CN105761778B - A kind of preparation method of low temperature curing type conductive silver paste - Google Patents

A kind of preparation method of low temperature curing type conductive silver paste Download PDF

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CN105761778B
CN105761778B CN201610253683.0A CN201610253683A CN105761778B CN 105761778 B CN105761778 B CN 105761778B CN 201610253683 A CN201610253683 A CN 201610253683A CN 105761778 B CN105761778 B CN 105761778B
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CN105761778A (en
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刘玉洁
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Guangdong Jinwu New Material Technology Co ltd
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Wuxi Nanligong Technology Development Co Ltd
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    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01BCABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B1/00Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
    • H01B1/20Conductive material dispersed in non-conductive organic material
    • H01B1/22Conductive material dispersed in non-conductive organic material the conductive material comprising metals or alloys
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01BCABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B13/00Apparatus or processes specially adapted for manufacturing conductors or cables
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01LSEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L31/00Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
    • H01L31/02Details
    • H01L31/0224Electrodes
    • H01L31/022408Electrodes for devices characterised by at least one potential jump barrier or surface barrier
    • H01L31/022425Electrodes for devices characterised by at least one potential jump barrier or surface barrier for solar cells

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  • Engineering & Computer Science (AREA)
  • Manufacturing & Machinery (AREA)
  • Physics & Mathematics (AREA)
  • Chemical & Material Sciences (AREA)
  • Dispersion Chemistry (AREA)
  • Spectroscopy & Molecular Physics (AREA)
  • Conductive Materials (AREA)

Abstract

The present invention relates to a kind of preparation methods of low temperature curing type conductive silver paste, include the following steps:(1)Raw material is weighed in proportion, it is spare;(2)Nano-silver powder and nanometer aluminium powder are put into ball mill, ground while stirring, nano-silver powder and nanometer aluminium powder is made to be uniformly mixed, and the grain size of mixed-powder is less than 100nm, it is spare;(3)Thermoplastic resin, additive and solvent are put into a mixing bowl and dissolved, and heating stirring, heating temperature is 80 ~ 90 DEG C, and mixing speed is 600 ~ 800 r/min, and stirring and heating time are 2 ~ 3h;(4)By step(2)In mixed-powder be added a mixing bowl, continue heating stirring, heating temperature be 40 ~ 60 DEG C, mixing speed be 2600 ~ 3500 r/min, stirring and heating time be 4 ~ 6h;It is mixed into paste-like, then low-temperature cured conductive silver paste is made;The preparation process is simple, and operability is strong, and productivity is high.

Description

A kind of preparation method of low temperature curing type conductive silver paste
Technical field
The present invention relates to a kind of field of new energy technologies, more particularly to a kind of preparation side of low temperature curing type conductive silver paste Method.
Background technology
Solar energy is a kind of inexhaustible, nexhaustible clean type energy, with non-renewable energy resources such as coal, oil Increasingly depleted, exploitation becomes big hot spot using solar energy, and solar cell is exactly a kind of important means using solar energy.
Currently, crystal silicon solar batteries technology is increasingly ripe, transfer efficiency is close to 20%;Most researchers are all being ground The transfer efficiency for how improving solar cell studied carefully;It is 29% that silicon/crystalline silicon heterojunction solar battery theoretical calculation, which goes out its transfer efficiency, Between the transfer efficiency for the silicon/crystalline silicon heterojunction solar battery produced at present is 22 ~ 23%, the transfer efficiency in laboratory is then up to 25%, and the temperature tolerance of the silicon/crystalline silicon heterojunction solar battery and stability are better than common crystal silicon solar batteries, mainly Because the electrode of silicon/crystalline silicon heterojunction solar battery is to use low-temperature conductive silver slurry, and the slurry of electrode influence crystal silicon is heterogeneous The fill factor of joint solar cell, to influence its transfer efficiency;There are many method for manufacturing electrode, and silk-screen printing and cofiring are A kind of presently the most universal production technology.Silicon/crystalline silicon heterojunction solar battery conductive slurry for front electrode and backplate are equal Conductive silver paste is coated on battery by silk-screen printing and positive and negative electrode is formed on silicon chip two sides by low-temperature sintering;Cofiring The electrode of silicon/crystalline silicon heterojunction solar battery after knot must adhesion-tight, do not fall ash, silicon chip is unlikely to deform, and is easy to weld It connects, convenient for the electric current collection for being generated illumination with conducting wire and export.Most of low-temperature conductive silver paste is due to its viscosity at present And the properties such as electric conductivity cause the fill factor of silicon/crystalline silicon heterojunction solar battery not high, it is therefore necessary to develop a kind of raising The low-temperature cured conductive silver paste of the fill factor of solar cell.
Invention content
The technical problem to be solved by the present invention is to provide a kind of preparation method of low temperature curing type conductive silver paste.
To solve the above-mentioned problems, the technical solution adopted by the present invention is the preparation of the low temperature curing type conductive silver paste Method, each component being formulated are by weight:86 ~ 92wt% of nano-silver powder, 0.5 ~ 2wt% of nanometer aluminium powder, thermoplastic resin 2 ~ 4wt%, additive 0.1 ~ 2 wt%, 1 ~ 10wt% of solvent.
Further improvement lies in that each component of formula is by weight:Nano-silver powder 92wt%, nanometer aluminium powder 0.5wt%, Thermoplastic resin 2wt%, additive 0.5 wt%, solvent 5wt%.
Further improvement lies in that the solvent is butyl carbitol acetate or/and butyl carbitol.
Further improvement lies in that thermoplastic resin takes polyamide with polycarbonate resin according to mass ratio 3: 97~10:The mixture of 90 mixing.
Further improvement lies in that the nano-silver powder is ball shape silver powder, the median particle size D50=50- of the ball shape silver powder 200nm。
Further improvement lies in that the additive is imidazole curing agent.
Using above-mentioned technical proposal, the preparation method of obtained low temperature curing type conductive silver paste have low-temperature setting and Hardening time is short, and the electrode depth-width ratio of obtained solar cell is big, improves the fill factor of solar cell, to carry The high transfer efficiency of solar cell.
The technical problem to be solved by the present invention is to provide a kind of preparation method of low temperature curing type conductive silver paste, make Standby simple for process, operability is strong, and productivity is high and using the preparation of the low temperature curing type conductive silver paste prepared by this method Method is at low cost, and yield is big, suitable for being commercially widely popularized.
To solve the above-mentioned problems, the technical solution adopted by the present invention is the preparation of the low temperature curing type conductive silver paste Method includes the following steps:
(1)Raw material is weighed in proportion, it is spare;
(2)Nano-silver powder and nanometer aluminium powder are put into ball mill, ground while stirring, keeps nano-silver powder and nanometer aluminium powder mixed It closes uniformly, and the grain size of mixed-powder is less than 100nm, it is spare;
(3)Thermoplastic resin, additive and solvent are put into a mixing bowl and dissolved, and heating stirring, heating temperature be 80 ~ 90 DEG C, mixing speed is 600 ~ 800 r/min, and stirring and heating time are 2 ~ 3h;
(4)By step(2)In mixed-powder be added a mixing bowl, continue heating stirring, heating temperature be 40 ~ 60 DEG C, stir It is 2600 ~ 3500 r/min to mix speed, and stirring and heating time are 4 ~ 6h;It is mixed into paste-like, then low-temperature setting is made Conductive silver paste.
Specific implementation mode
Embodiment 1:The low temperature curing type conductive silver paste, each component being formulated are by weight:Nano-silver powder 92wt%, nanometer aluminium powder 0.5wt%, thermoplastic resin 2wt%, additive 0.5 wt%, solvent 5wt%;The solvent is that butyl card must Alcohol acetate;Thermoplastic resin takes polyamide with polycarbonate resin according to mass ratio 6:The mixture of 94 mixing; The nano-silver powder is ball shape silver powder, the median particle size D50=50-200nm of the ball shape silver powder;The additive is imidazoles Curing agent.
The preparation method of the low temperature curing type conductive silver paste, includes the following steps:
(1)Raw material is weighed in proportion, it is spare;
(2)Nano-silver powder and nanometer aluminium powder are put into ball mill, ground while stirring, keeps nano-silver powder and nanometer aluminium powder mixed It closes uniformly, and the grain size of mixed-powder is less than 100nm, it is spare;
(3)Thermoplastic resin, additive and solvent are put into a mixing bowl and dissolved, and heating stirring, heating temperature 80 DEG C, mixing speed is 700 r/min, and stirring and heating time are 2.5h;
(4)By step(2)In mixed-powder be added a mixing bowl, continue heating stirring, heating temperature be 50 DEG C, stirring speed Degree is 3000 r/min, and stirring and heating time are 5h;It is mixed into paste-like, then low-temperature cured conductive silver paste is made.
Embodiment 2:The low temperature curing type conductive silver paste, each component being formulated are by weight proportion:Nano-silver powder 86wt%, nanometer aluminium powder 2wt%, thermoplastic resin 4wt%, additive 2 wt%, solvent 6wt%;The solvent is butyl carbitol; Thermoplastic resin takes polyamide with polycarbonate resin according to mass ratio 3:The mixture of 97 mixing;The nanometer Silver powder is ball shape silver powder, the median particle size D50=50-200nm of the ball shape silver powder;The additive is imidazole curing agent.
The preparation method of the low temperature curing type conductive silver paste, includes the following steps:
(1)Raw material is weighed in proportion, it is spare;
(2)Nano-silver powder and nanometer aluminium powder are put into ball mill, ground while stirring, keeps nano-silver powder and nanometer aluminium powder mixed It closes uniformly, and the grain size of mixed-powder is less than 100nm, it is spare;
(3)Thermoplastic resin, additive and solvent are put into a mixing bowl and dissolved, and heating stirring, heating temperature 90 DEG C, mixing speed is 800 r/min, and stirring and heating time are 2h;
(4)By step(2)In mixed-powder be added a mixing bowl, continue heating stirring, heating temperature be 60 DEG C, stirring speed Degree is 3500 r/min, and stirring and heating time are 4h;It is mixed into paste-like, then low-temperature cured conductive silver paste is made.
Embodiment 3:The low temperature curing type conductive silver paste, each component being formulated are by weight proportion:Nano-silver powder 90wt%, nanometer aluminium powder 1wt%, thermoplastic resin 3wt%, additive 1 wt%, solvent 5wt%;The solvent is butyl carbitol vinegar Acid esters and butyl carbitol;Thermoplastic resin takes polyamide with polycarbonate resin according to mass ratio 10:90 is mixed The mixture of conjunction;The nano-silver powder is ball shape silver powder, the median particle size D50=50-200nm of the ball shape silver powder;It is described to add It is imidazole curing agent to add agent.
The preparation method of the low temperature curing type conductive silver paste, includes the following steps:
(1)Raw material is weighed in proportion, it is spare;
(2)Nano-silver powder and nanometer aluminium powder are put into ball mill, ground while stirring, keeps nano-silver powder and nanometer aluminium powder mixed It closes uniformly, and the grain size of mixed-powder is less than 100nm, it is spare;
(3)Thermoplastic resin, additive and solvent are put into a mixing bowl and dissolved, and heating stirring, heating temperature 85 DEG C, mixing speed is 600 r/min, and stirring and heating time are 3h;
(4)By step(2)In mixed-powder be added a mixing bowl, continue heating stirring, heating temperature be 40 DEG C, stirring speed Degree is 2600r/min, and stirring and heating time are 6h;It is mixed into paste-like, then low-temperature cured conductive silver paste is made.
Silver paste is led using the low temperature obtained by above-described embodiment, the silicon/crystalline silicon heterojunction sun is applied to using silk-screen printing technique After energy battery, fill factor:1 > embodiments of embodiment, 3 > embodiments 2.
Finally, it should also be noted that it is listed above be only the present invention several specific embodiments.Obviously, this hair Bright to be not limited to above example, acceptable there are many deformations.Those skilled in the art can be from present disclosure All deformations for directly exporting or associating, are considered as protection scope of the present invention.

Claims (1)

1. a kind of preparation method of low temperature curing type conductive silver paste, includes the following steps:
(1) raw material is weighed in proportion, it is spare;
(2) nano-silver powder and nanometer aluminium powder are put into ball mill, ground while stirring, so that nano-silver powder and nanometer aluminium powder is mixed equal It is even, and the grain size of mixed-powder is less than 100nm, it is spare;
(3) thermoplastic resin, additive and solvent are put into a mixing bowl and are dissolved, and heating stirring, heating temperature is 80~90 DEG C, mixing speed is 600~800r/min, and stirring and heating time are 2~3h;
(4) a mixing bowl is added in the mixed-powder in step (2), continues heating stirring, heating temperature is 40~60 DEG C, stirring speed Degree is 2600~3500r/min, and stirring and heating time are 4~6h;It is mixed into paste-like, then low-temperature cured conductive is made Silver paste;It is formulated each component be by weight:86~92wt% of nano-silver powder, 0.5~2wt% of nanometer aluminium powder, thermoplasticity 2~4wt% of resin, 0.1~2wt% of additive, 1~10wt% of solvent;The solvent is butyl carbitol acetate or/and fourth Base carbitol;Thermoplastic resin takes polyamide with polycarbonate resin according to mass ratio 3:97~10:90 mixing Mixture;The additive is imidazole curing agent.
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US9972740B2 (en) 2015-06-07 2018-05-15 Tesla, Inc. Chemical vapor deposition tool and process for fabrication of photovoltaic structures
US9748434B1 (en) 2016-05-24 2017-08-29 Tesla, Inc. Systems, method and apparatus for curing conductive paste
US9954136B2 (en) 2016-08-03 2018-04-24 Tesla, Inc. Cassette optimized for an inline annealing system
US10115856B2 (en) 2016-10-31 2018-10-30 Tesla, Inc. System and method for curing conductive paste using induction heating
CN107978384A (en) * 2017-11-27 2018-05-01 西安工程大学 A kind of electrocondution slurry aerosol and preparation method thereof
CN114220587A (en) * 2021-11-23 2022-03-22 苏州思尔维纳米科技有限公司 Auxiliary agent for low-temperature silver paste and preparation method and application thereof

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KR20100029652A (en) * 2008-09-08 2010-03-17 주식회사 에프피 Low temperature dryable conductive paste composite for solar cell and printing method using the same
JP2011006740A (en) * 2009-06-25 2011-01-13 Mitsui Mining & Smelting Co Ltd Copper powder for conductive paste, and conductive paste
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CN104751942A (en) * 2015-04-23 2015-07-01 江苏欧耐尔新型材料有限公司 Lead-free conductive paste for filament screen printing of solar cells and preparation method of lead-free conductive paste

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KR20100029652A (en) * 2008-09-08 2010-03-17 주식회사 에프피 Low temperature dryable conductive paste composite for solar cell and printing method using the same
JP2011006740A (en) * 2009-06-25 2011-01-13 Mitsui Mining & Smelting Co Ltd Copper powder for conductive paste, and conductive paste
CN102470436A (en) * 2009-10-02 2012-05-23 户田工业株式会社 Fine silver particles, method for producing same, conductive paste containing the fine silver particles, conductive film, and electronic device
CN104010752A (en) * 2011-12-28 2014-08-27 户田工业株式会社 Silver fine particles, production process therefor, conductive paste, conductive membrane and electronic device, containing said silver fine particles
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