CN105817647A - Preparation method for flake sliver powder used for solar rear silver paste - Google Patents
Preparation method for flake sliver powder used for solar rear silver paste Download PDFInfo
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- CN105817647A CN105817647A CN201610322536.4A CN201610322536A CN105817647A CN 105817647 A CN105817647 A CN 105817647A CN 201610322536 A CN201610322536 A CN 201610322536A CN 105817647 A CN105817647 A CN 105817647A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
- B22F2009/042—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling using a particular milling fluid
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
- B22F2009/043—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by ball milling
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
Abstract
The invention relates to a preparation method for flake sliver powder used for solar rear silver paste. The method comprises the following steps that (1) a silver nitrate solution with the concentration being 1-1.5 mol/L is prepared; (2) a sodium hydroxide solution with the mass friction being 5%-10% is added into the silver nitrate solution, and pH is adjusted to be 8-11; (3) a triethanolamine solution is dripped to the silver nitrate solution obtained in the step (2) to obtain silver powder slurry;(4) a stearic acid ethanol solution with the mass friction being 5%-15% is added into the silver powder slurry to serve as a ball milling additive, and ball milling is conducted for 40 h; and (5) powder slurry subjected to ball milling is dried to obtain the flake sliver powder. The flake sliver powder prepared through the method has the low tap density and apparent density, the high specific area and the good dispersing performance, and the comprehensive performance of the flake sliver powder is better when mixed with superfine silver powder for use, the practical application ability of the flake sliver powder is improved, and the flake sliver powder is widely applied to solar rear silver paste. The preparation method is simple, low in production cost, capable of facilitating volume production and suitable for industrial mass production.
Description
Technical field
The present invention relates to the preparation method of a kind of argentum powder, a kind of flake silver powder for solar energy back of the body silver
Preparation method.
Background technology
Solar energy is as a kind of green energy resource, inexhaustible with it, pollution-free, do not limited by resource advantage
Advantage is increasingly subject to people's attention.Electrocondution slurry is the main auxiliary material making silica-based solar cell.
Silica-based solar cell, typically by being printed on silicon cell by electrocondution slurry, is then dried and fires and make
Standby electrode.Electrocondution slurry typically contains conductive metal powder, glass dust and organic carrier.Solar battery back
Used by electrode, electrocondution slurry is generally conductive silver paste, containing 70-85wt% or the most higher flake silver powder,
The price comparison of flake silver powder is expensive, result in the relatively costly of electrocondution slurry.
Conductive silver paste, as an important component part in electronic material, mainly includes curing type conductive silver paste
With slug type conductive silver paste, typically it is made up of argentum powder, organic carrier, binding agent and auxiliary agent etc..Argentum powder conduct
Conducting function phase in conductive silver paste, the physical characteristic such as its form, granularity and specific surface area to the viscosity of slurry,
Electric conductivity and adhesive force etc. all have certain impact.Argentum powder according to form can be divided into crystallite shape argentum powder, Bright Silver Powder,
Flake silver powder, ball shape silver powder and special shape argentum powder, be most widely used in conductive silver paste at present is ball
Shape argentum powder and flake silver powder.When flake silver powder conducts electricity as filler, it is face or linear contact lay each other, spherical silver
Powder is point cantact, so flake silver powder is much lower than the resistance of spherical argentum powder, even at relatively low silver content
With still there is during relatively thin printed coating higher electrical conductivity, be therefore widely used in carbon-film potentiometer termination, thin
In the electronic devices and components such as membrane switch, wave filter.The physical property of flake silver powder is the weight of impact silver slurry electrical property
Want factor, when the particle diameter of flake silver powder reaches submicron order yardstick, when pattern is the lamellar of light, to electronics
The printing effect of circuit, all has clear improvement including uniformity, flatness etc., and can save noble metal dosage
30%～50%.Chinese patent CN104475754A discloses a kind of rear surface of solar cell silver slurry with irregular
The preparation method of flake silver powder, the argentum powder of preparation can be directly as back silver paste argentum powder, it is not necessary to and its
His thin argentum powder collocation, but use single argentum powder to prepare electrode that back silver paste of solar cell formed
Welding pulling force is the highest, thus causes the reliability of the use of solaode poor.Chinese patent
CN103962569A discloses the preparation method of a kind of flake silver powder, by silver nitrate and the mixing water of polyvinyl alcohol
Solution through atomization, be pyrolyzed to obtain ball shape silver powder under protective atmosphere, after ball shape silver powder and water for ball milling are obtained flake silver powder,
By reactant liquor high-temperature atomizing, complexity and the production cost of process equipment substantially increase.
Summary of the invention
The present invention overcomes the deficiency that prior art exists, it is provided that a kind of flake silver powder for solar energy back of the body silver
Preparation method, prepares flake silver powder and super fine silver powder mixing that mean diameter is 6-11 μm, extensively should
For solar energy back of the body silver.
The technical solution adopted for the present invention to solve the technical problems is:
The preparation method of a kind of flake silver powder for solar energy back of the body silver, comprises the following steps:
(1) preparation silver nitrate solution, in solution, the concentration of silver nitrate is 1-1.5mol/L；
(2) in the silver nitrate solution that step (1) is prepared, the sodium hydroxide that mass fraction is 5-10% is added molten
Liquid, regulates pH to 8-11；
(3) triethanolamine solution is instilled in the silver nitrate solution of step (2) with the speed of 0.5-1mL/min,
Prepare argentum powder serosity；
(4) the argentum powder serosity that step (3) obtains first is filtered, be the diameter of 1:3-5 with mass ratio after washing
For 1mm and 2mm mixing rustless steel hoodle, press (5-10): after the ratio of grinding media to material mixing of 1, put into hexagon ball grinder
In, being subsequently adding the stearic acid ethanol solution that mass fraction is 5-15% as ball-milling additive, rotational speed of ball-mill is
80～100r/min, ball milling 40h；
(5) by ball milling slurry after complete, flake silver powder is the most i.e. obtained.
Specifically, described step (2), the temperature constant of (3) system are 25-40 DEG C.
Specifically, in described step (3), the ratio of triethanolamine and the amount of the material of silver nitrate is (1.5-5): 1.
Specifically, the ball-milling additive in described step (4) be mass fraction be the stearic ethanol of 5-15%
Aqueous solution, the mass ratio of described water and ethanol is 0.05-0.2:10.
Specifically, described step (4) described stearic acid concentration in argentum powder serosity is 0.5-1.5wt%.
Specifically, the mean diameter of the flake silver powder that described step (5) obtains is 6.00-11.00 μm.
The invention have the benefit that
(1) present invention is when preparing ultrapure argentum powder, and any protective agent and dispersant, nothing need not be added in centre
Any organic residual, during use, calcination thermal weight loss is little；
(2) flake silver powder prepared by the present invention has tap density and apparent density is low, and specific surface area is high, relatively
Good dispersive property, when being used in mixed way with super fine silver powder, combination property is more excellent, improves its actual application ability,
It is widely used in solar energy back of the body silver；
(3) preparation method of the present invention is simple, and production cost is low, be prone to volume production, be suitable for industrial on a large scale
Produce；
(4) preparation method of the present invention selects stearic ethanol water as ball-milling additive, can effectively control
The average particle size range of flake silver powder processed.
Detailed description of the invention
Presently in connection with embodiment, the present invention is further detailed explanation.
Embodiment 1
The preparation method of a kind of flake silver powder for solar energy back of the body silver, comprises the following steps:
(1) preparation silver nitrate solution, in solution, the concentration of silver nitrate is 1-1.5mol/L；
(2) in the silver nitrate solution that step (1) is prepared, the sodium hydroxide that mass fraction is 5-10% is added molten
Liquid, regulates pH to 8-11；
(3) triethanolamine solution is instilled in the silver nitrate solution of step (2) with the speed of 0.5-1mL/min,
Preparing argentum powder serosity, wherein triethanolamine is 1.5-5:1 with the ratio of the amount of the material of silver nitrate；
(4) the argentum powder serosity that step (3) obtains first is filtered, be the diameter of 1:3-5 with mass ratio after washing
For 1mm and 2mm mixing rustless steel hoodle, press (5-10): after the ratio of grinding media to material mixing of 1, put into hexagon ball grinder
In, be subsequently adding stearic ethanol water that mass fraction is 5-15% as ball-milling additive, wherein water and
The mass ratio of ethanol is 0.05-0.2:10, and rotational speed of ball-mill is 80～100r/min, and ball milling 40h, stearic acid is at silver
Concentration in slurry liquid is 0.5-1.5wt%；
(5) by ball milling slurry after complete, the average particle size range the most i.e. obtaining flake silver powder is 6-11 μm,
Wherein, step (2), the temperature constant of (3) system are 25-40 DEG C.
Embodiment 2-12 and other conditions of scheme with embodiment 1, difference such as following table:
With the above-mentioned desirable embodiment according to the present invention for enlightenment, by above-mentioned description, related work
Personnel can carry out various change and amendment completely in the range of without departing from this invention technological thought.
The content that the technical scope of this invention is not limited in description, it is necessary to according to right
Determine its technical scope.
Claims (7)
1. carry on the back a preparation method for the flake silver powder of silver for solar energy, comprise the following steps:
(1) preparation silver nitrate solution, in solution, the concentration of silver nitrate is 1-1.5mol/L；
(2) in the silver nitrate solution that step (1) is prepared, the sodium hydroxide that mass fraction is 5-10% is added molten
Liquid, regulates pH to 8-11；
(3) triethanolamine solution is instilled in the silver nitrate solution of step (2) with the speed of 0.5-1mL/min,
Prepare argentum powder serosity；
(4) the argentum powder serosity that step (3) obtains first is filtered, be the diameter of 1:3-5 with mass ratio after washing
For 1mm and 2mm mixing rustless steel hoodle, press (5-10): after the ratio of grinding media to material mixing of 1, put into hexagon ball grinder
In, it being subsequently adding ball-milling additive, rotational speed of ball-mill is 80～100r/min, ball milling 40h；
(5) by ball milling slurry after complete, flake silver powder is the most i.e. obtained.
The preparation method of a kind of flake silver powder for solar energy back of the body silver, it is special
Levy and be: described step (2), the temperature constant of (3) system are 25-40 DEG C.
The preparation method of a kind of flake silver powder for solar energy back of the body silver, it is special
Levy and be: in described step (3), triethanolamine is (1.5-5) with the ratio of the amount of the material of silver nitrate: 1.
The preparation method of a kind of flake silver powder for solar energy back of the body silver, it is special
Levy and be: the ball-milling additive in described step (4) be mass fraction be that the stearic ethanol of 5-15% is water-soluble
Liquid, the mass ratio of described water and ethanol is 0.05-0.2:10.
The preparation method of a kind of flake silver powder for solar energy back of the body silver, it is special
Levy and be: in described step (4), stearic acid concentration in argentum powder serosity is 0.5-1.5%.
The preparation method of a kind of flake silver powder for solar energy back of the body silver, it is special
Levy and be: the mean diameter of the flake silver powder that described step (5) obtains is 6-11 μm.
The preparation method of a kind of flake silver powder for solar energy back of the body silver, it is special
Levy and be: the average particle size range of the flake silver powder that described step (5) obtains is 6-11 μm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610322536.4A CN105817647A (en) | 2016-05-13 | 2016-05-13 | Preparation method for flake sliver powder used for solar rear silver paste |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610322536.4A CN105817647A (en) | 2016-05-13 | 2016-05-13 | Preparation method for flake sliver powder used for solar rear silver paste |
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| CN105817647A true CN105817647A (en) | 2016-08-03 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN201610322536.4A Pending CN105817647A (en) | 2016-05-13 | 2016-05-13 | Preparation method for flake sliver powder used for solar rear silver paste |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112296351A (en) * | 2020-09-29 | 2021-02-02 | 湖南诺尔得材料科技有限公司 | Preparation method of high-tap-density ultrafine silver powder |
| CN112809019A (en) * | 2021-02-07 | 2021-05-18 | 深圳市宏达瑞科技有限公司 | Preparation method of silver powder for low-temperature silver paste of heterojunction solar cell |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102784927A (en) * | 2012-08-28 | 2012-11-21 | 苏州东旭弘业新材料科技有限公司 | Method for preparing high-performance sheet silver powder |
| CN103143723A (en) * | 2013-03-27 | 2013-06-12 | 深圳市中金岭南科技有限公司 | Method for preparing flake silver powder with low bulk density |
| 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 |
-
2016
- 2016-05-13 CN CN201610322536.4A patent/CN105817647A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102784927A (en) * | 2012-08-28 | 2012-11-21 | 苏州东旭弘业新材料科技有限公司 | Method for preparing high-performance sheet silver powder |
| CN103143723A (en) * | 2013-03-27 | 2013-06-12 | 深圳市中金岭南科技有限公司 | Method for preparing flake silver powder with low bulk density |
| 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 |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112296351A (en) * | 2020-09-29 | 2021-02-02 | 湖南诺尔得材料科技有限公司 | Preparation method of high-tap-density ultrafine silver powder |
| CN112809019A (en) * | 2021-02-07 | 2021-05-18 | 深圳市宏达瑞科技有限公司 | Preparation method of silver powder for low-temperature silver paste of heterojunction solar cell |
| CN112809019B (en) * | 2021-02-07 | 2022-02-22 | 深圳市宏达瑞科技有限公司 | Preparation method of silver powder for low-temperature silver paste of heterojunction solar cell |
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| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20160803 |