CN102347091B - Composite silver powder, preparation method thereof, and conductive silver slurry containing composite silver powder - Google Patents
Composite silver powder, preparation method thereof, and conductive silver slurry containing composite silver powder Download PDFInfo
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- CN102347091B CN102347091B CN 201010240312 CN201010240312A CN102347091B CN 102347091 B CN102347091 B CN 102347091B CN 201010240312 CN201010240312 CN 201010240312 CN 201010240312 A CN201010240312 A CN 201010240312A CN 102347091 B CN102347091 B CN 102347091B
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- silver powder
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- vitreum
- powder
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Abstract
The invention provides a composite silver powder which is a core shell structure, wherein core material is silver particles, shell material is a vitreous body, and a particle size of the silver particles is 1 to 3 micrometers. The invention also provides a preparation method of the composite silver powder and conductive silver slurry containing the composite silver powder. The composite silver powder of the present invention has the characteristics of good dispersivity and simple preparation technology, and the conductive silver slurry employing the composite silver powder has high conductivity.
Description
Technical field
The invention belongs to area of solar cell, relate in particular to a kind of compound silver powder and preparation method thereof and the conductive silver paste that contains this compound silver powder.
Background technology
Along with the fast development of solar battery technology, conductive silver paste is widely used in making front electrode of solar battery with its low cost, advantage simple to operate.Conductive silver paste generally is comprised of silver powder, Binder Phase and organic carrier, and wherein Binder Phase is glass dust.Conductive silver paste of the prior art generally prepares by silver powder is mixed and is dispersed in the organic carrier with glass dust.But the particle diameter of silver powder is very little on the one hand, very easily reunites, and is difficult to mix with glass dust in preparation slurry process; On the other hand, the area coverage of conductive silver paste glass and substrate in sintering process increases, and makes electrode surface produce the space, increases the contact resistance of solar cell, and conductance descends greatly.
A kind of photosensitive silver slurry for concentration electrode for plasma scope is disclosed among the CN1290121C.Containing particle diameter in this silver paste is the silver coating glass dust of 0.8-1 μ m, and this silver coats glass dust to be mixed with nano-silver powder, silverskin generation viscosity and Plastic Flow during sintering, thus improve conductance.Argentiferous is more in this silver paste, and cost is higher; In addition, silver coats the glass dust complicated process of preparation.And the conductance of this conductive silver paste is still lower.
Summary of the invention
The invention solves that the silver powder that exists in the prior art is difficult to disperse, the conductance of conductive silver paste is low and the defective of complicated process of preparation.
The invention provides a kind of compound silver powder, described compound silver powder is nucleocapsid structure, and wherein nuclear material is silver-colored particle, and shell material is vitreum; The particle diameter of silver particle is 1-3 μ m.
The invention provides the preparation method of described compound silver powder, may further comprise the steps:
1) preparation contains the solution of silver nitrate, also contains acid corresponding to nonmetal oxide in metal oxide is corresponding in the vitreum metal nitrate and the vitreum in the described solution;
2) with step 1) solution by air-blast atomizing, 800-1200 ℃ of lower sintering obtains described compound silver powder.
At last, the present invention also provides a kind of conductive silver paste, contains silver powder and organic carrier in the described conductive silver paste; Wherein said silver powder is compound silver powder provided by the invention.
Compound silver powder of the present invention is nucleocapsid structure, and wherein nuclear material is silver-colored particle, and shell material is vitreum, and namely vitreum is coated on silver-colored particle surface, can effectively prevent silver-colored particle agglomeration, and therefore compound silver powder of the present invention has good dispersiveness.In addition, compound silver powder of the present invention is used for conductive silver paste, and during sintering, the vitreum of shell material softens melting, and homodisperse silver powder fully contacts with silicon substrate, and electrode is continuous, and contact resistance greatly reduces, so conductivity is very high.The preparation method of compound silver powder provided by the invention, technique are very simple.
Description of drawings
Fig. 1 is the TEM figure of compound silver powder of the present invention.
Embodiment
The invention provides a kind of compound silver powder, described compound silver powder is nucleocapsid structure, and wherein nuclear material is silver-colored particle, and shell material is vitreum; The particle diameter of silver particle is 1-3 μ m.The particle diameter of silver particle can be measured by transmission electron microscope.
Compound silver powder of the present invention is nucleocapsid structure, as shown in Figure 1; By high-resolution-ration transmission electric-lens HRTEM, find that nuclear material is silver-colored particle, shell material is vitreum, namely vitreum coats and silver-colored particle surface.In the compound silver powder of the present invention, vitreum is coated on silver-colored particle surface, can effectively prevent silver-colored particle agglomeration, and therefore compound silver powder of the present invention has good dispersiveness.When adopting compound silver powder of the present invention to prepare electrocondution slurry, conductivity is very good.
The present inventor thinks: contain the conductive silver paste of compound silver powder of the present invention in sintering process, the shell material vitreum elder generation melting of compound silver powder, and sink under the silver powder, wetting, as to corrode and penetrate silicon substrate surface antireflective coating, the silicon generation redox reaction on vitreum and silicon substrate surface, the vitreum Partial Conversion is simple substance; This simple substance contacts with silver powder, and silver powder melting speed is accelerated, and melts altogether body with vitreum generation Ag-glass; Subsequently, Ag-glass melts altogether body and contacts with silicon substrate, and Ag separates with glass, and recrystallization fully contacts with silicon substrate at silicon face, thereby increases conductivity.
Vitreum of the present invention is to well known to a person skilled in the art the class material with glassy phase that is formed by multiple inorganic oxide pre-burning.For example, contain SiO in the described vitreum
2, B
2O
3, Bi
2O
3, CaO, BaO, ZnO, Al
2O
3, TiO
2, ZrO
2, CuO, PbO one or more.Under the preferable case, for improving the conductivity of conductive silver paste, take Vitrea gross mass as benchmark, contain 10-15%ZnO in the described glass dust, 70-75%Bi
2O
3, surplus is BaO and Al
2O
3
In the compound silver powder of the present invention, silver powder is similar to the proportion of glass dust in the conductive silver paste of silver-colored particle and Vitrea proportion and prior art, does not have specific (special) requirements among the present invention.For example, take the gross mass of compound silver powder as benchmark, the content of silver-colored particle is 93-99%, and Vitrea content is 1-7%.
The particle diameter of compound silver powder of the present invention is 1.2-3.1 μ m.
The invention provides the preparation method of described compound silver powder, may further comprise the steps:
1) preparation contains the solution of silver nitrate, also contains acid corresponding to nonmetal oxide in metal oxide is corresponding in the vitreum metal nitrate and the vitreum in the described solution;
2) with step 1) solution by air-blast atomizing, 800-1200 ℃ of lower sintering obtains described compound silver powder.
According to preparation method provided by the invention, by preparing first the mixed solution of the corresponding ion of inorganic oxide in silver ion and the vitreum, silver ion is evenly mixed with the various inorganic ions in the vitreum are first, then under atomize, carry out high temperature sintering; In the sintering process, the ion in the solution generates first corresponding oxide, various oxide Uniform Dispersions; Temperature continues to raise, and other various oxide meltings also form vitreum, are dispersed in around the silver oxide; Temperature reaches the heat decomposition temperature of silver oxide, and the silver oxide thermal decomposition obtains silver-colored particle, and vitreum evenly is coated on around the silver-colored particle, thereby obtains compound silver powder of the present invention.
As previously mentioned, vitreum is formed by multiple inorganic oxide pre-burning, has both contained metal oxide in the described inorganic oxide and has also contained nonmetal oxide.For example, described metal oxide is ZnO, Bi
2O
3, BaO, Al
2O
3, the metal nitrate that then described metal oxide is corresponding is followed successively by Zn (NO
3)
2, Bi (NO
3)
3, Ba (NO
3)
2, Al (NO
3)
3Described nonmetal oxide is B
2O
3, SiO
2, the acid that then nonmetal oxide is corresponding and derivative thereof are H
3BO
3, H
2SiO
3, H
4SiO
4Or various esters of silicon acis.
In the solute of solution, the content of silver nitrate is 95.3-99.4wt%, and the total content of the acid that nonmetal oxide is corresponding in the metal nitrate that metal oxide is corresponding in the vitreum and the vitreum is 0.6-4.7wt%.
Among the present invention, solution carries out sintering under the air-blast atomizing state.Generally speaking, for reducing energy consumption, the flow of solution can not be too little; On the other hand, abundant for guaranteeing the various ion sintering in the solution, the flow of solution can not be too large.Under the preferable case, the flow of solution is 5-20ml/min during air-blast atomizing.
The carrier gas of air-blast atomizing can be adopted and well known to a person skilled in the art various inert gases, silver powder oxidation when preventing high temperature.Among the present invention, nitrogen is preferably adopted in carrier gas.More preferably in the situation, the flow of nitrogen is 2-20L/min.
Among the present invention, can adopt temperature programming to the sintering of the solution under the air-blast atomizing state, the highest sintering temperature need reach more than the heat decomposition temperature of silver oxide, guarantees the generation of silver-colored particle.Sintering temperature of the present invention is 800-1200 ℃, is preferably 1000-1100 ℃.The time of sintering is 15-45s, is preferably 20-30s.
Compound silver powder of the present invention because silver-colored particle is coated by vitreum, reduces the reunion of silver-colored particle greatly, and silver powder very easily disperses.In addition, in the compound silver powder of the present invention, silver-colored particle surface is coated with vitreum, so when the preparation conductive silver paste, need not to add glass dust, only needs directly compound silver powder to be dispersed in the organic carrier to get final product again.
Therefore, the invention provides a kind of conductive silver paste, contain silver powder and organic carrier in the described conductive silver paste; Silver powder wherein is compound silver powder provided by the invention.
As those skilled in the art's common practise, take the gross mass of conductive silver paste as benchmark, the content of silver powder is 80-90%, and the content of organic carrier is 10-20%.Described organic carrier is for well known to a person skilled in the art various organic carriers, such as thinking epoxy resin, diethanol glycidol ether etc.
Below in conjunction with embodiment and Comparative Examples the present invention is further explained.The raw material that adopts in embodiment and the Comparative Examples all is available commercially.
Embodiment 1
Present embodiment is used for illustrating compound silver powder provided by the invention and preparation method thereof.
(1) normal temperature obtain solution: get silver nitrate 120g, add the liquor argenti nitratis ophthalmicus that deionized water is made into 0.7mol/L, continue to add 1.4g Zn (NO
3)
2, 5g Bi (NO
3)
3, 0.12g Ba (NO
3)
2With 0.28g Al (NO
3)
3, and mix.
(2) solution of step (1) preparation is changed in the spray generator, it is 20ml/min that the adjustment jet size makes liquid inventory, and the nitrogen carrier gas amount is 10L/min; Jet expansion is connected to quartz ampoule, and it is 1000 ℃ that resistance heating makes the interior temperature of quartz ampoule, after spraying is finished, continues sintering 30s, and cooling obtains the compound silver powder of present embodiment, is designated as A1, and wherein silver-colored particle and Vitrea mass ratio are 95: 5.
Embodiment 2
Adopt the step identical with embodiment 1 to prepare compound silver powder, difference is:
In the step (1), add 1.33g Zn (NO
3)
2, 6.78g Bi (NO
3)
3, 0.27g Ba (NO
3)
2And 0.67gAl (NO
3)
3
By above-mentioned steps, obtain the compound silver powder of present embodiment, be designated as A2, wherein silver-colored particle and Vitrea mass ratio are 93: 7.
Embodiment 3
Adopt the step identical with embodiment 1 to prepare compound silver powder, difference is:
In the step (1), add 0.21g Zn (NO
3)
2, 0.95g Bi (NO
3)
3, 0.02g Ba (NO
3)
2And 0.07gAl (NO
3)
3
By above-mentioned steps, obtain the compound silver powder of present embodiment, be designated as A3, wherein silver-colored particle and Vitrea mass ratio are 99: 1.
Embodiment 4
Adopt the step identical with embodiment 1 to prepare compound silver powder, difference is:
In the step (2), liquid inventory is 10ml/min, and the nitrogen carrier gas amount is 20L/min; Temperature is 800 ℃ in the quartz ampoule, and the time of continuing sintering is 30s.
By above-mentioned steps, obtain the compound silver powder of present embodiment, be designated as A4, wherein silver-colored particle and Vitrea mass ratio are 95: 5.
Embodiment 5
Present embodiment is used for illustrating conductive silver paste provided by the invention and preparation method thereof.
(1) preparation organic carrier: E-51 epoxy resin: 7 weight portions;
6458 epoxy resin: 6 weight portions;
Diethanol and glycidol ether: 2 weight portions;
Benzyl dimethylamine modifier: 0.05 weight portion.
(2) be to mix at 85: 15 the compound silver powder A1 of embodiment 1 preparation and organic carrier according to mass ratio, obtain the conductive silver paste of present embodiment, be designated as S1.
Embodiment 6-8
Adopt the step identical with embodiment 5 to prepare conductive silver paste S2-S4, difference is:
Adopt respectively the A1 among the compound silver powder A2-A4 replacement embodiment 1 in the step (2), the conductive silver paste that obtains is designated as S2-S4 successively.
Comparative Examples 1
Adopt the step identical with embodiment 5 to prepare the conductive silver paste DS1 of this Comparative Examples, difference is:
In the step (2), be 1.2 μ m silver powder, organic carrier and glass dust (12%ZnO, 75%Bi with particle diameter
2O
3, 3%B
2O
3And 3%BaO, 2%Al
2O
3, 5%SiO
2) be to mix at 81: 4: 15 according to mass ratio.
By above-mentioned steps, obtain the conductive silver paste of this Comparative Examples, be designated as DS1.
Comparative Examples 2
Adopt the step identical with embodiment 5 to prepare the conductive silver paste DS2 of this Comparative Examples, difference is:
In the step (2), adopt the A1 among the silver coating glass dust replacement embodiment 1 among the CN1290121C embodiment 1, the conductive silver paste that obtains is designated as DS2 successively.
Performance test:
1, silver-colored grain diameter test in the compound silver powder:
Adopt the particle diameter of silver-colored particle among transmission electron microscope (JEM-2010 (HT), NEC) the test compound silver powder A1-A4.Test result is as shown in table 1.
2, the dispersed test of silver powder in the conductive silver paste:
Adopt Hegman grind gage to come the scraper plate fineness of silver powder among testing conductive silver slurry S1-S4 and the DS1-DS2.Test result is as shown in table 1.
3, conductive silver paste conductivity test:
Adopt " wetability of glass dust is on the impact of silicon solar cell performance ", Zhang Yaping etc., the disclosed step of the preparation of the 36th volume the 7th phases 1.3 battery (the 2nd page left hurdle the 5th section) prepares the solar cell silicon substrate, and wherein the silver slurry adopts respectively conductive silver paste S1-S4 and the DS1-DS2 of embodiment and Comparative Examples preparation; Adopt the Shanghai single flash operation solar cell tester model HSC1 of He Shuan Thermo-Solar Energietechnik GmbH, test the electricity conversion of each solar cell silicon substrate.Test result is as shown in table 1.
Table 1
| Compound silver powder | Silver grain diameter/μ m | Electrocondution slurry | Scraper plate fineness/μ m | Electricity conversion/% |
| A1 | 1.4 | S1 | 16 | 17.03 |
| A2 | 1.3 | S2 | 15 | 16.86 |
| A3 | 1.5 | S3 | 15 | 16.91 |
| A4 | 1.0 | S4 | 12 | 16.95 |
| - | - | DS1 | 20 | 16.21 |
| - | - | DS2 | 19 | 15.90 |
Can find out that from the test result of table 1 particle diameter of the middle silver-colored particle of compound silver powder of the present invention is 1-3 μ m.
The test result of S1-S4 and DS1-DS2 relatively can be found out in the table 1, and the scraper plate fineness of silver-colored particle is significantly less than Comparative Examples in the electrocondution slurry provided by the invention, illustrates that the compound silver powder of silica has dispersed preferably in the electrocondution slurry of the present invention.In addition, adopt electrocondution slurry of the present invention preparation the solar cell silicon substrate electricity conversion up to 16.86 and more than, and the conductive silver paste DS1 of Comparative Examples 1 to be used for the electricity conversion of solar cell silicon substrate only be 16.21, the electricity conversion that the conductive silver paste DS2 of Comparative Examples 2 is used for the solar cell silicon substrate is 15.90; The conductivity that conductive silver paste of the present invention is described obviously is better than various conductive silver paste of the prior art.
Claims (12)
1. a compound silver powder is characterized in that, described compound silver powder is nucleocapsid structure, and wherein nuclear material is silver-colored particle, and shell material is vitreum; The particle diameter of silver particle is 1-3 μ m.
2. compound silver powder according to claim 1 is characterized in that, take Vitrea gross mass as benchmark, contains 10-15%ZnO in the described vitreum, 70-75%Bi
2O
3, surplus is BaO and Al
2O
3
3. compound silver powder according to claim 1 and 2 is characterized in that, take the gross mass of compound silver powder as benchmark, the content of silver-colored particle is 93-99%, and Vitrea content is 1-7%.
4. compound silver powder according to claim 1 is characterized in that, the particle diameter of described compound silver powder is 1.2-3.1 μ m.
5. the preparation method of compound silver powder claimed in claim 1 may further comprise the steps:
1) preparation contains the solution of silver nitrate, also contains corresponding acid and the derivative thereof of nonmetal oxide in metal oxide is corresponding in the vitreum metal nitrate and the vitreum in the described solution;
2) with step 1) solution by air-blast atomizing, 800-1200 ℃ of lower sintering obtains described compound silver powder.
6. method according to claim 5 is characterized in that, take Vitrea gross mass as benchmark, contains 10-15%ZnO in the described vitreum, 70-75%Bi
2O
3, 1-5%B
2O
3, surplus is BaO, Al
2O
3And SiO
2
7. method according to claim 5, it is characterized in that, the content of silver nitrate is 95.3-99.4wt% in the solute of solution, and the total content of the acid that nonmetal oxide is corresponding in the metal nitrate that metal oxide is corresponding in the vitreum and the vitreum is 0.6-4.7wt%.
8. method according to claim 5 is characterized in that, the flow of solution is 5-20ml/min during air-blast atomizing.
9. method according to claim 5 is characterized in that, the carrier gas of air-blast atomizing is nitrogen, and nitrogen flow is 2-20L/min.
10. method according to claim 5 is characterized in that, sintering temperature is 1000-1100 ℃, and sintering time is 15-45s.
11. a conductive silver paste contains silver powder and organic carrier in the described conductive silver paste; It is characterized in that described silver powder is compound silver powder claimed in claim 1.
12. conductive silver paste according to claim 11 is characterized in that, take the gross mass of conductive silver paste as benchmark, the content of compound silver powder is 80-90%, and the content of organic carrier is 10-20%.
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|---|---|---|---|
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| CN102347091B true CN102347091B (en) | 2013-03-27 |
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| CN104318978B (en) * | 2014-10-25 | 2017-05-10 | 苏州华琼电子材料有限公司 | Electro-conductive paste with core shell conductive particles and preparation method thereof |
| CN104575672A (en) * | 2014-12-23 | 2015-04-29 | 合肥中南光电有限公司 | Conductive silver paste taking coating silver powder as main material |
| JP6209666B1 (en) * | 2016-12-02 | 2017-10-04 | 田中貴金属工業株式会社 | Conductive bonding material and method for manufacturing semiconductor device |
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| CN1655285A (en) * | 2005-03-08 | 2005-08-17 | 东南大学 | Photosensitive silver slurry for concentration electrode and method for preparing same |
| CN2786773Y (en) * | 2005-03-15 | 2006-06-07 | 东南大学 | Glass particle for conflux electrode silver slurry material |
| CN101045828A (en) * | 2006-07-03 | 2007-10-03 | 张义纲 | Phosphate film-coated powder and preparation method thereof |
| CN101295586A (en) * | 2008-06-11 | 2008-10-29 | 中国科学院上海硅酸盐研究所 | Production method of nanocrystalline TiO2 solar battery prototype device |
| CN101712076A (en) * | 2009-11-17 | 2010-05-26 | 武汉理工大学 | Preparation method as well as application of novel electromagnetic shielding filler |
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| US7132922B2 (en) * | 2002-04-08 | 2006-11-07 | Littelfuse, Inc. | Direct application voltage variable material, components thereof and devices employing same |
| CN1780729A (en) * | 2003-02-25 | 2006-05-31 | 曼弗雷德·R·库赫奈利 | Encapsulated nanoparticles for the absorption of electromagnetic energy |
| US20090068089A1 (en) * | 2007-09-08 | 2009-03-12 | Quaid-E-Azam University | Novel method of manufacture of silver oxide nano particles |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1655285A (en) * | 2005-03-08 | 2005-08-17 | 东南大学 | Photosensitive silver slurry for concentration electrode and method for preparing same |
| CN2786773Y (en) * | 2005-03-15 | 2006-06-07 | 东南大学 | Glass particle for conflux electrode silver slurry material |
| CN101045828A (en) * | 2006-07-03 | 2007-10-03 | 张义纲 | Phosphate film-coated powder and preparation method thereof |
| CN101295586A (en) * | 2008-06-11 | 2008-10-29 | 中国科学院上海硅酸盐研究所 | Production method of nanocrystalline TiO2 solar battery prototype device |
| CN101712076A (en) * | 2009-11-17 | 2010-05-26 | 武汉理工大学 | Preparation method as well as application of novel electromagnetic shielding filler |
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Inventor after: Ao Yiwei Inventor after: Yan Haiyong Inventor after: Jiang Ansong Inventor before: Peng Changchun Inventor before: Zhou Wei |
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Effective date of registration: 20170105 Address after: 213000 Hsinchu New District, Jiangsu, North Road, No. two, No. 88, No. Patentee after: CHANGZHOU JUHE NEW MATERIAL CO., LTD. Address before: BYD 518118 Shenzhen Road, Guangdong province Pingshan New District No. 3009 Patentee before: BYD Co. Ltd. |