CN108941609A - Solar cell conductive silver paste high performance spherical super fine silver powder and preparation method thereof - Google Patents
Solar cell conductive silver paste high performance spherical super fine silver powder and preparation method thereof Download PDFInfo
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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
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/06—Metallic powder characterised by the shape of the particles
- B22F1/065—Spherical particles
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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
- B22F2009/245—Reduction reaction in an Ionic Liquid [IL]
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Abstract
The invention discloses a kind of solar cell conductive silver paste high performance spherical super fine silver powders and preparation method thereof, and this method includes: silver nitrate is dissolved in distilled water by step 1, is stirred evenly, and dispersing agent and pH adjusting agent is added；Hydroquinone is dissolved in distilled water obtains quinol solution again by step 2, and under agitation, resulting quinol solution is rapidly added in silver nitrate solution, makes its reaction；Step 3, after the reaction was completed, staticly settles, and filters, washs precipitating repeatedly with dehydrated alcohol, be finally dried to obtain silver powder.The present invention also provides the solar cell conductive silver paste high performance spherical super fine silver powders of this method preparation.Solar cell conductive silver paste high performance spherical super fine silver powder and preparation method thereof provided by the invention, easy control of process conditions, the high density of preparation, the silver powder easily dispersed, performance meet solar cell conductive silver paste production requirement.
Description
Technical field
The present invention relates to a kind of new energy and the super fine silver powder of field of new materials and preparation method thereof, and in particular, to one
Kind solar cell conductive silver paste high performance spherical super fine silver powder and preparation method thereof.
Background technique
Silver powder is the important component of solar battery anode sizing agent, only meets leading for the silver powder preparation of specified conditions
Plasma-based material just has good silk-screen printing performance, could be formed after oversintering with the front silver compared with high square resistance and thin grid line
Electrode.Front electrode is divided into gate electrode line and main electrode line, and grid line mainly collects the carrier of photoelectric conversion generation, main electrode master
It connect cell piece with outside line.Positive electrode gate line width 0.15mm or so, sintering temperature reach 930 DEG C, high-temperature region sintering
Time only 5-8 seconds.If silver powder granularity is excessive, silver paste print when cannot pass through silk screen completely, in the short time can not densified sintering product,
Sintered membrane is easy to appear cavity, to influence electric conductivity.
Document mainly concentrates research nano-silver powder at present, since nano-silver powder activity is high, is easy to happen at normal temperature from burning
Knot or agglomeration, cause that nano-silver powder dispersibility is very poor, and tap density is low.Nano-silver powder modulation slurry is not easy to be had airborne
Body complete wetting causes printing effect bad, silverskin shrinking percentage is big after sintering, hole mostly with connect it is not fine and close.In addition, nano silver
Powder is difficult to improve the silver content of conductive silver paste, and electric conductivity is poor.Silver powder used for solar batteries needs to meet moderate in grain size, crystallization
Degree is high, tap density is big, good dispersion, spherical shape or the conditions such as spherical.
Application practice prove average grain diameter 0.23 μm, especially average grain diameter 12 μm silver powder modulate solar-electricity
Pond silver paste can preferably coordinate the relationship between sintering time and silver-colored meltage, so that silver wire is formed good ohm with silicon wafer and connect
Touching.The high dispersive high-density spherical silver powder for preparing 12 μm of partial size, for the printing of current silver paste of solar cells and electric conductivity
It improves and the promotion of solar cell photoelectric transfer efficiency is of great significance.
The preparation method of silver powder has high-energy ball milling method, spray heating decomposition (SP method), plasma evaporation condensation method, chemistry
Liquid phase reduction and microemulsion method etc., wherein chemical liquid phase reduction method because production equipment is simple, technique is easy to control, low cost,
The advantages that low energy consumption, has obtained extensive attention.
Liquid phase reduction principle be exactly with reducing agent from the solution of silver salt or silver complex by silver ion with the shape of silver powder
Formula is deposited.The silver salt of use is usually silver nitrate [AgNO3], silver carbonate [Ag2CO3] and silver ammino ion [Ag (NH3)2
+]。
During entire reduction reaction, the selection of reducing agent is extremely important.Inorganic reducing agent reported in the literature mainly has
Hydrazine hydrate, hydrogen peroxide, sodium hypophosphite, sodium dithionite, sodium borohydride, ferrous sulfate, sodium thiosulfate, potassium sulfite
Deng；Organic reducing agent reported in the literature mainly have ascorbic acid, formaldehyde, formic acid, sodium potassium tartrate tetrahydrate, ethyl alcohol, glycerol, glucose,
Reduced sugar, triethanolamine, quinhydrones etc..If the reproducibility of reducing agent is too strong, obtained silver particles are not easy to shift, and partial size is easy
Increase it is excessive, comprising impurity or reunite, cannot the uniform Argent grain easily dispersed.Dispersing agent is generally needed to be added to life
At silver particles carry out dispersion protection, prevent the reunion of silver powder.Dispersion protective agent reported in the literature is usually high molecular material, table
Face activating agent and ligand mainly have polyvinylpyrrolidone (PVP), polyvinyl alcohol (PVA), gelatin, carboxymethyl cellulose, chain
Alkanolamine, lauryl sodium sulfate (DBS), cetyl trimethylammonium bromide, polyethylene glycol, tween, succinic acid, sulfuric acid etc.,
Wherein being most widely used with PVP.
There are many patent about silver powder preparation method, for example, Chinese patent CN102921944 (2013-02-13) discloses one
Kind silver powder for conductive silver paste of solar battery electrode and preparation method thereof, using glucose, hydrazine hydrate, hydroquinone or Vitamin C
Acid and its mixture are reducing agent；Chinese patent CN102632248 (2012-08-15) discloses a kind of ball shape silver powder and its preparation
Method uses ascorbic acid for reducing agent, and polyvinylpyrrolidone is protective agent；Chinese patent CN101941078 (2011-01-
12) a kind of silver powder for conductive silver paste of solar battery electrode and preparation method thereof is disclosed, using hydrazine hydrate, formaldehyde, thiosulfuric acid
Sodium or sodium borohydride are reducing agent；Japan Patent JP2013189704 (2013-09-26) disclose it is a kind of use formaldehyde for reduction
Agent, stearic acid are made to disperse protectant silver powder production method；United States Patent (USP) US4456473 (1984-06-26) discloses a kind of use
Hydrazine hydrate is that reducing agent produces high-purity silver powder method；The open time Asia Korean Patent KR20100100210 (2010-09-15)
The method of sodium phosphate production silver powder.
There is also many deficiencies for existing silver powder technology of preparing: (1) reducing agent hydrazine hydrate, formaldehyde and quinhydrones are toxic, irritation
Very strong, environmental protection and safety problems are difficult to solve；(2) sodium borohydride, quinhydrones reducing agent cost are excessively high, influence silver powder production effect
Benefit；(3) reducing agent ascorbic acid changes the conditions such as system acidity, concentration and temperature sensitive, and working condition is not easy to control；(4)
Common reducing agent reproducibility is too strong, need to usually be used cooperatively with a large amount of dispersing agents, causes subsequent silver powder separation difficult.
China is maximum crystal silicon solar battery component producing country in the world, is needed according to 1MW photovoltaic module 64 public
Jin silver powder meter, the country reaches 750 tons or so to silver powder demand, with the continuous expansion of photovoltaic market, inexpensive silver powder market
It will constantly expand, and develop environmental-friendly, at low cost and good conductivity silver powder, it will promotion solar cell industry development.
Summary of the invention
The object of the present invention is to provide a kind of super fine silver powders and preparation method thereof, can overcome the deficiencies of existing technologies, system
Standby high density, the super fine silver powder easily dispersed.
In order to achieve the above object, the present invention provides a kind of solar cell conductive silver paste high performance spherical ultra-fine silvers
The preparation method of powder, wherein the method includes: silver nitrate is dissolved in distilled water by step 1, is stirred evenly, and is added and is divided
Powder and pH adjusting agent；Hydroquinone is dissolved in distilled water obtains quinol solution again by step 2, under agitation,
Resulting quinol solution is rapidly added in silver nitrate solution, its reaction is made；Step 3, after the reaction was completed, staticly settles,
It filters, washs precipitating repeatedly with dehydrated alcohol, be finally dried to obtain silver powder.
The preparation method of above-mentioned solar cell conductive silver paste high performance spherical super fine silver powder, wherein the step
The mass volume ratio of silver nitrate and distilled water is 1: 5 in rapid 1.Silver nitrate uses pure dose of nitric acid of reagent silver nitrate or Industrial Analysis
Silver, the pure a small amount of nitric acid of Industrial Analysis are practiced without influence to invention.
The preparation method of above-mentioned solar cell conductive silver paste high performance spherical super fine silver powder, wherein the step
Dispersing agent in rapid 1 is Arabic gum, and the Arabic gum of addition accounts for solution total amount obtained in step 1 by mass percentage
2.5~4%.
The preparation method of above-mentioned solar cell conductive silver paste high performance spherical super fine silver powder, wherein the step
PH adjusting agent in rapid 1 is ammonium hydroxide, and the ammonium hydroxide additive amount is the 100~225% of silver nitrate quality, the pH model after adjusting
Enclose is 6~7.
The preparation method of above-mentioned solar cell conductive silver paste high performance spherical super fine silver powder, wherein the step
The mass volume ratio of hydroquinone and distilled water is 1: 10 in rapid 2, in the volume and step 1 of the distilled water in the step 2
The volume ratio of distilled water is 1: 1；Reaction time in step 2 is 15min, i.e. completes reaction after 15min, carry out subsequent step
3.Hydroquinone is using commercially available industrial hydroquinone, wherein being practiced without influence to the present invention containing impurity.
The preparation method of above-mentioned solar cell conductive silver paste high performance spherical super fine silver powder, wherein the step
Drying temperature is 60 DEG C in rapid 3.
The present invention also provides the solar cell conductive silver paste high performance spherical super fine silver powders of above-mentioned method preparation.
Above-mentioned solar cell conductive silver paste high performance spherical super fine silver powder, wherein the silver powder, particle are in
Close spherical, surface is smooth, glossy, and preferably, average grain diameter is 0.8~2.6 μm to dispersibility, and apparent density is 2.3~2.9g/
cm3, tap density is 5.0~6.0g/cm3, molar yield is 98%~99.2%.
Solar cell conductive silver paste provided by the invention with high performance spherical super fine silver powder and preparation method thereof have with
Lower advantage:
The present invention is to provide one kind to restore silver nitrate using hydroquinone as reducing agent, with Arabic gum as silver powder point
It dissipates protective agent component and makees pH regulator with ammonium hydroxide, properties of product meet the highly dense of solar cell conductive silver paste production requirement
Degree, easy dispersible silver powder and preparation method thereof can reduce production cost, improve productivity effect, also there is working condition more may be used
The advantages that control is easy to subsequent silver powder separation, is conducive to environmental protection, and safety is obviously improved.
Specific embodiment
A specific embodiment of the invention is further described below.
The solar cell conductive silver paste preparation method of high performance spherical super fine silver powder provided by the invention includes: step
Rapid 1, silver nitrate is dissolved in distilled water, is stirred evenly, and dispersing agent and pH adjusting agent is added；Step 2, again by hydroquinone
It is dissolved in distilled water and obtains quinol solution, under agitation, resulting quinol solution is rapidly added silver nitrate
In solution, make its reaction；Step 3, after the reaction was completed, staticly settles, and filters, washs precipitating repeatedly with dehydrated alcohol, finally do
It is dry to obtain silver powder.
The mass volume ratio of silver nitrate and distilled water is 1: 5 in step 1.
Dispersing agent in step 1 is Arabic gum, and the Arabic gum of addition is accounted for by mass percentage obtained in step 1
The 2.5~4% of solution total amount.
PH adjusting agent in step 1 is ammonium hydroxide, and ammonium hydroxide additive amount is the 100~225% of silver nitrate quality, after adjusting
PH range is 6~7.
The mass volume ratio of hydroquinone and distilled water is 1: 10 in step 2, the volume and step of the distilled water in step 2
The volume ratio of distilled water is 1: 1 in 1；Reaction time in step 2 is 15min.
Drying temperature is 60 DEG C in step 3.
The present invention also provides the solar cell conductive silver paste high performance spherical super fine silver powders of this method preparation.
The silver powder particles are in close spherical, and surface is smooth, glossy, and preferably, average grain diameter is 0.8~2.6 μm to dispersibility, pine
Dress density is 2.3~2.9g/cm3, tap density is 5.0~6.0g/cm3, molar yield is 98%~99.2%.
Below with reference to embodiment to solar cell conductive silver paste provided by the invention high performance spherical super fine silver powder and
Preparation method is further described.
Embodiment 1
A kind of solar cell conductive silver paste preparation method of high performance spherical super fine silver powder includes:
40g silver nitrate is dissolved in 200ml distilled water by step 1, is stirred evenly, and dispersing agent and pH adjusting agent is added.
Silver nitrate uses pure dose of silver nitrate of reagent silver nitrate or Industrial Analysis, and the pure a small amount of nitric acid of Industrial Analysis implements invention
Do not influence.
Dispersing agent is Arabic gum, and the Arabic gum of addition accounts for solution total amount obtained in step 1 by mass percentage
3%.PH adjusting agent is ammonium hydroxide, and ammonium hydroxide additive amount is preferably that the pH range after 200% adjusting of silver nitrate quality is 6~7.
20g hydroquinone is dissolved in 200ml distilled water obtains quinol solution again by step 2, under agitation,
Resulting quinol solution is rapidly added in silver nitrate solution, its reaction is made.
Reaction time is 15min, i.e. completes reaction after 15min, carry out subsequent step 3.Hydroquinone uses commercially available work
Industry hydroquinone, wherein being practiced without influence to the present invention containing impurity.
Step 3, after the reaction was completed, staticly settles, and filters, washs precipitating repeatedly with dehydrated alcohol, be finally dried to obtain silver
Powder.
Drying temperature is 60 DEG C.
The present embodiment additionally provides the solar cell conductive silver paste high performance spherical super fine silver powder of this method preparation.
The silver powder particles are in close spherical, and surface is smooth, glossy, and preferably, average grain diameter is 0.8~2.6 μm to dispersibility, pine
Dress density is 2.3~2.9g/cm3, tap density is 5.0~6.0g/cm3, molar yield is 98%~99.2%.
Hydroquinone (C6H4(OH)2) carry out that there is very strong reproducibility under alkaline condition.Ag+ is reduced into simple substance by it
When Ag, it itself is oxidized to 1,4-benzoquinone, while generating nitric acid and pH value of reaction system is caused to reduce, chemical equation is as follows:
(C6H4(OH)2)+2AgNO3→C6H4O2+2HNO3+2Ag↓
Reproducibility is lost since the reduction of pH value will lead to hydroquinone, the change of pH value will cause the end of reaction
Only, therefore the forming core of silver powder and growth moment complete, this is to realize the uniform prerequisite of silver powder.However Arabic gum is dissolved in water
In, there is emulsification, the reunion of silver powder can be prevented.Therefore this reduction system can prepare high performance spherical silver powder.
Ammonium hydroxide has a great impact to the performance for preparing silver powder, and with the increase of ammonia volume, the partial size of silver powder gradually subtracts
Small, tap density is gradually increased；This is because it is not enough to maintain the pH stable of reduction system when ammonia volume is inadequate,
Reduction system pH value increases, and hydroquinone reproducibility weakens, and long macro aggregate occurs for silver powder nucleus, therefore partial size is big, and apparent density is small.
When ammonium hydroxide increases to it is a certain amount of when, can constantly neutralize reduction reaction generation hydrogen ion, the pH stable of maintenance system, silver powder shape
Crystalline nucleation is rapid, has little time to grow up to react and complete, therefore unijunction crystal size and higher tap density is presented in silver powder.With ammonia
Water consumption continues growing, and silver powder granularity and tap density tend towards stability, and there is no too much influences, but if ammonium hydroxide excess, meeting
It causes silver powder impurity concentration high, causes subsequent wash difficult.The tap density of comprehensive silver powder and the partial size of laser particle analyzer measurement
As a result, the silver powder of preparation has optimal particle diameter distribution and tap density when ammonium hydroxide additive amount is the 200% of silver nitrate quality,
Its average grain diameter D50It is 1.49 μm, tap density reaches 5.67g/cm3Regular spherical silver powder.So subsequent characterizations, slurry system
Make using this silver powder as raw material.
Solar cell conductive silver paste high performance spherical super fine silver powder and preparation method thereof provided by the invention, to benzene
Diphenol restores silver nitrate as reducing agent, passes through addition ammonium hydroxide control as silver powder dispersion protective agent component and simultaneously with Arabic gum
The pH value of system processed, easy control of process conditions, properties of product meet solar cell conductive silver paste production requirement.
It is discussed in detail although the contents of the present invention have passed through above preferred embodiment, but it should be appreciated that above-mentioned
Description is not considered as limitation of the present invention.After those skilled in the art have read above content, for of the invention
A variety of modifications and substitutions all will be apparent.Therefore, protection scope of the present invention should be limited to the appended claims.
Claims (8)
1. a kind of preparation method of solar cell conductive silver paste high performance spherical super fine silver powder, which is characterized in that described
Method includes:
Silver nitrate is dissolved in distilled water by step 1, stirs evenly, and dispersing agent and pH adjusting agent is added, it is molten to obtain silver nitrate
Liquid；
Hydroquinone is dissolved in distilled water obtains quinol solution again by step 2, under agitation, by resulting to benzene
Two phenol solutions are added in silver nitrate solution, make its reaction；
Step 3, after the reaction was completed, staticly settles, and filters, washs precipitating with dehydrated alcohol, be finally dried to obtain silver powder.
2. the preparation method of solar cell conductive silver paste high performance spherical super fine silver powder as described in claim 1, special
Sign is that the mass volume ratio of silver nitrate and distilled water is 1: 5 in the step 1.
3. the preparation method of solar cell conductive silver paste high performance spherical super fine silver powder as claimed in claim 2, special
Sign is that the dispersing agent in the step 1 is Arabic gum, and the Arabic gum of addition accounts in step 1 by mass percentage
The 2.5~4% of resulting solution total amount.
4. the preparation method of solar cell conductive silver paste high performance spherical super fine silver powder as claimed in claim 3, special
Sign is, the pH adjusting agent in the step 1 is ammonium hydroxide, the ammonium hydroxide additive amount be silver nitrate quality 100~
225%, the pH range after adjusting is 6~7.
5. the preparation method of solar cell conductive silver paste high performance spherical super fine silver powder as described in claim 1, special
Sign is that the mass volume ratio of hydroquinone and distilled water is 1: 10 in the step 2, the distilled water in the step 2
Volume and step 1 in distilled water volume ratio be 1: 1；Reaction time in step 2 is 15min.
6. the preparation method of solar cell conductive silver paste high performance spherical super fine silver powder as described in claim 1, special
Sign is that drying temperature is 60 DEG C in the step 3.
7. a kind of solar cell conductive silver paste high-performance of the method preparation as described in any one of claim 1~6
Spherical super fine silver powder.
8. solar cell conductive silver paste high performance spherical super fine silver powder as claimed in claim 7, which is characterized in that described
Silver powder, particle is in close spherical, and surface is smooth, glossy, and average grain diameter is 0.8~2.6 μm, apparent density is 2.3~
2.9g/cm3, tap density is 5.0~6.0g/cm3, molar yield is 98%~99.2%.
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| CN110238384A (en) * | 2019-08-01 | 2019-09-17 | 河南金渠银通金属材料有限公司 | The preparation method of nanometer monocrystalline silver powder |
| CN111940761A (en) * | 2020-09-01 | 2020-11-17 | 苏州银瑞光电材料科技有限公司 | Preparation method of silver powder for N-type solar cell |
| CN111940760A (en) * | 2020-08-20 | 2020-11-17 | 湖南泽宇新材料有限公司 | Spherical nano silver powder and preparation method and application thereof |
| CN112008094A (en) * | 2020-09-08 | 2020-12-01 | 西安汇创贵金属新材料研究院有限公司 | Preparation method of silver powder |
| CN112371993A (en) * | 2020-10-16 | 2021-02-19 | 湖南诺尔得材料科技有限公司 | Preparation method of silver powder |
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| CN116713475A (en) * | 2023-05-30 | 2023-09-08 | 上海银波生物科技有限公司 | Method for preparing silver powder with high specific surface area for TOPCO solar cell |
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| CN110238384A (en) * | 2019-08-01 | 2019-09-17 | 河南金渠银通金属材料有限公司 | The preparation method of nanometer monocrystalline silver powder |
| CN111940760A (en) * | 2020-08-20 | 2020-11-17 | 湖南泽宇新材料有限公司 | Spherical nano silver powder and preparation method and application thereof |
| CN111940761A (en) * | 2020-09-01 | 2020-11-17 | 苏州银瑞光电材料科技有限公司 | Preparation method of silver powder for N-type solar cell |
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