grease is selected from one or more in lithium base grease, urea-base grease, complex calcium lubricating grease, complex lithium grease, composite barium-base grease, is preferably lithium base grease or complex lithium grease; Temperature when dropping point represents that lubricating grease the first dropping liquid occurs in heating process.If the dropping point of the lubricating grease that adopts is lower than 180 ℃, this moment, solvent not yet volatilized fully, if softening as the lubricating grease of the main skeleton of organic carrier, subsiding was appearred in the pattern that makes the silver electrode grid line.In the preferred case, the dropping point of high temperature resistant lubricating grease is lower than 220 ℃.
If use high temperature resistant lubricating grease as the chief component component of organic carrier, organic solvent can be heated to 50-80 ℃ in reaction vessel, then add high temperature resistant lubricating grease, more than continuing to stir 5min, then add additive, more than continuing to stir 5min, be cooled to room temperature, make organic carrier.If heating-up temperature is lower than 50 ℃, organic solvent is poor to the solvability of lubricating grease and additive, and the required process time is longer.If heating-up temperature is higher than 80 ℃, the organic solvent evaporation rate is fast, is difficult to guarantee the organic carrier stability of system.
Because Hmp grease mainly is comprised of base oil, thickening agent and additive three parts, these two kinds of key components of thickening agent and base oil are neither simple dissolving, neither simply mix, but be evenly dispersed in stable dispersion in base oil by thickening agent; Wherein, the particulate of dispersion is called decentralized photo (thickening agent), and size is between the 0.001-0.1 micron, and the material that surrounds decentralized photo is called continuous phase (base oil).The soap base thickening agent is fibrous, and in its mesh skeleton, base oil in occlusion, forms the butter state, has neither and flows voluntarily, the high thixotropic energy that can pave rapidly when shearing again.In the indefinite situation of performance to the constituent of commercially available Hmp grease, adopt commercially available Hmp grease to introduce unfavorable material at silver paste.The present invention in the preferred case, directly use high temperature resistant thickening agent, for example: one or more that are selected from lithium soap thickening agent, polyurea thickening agent, compound lithium soap thickening agent, compound barium soap thickening agent, calcium complex soap thickening agent prepare organic carrier, preferred lithium soap thickening agent or compound lithium soap thickening agent prepare organic carrier, above-mentioned high temperature resistant thickening agent generally is used for preparing high temperature resistant lubricating grease, can be evenly dispersed in organic solvent and form high temperature resistant lubricating grease in organic solvent.In the present invention, itself and organic solvent can be reacted directly that preparation is high temperature resistant, low-viscosity, the good organic carrier of thixotropy; The preparation method adds above-mentioned high temperature resistant thickening agent for organic solvent is heated to 80-120 ℃ in closed reaction vessel, stirs and be warming up to 150-200 ℃, continues to stir 1-5min, then adds additive, continues to stir, and is cooled to room temperature and obtains organic carrier.
The additive that organic carrier of the present invention adopts can be selected as required, comprising: the cellulose substances that is used for adjusting viscosity; Adjust the thixotropic agent of thixotropic property, for example: rilanit special or polyamide wax; Form the thermoplastic resin of the skeleton of organic carrier, such as: alkyd resins or acrylic resin etc.; Adjust the essence of smell; Improve the auxiliary agents such as wetting dispersing agent of the moisture dispersibility energy of inorganic particle.Can add corresponding additive according to viscosity and the rheological property of organic carrier or silver paste.Adding cellulose substances will increase viscosity and the viscosity of organic carrier and slurry, improve the high temperature slump resistance energy of slurry and the uniformity of grid line height, cellulose in organic carrier is known in those skilled in the art, such as methylcellulose, ethyl cellulose etc., propyl cellulose, butyl cellulose etc.Add the skeleton that resin can be used as carrier, effect and cellulose family are seemingly, and be but less to the increase of viscosity.Add appropriate thixotropic agent and can significantly improve the depth-width ratio of conductive silver paste printing gate electrode line later, and can effectively prevent in storage, the separation of the silver powder in slurry and precipitation, the net performance excessively of lifting silk screen printing; Thixotropic agent commonly used has one or more in hexadecanol, class of department 85, rilanit special, polyamide wax.If add one or more in cellulose, thixotropic agent, resin, addition is the 2-13 % by weight.Add the smell that essence can effectively cover organic solvent, thickening agent or lubricating grease, improve operational environment.Add the wetting and dispersion that wetting dispersing agent can significantly accelerate inorganic particle in silver slurry preparation process, reduce the viscosity of slurry, prevent the reunion of inorganic particle in storage and separating out of organic solvent, preferably one or more in oleic acid, stearic acid, lecithin.If add essence or wetting dispersing agent, addition is generally the 0.5-2 % by weight.
The present invention also provides the preparation method of above-mentioned front electrode of solar battery silver slurry, comprises the following steps:
Step 1, add high temperature resistant lubricating grease or high temperature resistant thickening agent in organic solvent, stir, obtain organic carrier;
Step 2, with above-mentioned organic carrier with after silver powder, glass dust mix, grind, obtain described front electrode of solar battery silver slurry.
In step 1, in order to prepare the organic carrier that contains high temperature resistant lubricating grease, organic solvent can be heated to 50-80 ℃, add high temperature resistant lubricating grease, stir 5-30min, then add additive, continue to stir 5-30min, be cooled to room temperature and can obtain organic carrier.
In step 1, in order to prepare the organic carrier that contains high temperature resistant thickening agent, organic solvent can be heated to 80-120 ℃, add high temperature resistant thickening agent, stir and be warming up to 150-200 ℃, continue to stir 1-5min, then add additive, continue to stir, be cooled to room temperature and obtain organic carrier.
In step 2, after the organic carrier that will make by step 1 and silver powder, glass dust carry out premixed, even by the three-roll grinder grinding distribution, silver powder, glass dust are dispersed in organic carrier, and fineness reaches can obtain front electrode of solar battery silver slurry of the present invention below 10 μ m.
The present invention also provides a kind of solar battery sheet, and described solar battery sheet comprises silicon chip and the silver electrode grid line of being located on silicon chip, and then described silver electrode grid line obtains after drying, sintering by the above-mentioned conductive silver paste of silk screen printing on silicon chip.
Crystal silicon solar energy battery front electrode silver slurry of the present invention, make front electrode silver slurry by adding Hmp grease as the key component of organic carrier, thixotropic property is good, and have advantages of that viscosity is low, powder is uniformly dispersed, the easy net of crossing, be used for making gate electrode line, at high temperature can not subside, can significantly improve the final depth-width ratio of gate electrode line, obtain good pattern, and then improve the optoelectronic transformation efficiency of solar cell and produce yield.
Below in conjunction with technology embodiment, the present invention is described in further detail.
Embodiment 1
Embodiment 1 is for the front electrode of solar battery slurry that the preparation method of front electrode of solar battery slurry of the present invention is described and adopts this preparation method to make;
1, supply raw materials: silver powder 79 % by weight, 1.5 microns of specific areas; Glass dust 6 % by weight PbO-B
2O
3-SiO
2(wherein, PbO 70wt%), 1.5 microns of average grain diameters; Organic carrier 15 % by weight, wherein, organic solvent accounts for 80 % by weight, and the lithium soap thickening agent accounts for 14 % by weight, and wetting dispersing agent accounts for 1 % by weight, and ethyl cellulose accounts for 5 % by weight;
2, preparation organic carrier: organic solvent is heated to 120 ℃ in closed reaction vessel, adds lithium base thickening agent, stir and be warming up to 180 ℃, continue to stir 3min, then add wetting dispersing agent and ethyl cellulose, stir and be cooled to room temperature;
3, with after above-mentioned silver powder, glass dust and prepared organic carrier premixed, mix and grind at three-roll grinder, make the fineness of silver powder, glass dust reach 8 microns, namely obtain front electrode of solar battery slurry A1.
Embodiment 2
Embodiment 2 is for the front electrode of solar battery slurry that the preparation method of front electrode of solar battery slurry of the present invention is described and adopts this preparation method to make;
1, supply raw materials: silver powder 83 % by weight, 0.8 micron of specific area; Glass dust 4 % by weight PbO-B
2O
3-SiO
2(wherein, PbO 85wt%), 1.0 microns of average grain diameters; Organic carrier 13 % by weight, wherein, organic solvent accounts for 70 % by weight, and polyurea thickening agent accounts for 20 % by weight, and wetting dispersing agent accounts for 2 % by weight, and rilanit special accounts for 3 % by weight, and ethyl cellulose accounts for 5 % by weight;
2, preparation organic carrier: organic solvent is heated to 100 ℃ in closed reaction vessel, add polyurea thickening agent, stirring is warming up to 200 ℃, continue to stir 1min, then add wetting dispersing agent and ethyl cellulose, stir and be cooled to 50 ℃, then add rilanit special, stir 10min, be cooled to room temperature;
3, with after above-mentioned silver powder, glass dust and prepared organic carrier premixed, mix and grind at three-roll grinder, make the fineness of silver powder, glass dust reach 5 microns, namely obtain front electrode of solar battery slurry A2.
Embodiment 3
Embodiment 3 is for the front electrode of solar battery slurry that the preparation method of front electrode of solar battery slurry of the present invention is described and adopts this preparation method to make;
1, supply raw materials: silver powder 86 % by weight, 0.4 micron of specific area; Glass dust 3 % by weight PbO-B
2O
3-ZnO(wherein, PbO 80wt%), 0.7 micron of average grain diameter; Organic carrier 11 % by weight, wherein, organic solvent accounts for 75 % by weight, and the calcium complex soap thickening agent accounts for 18 % by weight, and wetting dispersing agent accounts for 1.5 % by weight, and ethyl cellulose accounts for 4.5 % by weight, essence 1 % by weight;
2, preparation organic carrier: organic solvent is heated to 80 ℃ in closed reaction vessel, adds the composite calcium-base thickening agent, stir and be warming up to 160 ℃, continue to stir 5min, then add wetting dispersing agent, essence and ethyl cellulose, stir and be cooled to room temperature;
3, with after above-mentioned silver powder, glass dust and prepared organic carrier premixed, mix and grind at three-roll grinder, make the fineness of silver powder, glass dust reach 10 microns, namely obtain front electrode of solar battery slurry A3.
Embodiment 4
Embodiment 4 is for the front electrode of solar battery slurry that the preparation method of front electrode of solar battery slurry of the present invention is described and adopts this preparation method to make;
1, supply raw materials: silver powder 84 % by weight, 0.8 micron of specific area; Glass dust 4.5 % by weight PbO-B
2O
3-SiO
2(wherein, PbO 82wt%), 0.9 micron of average grain diameter; Organic carrier 11.5 % by weight, wherein, organic solvent accounts for 65 % by weight, and complex lithium grease accounts for 25 % by weight, and wetting dispersing agent accounts for 1 % by weight, and ethyl cellulose accounts for 8 % by weight, and essence accounts for 1 % by weight;
2, preparation organic carrier: organic solvent is heated to 65 ℃ in reaction vessel, adds complex lithium grease, wetting dispersing agent, ethyl cellulose and essence, continue to stir 30min, be cooled to room temperature;
3, with after above-mentioned silver powder, glass dust and prepared organic carrier premixed, mix and grind at three-roll grinder, make the fineness of silver powder, glass dust reach 8 microns, namely obtain front electrode of solar battery slurry A4.
Embodiment 5
Embodiment 5 is for the front electrode of solar battery slurry that the preparation method of front electrode of solar battery slurry of the present invention is described and adopts this preparation method to make;
1, supply raw materials: silver powder 73 % by weight, 1.8 microns of specific areas; Glass dust 6 % by weight Bi
2O
3-B
2O
3-SiO
2(wherein, Bi
2O
378wt%), average grain diameter is 1.1 microns; Organic carrier 21 % by weight, wherein, organic solvent accounts for 60 % by weight, and composite barium-base grease accounts for 20 % by weight, and wetting dispersing agent accounts for 1 % by weight, and acrylic resin accounts for 8 % by weight, and polyamide wax accounts for 10 % by weight, and essence accounts for 1 % by weight;
2, preparation organic carrier: organic solvent is heated to 60 ℃ in reaction vessel, adds composite barium-base grease, wetting dispersing agent, ethyl cellulose, polyamide wax and essence, continue to stir 45min, be cooled to room temperature;
3, with after above-mentioned silver powder, glass dust and prepared organic carrier premixed, mix and grind at three-roll grinder, make the fineness of silver powder, glass dust reach 7 microns, namely obtain front electrode of solar battery slurry A5.
Embodiment 6
Embodiment 6 is for the front electrode of solar battery slurry that the preparation method of front electrode of solar battery slurry of the present invention is described and adopts this preparation method to make;
1, supply raw materials: silver powder 85 % by weight, 1.1 microns of specific areas; Glass dust 4 % by weight Bi
2O
3-B
2O
3-SiO
2(wherein, Bi
2O
376wt%), average grain diameter is 0.9 micron; Organic carrier 11 % by weight, wherein, organic solvent accounts for 80 % by weight, and urea-base grease accounts for 14 % by weight, and wetting dispersing agent accounts for 1 % by weight, and ethyl cellulose accounts for 4 % by weight, and essence accounts for 1 % by weight;
2, preparation organic carrier: organic solvent is heated to 80 ℃ in reaction vessel, adds compound urea-base grease, wetting dispersing agent, ethyl cellulose and essence, continue to stir 30min, be cooled to room temperature;
3, with after above-mentioned silver powder, glass dust and prepared organic carrier premixed, mix and grind at three-roll grinder, make the fineness of silver powder, glass dust reach 8 microns, namely obtain front electrode of solar battery slurry A6.
Comparative Examples 1
1, supply raw materials: silver powder 85 % by weight, 1.1 microns of specific areas; Glass dust 4 % by weight Bi
2O
3-B
2O
3-SiO
2(wherein, Bi
2O
376wt%), average grain diameter is 0.9 micron; Organic carrier 11 % by weight, wherein, organic solvent accounts for 80 % by weight, and rilanit special accounts for 9 % by weight, and wetting dispersing agent accounts for 1 % by weight, and ethyl cellulose accounts for 10 % by weight;
2, preparation organic carrier: organic solvent is heated to 55 ℃ in reaction vessel, adds rilanit special, wetting dispersing agent and ethyl cellulose, continue to stir 30min, be cooled to room temperature;
3, with after above-mentioned silver powder, glass powder and organic carrier premixed, mix and grind at three-roll grinder, make the fineness of silver powder, glass dust reach 8 microns, namely obtain front electrode of solar battery slurry B1.
Comparative Examples 2
1, supply raw materials: silver powder 83 % by weight, 1.2 microns of specific areas; Glass dust 4.5 % by weight Bi
2O
3-B
2O
3-SiO
2(wherein, Bi
2O
376wt%), average grain diameter is 0.9 micron; Organic carrier 12.5 % by weight, wherein, organic solvent accounts for 81 % by weight, and wetting dispersing agent accounts for 1 % by weight, and ethyl cellulose accounts for 18 % by weight;
2, preparation organic carrier: organic solvent is heated to 60 ℃ in reaction vessel, adds wetting dispersing agent and ethyl cellulose, continue to stir 30min, be cooled to room temperature;
3, with after above-mentioned silver powder, glass powder and organic carrier premixed, mix and grind at three-roll grinder, make the fineness of silver powder, glass dust reach 8 microns, namely obtain front electrode of solar battery slurry B2.
Comparative Examples 3
1, supply raw materials: silver powder 79 % by weight, 0.8 micron of specific area; Glass dust 6 % by weight PbO-B
2O
3-SiO
21.5 microns of (wherein, PbO 70wt%) average grain diameters; Organic carrier 15 % by weight, wherein, organic solvent accounts for 80 % by weight, and polyamide wax accounts for 14 % by weight, and wetting dispersing agent accounts for 6 % by weight;
2, preparation organic carrier: organic solvent is heated to 80 ℃ in reaction vessel, adds polyamide wax, wetting dispersing agent, continue to stir 30min, be cooled to room temperature;
3, with after above-mentioned silver powder, glass powder and organic carrier premixed, mix and grind at three-roll grinder, make the fineness of silver powder, glass dust reach 8 microns, namely obtain front electrode of solar battery slurry B3.
Comparative Examples 4
1, supply raw materials: silver powder 79 % by weight, 0.8 micron of specific area; Glass dust 6 % by weight PbO-B
2O
3-SiO
2(wherein, PbO 70wt%), 1.2 microns of average grain diameters; Organic carrier 15 % by weight, wherein, organic solvent accounts for 74 % by weight, and polyamide wax accounts for 10 % by weight, and wetting dispersing agent accounts for 1 % by weight, and acrylic resin accounts for 15 % by weight;
2, preparation organic carrier: organic solvent is heated to 80 ℃ in reaction vessel, adds polyamide wax, wetting dispersing agent and acrylic resin, continue to stir 30min, be cooled to room temperature;
3, with after above-mentioned silver powder, glass powder and organic carrier premixed, mix and grind at three-roll grinder, make the fineness of silver powder, glass dust reach 8 microns, namely obtain front electrode of solar battery slurry B4.
Performance test:
1, the size of the silver electrode grid line after testing of printed, oven dry and sintering and pattern situation:
The front electrode of solar battery slurry B1-B4 that the front electrode of solar battery slurry A1-A6 that above-described embodiment 1-6 is made and Comparative Examples 1-4 make is by screen process press (Dongguan excellent seal silk screen bat printing machinery plant, UP-S7090) coordinate 290 order screen printings of 60 microns of thin grid line width positive at the polysilicon chip of 156 * 156mm, use the height and width of the grid line after the 3D optical microscope measuring prints, and observe situations such as whether having empty seal and broken string, test result is as shown in table 1; Dry by continuous tunnel furnace subsequently, 160 ℃ of furnace temperature, dry 3min re-uses the grid line height and width after the 3D optical microscope measuring is dried, and test result is as shown in table 2; The silicon chip that is printed at last gate electrode line at the uniform velocity passed through the tunnel sintering furnace in 2 minutes and 12 seconds, since 300 ℃ of sintering, 870 ℃ of sintering final temperatures, make solar battery sheet AA1-AA6 and BB1-BB4, re-use the grid line height and width after 3D optical microscope measuring sintering, test result is as shown in table 3.
2, electricity conversion test:
(Shang Haiju receives Science and Technology Ltd. to use the solar battery sheet special test equipment, NELC-140A), under standard test condition (STC), electricity conversion, short circuit current and the series resistance of the solar battery sheet BB1-BB4 that the front electrode of solar battery slurry B1-B4 that the solar battery sheet AA1-AA6 that the front electrode of solar battery slurry A1-A6 that test employing embodiment 1-6 makes makes and Comparative Examples 1-4 make makes; Standard test condition (STC) is: light intensity: 1000W/m
2Spectrum: AM1.5; Temperature: 25 ℃, test result is as shown in table 4.
Table 1
| ? | Height μ m | Width μ m | Depth-width ratio | Gross imperfection | Microdefect |
| A1 | 42 | 71 | 0.59 | Nothing | Nothing |
| A2 | 45 | 75 | 0.60 | Nothing | Nothing |
| A3 | 41 | 71 | 0.58 | Nothing | Nothing |
| A4 | 43 | 72 | 0.60 | Nothing | Nothing |
| A5 | 40 | 68 | 0.59 | Nothing | Nothing |
| A6 | 41 | 70 | 0.59 | Nothing | Nothing |
| B1 | 38 | 72 | 0.53 | Nothing | Nothing |
| B2 | 28 | 68 | 0.41 | Nothing | Nothing |
| B3 | 34 | 75 | 0.45 | 3 above breakpoints | Nothing |
| B4 | 35 | 76 | 0.46 | 3 above breakpoints | Nothing |
Table 2
| ? | Height μ m | Width μ m | Depth-width ratio | Gross imperfection | Microdefect |
| A1 | 38 | 78 | 0.49 | Nothing | Nothing |
| A2 | 39 | 78 | 0.5 | Nothing | Nothing |
| A3 | 37 | 76 | 0.49 | Nothing | Nothing |
| A4 | 38 | 78 | 0.49 | Nothing | Nothing |
| A5 | 36 | 75 | 0.48 | Nothing | Nothing |
| A6 | 37 | 79 | 0.47 | Nothing | Nothing |
| B1 | 20 | 83 | 0.24 | Nothing | Nothing |
| B2 | 25 | 73 | 0.34 | Nothing | Nothing |
| B3 | 21 | 85 | 0.25 | 3 above breakpoints | Nothing |
| B4 | 22 | 80 | 0.28 | 3 above breakpoints | Nothing |
Table 3
| ? | Height μ m | Width μ m | Depth-width ratio | Gross imperfection | Microdefect |
| A1 | 28 | 72 | 0.39 | Nothing | Nothing |
| A2 | 27 | 74 | 0.36 | Nothing | Nothing |
| A3 | 26 | 73 | 0.36 | Nothing | Nothing |
| A4 | 27 | 71 | 0.38 | Nothing | Nothing |
| A5 | 25 | 70 | 0.36 | Nothing | Nothing |
| A6 | 27 | 71 | 0.38 | Nothing | Nothing |
| B1 | 13 | 87 | 0.15 | Nothing | Empty seal is arranged |
| B2 | 15 | 78 | 0.19 | Nothing | Nothing |
| B3 | 13 | 89 | 0.15 | 3 above breakpoints | Empty seal is arranged |
| B4 | 16 | 82 | 0.20 | 3 above breakpoints | Nothing |
Table 4
| ? | Short circuit current A | Series resistance m Ω | Electricity conversion % |
| AA1 | 8.478 | 2.6 | 16.83 |
| AA2 | 8.476 | 2.8 | 16.79 |
| AA3 | 8.475 | 2.7 | 16.80 |
| AA4 | 8.478 | 2.6 | 16.82 |
| AA5 | 8.476 | 2.7 | 16.81 |
| AA6 | 8.477 | 2.7 | 16.82 |
| BB1 | 8.432 | 2.9 | 16.73 |
| BB2 | 8.451 | 2.8 | 16.75 |
| BB3 | 8.436 | 3.0 | 16.71 |
| BB4 | 8.453 | 2.8 | 16.72 |
Can find out from the experimental result of above-mentioned table 1-4, adopt solar cell front side silver paste material of the present invention in printing, oven dry and sintering process process, all can keep depth-width ratio and grid line pattern preferably, the situation that there is no empty seal and broken string, printing adaptability is good, and prepared solar battery sheet short circuit current is large, electricity conversion is high.
The above is only preferred embodiment of the present invention, not in order to limiting the present invention, all any modifications of doing within the spirit and principles in the present invention, is equal to and replaces and improvement etc., within all should being included in protection scope of the present invention.
Claims (12)
1. front electrode of solar battery silver slurry, is characterized in that, described silver slurry comprises organic carrier and is dispersed in silver powder and glass dust in organic carrier; Described organic carrier comprises organic solvent and high temperature resistant lubricating grease or high temperature resistant thickening agent.
2. front electrode of solar battery as claimed in claim 1 silver slurry, is characterized in that, take the total weight of silver slurry as benchmark, the content of described silver powder is the 70-90 % by weight, and the content of described glass dust is the 1-8 % by weight, and the content of described organic carrier is the 6-25 % by weight.
3. front electrode of solar battery silver slurry as claimed in claim 1, is characterized in that, the specific area of described silver powder is 0.2-2.5m
2/ g; The particle diameter of described glass dust is 0.1-5 μ m; Described glass dust contains the compound of Pb or Bi, and the content of the compound of described Pb or Bi is 65-90wt%.
4. front electrode of solar battery silver as claimed in claim 1 is starched, it is characterized in that, described organic carrier also comprises additive, take the total weight of organic carrier as benchmark, the content of described organic solvent is the 60-90 % by weight, the content of described high temperature resistant lubricating grease or high temperature resistant thickening agent is the 5-30 % by weight, and the content of described additive is the 0.5-15 % by weight.
5. according to claim 1 or 4 described front electrode of solar battery silver are starched, and it is characterized in that: the boiling point of described organic solvent is 180-340 ℃, is selected from one or more in fourth card, fourth card ester, terpinol, tributyl phosphate, lauryl alcohol ester.
6. according to claim 1 or 4 described front electrode of solar battery silver are starched, it is characterized in that: the dropping point of described high temperature resistant lubricating grease is selected from one or more in lithium base grease, urea-base grease, complex calcium lubricating grease, complex lithium grease, composite barium-base grease higher than 180 ℃-220 ℃.
7. according to claim 1 or 4 described front electrode of solar battery silver are starched, and it is characterized in that: described high temperature resistant thickening agent is selected from one or more in lithium soap thickening agent, polyurea thickening agent, compound lithium soap thickening agent, compound barium soap thickening agent, calcium complex soap thickening agent.
8. front electrode of solar battery silver according to claim 4 is starched, and it is characterized in that: described additive comprises one or more in cellulose, thixotropic agent, wetting dispersing agent, essence.
9. the preparation method of as described in a claim 1-8 any one front electrode of solar battery silver slurry comprises the following steps:
Step 1, add high temperature resistant lubricating grease or high temperature resistant thickening agent in organic solvent, stir, obtain organic carrier;
Step 2, with above-mentioned organic carrier with after silver powder, glass dust mix, grind, obtain described front electrode of solar battery silver slurry.
10. preparation method as claimed in claim 9, is characterized in that: in step 1, organic solvent is heated to 50-80 ℃, adds high temperature resistant lubricating grease, stir 5-30min, then add additive, continue to stir 5-30min, be cooled to room temperature and obtain organic carrier.
11. preparation method according to claim 9, it is characterized in that: in step 1, organic solvent is heated to 80-120 ℃, add high temperature resistant thickening agent, stir and be warming up to 150-200 ℃, continue to stir 1-5min, then add additive, continue to be stirred to cool to room temperature and obtain organic carrier.
12. solar battery sheet, described solar battery sheet comprises silicon chip and the silver electrode grid line of being located on silicon chip, it is characterized in that: then described silver electrode grid line obtains after drying, sintering by silk screen printing such as the described conductive silver paste of claim 1-8 any one on silicon chip.
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| CN103337277A (en) * | 2013-07-11 | 2013-10-02 | 中国工程物理研究院化工材料研究所 | Conductive silver paste for front electrode of solar battery and preparation method of conductive silver paste |
| CN104008789A (en) * | 2013-10-28 | 2014-08-27 | 苏州晶银新材料股份有限公司 | Front conductive silver paste for crystal silicon solar cells |
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