CN102262914B - Conductive silver paste and preparation method thereof as well as solar cell slice - Google Patents
Conductive silver paste and preparation method thereof as well as solar cell slice Download PDFInfo
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Abstract
The invention provides a conductive silver paste which comprises a silver powder, a glass powder, a size carrier and a dispersing agent, wherein the silver powder is a mixture containing a nanometer silver powder and a fine silver powder; and the grain size of the nanometer silver powder is 50-180nm, the grain size of the fine silver powder is 1-10mu m, and the mass ratio of the nanometer silver powder and the fine silver powder is 1: (50-100). The electric conductivity of the conductive silver paste can be improved effectively by using the mixture of the nanometer silver powder and the fine silver powder.
Description
Technical field
The present invention relates to a kind of conductive silver paste and preparation method thereof and a kind of solar battery sheet.
Background technology
Conductive silver paste is generally comprised of silver powder, glass dust and organic component.But because silver powder is easy to reunite, the existence of glass dust on the other hand, makes the conductivity of conductive silver paste very poor on the one hand.In conductive silver paste, the dispersing uniformity of silver powder has a great impact the conductivity of conductive silver paste.So in order to improve the conductivity of conductive silver paste, prior art seeks effectively to improve the method for silver powder dispersing uniformity always.
For example, adopt by sheet and spherical compound silver powder in the electrocondution slurry in CN101246760A, and the ratio of the weight of spherical and flake silver powder is 5-15: 95-85, the average grain diameter of compound silver powder is less than 4 μ m.Thereby still existing silver powder to reunite, this electrocondution slurry causes the dispersed poor defect that reduces conductivity.In CN101604557A, disclose a kind of plasma display electrode electrocondution slurry, comprised silver powder, organic principle and glass powder with low melting point, wherein, silver powder adopts the silver powder of particle size range different-grain diameter specification between 0.2-3.5 micron.This electrocondution slurry adopts ball silver and the combination of sheet silver of different-grain diameter, and the blind of small particle diameter sheet silver, effectively improves the contact area of silver powder and base material, thereby improves conductance.But the small particle diameter silver powder between this particle size range 0.2-3.5 micron can make grain boundary face increase, and the less silver powder of particle diameter more easily reunites, and can reduce conductance again.
Summary of the invention
The invention solves the low technical problem of conductive silver paste conductance existing in prior art.
The invention provides a kind of conductive silver paste, in described conductive silver paste, contain silver powder, glass dust, slurry carrier and dispersant; Described silver powder is the mixture that contains nano-silver powder and micro aluminum powder, and wherein the particle diameter of nano-silver powder is 50-180nm, and the particle diameter of micro aluminum powder is 1-10 μ m, and the mass ratio of nano-silver powder and micro aluminum powder is 1: 50-100.
The present invention also provides the preparation method of described conductive silver paste, comprises the following steps:
A. nano-silver powder is scattered in the organic solvent that boiling point is less than 90 ℃, adds dispersant, be uniformly dispersed;
B. add slurry carrier, be uniformly dispersed; The organic solvent that described boiling point is less than 90 ℃ is removed in distillation;
C. add micro aluminum powder and glass dust, be uniformly dispersed, obtain described conductive silver paste.
The present invention also provides a kind of solar battery sheet, and described solar battery sheet comprises silicon substrate and be positioned at the conduction grid line on silicon substrate, and wherein, described conduction grid line is by silk screen printing conductive silver paste claimed in claim 1 on silicon substrate, and then sintering obtains.
Conductive silver paste provided by the invention, by adopting the mixture of nano-silver powder and micro aluminum powder, this conductive silver paste nano-silver powder and first congruent melting of glass dust in sintering and solidification process on the one hand, nano-silver powder is filled micro aluminum powder interface around, reduces the contact area of glass dust; On the other hand, after this conductive silver paste sintering, silver powder can be formed the larger and uniform silver-colored crystal grain of particle, and silver-colored particle is uniformly dispersed, thereby improves the conductance of conductive silver paste.
Embodiment
The invention provides a kind of conductive silver paste, in described conductive silver paste, contain silver powder, glass dust, slurry carrier, contain or do not contain dispersant; Described silver powder is the mixture that contains nano-silver powder and micro aluminum powder, and wherein the particle diameter of nano-silver powder is 50-180nm, and the particle diameter of micro aluminum powder is 1-10 μ m, and the mass ratio of nano-silver powder and micro aluminum powder is 1: 50-100.
Generally, the silver powder particle diameter adopting in conductive silver paste is less, and silver powder is more easily reunited, and is difficult to be uniformly dispersed, and can significantly reduce the conductance of conductive silver paste.The present inventor surprisingly finds: in conductive silver paste of the present invention, silver powder adopts the silver powder combination of two particle diameter sections, and during the mixture of nano-silver powder and micro aluminum powder, the conductance of conductive silver paste is very high.
The present inventor thinks: the silver powder fusing point of different-grain diameter is different, nano-silver powder and micro aluminum powder have fusing point difference, in high temperature sintering and curing process, the first congruent melting of nano-silver powder and glass dust, and after micro aluminum powder congruent melting, from micro aluminum powder, around supplement contacting of silver-colored particle and substrate, the contact area of minimizing glass dust and substrate; In addition, after silver powder congruent melting, can form the larger and uniform silver-colored crystal grain of particle, be dispersed in substrate surface, thereby improve conductance.
Described silver powder is the mixture that contains nano-silver powder and micro aluminum powder, and wherein the particle diameter of nano-silver powder is 50-180nm, and the particle diameter of micro aluminum powder is 1-10 μ m, and the mass ratio of nano-silver powder and micro aluminum powder is 1: 50-100.Under preferable case, the mass ratio of nano-silver powder and micro aluminum powder is 1: 70-100.In the present invention, described nano-silver powder, micro aluminum powder can directly adopt and be purchased product.
The quality of conductive silver paste of take is benchmark, and the content of silver powder is 65-85%, and the content of glass dust is 3-10%, and the content of dispersant is 0.01-0.05%, and the content of slurry carrier is 10-20%, sizing agent 1-5%.Under preferable case, the quality of conductive silver paste of take is benchmark, and the content of silver powder is 75-81%, and the content of glass dust is 3-5%, and the content of dispersant is 0.02-0.03%, and the content of slurry carrier is 10-20%, sizing agent content 2-4%.
Described glass dust, for improving the caking property of conductive silver paste, reduces sintering temperature.The average grain diameter of described glass dust is generally 0.1-10 μ m.The class material with glassy phase being formed by multiple inorganic oxide pre-burning that described glass dust is known to the skilled person.For example, in described glass dust, contain SiO
2, B
2o
3, Bi
2o
3, CaO, BaO, ZnO, Al
2o
3, TiO
2, ZrO
2, CuO, PbO at least three kinds.Under preferable case, be to improve the conductivity of wire silver slurry, the quality of glass dust of take is benchmark, contains the PbO of 45-65wt%, the TiO of 5-15wt% in described glass dust
2, the SiO of 20-30wt%
2and 5-10wt%Al
2o
3.
Described dispersant is various organic dispersing agents conventional in prior art, for example, can be selected from one or more in lauryl sodium sulfate (SDS), cetyl benzene sulfonic acid sodium salt (SDBS), softex kw (CTMAB), cetyl pyridinium (CPB), polyvinylpyrrolidone (PVP), glycerol, stearic acid and stearate.The various stearic acid that described stearic acid is known to the skilled person can be for example enanthic acid, sad or n-nonanoic acid.
Described slurry carrier improves the stability of coating property and coated film while being mainly used in conductive silver paste to be applied on substrate.Described slurry carrier contains resin and auxiliary agent; At 25 ℃ of described vector resins, viscosity is 500-50000mPas, and described auxiliary agent comprises reactive diluent, levelling agent and defoamer.The quality of slurry carrier of take is benchmark, and the content of resin is 75-97%, and the content of carrier auxiliary agent is 3-25%.
Described resin for the various resins that those skilled in the art commonly use, for example, can comprise epoxy resin, acrylic resin, amino resins and/or silane resin.Under preferable case, described resin is epoxy resin.Described epoxy resin is selected from a kind of or many in glycidol ether bisphenol A-type, bisphenol f type epoxy resin, glycidol alicyclic ring epoxy resins, aliphatic epoxy resin, cycloaliphatic epoxy resin, and the epoxide number of described epoxy resin is 0.4-0.8.Described epoxy resin also can directly adopt and be purchased product, for example, can adopt E-51 epoxy resin and/or 6458 epoxy resin.
Described reactive diluent is selected from one or more in diglycidyl ether, polyglycidyl ether, ethylene glycol diglycidylether, many diglycidyl ether of ethylene glycol, butanediol diglycidyl ether, glycerine epoxy.Described curing accelerator is selected from the modifier of benzyl dimethylamine, DMP-30,2-ethyl-4-methylimidazole, one or more in the modifier of cyano group-2-ethyl-4-methylimidazole.
The kind of levelling agent, defoamer and consumption are conventionally known to one of skill in the art.For example, described levelling agent can be selected from EFKA3883, EFKA3886, EFKA3600, BYK366, BYK333, in BYK307, DEGO410, DEGO Glide410, Glide450, Rad2300, Rad2500, TEGORad 2100 one or more.Defoamer can be selected from EFKA2022, EFKA2527, EFKA2040, BYK352, BYK354, BYK357, TEGO Airex900, TEGO Airex920, TEGO Airex900, FOAMEXN one or more.
The preparation method who the invention provides described conductive silver paste, comprises the following steps:
A. nano-silver powder is scattered in the organic solvent that boiling point is less than 90 ℃, adds dispersant, be uniformly dispersed;
B. add slurry carrier, be uniformly dispersed; The organic solvent that described boiling point is less than 90 ℃ is removed in distillation;
C. add micro aluminum powder and glass dust, be uniformly dispersed, obtain described conductive silver paste.
Due to after nano-silver powder, micro aluminum powder mix with glass dust, the particle diameter of nano-silver powder is too little, directly disperses to be difficult to be uniformly dispersed, and easily reunite in slurry carrier.Therefore, in the present invention, first nano-silver powder is scattered in the organic solvent that boiling point is less than 90 ℃, and then mixes with slurry carrier, the organic solvent that boiling point is less than 90 ℃ is removed in distillation; Finally add micro aluminum powder and glass dust.
Described boiling point is less than the various low boiling point organic solvents that the organic solvent of 90 ℃ is commonly used for those skilled in the art, preferably employing boiling point is the organic solvent of 20-90 ℃, for example, can be selected from one or more in thiacyclohexane, ethyl acetate, butanone, oxolane, normal heptane, methyl alcohol, isopropyl alcohol, ethanol, butyl acetate.
In order to make the nano-silver powder simultaneously production control cost that is uniformly dispersed, the mass ratio that described nano-silver powder and described boiling point are less than the organic solvent of 90 ℃ is 1: 1-10; Be preferably 1: 3-8.In the present invention, the temperature of described distillation is 20-60 ℃, is preferably 35-55 ℃.
As a kind of preferred implementation of the present invention, described slurry carrier also can add step by step, for example, can after step a completes, add part slurry carrier, and after being uniformly dispersed, the organic solvent that boiling point is less than 90 ℃ is removed in distillation; And then add micro aluminum powder, glass dust and remaining slurry carrier.Adopt substep to add the technique of slurry carrier can avoid nano-silver powder in resin, to occur the phenomenon of reuniting.
Conductive silver paste of the present invention can be applicable to print fine circuitry field, especially the less circuit of live width; For example, for making FPC plate or photoelectric conversion assembly substrate.
The invention provides a kind of solar battery sheet, described solar battery sheet comprises silicon substrate and be positioned at the conduction grid line on silicon substrate, and wherein, described conduction grid line is by silk screen printing conductive silver paste claimed in claim 1 on silicon substrate, dries, sintering obtains.
In the present invention, the various silicon substrates that described silicon substrate is known to the skilled person.Mode by conductive silver paste of the present invention by silk screen printing is printed on silicon substrate, oven dry, sintering, and conductive silver paste solidify to form conduction grid line, thereby prepares solar battery sheet of the present invention.The temperature of drying is 100-200 ℃.Described silk screen printing preferably adopts 280-330 order nylon mesh; The temperature of described sintering is 300-950 ℃.Under preferable case, in the present invention, the sintering of described conductive silver paste can adopt various sintering furnaces on direct employing market to realize, for example, can adopt the HSH3003-0910 solar cell fast-burning furnace of Hefei Hengli Electronic Technology Development Co., Ltd..
Below in conjunction with embodiment, the invention will be further described.The raw material adopting in embodiment and comparative example is all available commercially.
Embodiment 1
The present embodiment is used for illustrating conductive silver paste provided by the invention and preparation method thereof.
A. inorganic raw material: nano-silver powder: particle diameter 80-100nm silver powder 10g;
Micro aluminum powder: particle diameter 2 μ m flake silver powder 800g;
Glass dust: 40g (mass ratio PbO: TiO
2: SiO
2: Al
2o
3=50: 12:
30∶8)；
Organic Ingredients: low boiling point organic solvent: ethanol 30g;
Dispersant: PVP 0.08g, SDBS 0.06g, glycerol 0.1g;
Slurry carrier: epoxy resin: E-5180g, 645860g;
Reactive diluent: ethylene glycol diglycidylether 20g;
Levelling agent: BYK36610g;
Defoamer: EFKA25275g.
B. nano-silver powder is added in low boiling point organic solvent, then add dispersant, ultrasonic dispersion 10 minutes, adds 50g epoxy resin, mechanical agitation; Low boiling point organic solvent is removed in 55 ℃ of distillations.
C. micro aluminum powder is mixed with glass dust, add remaining slurry carrier to mix.
D. the system of step b and c is mixed, mechanical agitation is even, and three-roller disperses (depolymerisation) 5 times, obtains the conductive silver paste of the present embodiment, and wherein the content of silver powder is 79%, and described conductive silver paste is designated as S1.
Embodiment 2
Adopt the method similar to embodiment 1 to prepare the conductive silver paste of the present embodiment, difference is: in step a, the quality of nano-silver powder is 16g, and the quality of micro aluminum powder is 800g, and the mass ratio that makes nano-silver powder and micro aluminum powder is 1: 50.
By above-mentioned steps, obtain the conductive silver paste of the present embodiment, wherein the content of silver powder is 79.4%, described conductive silver paste is designated as S2.
Embodiment 3
Adopt the method similar to embodiment 1 to prepare the conductive silver paste of the present embodiment, difference is: in step a, the quality of nano-silver powder is 8g, and the quality of micro aluminum powder is 800g, and the mass ratio that makes nano-silver powder and micro aluminum powder is 1: 100.
By above-mentioned steps, obtain the conductive silver paste of the present embodiment, wherein the content of silver powder is 79%, described conductive silver paste is designated as S4.
Embodiment 4
Adopt the method similar to embodiment 1 to prepare the conductive silver paste of the present embodiment, difference is: in step a, the quality of nano-silver powder is 5g, and the quality of micro aluminum powder is 394g, and the mass ratio that makes nano-silver powder and micro aluminum powder is 1: 78.8.
By above-mentioned steps, obtain the conductive silver paste of the present embodiment, wherein the content of silver powder is 65%, is designated as S4.
Embodiment 5
Adopt the method similar to embodiment 1 to prepare the conductive silver paste of the present embodiment, difference is: in step a, the quality of nano-silver powder is 15g, and the quality of micro aluminum powder is 1204.7g, and the mass ratio that makes nano-silver powder and micro aluminum powder is 1: 78.8.
By above-mentioned steps, obtain the conductive silver paste of the present embodiment, wherein the content of silver powder is 85%, is designated as S5.
Embodiment 6
A. inorganic raw material: nano-silver powder: particle diameter 80-100nm silver powder 16g;
Micro aluminum powder: particle diameter 2 μ m flake silver powder 800g;
Glass dust: 30g (mass ratio PbO: TiO
2: SiO
2: Al
2o
3=50: 12:
30∶8)；
Organic Ingredients: low boiling point organic solvent: ethanol 40g;
Dispersant: SDS 0.06g, CPB 0.08g, sad 0.04g, glycerol 0.08g;
Slurry carrier: epoxy resin: E-51100g, 645880g;
Reactive diluent: butanediol diglycidyl ether 20g;
Levelling agent: EFKA36005g;
Defoamer: BYK3545g.
B. nano-silver powder is added in low boiling point organic solvent, then add dispersant, ultrasonic dispersion 15 minutes, adds 50g epoxy resin, mechanical agitation; Low boiling point organic solvent is removed in 50 ℃ of distillations.
C. micro aluminum powder is mixed with glass dust, add remaining slurry carrier to mix.
D. the system of step b and c is mixed, mechanical agitation is even, and three-roller disperses (depolymerisation) 5 times, obtains the conductive silver paste of the present embodiment, and wherein the content of silver powder is 75.83%, and described conductive silver paste is designated as S6.
Embodiment 7
A. inorganic raw material: nano-silver powder: particle diameter 80-100nm silver powder 8g;
Micro aluminum powder: particle diameter 2 μ m flake silver powder 800g;
Glass dust: 50g (mass ratio PbO: TiO
2: SiO
2: Al
2o
3=50: 12:
30∶8)；
Organic Ingredients: low boiling point organic solvent: ethanol 40g;
Dispersant: PVP 0.06g, SDBS 0.02g, glycerol 0.04g;
Slurry carrier: epoxy resin: E-5160g, 645850g;
Reactive diluent: ethylene glycol diglycidylether 20g;
Levelling agent: BYK33310g;
Defoamer: TEGO Airex9205g BYK3525g.
B. nano-silver powder is added in low boiling point organic solvent, then add dispersant, ultrasonic dispersion 10 minutes, adds 50g epoxy resin, mechanical agitation; Low boiling point organic solvent is removed in 50 ℃ of distillations.
C. micro aluminum powder is mixed with glass dust, add remaining slurry carrier to mix.
D. the system of step b and c is mixed, mechanical agitation is even, and three-roller disperses 5 times, obtains the conductive silver paste of the present embodiment, and wherein the content of silver powder is 75.83%, and described conductive silver paste is designated as S7.
Comparative example 1
Adopt with embodiment 4 same procedure and prepare conductive silver paste, difference is: in step a, directly adopt 400g particle diameter 2 μ m flake silver powders, and no longer add nano-silver powder.
Comparative example 2
Adopt CN101246760A embodiment 1 disclosed method to prepare the electrocondution slurry of this comparative example, be designated as DS2.
Comparative example 3
Adopt CN101604557A embodiment 1 disclosed method to prepare the electrocondution slurry of this comparative example, be designated as DS3.
Embodiment 8-14
Respectively by conductive silver paste S1-S5 and DS1-DS2, adopt 280 order nylon mesh to be coated on the electrode zone on solar power silicon substrate back by silk screen printing, then (constant force electronic technology exploitation in Hefei is public to proceed to solar cell fast-burning furnace, HSH3003-0910) in, dry, sintering, conductive silver paste is solidified, obtain solar battery sheet, be designated as S11-S77.
Comparative example 3-4
Employing electrocondution slurry DS1-DS2 to solar power silicon substrate back top electrode region, prepares solar battery sheet according to the method silk screen printing identical with embodiment 8-14, is designated as DS11-DS22.
Performance test:
Solar battery sheet S11-S77 and DS11-DS22 are respectively got to 150, adopt the single flash operation solar cell tester model HSC1 of Shanghai He Shuan Thermo-Solar Energietechnik GmbH, the average photoelectric conversion efficiency of testing respectively each solar battery sheet S11-S55 and DS11-DS22.Test result is as shown in table 1.
Table 1
| Electrocondution slurry | Electricity conversion (%) |
| S11 | 15.61 |
| S22 | 15.60 |
| S33 | 15.58 |
| S44 | 15.02 |
| S55 | 15.60 |
| S66 | 15.35 |
| S77 | 15.21 |
| DS11 | 14.01 |
| DS22 | 11.63 |
| DS33 | 12.56 |
From upper table 1, in electrocondution slurry provided by the invention, the scraper plate fineness of silver-colored particle is significantly less than comparative example, illustrates that in electrocondution slurry of the present invention, the compound silver powder of silica has good dispersiveness; In addition, the electricity conversion that adopts solar cell silicon substrate prepared by electrocondution slurry of the present invention up to 15.02% and more than, illustrate that electrocondution slurry of the present invention has good conductivity.
Claims (11)
1. a preparation method for solar cell conductive silver slurry, contains silver powder, glass dust, slurry carrier and dispersant in described solar cell conductive silver slurry; It is characterized in that, described silver powder is the mixture that contains nano-silver powder and micro aluminum powder, and wherein the particle diameter of nano-silver powder is 50-180nm, and the particle diameter of micro aluminum powder is 1-10 μ m, and the mass ratio of nano-silver powder and micro aluminum powder is 1:50-1:100;
Comprise the following steps:
A. nano-silver powder is scattered in the organic solvent that boiling point is less than 90 ℃, adds dispersant, be uniformly dispersed;
B. add slurry carrier, be uniformly dispersed; The organic solvent that described boiling point is less than 90 ℃ is removed in distillation;
C. add micro aluminum powder and glass dust, be uniformly dispersed, obtain described solar cell conductive silver slurry.
2. method according to claim 1, is characterized in that, the quality that the solar cell conductive silver of take is starched is benchmark, and the content of silver powder is 65-85%, and the content of glass dust is 3-10%, and the content of dispersant is 0.01-0.05%, and the content of slurry carrier is 10-25%.
3. method according to claim 1 and 2, is characterized in that, in described glass dust, contains SiO
2, B
2o
3, Bi
2o
3, CaO, BaO, ZnO, Al
2o
3, TiO
2, ZrO
2, CuO, PbO at least three kinds.
4. method according to claim 3, is characterized in that, the quality of glass dust of take is benchmark, contains the PbO of 45-65wt%, the TiO of 5-15wt% in described glass dust
2, the SiO of 20-30wt%
2with 5-10wt% Al
2o
3.
5. method according to claim 1 and 2, it is characterized in that, described dispersant is selected from one or more in lauryl sodium sulfate, cetyl benzene sulfonic acid sodium salt, softex kw, cetyl pyridinium, polyvinylpyrrolidone, glycerol, stearic acid and stearate.
6. method according to claim 1 and 2, is characterized in that, described slurry carrier contains resin and auxiliary agent; At 25 ℃ of described resins, viscosity is 500-50000mPas; Described auxiliary agent comprises reactive diluent, levelling agent and defoamer.
7. method according to claim 6, is characterized in that, described slurry vector resin comprises epoxy resin, acrylic resin, amino resins and/or silane resin; Described epoxy resin is selected from one or more in glycidol ether bisphenol A-type, bisphenol f type epoxy resin, glycidol alicyclic ring epoxy resins, aliphatic epoxy resin, cycloaliphatic epoxy resin, and the epoxide number of described epoxy resin is 0.4-0.8.
8. method according to claim 6, it is characterized in that, described reactive diluent is selected from one or more in diglycidyl ether, polyglycidyl ether, ethylene glycol diglycidylether, many diglycidyl ether of ethylene glycol, butanediol diglycidyl ether, glycerine epoxy.
9. method according to claim 1, is characterized in that, described boiling point is less than the organic solvent of 90 ℃ and is selected from one or more in thiacyclohexane, ethyl acetate, butanone, oxolane, normal heptane, methyl alcohol, isopropyl alcohol, ethanol, butyl acetate.
10. according to the method described in claim 1 or 9, it is characterized in that, the mass ratio that nano-silver powder and described boiling point are less than the organic solvent of 90 ℃ is 1:1-1:10.
11. methods according to claim 1, is characterized in that, the temperature of described distillation is 20-60 ℃.
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