CN109079152A - A kind of solar battery silver powder preparation method - Google Patents
A kind of solar battery silver powder preparation method Download PDFInfo
- Publication number
- CN109079152A CN109079152A CN201810789880.3A CN201810789880A CN109079152A CN 109079152 A CN109079152 A CN 109079152A CN 201810789880 A CN201810789880 A CN 201810789880A CN 109079152 A CN109079152 A CN 109079152A
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- Prior art keywords
- solution
- silver
- reducing agent
- silver powder
- mixed solution
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Classifications
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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
-
- 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
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/10—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material
- B22F1/102—Metallic powder coated with organic material
Abstract
The invention discloses a kind of solar battery silver powder preparation methods, first mixed solution is reacted to the nano silver crystal seed for generating size tunable, high dispersive with reducing agent first, the second mixed solution and reducing agent is added into the solution after reaction again, the nucleation process of silver-colored crystal seed is separated with growth course, micron order silver powder needed for preparing solar panel front side silver paste by the method that silver-colored crystal seed induces, the defects of silver powder particle diameter distribution existing in the prior art is wide, crystallinity is poor, pattern is various is overcome, it is with good economic efficiency.
Description
Technical field
The present invention relates to solar panel technology fields, and in particular to a kind of solar battery silver powder preparation method.
Background technique
Solar cell front side silver paste is the core starting materials for preparing front electrode of solar battery.Front electrode plays remittance
Colleeting comb, the important function of derived current.The performances such as the ratio of width to height, compactness, the adhesive force of front electrode are all to solar battery
Battery efficiency and the service life have important influence.Solar cell front side silver paste includes super fine silver powder, glass powder, You Jirong
Agent.Wherein, silver powder accounts for 90% or so of solar cell front side silver paste solid content, and quality directly affects the efficiency of battery;Mesh
Preceding industrialization prepares the method for super fine silver powder based on solution phase chemical reduction.Its traditional handicraft is to be held with reaction kettle for reaction
Device, using churned mechanically mode, by the precipitating for putting into reducing agent solution realization Argent grain in silver salt solution.This method
Nucleation carried out simultaneously with nucleus growth, cannot achieve the control to silver powder key parameter, cause production silver powder particle diameter distribution
Width, crystallinity is poor, pattern multiplicity, and tap density is low, it is difficult to meet the technical need of solar cell front side silver paste.
The Chinese invention patent of Publication No. CN103624267A discloses a kind of continuity method preparation on March 12nd, 2014
Silver nitrate, pH adjusting agent, complexing agent, dispersing agent are dissolved in deionized water by the method for silver powder, are configured to concentration of silver ions and are
The solution of 0.3-3mol/L;Reducing agent, pH adjusting agent are dissolved in deionized water and prepare reducing agent solution, it is molten by adjusting silver ion
Temperature, pH value, flow when liquid is reacted with reducing agent solution control the partial size of silver powder with injection angle, so that it is steady to obtain performance
Fixed, dispersibility height, the uniform silver powder of particle diameter distribution.
Summary of the invention
It is wide for silver powder particle diameter distribution existing in the prior art, shape partial size is irregular and reaction effect is poor etc. lacks
It falls into, the invention discloses a kind of solar battery silver powder preparation methods, using solar panel silver paste silver produced by the invention
Powder has many advantages, such as that strong even particle size distribution, morphological rules, crystallinity, good dispersion, tap density are high.It can effectively mention simultaneously
The utilization rate of high reaction solution is reduced with production cost pressure in the environmental discharge pressure of enterprise, with good economic efficiency.
Above-mentioned purpose that the invention is realized by the following technical scheme:
A kind of solar battery silver powder preparation method, it is characterised in that: include the following steps
A, silver chlorate, dispersing agent and deionized water being added in the first Agitation Tank and being configured to concentration of silver ions is 0.2-2mol/L's
The mass ratio of first mixed solution, dispersing agent and corresponding silver salt is 0.002-0.4, and the pH value of the first mixed solution is 3;By carbonic acid
The second mixed solution for preparing that concentration of silver ions is 0.2-2mol/L is added in the second Agitation Tank in silver, dispersing agent and deionized water,
The mass ratio of dispersing agent and corresponding silver salt is 0.002-0.4, and the pH value of the second mixed solution is 1-10;
B, reducing agent and deionized water are separately added into the first reducing agent tank and the second reducing agent tank and prepare reducing agent solution, also
The mole of former agent solution is the 0.6- of silver ion mole in the first mixed solution described in step A and the second mixed solution
1.5 again;
C, the first mixed solution prepared in step A and the reducing agent solution in step B in the first reducing agent tank are pumped respectively
Carry out hybrid reaction into mixing reactor, the feed flow of the first mixed solution and reducing agent solution is 1-90 L/
min;
D, by the mixed solution generated in step C be sent into hybrid reactor in, and by the second mixed solution prepared in step A with
Reducing agent solution in step B in the second reducing agent tank is pumped into hybrid reactor respectively, the second mixed solution and reducing agent
Feed flow be 0.2-15L/min, open simultaneously the ultrasonic generator and blender being arranged on hybrid reactor;
E, after the second mixed solution in step D and reducing agent solution are added, the Mixing Machine of hybrid reactor continues to stir
It mixes, mixing time 30-50min, reaction generates silver powder solution;
F, the silver powder solution that step E is generated is sent into stillpot and carries out ageing reaction 10-50min, reaction temperature 20-90
℃;
G, the silver powder solution in stillpot is transported in centrifuge, and surfactant is added in the silver powder solution into centrifuge;
The dosage of surfactant is 0.002-0.4 times of silver salt quality in silver powder solution;
H, the silver powder solution of processing surface-modified in step G is sent into drying in drying machine can be obtained silver powder.
The dispersing agent is in polyvinyl alcohol, polyvinyl pyrrole network alkanone, gum arabic, methylcellulose or gelatin
It is one or more of.
The reducing agent includes one or more of D- ascorbic acid, L-AA.
The surfactant is polyethylene glycol, polyvinylpyrrolidone, gelatin, polyvinyl alcohol, gum arabic, methyl
The mixture of any ratio of one or more of cellulose.
Compared with prior art, the invention has the following advantages:
1, the present invention, which first reacts the first mixed solution with reducing agent solution, generates nano-Ag particles solution, then the second mixing is molten
Liquid and reducing agent solution are added in nano-Ag particles solution, make the nucleation process and growth course separation of silver-colored nucleus, silver-colored crystal seed at
The silver-colored crystal seed partial size generated in nuclear process has stronger controllability, and silver-colored crystal seed during the growth process directly inhales newborn silver atoms
Seed surface is invested, directly the growth of participation crystal seed, so that it be avoided to repeatedly generate silver-colored crystal seed, has both improved the utilization of silver atoms
Rate, and be avoided that a large amount of silver-colored crystal seeds be combined with each other and generate silver powder, be conducive to the partial size and pattern that control silver powder.
2, keep reaction solution mixing more uniform by the stirring action of agitating paddle in silver-colored crystal seed growth course of the invention, mention
The rate and raw material availability of height reaction;Silver-colored crystal seed growth course is controlled by ultrasonic unit simultaneously, it can be effective
The reunion for inhibiting silver-colored crystal seed, not only can control silver powder particle size and pattern, but also can improve the yield of silver powder.
3, the present invention will also carry out the ageing reaction of 10-50min after terminating stirring, and being aged reaction in temperature is 20-
It is carried out in 90 DEG C of ultrasonic environment, the small particle silver particles in solution can be made to dissolve again, recrystallized, improve silver powder table
The crystallinity and smoothness in face, while by being reacted in ultrasonic environment, avoid large-sized silver powder from generating, Jin Erti
The tap density of high silver powder.
4, the present invention is modified to be re-fed into drying machine after processing and be dried using surfactant to silver powder solution
Processing, can be improved the dispersibility of silver powder, to avoid the aggregation of silver powder particle, be conducive to improve the uniform of silver powder partial size
Degree.
Detailed description of the invention
Fig. 1 is reaction system schematic diagram of the invention;
Appended drawing reference: 1, first Agitation Tank, the 2, second Agitation Tank, the 3, first reducing agent tank, the 4, second reducing agent tank, 5, mixing it is anti-
Answer device, 6, hybrid reactor, 7, stillpot, 8, centrifuge, 9, drying machine.
Specific embodiment
It below will the invention will be further described by specific embodiment:
Embodiment 1
The present embodiment is as a preferred embodiment of the invention, and it discloses a kind of preparation method of solar battery silver powder, packets
Include following steps:
A, silver chlorate, dispersing agent and deionized water are added in the first Agitation Tank to be configured to that concentration of silver ions is 0.2mol/L the
The mass ratio of one mixed solution, dispersing agent and corresponding silver salt is 0.002, and the pH value of the first mixed solution is 3;By silver carbonate, divide
Powder and deionized water are added in the second Agitation Tank the second mixed solution for preparing that concentration of silver ions is 0.2mol/L, dispersing agent with
The mass ratio of corresponding silver salt is 0.002, and the pH value of the second mixed solution is 1;
B, reducing agent and deionized water are separately added into the first reducing agent tank and the second reducing agent tank and prepare reducing agent solution, also
The mole of former agent solution is 0.6 times of silver ion mole in the first mixed solution described in step A and the second mixed solution;
C, the first mixed solution prepared in step A and the reducing agent solution in step B in the first reducing agent tank are pumped respectively
Carry out hybrid reaction into mixing reactor, the feed flow of the first mixed solution and reducing agent solution is 1L/min;
D, by the mixed solution generated in step C be sent into hybrid reactor in, and by the second mixed solution prepared in step A with
Reducing agent solution in step B in the second reducing agent tank is pumped into hybrid reactor respectively, the second mixed solution and reducing agent
Feed flow be 0.2L/min, open simultaneously the ultrasonic generator and blender being arranged on hybrid reactor;
E, after the second mixed solution in step D and reducing agent solution are added, the Mixing Machine of hybrid reactor continues to stir
It mixes, mixing time 30min, reaction generates silver powder solution;
F, the silver powder solution that step E is generated is sent into stillpot and carries out ageing reaction 10min, reaction temperature is 20 DEG C;
G, the silver powder solution in stillpot is transported in centrifuge, and surfactant is added in the silver powder solution into centrifuge;
The dosage of surfactant is 0.002 times of silver salt quality in silver powder solution;
H, the silver powder solution of processing surface-modified in step G is sent into drying in drying machine can be obtained silver powder.
Embodiment 2
The present embodiment is as another preferred embodiment of the invention, and it discloses a kind of preparation sides of solar panel silver powder
Method, comprising the following steps:
A, silver chlorate, dispersing agent and deionized water are added in the first Agitation Tank and are configured to concentration of silver ions as the first of 2mol/L
The mass ratio of mixed solution, dispersing agent and corresponding silver salt is 0.4, and the pH value of the first mixed solution is 3;By silver carbonate, dispersing agent
It is added in the second Agitation Tank with deionized water and prepares the second mixed solution that concentration of silver ions is 2mol/L, dispersing agent and corresponding silver
The mass ratio of salt is 0.4, and the pH value of the second mixed solution is 10;
B, reducing agent and deionized water are separately added into the first reducing agent tank and the second reducing agent tank and prepare reducing agent solution, also
The mole of former agent solution is 1.5 times of silver ion mole in the first mixed solution described in step A and the second mixed solution;
C, the first mixed solution prepared in step A and the reducing agent solution in step B in the first reducing agent tank are pumped respectively
Carry out hybrid reaction into mixing reactor, the feed flow of the first mixed solution and reducing agent solution is 90 L/min;
D, by the mixed solution generated in step C be sent into hybrid reactor in, and by the second mixed solution prepared in step A with
Reducing agent solution in step B in the second reducing agent tank is pumped into hybrid reactor respectively, the second mixed solution and reducing agent
Feed flow be 15L/min, open simultaneously the ultrasonic generator and blender being arranged on hybrid reactor;
E, after the second mixed solution in step D and reducing agent solution are added, the Mixing Machine of hybrid reactor continues to stir
It mixes, mixing time 50min, reaction generates silver powder solution;
F, the silver powder solution that step E is generated is sent into stillpot and carries out ageing reaction 50min, reaction temperature is 90 DEG C;
G, the silver powder solution in stillpot is transported in centrifuge, and surfactant is added in the silver powder solution into centrifuge;
The dosage of surfactant is 0.4 times of silver salt quality in silver powder solution;
H, the silver powder solution of processing surface-modified in step G is sent into drying in drying machine can be obtained silver powder.
Embodiment 3
A kind of preparation method of solar panel silver powder described in based on the above embodiment:
The dispersing agent is one of polyvinyl alcohol, polyvinyl pyrrole network alkanone, gum arabic, methylcellulose or gelatin
Or it is several.
The reducing agent includes one or more of D- ascorbic acid, L-AA.
The surfactant is polyethylene glycol, polyvinylpyrrolidone, gelatin, polyvinyl alcohol, gum arabic, methyl
The mixture of any ratio of one or more of cellulose.
The working principle of the invention is: the first mixed solution being added in mixing reactor with reducing agent solution react first
Nano-Ag particles solution is generated, then nano-Ag particles solution, the second mixed solution are mixed with reducing agent solution, reacts generation
Nano-Ag particles can make newborn silver atoms be adsorbed in silver-colored seed surface as the silver-colored crystal seed in subsequent reactions, silver-colored crystal seed, directly
Participate in the growth of silver-colored crystal seed, to inhibit the nucleating course of newborn silver atoms, can improve silver atoms utilization rate and
The control of silver powder partial size.
Claims (4)
1. a kind of solar battery silver powder preparation method, it is characterised in that: include the following steps
A, silver chlorate, dispersing agent and deionized water being added in the first Agitation Tank (1) and being configured to concentration of silver ions is 0.2-2mol/
The mass ratio of the first mixed solution of L, dispersing agent and corresponding silver salt is 0.002-0.4, and the pH value of the first mixed solution is 3;It will
Silver carbonate, dispersing agent and deionized water are added preparation concentration of silver ions in the second Agitation Tank (2) and mix for the second of 0.2-2mol/L
The mass ratio of conjunction solution, dispersing agent and corresponding silver salt is 0.002-0.4, and the pH value of the second mixed solution is 1-10;
B, reducing agent and deionized water are separately added into the first reducing agent tank (3) and the second reducing agent tank (4) and prepare reducing agent
Solution, the mole of reducing agent solution are silver ion moles in the first mixed solution described in step A and the second mixed solution
0.6-1.5 times;
C, the first mixed solution prepared in step A and the reducing agent solution in step B in the first reducing agent tank (3) are pumped respectively
It is sent in mixing reactor (5) and carries out hybrid reaction, the feed flow of the first mixed solution and reducing agent solution is 1-90
L/min;
D, the mixed solution generated in step C is sent into hybrid reactor (6), and the prepare in step A second mixing is molten
Liquid is pumped into hybrid reactor (6) respectively with the reducing agent solution in the second reducing agent tank (4) in step B, and the second mixing is molten
The feed flow of liquid and reducing agent is 0.2-15L/min, opens simultaneously the ultrasonic wave being arranged on hybrid reactor (6) and fills
It sets and blender;
E, after the second mixed solution in step D and reducing agent solution are added, the Mixing Machine of hybrid reactor (6) continues
Stirring, mixing time 30-50min, reaction generate silver powder solution;
F, the silver powder solution that step E is generated is sent into stillpot (7) and carries out ageing reaction 10-50min, reaction temperature is
20-90℃;
G, the silver powder solution in stillpot (7) is transported in centrifuge (8), and the silver powder solution in centrifuge (8) is added
Surfactant;The dosage of surfactant is 0.002-0.4 times of silver salt quality in silver powder solution;
H, the silver powder solution of processing surface-modified in step G is sent into drying in drying machine (9) can be obtained silver powder.
2. a kind of solar battery silver powder preparation method according to claim 1, it is characterised in that: the dispersing agent is
One or more of polyvinyl alcohol, polyvinyl pyrrole network alkanone, gum arabic, methylcellulose or gelatin.
3. a kind of solar battery silver powder preparation method according to claim 1, it is characterised in that: the reducing agent packet
One or more of ascorbic acid containing D-, L-AA.
4. a kind of solar battery silver powder preparation method according to claim 1, it is characterised in that: the surface-active
Agent is one of polyethylene glycol, polyvinylpyrrolidone, gelatin, polyvinyl alcohol, gum arabic, methylcellulose or more
The mixture of any ratio of kind.
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Cited By (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN111299608A (en) * | 2020-04-15 | 2020-06-19 | 河南金渠银通金属材料有限公司 | Silver powder for silicon solar cell main grid slurry and preparation method thereof |
CN111618316A (en) * | 2020-06-29 | 2020-09-04 | 河南金渠银通金属材料有限公司 | Surface-modified silver powder and coating preparation method thereof |
CN114682792A (en) * | 2022-04-14 | 2022-07-01 | 宁夏中色新材料有限公司 | Spherical silver powder with high specific surface area and preparation method thereof |
CN115780824A (en) * | 2023-01-29 | 2023-03-14 | 苏州银瑞光电材料科技有限公司 | Preparation method and application of silver powder with high sintering activity |
CN116984622A (en) * | 2023-09-26 | 2023-11-03 | 东方电气集团科学技术研究院有限公司 | Preparation method of nano seed crystal for inducing growth of crystallization type micron-sized silver powder |
CN117047121A (en) * | 2023-10-11 | 2023-11-14 | 长春黄金研究院有限公司 | Silver powder preparation method |
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CN1600477A (en) * | 2003-09-28 | 2005-03-30 | 中国印钞造币总公司 | Method for preparing nano silver powder |
CN106583746A (en) * | 2016-11-30 | 2017-04-26 | 中国东方电气集团有限公司 | Preparation method of solar battery panel silver powder |
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2018
- 2018-07-18 CN CN201810789880.3A patent/CN109079152A/en active Pending
Patent Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
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CN1600477A (en) * | 2003-09-28 | 2005-03-30 | 中国印钞造币总公司 | Method for preparing nano silver powder |
CN106583746A (en) * | 2016-11-30 | 2017-04-26 | 中国东方电气集团有限公司 | Preparation method of solar battery panel silver powder |
Cited By (9)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN111299608A (en) * | 2020-04-15 | 2020-06-19 | 河南金渠银通金属材料有限公司 | Silver powder for silicon solar cell main grid slurry and preparation method thereof |
CN111618316A (en) * | 2020-06-29 | 2020-09-04 | 河南金渠银通金属材料有限公司 | Surface-modified silver powder and coating preparation method thereof |
CN114682792A (en) * | 2022-04-14 | 2022-07-01 | 宁夏中色新材料有限公司 | Spherical silver powder with high specific surface area and preparation method thereof |
CN114682792B (en) * | 2022-04-14 | 2024-02-13 | 宁夏中色新材料有限公司 | Spherical silver powder with high specific surface area and preparation method thereof |
CN115780824A (en) * | 2023-01-29 | 2023-03-14 | 苏州银瑞光电材料科技有限公司 | Preparation method and application of silver powder with high sintering activity |
CN116984622A (en) * | 2023-09-26 | 2023-11-03 | 东方电气集团科学技术研究院有限公司 | Preparation method of nano seed crystal for inducing growth of crystallization type micron-sized silver powder |
CN116984622B (en) * | 2023-09-26 | 2024-02-09 | 东方电气集团科学技术研究院有限公司 | Preparation method of nano seed crystal for inducing growth of crystallization type micron-sized silver powder |
CN117047121A (en) * | 2023-10-11 | 2023-11-14 | 长春黄金研究院有限公司 | Silver powder preparation method |
CN117047121B (en) * | 2023-10-11 | 2024-01-05 | 长春黄金研究院有限公司 | Silver powder preparation method |
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Application publication date: 20181225 |