CN102903420B - A kind of electrocondution slurry and preparation method thereof - Google Patents
A kind of electrocondution slurry and preparation method thereof Download PDFInfo
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- CN102903420B CN102903420B CN201110212973.8A CN201110212973A CN102903420B CN 102903420 B CN102903420 B CN 102903420B CN 201110212973 A CN201110212973 A CN 201110212973A CN 102903420 B CN102903420 B CN 102903420B
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Abstract
The invention provides a kind of electrocondution slurry and preparation method thereof, electrocondution slurry comprises silver powder, glass dust, organic carrier and additive, and wherein, additive comprises bleeding agent.With the mass percentage of electrocondution slurry for benchmark, wherein, the content of silver powder is 60-85%; The content of glass dust is 1-10%; The content of organic carrier is 3-20%; The content of bleeding agent is 0.1-5%.With electrocondution slurry of the present invention after solar cell surface printing, sintering, can surfacing be formed, the silver grating line that height is consistent, depth-width ratio is high, and then the battery efficiency of solar cell can be improved.
Description
Technical field
The invention belongs to area of solar cell, particularly relate to a kind of electrocondution slurry and preparation method thereof.
Background technology
Along with the increasingly sharpening of day by day exhausted, problem of environmental pollution of traditional energy, the development and application of new forms of energy has become the focus of human research.Solar energy that is inexhaustible, green non-pollution is one of emphasis of new energy development utilization.
Electrocondution slurry is the important materials making silica-based solar cell.Silica-based solar cell is generally by being printed on silicon substrate by electrocondution slurry, and then drying prepares electrode with firing.
The quality of the metal electrode of solar cell, especially sensitive surface metal electrode (i.e. front electrode) can produce material impact to performance parameters such as the fill factor, curve factor of battery, electricity conversions.The front side conductive slurry of current use generally comprises silver powder, glass dust, organic carrier, electrocondution slurry gate electrode line when sintering prepares electrode of solar battery of printing easily caves in, situation low between the senior middle school of both sides is easily there is in the electrocondution slurry grid line of printing at Width, in number to be printed one timing of electrocondution slurry, cave in the middle of the electrocondution slurry grid line of printing extruding margin slurry, the electrocondution slurry grid line width of printing is broadened, decrease the light-receiving area of solar cell, have impact on the photoelectric conversion efficiency of battery, existing electrocondution slurry after sintering simultaneously, also there is formed silver grating line height inconsistent, electrode surface out-of-flatness, electrode resistance is larger, the problem that cell photoelectric conversion efficiency is not high.
Summary of the invention
The present invention is silver grating line height inconsistent, the depth-width ratio comparatively end sintering formation after solving existing electrocondution slurry silk screen printing, reduce the light-receiving area of the solar cell of preparation, and then affect the problem of cell photoelectric conversion efficiency, a kind of Novel conductive paste and preparation method thereof is provided.
The invention provides a kind of electrocondution slurry, comprise silver powder, glass dust, organic carrier and additive, wherein, additive comprises bleeding agent.
In electrocondution slurry provided by the invention, with the mass percentage of electrocondution slurry for benchmark, wherein, the content of silver powder is 60-85%; The content of glass dust is 1-10%; The content of organic carrier is 3-20%; The content of bleeding agent is 0.1-5%.
In electrocondution slurry provided by the invention, preferably, additive also comprises coupling agent.
The present invention also provides a kind of preparation method of electrocondution slurry, comprising:
1) additive is mixed with organic carrier, heating for dissolving, obtain organic carrier solution;
2) under stirring, mixed by organic carrier solution with glass dust and silver powder, grinding, obtains electrocondution slurry.
The present inventor surprisingly finds, with electrocondution slurry of the present invention after solar cell surface printing, sintering, can form surfacing, the silver grating line that height is consistent, depth-width ratio is high, and then can improve the battery efficiency of solar cell.
Infer that reason may be, when bleeding agent adds in electrocondution slurry, when the pressed powder that organic carrier mixes with silver powder and glass dust mixes, understand some agglomerated particle in pressed powder and be difficult to infiltrate, bleeding agent can play pioneering role in organic flowing, organic substance is led progressively to permeate, be separated agglomerated particle, wrap up all independently pressed powders, the firm distribution of organic substance and pressed powder, when making silk screen printing, pulp flow is even, and can not cause highly inconsistent situation.Simultaneously, after interpolation coupling agent, coupling agent is dissolved in organic carrier, when stirring with pressed powder, one end of coupling agent connects organic substance, one end connects pressed powder, make the combination between organic substance and pressed powder more firm, complete wetting powder is issued in the effect of bleeding agent, be coated on solid powder surfaces, under the acting in conjunction of bleeding agent and coupling agent, slurry there will not be the phenomenon because shearing force causes solid to be separated with organic substance in silk screen printing disposed slurry, better can improve the situation that the inside and outside height of gained grid line after existing electrocondution slurry printing is inconsistent.
Combination between the composition of electrocondution slurry provided by the present invention, electrocondution slurry is made to sinter the silver grating line height of formation after screen printing more consistent, high wide higher, improve the light-receiving area of prepared solar cell, also improve the photoelectric conversion efficiency of battery simultaneously.
Accompanying drawing explanation
Fig. 1 is the wide collection of illustrative plates of height of silver grating line obtained by the electrocondution slurry that provides of the embodiment of the present invention;
Fig. 2 is the wide collection of illustrative plates of height of silver grating line obtained by the electrocondution slurry that provides of prior art;
Fig. 3 is the SEM collection of illustrative plates of the electrocondution slurry that the embodiment of the present invention provides;
Fig. 4 is the SEM collection of illustrative plates of the electrocondution slurry that prior art provides.
Embodiment
In order to make technical problem solved by the invention, technical scheme and beneficial effect clearly understand, below in conjunction with drawings and Examples, the present invention is further elaborated.Should be appreciated that specific embodiment described herein only in order to explain the present invention, be not intended to limit the present invention.
In order to make technical problem solved by the invention, technical scheme and beneficial effect clearly understand, 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, be not intended to limit the present invention.
The invention provides a kind of electrocondution slurry, comprise silver powder, glass dust, organic carrier and additive, wherein, additive comprises bleeding agent.
In electrocondution slurry provided by the invention, bleeding agent preferably can be ether alcohol class long-chain material, and further preferably, bleeding agent can be one or more in the secondary alkyl alcohol ether of polyoxyethylene phenolic ether, aliphatic alcohol polyoxyvinethene phosphate or polyoxyethylene; With the mass percentage of electrocondution slurry for benchmark, the preferred content of bleeding agent is 0.1-5%, and preferred content is 0.1-3% further; Better play the effect of infiltration, after improving printing, institute forms the high consistency of silver grating line, thus the photoelectric conversion efficiency of better raising battery.
In electrocondution slurry provided by the invention, preferably, additive also comprises coupling agent, and coupling agent can be the various coupling agent such as silane coupling agent or titante coupling agent; Preferred, coupling agent is titanate esters; Preferred further, coupling agent can be one or more in isopropyl three (methacryl) titanate esters, isopropyl three (different caprylyl) titanate esters, isopropyl three (capryl) titanate esters; Titante coupling agent can be applicable to thermosetting resin and thermoplastic resin simultaneously, can better with containing thermoplastic resin organic carrier with the use of, the obtained better slurry of mobility, can print simultaneously and obtain thinner grid line; And titante coupling agent is tetrahedral network structure not, adds in electrocondution slurry and can not play fixation or cause not having toughness, can have plasticity on the contrary after coupling, make slurry have better mobility equally.With the mass percentage of electrocondution slurry for benchmark, the preferred content of coupling agent is 0.1-10%, and preferred content is 1-6% further, and when solution silk screen printing preferably, pulp flow is uneven, while the silver grating line height inconsistence problems formed, better cost-saving.
In electrocondution slurry provided by the invention, preferably, silver powder is sheet or spherical, and purity is greater than 99%.Further preferred, silver powder is the mixing of the dissimilar silver powder such as sheet, spherical or other shapes.With the mass percentage of electrocondution slurry for benchmark, the preferred content of silver powder is 60-85%; Preferably, the particle size range of flake silver powder is 2-5 μm, and the particle size range of spherical silver powder is 0.1-2 μm, can improve the performance of positive silver paste further, optimizes the sintering velocity of slurry further.
In electrocondution slurry provided by the invention, glass dust is inorganic bond.The softening point of preferred glass powder is 400-600 DEG C, can be moistening when sintering for 800-900 DEG C at electrocondution slurry, be adhered to silicon substrate, the performance of further optimization electrocondution slurry, avoids burning or the fusing of melt and appearance that is insufficient, insufficient, the sintered situation such as slowly of adhering of flowing in sintering process.
The component of glass dust can be preferably the materials such as lead silicate, lead borosilicate, zinc borosilicate.With the mass percentage of electrocondution slurry for benchmark, the preferred content of glass dust is 1wt%-10wt%, further optimizes electrocondution slurry performance, avoids occurring that adhesive performance is not enough, or the welding of the situation hindrance electrode such as glass is floating.
In electrocondution slurry provided by the invention, organic carrier preferably comprises solvent and solute, and wherein, solvent can be alcohols or the Esters such as terpinol, butyl carbitol, tributyl citrate, with the mass percentage of organic carrier for benchmark, the content of solvent is preferably 10-70%; Solute can be the organic substance of some specific functions such as dispersant, thixotropic agent, thickener, and as ethyl cellulose, organic silicone oil, ethylene glycol, lecithin etc., with the mass percentage of organic carrier for benchmark, the content of solute is preferably 30-90wt%.
In electrocondution slurry provided by the invention, have no particular limits organic carrier, be applicable to the key property of this electrocondution slurry, preferably, with the mass percentage of electrocondution slurry for benchmark, the content of organic carrier is 3-20%.
The present invention also provides a kind of preparation method of electrocondution slurry, comprising:
1) additive is mixed with organic carrier, heating for dissolving, obtain organic carrier solution;
2) under stirring, mixed by organic carrier solution with glass dust and silver powder, grinding, obtains electrocondution slurry.
The preparation method of electrocondution slurry provided by the invention, specifically comprises the following steps:
A) by organic carrier and additive, put into the water-bath of 60-90 DEG C, under the stirring of homogenizer, be dissolved into uniform liquid, mixing time is 0.5-2h, takes out for subsequent use;
B) glass dust raw material is put into alumina crucible, the sintering furnace being placed in 1200-1400 DEG C melts, and high temperature takes out, and enters quenching-in water, obtains quenching material, quenching material is put into ball mill and be milled to granularity and be less than 10 μm, obtain glass dust, take out for subsequent use;
C) by silver powder, the organic carrier, the glass dust that are dissolved with additive stir into pulpous state together, three-roll grinder grinds, obtains electrocondution slurry.
The electrocondution slurry of above-mentioned preparation can be directly used in the electrode preparation of solar cell, such as by silk screen printing at the front surface of silicon chip, rear sintering for the preparation of the front electrode of solar cell.
Below in conjunction with embodiment, the invention will be further described.
Embodiment 1
Raw material (with the mass percentage of electrocondution slurry for benchmark) is taken according to following ratio:
Silver powder: 80%(granularity: 1 μm; Shape: spherical; )
Glass dust: 4%(raw material: with the mass percentage of glass dust for benchmark, boron oxide 8%, silica 25%, lead oxide 60%, aluminium oxide 7%)
Organic carrier: 13%(solvent: butyl carbitol; Solute: ethyl cellulose; With the mass percentage of organic carrier for benchmark, butyl carbitol 90%, ethyl cellulose 10%)
Coupling agent: 2%; Isopropyl three (methacryl) titanate esters
Bleeding agent: 1%; Polyoxyethylene phenolic ether
Electrocondution slurry is prepared by following steps:
A) organic carrier of precise aforementioned proportion, coupling agent and bleeding agent, put into the water-bath of 75 DEG C, under the stirring of homogenizer, stirs 1h, be dissolved into uniform liquid, take out for subsequent use;
B) the glass dust raw material of precise aforementioned proportion again, put into alumina crucible, the sintering furnace being placed in 1250 DEG C melts, high temperature takes out, and enters quenching-in water, obtains quenching material, quenching material is put into ball mill and is milled to the glass dust that granularity is 3 μm of microns, take out for subsequent use;
C) silver powder of last precise aforementioned proportion, stir into pulpous state by being dissolved with together with the organic carrier of coupling agent with bleeding agent, glass dust, then grind on three-roll grinder, obtained electrocondution slurry is denoted as S1.
Embodiment 2
Be with the difference of embodiment 1: the content of bleeding agent is 3%, the content of organic carrier is 11%, and obtained electrocondution slurry is denoted as S2.
Embodiment 3
Be with the difference of embodiment 1: the content of coupling agent is 6%, the content of organic carrier is 9%, and obtained electrocondution slurry is denoted as S3.
Embodiment 4
Be with the difference of embodiment 1: the content of coupling agent is 7%, the content of bleeding agent is 0.05%, and the content of organic carrier is 8.95%, and obtained electrocondution slurry is denoted as S4.
Embodiment 5
Be with the difference of embodiment 1: the content of coupling agent is 8%, the content of bleeding agent is 4%, and the content of organic carrier is 4%, and obtained electrocondution slurry is denoted as S5.
Embodiment 6
Be with the difference of embodiment 1: the content of coupling agent is 0%, the content of bleeding agent is 0.1%, and the content of organic carrier is 15.9%, and obtained electrocondution slurry is denoted as S6.
Embodiment 7
Be with the difference of embodiment 1: the content of coupling agent is 0%, the content of bleeding agent is 1.5%, and the content of organic carrier is 14.5%, and obtained electrocondution slurry is denoted as S7.
Embodiment 8
Be with the difference of embodiment 1: coupling agent used is vinyltrimethoxy silane, and obtained electrocondution slurry is denoted as S8.
Embodiment 9
Be with the difference of embodiment 1: coupling agent used is isopropyl three (capryl) titanate esters, and obtained electrocondution slurry is denoted as S9.
Comparative example 1
Be with the difference of embodiment 1: the content of coupling agent is 0%, the content of bleeding agent is 0%, and the content of organic carrier is 16%, and obtained electrocondution slurry is denoted as D1.
performance test
By the electrocondution slurry silk screen printing of S1-S9 and D1, the solar battery sheet obtained after sintering is denoted as S11-S99 and D11 accordingly respectively, carries out performance test.
1, sheet resistance test
The method adopting GB/T17473.3-1998 to specify is carried out, and the model adopting Guangzhou four point probe Electronic Science and Technology Co., Ltd. to produce is that the solar battery sheet of sheet resistance instrument to S11-S99 and D11 of RTS-4 is tested, and unit is milliohm/, and test result is in table 1.
2, depth-width ratio
Adopt height and the width of silver grating line in ambiosXP-1 type step instrument test S11-S99 and D11 solar battery sheet produced in USA, respectively as depicted in figs. 1 and 2, calculate depth-width ratio, result of calculation is in table 1 for high wide collection of illustrative plates.
3, light conversion ratio
The model adopting He Shuan Science and Technology Ltd. of Shanghai Communications University to produce is that the solar battery sheet of solar battery sheet electricity conversion special test equipment to S11-S99 and D11 of HSC1/XSCM-9 is tested, and test result is in table 1.
4, microscopic appearance
Carry out SEM detection to S1 and D1, gained collection of illustrative plates respectively as shown in Figure 3 and Figure 4.
Table 1
| Sheet resistance (milliohm/) | Depth-width ratio | Optoelectronic transformation efficiency % | |
| S11 | 1.5 | 0.0068 | 16.7 |
| S22 | 1.9 | 0.0061 | 16.3 |
| S33 | 2.1 | 0.0059 | 16.2 |
| S44 | 2.4 | 0.0056 | 15.9 |
| S55 | 3 | 0.0051 | 15.1 |
| S66 | 2.5 | 0.0055 | 15.7 |
| S77 | 2.5 | 0.0056 | 15.8 |
| S88 | 2.9 | 0.0046 | 14.8 |
| S99 | 2.6 | 0.0054 | 15.6 |
| D11 | 3.2 | 0.0041 | 14.5 |
Can find out according to the data result in table 1 and Fig. 1 to Fig. 4, the depth-width ratio that with the addition of the silver grating line obtained by electrocondution slurry S1-S9 of bleeding agent is obviously higher than the silver grating line obtained by electrocondution slurry D1, the solar battery sheet S11-S99 sheet resistance that electrocondution slurry S1-S9 obtains is starkly lower than the solar battery sheet of D11, electricity conversion also obviously increases, wherein, with the addition of the bleeding agent of preferable range content and the electrocondution slurry of coupling agent, the performance of obtained solar battery sheet improves more remarkable simultaneously.In addition, can clearly find out from step instrument test collection of illustrative plates, S1 surfacing, and D1 occurs that both sides are high, middle low state; Scheme also as can be seen from the SEM of S1, after slurry sintering, hole is less, and sintering is even, and D1 hole is more, and out-of-flatness.
The foregoing is only preferred embodiment of the present invention, not in order to limit the present invention, all any amendments done within the spirit and principles in the present invention, equivalent replacement and improvement etc., all should be included within protection scope of the present invention.
Claims (6)
1. an electrocondution slurry, comprises silver powder, glass dust, organic carrier and additive, it is characterized in that, described additive comprises bleeding agent and coupling agent; And with the mass percentage of this electrocondution slurry for benchmark, the content of described silver powder is 60-85 quality %, the content of described glass dust is 1-10 quality %, the content of described organic carrier is 3-20 quality %, the content of described coupling agent is 0.1-10 quality %, the content of described bleeding agent is 0.1-5 quality %, and described coupling agent is titanate esters; Wherein, described bleeding agent is selected from one or more in the secondary alkyl alcohol ether of polyoxyethylene phenolic ether, aliphatic alcohol polyoxyvinethene phosphate and polyoxyethylene.
2. electrocondution slurry as claimed in claim 1; wherein, described titanate esters is selected from one or more in isopropyl three (methacryl) titanate esters, isopropyl three (different caprylyl) titanate esters and isopropyl three (capryl) titanate esters.
3. electrocondution slurry as claimed in claim 1, wherein, described silver powder comprises flake silver powder and/or spherical silver powder.
4. electrocondution slurry as claimed in claim 3, wherein, the particle size range of described flake silver powder is 2-5 μm; The particle size range of described spherical silver powder is 0.1-2 μm.
5., as a preparation method for electrocondution slurry as described in any one in Claims 1-4, comprising:
1) additive is mixed with organic carrier, heating for dissolving, obtain organic carrier solution;
2) under stirring, mixed by organic carrier solution with glass dust and silver powder, grinding, obtains electrocondution slurry.
6., as a preparation method for electrocondution slurry as described in any one in Claims 1-4, comprising:
A) by organic carrier and additive, put into the water-bath of 60-90 DEG C, under the stirring of homogenizer, be dissolved into uniform liquid, mixing time is 0.5-2h, takes out for subsequent use;
B) glass dust raw material is put into alumina crucible, the sintering furnace being placed in 1200-1400 DEG C melts, and high temperature takes out, and enters quenching-in water, obtains quenching material, quenching material is put into ball mill and be milled to granularity and be less than 10 μm, obtain glass dust, take out for subsequent use;
C) by silver powder, the organic carrier, the glass dust that are dissolved with additive stir into pulpous state together, three-roll grinder grinds, obtains electrocondution slurry.
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| CN104078099A (en) * | 2014-06-04 | 2014-10-01 | 乐凯特科技铜陵有限公司 | Environmentally-friendly printed circuit board conductive silver paste and preparing method thereof |
| CN112133469B (en) * | 2020-09-28 | 2022-03-11 | 长春黄金研究院有限公司 | Mixed organic solvent for preparing high-temperature sintering conductive slurry |
| CN114792588B (en) * | 2022-06-24 | 2022-09-20 | 江西理工大学南昌校区 | Preparation method of conductive silver paste for spraying electrode silver grid aerosol of solar cell |
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| CN101239246A (en) * | 2008-02-20 | 2008-08-13 | 江南大学 | Method for recovering cutting solution from by-product of silicon chip cutting processing |
| CN101457116A (en) * | 2007-12-12 | 2009-06-17 | 上海海悦涂料有限公司 | Long acting low surface treatment epoxy coating priming lacquer |
| CN101630695A (en) * | 2009-08-05 | 2010-01-20 | 贵研铂业股份有限公司 | Lead-free cadmium-free electrode slurry for crystalline silicon solar battery and preparation method thereof |
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| CN101457116A (en) * | 2007-12-12 | 2009-06-17 | 上海海悦涂料有限公司 | Long acting low surface treatment epoxy coating priming lacquer |
| CN101239246A (en) * | 2008-02-20 | 2008-08-13 | 江南大学 | Method for recovering cutting solution from by-product of silicon chip cutting processing |
| CN101630695A (en) * | 2009-08-05 | 2010-01-20 | 贵研铂业股份有限公司 | Lead-free cadmium-free electrode slurry for crystalline silicon solar battery and preparation method thereof |
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