CN112809019A - Preparation method of silver powder for low-temperature silver paste of heterojunction solar cell - Google Patents

Preparation method of silver powder for low-temperature silver paste of heterojunction solar cell Download PDF

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Publication number
CN112809019A
CN112809019A CN202110175583.1A CN202110175583A CN112809019A CN 112809019 A CN112809019 A CN 112809019A CN 202110175583 A CN202110175583 A CN 202110175583A CN 112809019 A CN112809019 A CN 112809019A
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silver powder
low
silver
temperature
solar cell
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CN202110175583.1A
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CN112809019B (en
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孙立志
唐飞勇
杨华明
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Shenzhen Hongdarui Technology Co ltd
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Shenzhen Hongdarui Technology Co ltd
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00Making metallic powder or suspensions thereof
    • B22F9/16Making metallic powder or suspensions thereof using chemical processes
    • B22F9/18Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
    • B22F9/24Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/06Metallic powder characterised by the shape of the particles
    • B22F1/068Flake-like particles
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/14Treatment of metallic powder
    • B22F1/142Thermal or thermo-mechanical treatment
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00Making metallic powder or suspensions thereof
    • B22F9/02Making metallic powder or suspensions thereof using physical processes
    • B22F9/04Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00Making metallic powder or suspensions thereof
    • B22F9/02Making metallic powder or suspensions thereof using physical processes
    • B22F9/04Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
    • B22F2009/042Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling using a particular milling fluid
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00Making metallic powder or suspensions thereof
    • B22F9/02Making metallic powder or suspensions thereof using physical processes
    • B22F9/04Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
    • B22F2009/043Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by ball milling

Abstract

The invention provides a preparation method of silver powder for low-temperature silver paste of a heterojunction solar cell. Firstly, preparing spherical silver powder by a chemical method, then dissociating a silver powder coating layer by a ball milling method to simultaneously prepare flaky silver powder, and finally, carrying out low-temperature annealing treatment, crushing and sieving to prepare the silver powder for the low-temperature silver paste of the heterojunction solar cell. The prepared silver powder has good conductivity and strong activity, and the preparation conditions are mild, the period is short, the efficiency is high, the process is simple, the requirement on equipment is low, and the large-scale industrial production is easy to realize.

Description

Preparation method of silver powder for low-temperature silver paste of heterojunction solar cell
Technical Field
The invention mainly relates to a preparation method of silver powder for electronic conductive paste, and particularly relates to a preparation method of silver powder for low-temperature silver paste of a heterojunction solar cell.
Background
Among the structural costs of the solar cell, the silver paste for the solar cell is the most important material affecting the cost of the solar cell, in addition to the silicon material. The traditional crystalline silicon battery usually adopts high-temperature silver paste and has better conductivity, while the heterojunction battery adopts a low-temperature process and needs to use low-temperature conductive silver paste. The low-temperature conductive paste is poorer in conductivity and printing performance than the high-temperature conductive paste, so that the paste weight of the heterojunction solar cell is increased greatly, the cost is high, and the industrial development of the silver paste of the heterojunction solar cell is limited. At present, the reason for influencing the conductivity of the silver paste of the heterojunction solar cell is mainly that the surface of the silver powder is coated with a layer of organic dispersant, the silver powder cannot be dissociated under the low-temperature process condition, the conductivity of an electrode is greatly lowered, and the efficiency of the cell is influenced.
In view of the above, a special method for dissociating silver powder coating layers at low temperature is adopted, targeted innovation is performed aiming at the defects of other methods, and silver powder for the low-temperature silver paste of the heterojunction solar cell, which is good in conductivity and strong in activity, is prepared.
Disclosure of Invention
The invention aims to provide a method for preparing silver powder for low-temperature silver paste of a heterojunction solar cell, aiming at the defect of poor conductivity of the silver powder prepared by the existing method.
The invention comprises the following steps:
(1) preparing spherical silver powder by a chemical method;
(2) adding spherical silver powder, corundum balls, a dissociating agent and the like into a ball milling tank according to a certain ball material ratio, and obtaining dissociated flake silver powder after ball milling;
(3) preserving the heat of the obtained flaky silver powder at the temperature of 120-180 ℃ for 15-60 minutes;
(4) and crushing and sieving the silver powder after annealing treatment to obtain the silver powder for the low-temperature silver paste of the heterojunction solar cell.
The silver powder prepared by the invention has good conductivity and strong activity, and the preparation conditions are mild, the period is short, the efficiency is high, the process is simple, the requirement on equipment is low, and the large-scale industrial production is easy to realize.
Drawings
FIG. 1 is an X-ray diffraction pattern of a silver powder sample prepared according to the present invention. In fig. 1, the abscissa represents the diffraction angle, and the ordinate represents the diffraction intensity. The lower vertical line is the theoretical diffraction peak position of silver.
DETAILED DESCRIPTION OF EMBODIMENT (S) OF INVENTION
Example 1
Weighing 100g of silver nitrate, dissolving the silver nitrate in 500mL of deionized water to dissolve the silver nitrate, then adding 60g of nucleating agent into a silver nitrate solution in a dropwise manner, adjusting the pH value to 7 after brown precipitates do not appear any more, adding a prepared dispersant solution, and fully stirring; adding a reducing agent for reaction, washing, centrifugally separating and drying after the reaction is completed to obtain the spherical silver powder. And then, adding spherical silver powder, corundum balls, ethanol and acetone into a ball milling tank according to the ball-to-material ratio of 5:3:2:2, and obtaining the dissociated flake silver powder after ball milling. The obtained silver flakes were then incubated at a temperature of 120 ℃ for 15 minutes. And finally, crushing and sieving the silver powder subjected to annealing treatment to obtain the silver powder for the low-temperature silver paste of the heterojunction solar cell.
Example 2
Weighing 100g of silver nitrate, dissolving the silver nitrate in 500mL of deionized water to dissolve the silver nitrate, then adding 60g of nucleating agent into a silver nitrate solution in a dropwise manner, adjusting the pH value to 7 after brown precipitates do not appear any more, adding a prepared dispersant solution, and fully stirring; adding a reducing agent for reaction, washing, centrifugally separating and drying after the reaction is completed to obtain the spherical silver powder. And then, adding spherical silver powder, corundum balls, isopropanol and dilute hydrochloric acid into a ball-milling tank according to the ball-to-material ratio of 5:3:2:2, and carrying out ball milling to obtain the dissociated flake silver powder. The obtained silver flakes were then incubated at a temperature of 140 ℃ for 30 minutes. And finally, crushing and sieving the silver powder subjected to annealing treatment to obtain the silver powder for the low-temperature silver paste of the heterojunction solar cell.
Example 3
Weighing 100g of silver nitrate, dissolving the silver nitrate in 500mL of deionized water to dissolve the silver nitrate, then adding 60g of nucleating agent into a silver nitrate solution in a dropwise manner, adjusting the pH value to 7 after brown precipitates do not appear any more, adding a prepared dispersant solution, and fully stirring; adding a reducing agent for reaction, washing, centrifugally separating and drying after the reaction is completed to obtain the spherical silver powder. And then, adding spherical silver powder, corundum balls, acetone and melamine into a ball milling tank according to the ball-to-material ratio of 5:3:2:2, and obtaining the dissociated flake silver powder after ball milling. The obtained silver flakes were then incubated at a temperature of 160 ℃ for 45 minutes. And finally, crushing and sieving the silver powder subjected to annealing treatment to obtain the silver powder for the low-temperature silver paste of the heterojunction solar cell.
Example 4
Weighing 100g of silver nitrate, dissolving the silver nitrate in 500mL of deionized water to dissolve the silver nitrate, then adding 60g of nucleating agent into a silver nitrate solution in a dropwise manner, adjusting the pH value to 7 after brown precipitates do not appear any more, adding a prepared dispersant solution, and fully stirring; adding a reducing agent for reaction, washing, centrifugally separating and drying after the reaction is completed to obtain the spherical silver powder. And then, adding spherical silver powder, corundum balls, acetone and dilute hydrochloric acid into a ball-milling tank according to the ball-to-material ratio of 5:3:2:2, and carrying out ball milling to obtain dissociated flake silver powder. The obtained silver flakes were then incubated at a temperature of 180 ℃ for 60 minutes. And finally, crushing and sieving the silver powder subjected to annealing treatment to obtain the silver powder for the low-temperature silver paste of the heterojunction solar cell.
The embodiments of the present invention are not limited to the above-mentioned embodiments, and any other embodiments of the present invention can be conceived without departing from the spirit of the invention or with creative efforts, and will fall within the protection scope of the present invention.

Claims (3)

1. A preparation method of silver powder for low-temperature silver paste of a heterojunction solar cell is characterized by firstly preparing spherical silver powder by a chemical method, then dissociating a silver powder coating layer by a ball milling method to simultaneously prepare flaky silver powder, and finally, carrying out low-temperature annealing treatment, crushing and sieving to obtain the silver powder for the low-temperature silver paste of the heterojunction solar cell.
2. The method for preparing silver powder for the low-temperature silver paste of the heterojunction solar cell according to claim 1, wherein the silver powder coating layer is dissociated by the ball milling method by using one or more of ethanol, acetone, isopropanol, dilute hydrochloric acid and melamine as a dissociating agent.
3. The method for preparing silver powder for the low-temperature silver paste of the heterojunction solar cell according to claim 1, wherein the low-temperature annealing treatment temperature is 120-180 ℃ and the time is 15-60 minutes.
CN202110175583.1A 2021-02-07 2021-02-07 Preparation method of silver powder for low-temperature silver paste of heterojunction solar cell Active CN112809019B (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112863733A (en) * 2021-02-05 2021-05-28 苏州思尔维纳米科技有限公司 Low-temperature silver paste for HIT solar cell and preparation method thereof
CN114734033A (en) * 2022-04-14 2022-07-12 宁夏中色新材料有限公司 Flake silver powder suitable for heterojunction solar cell conductive adhesive and preparation method thereof

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CN104475754A (en) * 2014-12-30 2015-04-01 山西森达源科技有限公司 Preparation method of irregular flaky silver powder for silver slurry on back surface of solar cell
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CN105772743A (en) * 2016-05-13 2016-07-20 江苏理工学院 Preparing method for flake silver powder applied to touch screen
CN105817647A (en) * 2016-05-13 2016-08-03 溧阳市立方贵金属材料有限公司 Preparation method for flake sliver powder used for solar rear silver paste
CN108405869A (en) * 2018-04-03 2018-08-17 金川集团股份有限公司 A kind of preparation method of small particle flake silver powder
CN108555312A (en) * 2018-04-19 2018-09-21 湖南省国银新材料有限公司 A kind of preparation method of flake silver powder
CN111145934A (en) * 2019-12-16 2020-05-12 苏州瑞力博新材科技有限公司 Silver paste capable of being stored at room temperature and used for Heterojunction (HIT) solar cell and preparation method

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CN104475754A (en) * 2014-12-30 2015-04-01 山西森达源科技有限公司 Preparation method of irregular flaky silver powder for silver slurry on back surface of solar cell
CN105345012A (en) * 2015-07-20 2016-02-24 昆明贵金属研究所 Preparation method and application for high-conductivity flake-shaped silver powder
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CN111145934A (en) * 2019-12-16 2020-05-12 苏州瑞力博新材科技有限公司 Silver paste capable of being stored at room temperature and used for Heterojunction (HIT) solar cell and preparation method

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112863733A (en) * 2021-02-05 2021-05-28 苏州思尔维纳米科技有限公司 Low-temperature silver paste for HIT solar cell and preparation method thereof
CN112863733B (en) * 2021-02-05 2022-04-26 苏州思尔维纳米科技有限公司 Low-temperature silver paste for HIT solar cell and preparation method thereof
CN114734033A (en) * 2022-04-14 2022-07-12 宁夏中色新材料有限公司 Flake silver powder suitable for heterojunction solar cell conductive adhesive and preparation method thereof

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