CN106112004B - A kind of preparation method of conductive silver paste strong adhesive force conductive silver powder - Google Patents
A kind of preparation method of conductive silver paste strong adhesive force conductive silver powder Download PDFInfo
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- CN106112004B CN106112004B CN201610484288.3A CN201610484288A CN106112004B CN 106112004 B CN106112004 B CN 106112004B CN 201610484288 A CN201610484288 A CN 201610484288A CN 106112004 B CN106112004 B CN 106112004B
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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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- H—ELECTRICITY
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- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
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Abstract
A kind of preparation method the invention discloses conductive silver paste with strong adhesive force conductive silver powder, belongs to conductive silver powder preparing technical field.The present invention is made using the treaster after making wine as raw material and dries calcium tartrate, adds deionized water and sulfuric acid, filtering, filtrate is rotated, obtains drying crystalline, mixed with deionized water, polyethylene glycol, cetyl trimethylammonium bromide and Tea Polyphenols, heating water bath, end to be heated, silver nitrate is being added thereto, centrifuge, and with absolute ethyl alcohol and deionized water washing sediment, cooled down and grinding by drying, you can a kind of conductive silver paste strong adhesive force conductive silver powder.Example proves, present invention process is simple, equipment investment is few, cost of material is relatively low, obtained powdered silver powder has the characteristics of photocureable energy is low, and lines surface is fine and smooth, and loading is small and resistance is small, so as to greatly strengthen the stability of conductive silver paste and electric conductivity, mass produced suitable for industrialization.
Description
Technical field
A kind of preparation method the invention discloses conductive silver paste with strong adhesive force conductive silver powder, belong to conductive silver powder preparation
Technical field.
Background technology
Solar energy is that the inexhaustible regenerative resource of the mankind is also clean energy resource, does not produce any ring
Pollute in border.Among effective utilization of solar energy；Big sun energy solar photovoltaic utilization is research with fastest developing speed in the last few years, most active
Field, it is one of project wherein to attract most attention.Large-scale development and utilization photovoltaic solar generate electricity, and the photoelectricity for improving battery turns
It is its core place to change efficiency and reduce production cost, because last decade people are to the further depth of solar cell theoretic knowledge
Enter, the improvement of production technology, the infiltration of IC technologies and the appearance of new battery structure, the conversion efficiency of battery obtain larger carry
It is high.
As solar power generation is increasingly valued by the people, countries in the world are modern one after another in exploitation solar cell module
The production of 10 years photovoltaic modulies will be developed with the increasing velocity of 20-30% even more highs afterwards.It is fast-developing roof project, various
Tax reduction and exemption policy and subsidy policy and gradually ripe green electric power supply price provide solid base for the development of photovoltaic market
Plinth.Market is by progressively from the supplement alternative energy source transition of the energy to the whole society in outlying district and rural area.Predict in next century, light
Volt generates electricity as one of basic energy resource of the mankind.
Solar cell is a kind of solid device that electric energy is converted optical energy into using semiconductor P-N junction photovoltaic effect
Part, also known as photovoltaic device, mainly by mixing 5 valency element phosphors (Phosphors) and relying on the N-type semiconductor of a large amount of electronic conductions,
And mix trivalent element boron (Boron) and formed by the P-type semiconductor of hole conduction, its interface is just to have tied, and is crystal silicon
The significant components of solar cell system.One layer of special antireflection will be covered by being made as the whole battery surface of reduction reflection afterwards
Film.Usual N-type semiconductor surface is furnished with very thin metal grid lines, and another side is close to P-type silicon, but it is important to make this metal grid lines
Material is conductive silver paste, and the design of conductive silver paste has significant impact to silk-screen, sintering process and conversion efficiency.
According to the market demand of touch-screen silver paste, silver paste is divided into capacitance plate silver paste, touch screens silver paste, laser engraving silver paste etc.
Conventional species, to toast as handling process, silver powder on the market toasts for satisfaction for the use of silver paste on the touchscreen at present
The demand that type silver paste is, based on flake silver powder, it has photocureable energy height, lines rough surface in UV system silver pastes, filled out
The shortcomings of charge is greatly and resistance is big, it is impossible to meet the use of UV type laser engraving silver pastes, thus conductive silver paste stability can be caused
Reduction, i.e., as the extension of standing time, the electric conductivity of silver paste can be deteriorated, resistance value rise.
The content of the invention
Present invention mainly solves technical problem：For current market sales of silver powder typically based on flake silver powder,
There is photocureable energy height, lines rough surface, loading is big and resistance is big, thus conductive silver paste stability can be caused
Reduce, the electric conductivity of silver paste can be deteriorated, a kind of elevated present situation of resistance value, there is provided conductive silver paste strong adhesive force conductive silver
The preparation method of powder.This method is made using the treaster after making wine as raw material and dries calcium tartrate, adds deionized water and sulphur
Acid, filtering, filtrate is rotated, obtains drying crystalline, with deionized water, polyethylene glycol, cetyl trimethylammonium bromide and tea
Polyphenol mixes, and heating water bath, end to be heated, is adding silver nitrate thereto, centrifuges, and with absolute ethyl alcohol and deionization
Water washing precipitate, cool down and grind by drying, you can obtain a kind of conductive silver paste strong adhesive force conductive silver powder.The present invention
Technique is simple, and equipment investment is few, and cost of material is relatively low, and obtained powdered silver powder has that photocureable energy is low, lines table
The characteristics of face is fine and smooth, and loading is small and resistance is small, so as to greatly strengthen the stability of conductive silver paste and electric conductivity, it is applicable
Mass produced in industrialization.
In order to solve the above-mentioned technical problem, the technical solution adopted in the present invention is：
（1）In mass ratio 1:5, the treaster after wine brewing and the sulfuric acid of mass concentration 10% are stirred, at 35~40 DEG C
Extraction 2~3h of processing, then filters and collects filtrate, count in parts by weight, weigh 10~15 parts of sodium hydroxides, 20~25 respectively
Part calcium carbonate and 45~50 parts of filtrates are stirred, and staticly settle 1~2h, filter and collect filter cake, and 3 are dried at 65~80 DEG C
~5h, it is prepared into dry calcium tartrate；
（2）In mass ratio 1:8, calcium tartrate and deionized water will be dried it is stirred and is placed in beaker, then 200~
Sonic oscillation handles 10~15min under 300W, then to the sulfuric acid of mass concentration 98% is added dropwise in beaker, waits to be added dropwise to and is produced without precipitation
After life, 1~2h is stood, filters and collects filtrate, the rotary evaporated to dryness at 65~80 DEG C, collect drying crystalline；
（3）Count in parts by weight, respectively weigh 45~50 parts of deionized waters, 10~15 parts of polyethylene glycol, 3~5 part 16
The drying crystalline of alkyl trimethyl ammonium bromide, 5~8 parts of Tea Polyphenols and 10~15 parts of above-mentioned preparations is placed in three-necked flask, stirring
Mixing is placed in 1~2h of heating water bath at 65~70 DEG C；
（4）After the completion for the treatment of heating water bath, the silver nitrate solution of deionized water quality 1/2 is added to three-necked flask, controls nitre
The silver-colored concentration of polymer solution of acid is 15%, and time for adding is 10~15min, after being added dropwise to complete, then is stirred under 600~800r/min
1~2h of mixing is mixed, 10~15min is then centrifuged under 6800~9000r/min, lower sediment is collected, uses absolute ethyl alcohol
Washed respectively with deionized water 3~5 times, then 6~8h is dried at 40~45 DEG C, standing is milled after being cooled to room temperature, you can system
It is standby to obtain a kind of conductive silver paste strong adhesive force conductive silver powder.
Conductive silver powder produced by the present invention is brown toner, and particle size is 150~200nm.
The present invention application process be：In mass ratio 7: 1~9: 1, water and polyvinyl alcohol are placed in container, stirring is equal
It is even, then 12~15% conductive silver powder produced by the present invention of mixed liquor quality is added into container, it is again stirring for being well mixed, with rotation
Turn coating method and be coated on PU substrates to form a film, be placed in 10~15min of heating at 135~150 DEG C, survey its resistance, obtain
Average resistivity is 5.2~5.4 Ω .cm, enhances the stability and electric conductivity of conductive silver paste.
The beneficial effects of the invention are as follows：
（1）Present invention process is simple, and equipment investment is few, is raw material using the treaster after wine brewing, cost of material is relatively
It is low, realize twice laid；
（2）Powdered silver powder produced by the present invention has that photocureable energy is low, and lines surface is fine and smooth, and loading is small and electric
The characteristics of small is hindered, so as to greatly strengthen the stability of conductive silver paste and electric conductivity, is mass produced suitable for industrialization.
Embodiment
First in mass ratio 1:5, the treaster after wine brewing and the sulfuric acid of mass concentration 10% are stirred, at 35~40 DEG C
It is lower extraction processing 2~3h, then filter and collect filtrate, count in parts by weight, respectively weigh 10~15 parts of sodium hydroxides, 20~
25 parts of calcium carbonate and 45~50 parts of filtrates are stirred, and staticly settle 1~2h, filter and collect filter cake, are done at 65~80 DEG C
Dry 3~5h, it is prepared into dry calcium tartrate；Last in mass ratio 1:8, calcium tartrate will be dried and be stirred simultaneously with deionized water
It is placed in beaker, then sonic oscillation handles 10~15min under 200~300W, then to the sulphur of mass concentration 98% is added dropwise in beaker
Acid, after being added dropwise to and being produced without precipitation, 1~2h is stood, filters and collects filtrate, the rotary evaporated to dryness at 65~80 DEG C, received
Collect drying crystalline；Count in parts by weight afterwards, respectively weigh 45~50 parts of deionized waters, 10~15 parts of polyethylene glycol, 3~5 parts
The drying crystalline of cetyl trimethylammonium bromide, 5~8 parts of Tea Polyphenols and 10~15 parts of above-mentioned preparations is placed in three-necked flask,
It is stirred and is placed in 1~2h of heating water bath at 65~70 DEG C；After the completion of finally treating heating water bath, to three-necked flask addition go from
The silver nitrate solution of sub- water quality 1/2, it is 15% to control silver nitrate solution mass concentration, and time for adding is 10~15min, waits to drip
After the completion of adding, then 1~2h is stirred under 600~800r/min, then under 6800~9000r/min centrifuge 10~
15min, lower sediment is collected, is washed respectively 3~5 times with absolute ethyl alcohol and deionized water, then dry 6 at 40~45 DEG C~
8h, standing are milled after being cooled to room temperature, you can are prepared into a kind of conductive silver paste strong adhesive force conductive silver powder.
Example 1
First in mass ratio 1:5, the treaster after wine brewing and the sulfuric acid of mass concentration 10% are stirred, soaked at 35 DEG C
Processing 2h is carried, then filters and collects filtrate, count in parts by weight, weighs 10 parts of sodium hydroxides, 20 parts of calcium carbonate and 45 respectively
Part filtrate is stirred, and staticly settles 1h, filters and collect filter cake, and 3h is dried at 65 DEG C, is prepared into dry calcium tartrate；Most
Afterwards in mass ratio 1:8, calcium tartrate will be dried and deionized water is stirred and is placed in beaker, then the sonic oscillation under 200W
10min is handled, then to the sulfuric acid of mass concentration 98% is added dropwise in beaker, after being added dropwise to and being produced without precipitation, stands 1h, filtering is simultaneously
Filtrate is collected, the rotary evaporated to dryness at 65 DEG C, collects drying crystalline；Count in parts by weight afterwards, respectively weigh 45 parts go from
Sub- water, 10 parts of polyethylene glycol, 3 parts of cetyl trimethylammonium bromides, 5 parts of Tea Polyphenols and the drying crystalline of 10 parts of above-mentioned preparations are put
In three-necked flask, it is stirred and is placed in heating water bath 1h at 65 DEG C；After the completion of finally treating heating water bath, three-necked flask is added
Add the silver nitrate solution of deionized water quality 1/2, it is 15% to control silver nitrate solution mass concentration, time for adding 10min, is treated
After being added dropwise to complete, then 1h is stirred under 600r/min, 10min is then centrifuged under 6800r/min, collected lower floor and sink
Form sediment, washed respectively 3 times with absolute ethyl alcohol and deionized water, then 6h is dried at 40 DEG C, standing is milled after being cooled to room temperature, you can
It is prepared into a kind of conductive silver paste strong adhesive force conductive silver powder.
This example operation is easy, in use, in mass ratio 7: 1, water and polyvinyl alcohol are placed in container, stirred,
12% conductive silver powder produced by the present invention of mixed liquor quality is added into container again, is again stirring for being well mixed, with rotary coating
Mode, which is coated on PU substrates, forms a film, is placed at 135 DEG C and heats 10min, surveys its resistance, and obtaining average resistivity is
5.2 Ω .cm, enhance the stability and electric conductivity of conductive silver paste.
Example 2
First in mass ratio 1:5, the treaster after wine brewing and the sulfuric acid of mass concentration 10% are stirred, soaked at 38 DEG C
Carry processing 2.5h, then filter and collect filtrate, count in parts by weight, respectively weigh 13 parts of sodium hydroxides, 23 parts of calcium carbonate and
48 parts of filtrates are stirred, and staticly settle 1.5h, filter and collect filter cake, and 4h is dried at 70 DEG C, is prepared into dry tartaric acid
Calcium；Last in mass ratio 1:8, calcium tartrate will be dried and deionized water is stirred and is placed in beaker, then surpassed under 250W
Sound oscillation handles 13min, then to the sulfuric acid of mass concentration 98% is added dropwise in beaker, after being added dropwise to and being produced without precipitation, stands
1.5h, filter and collect filtrate, the rotary evaporated to dryness at 75 DEG C, collect drying crystalline；Count, claim respectively in parts by weight afterwards
Measure 48 parts of deionized waters, 13 parts of polyethylene glycol, 4 parts of cetyl trimethylammonium bromides, 7 parts of Tea Polyphenols and 13 parts of above-mentioned preparations
Drying crystalline is placed in three-necked flask, is stirred and is placed in heating water bath 1.5h at 68 DEG C；After the completion of finally treating heating water bath,
To the silver nitrate solution of three-necked flask addition deionized water quality 1/2, control silver nitrate solution mass concentration as 15%, during dropwise addition
Between be 13min, after being added dropwise to complete, then 1.5h is stirred under 700r/min, is then centrifuged under 7500r/min
13min, lower sediment is collected, is washed respectively 4 times with absolute ethyl alcohol and deionized water, then 7h is dried at 43 DEG C, stand cooling
Milled after to room temperature, you can be prepared into a kind of conductive silver paste strong adhesive force conductive silver powder.
This example operation is easy, in use, in mass ratio 8: 1, water and polyvinyl alcohol are placed in container, stirred,
14% conductive silver powder produced by the present invention of mixed liquor quality is added into container again, is again stirring for being well mixed, with rotary coating
Mode, which is coated on PU substrates, forms a film, is placed at 145 DEG C and heats 13min, surveys its resistance, and obtaining average resistivity is
5.3 Ω .cm, enhance the stability and electric conductivity of conductive silver paste.
Example 3
First in mass ratio 1:5, the treaster after wine brewing and the sulfuric acid of mass concentration 10% are stirred, soaked at 40 DEG C
Processing 3h is carried, then filters and collects filtrate, count in parts by weight, weighs 15 parts of sodium hydroxides, 25 parts of calcium carbonate and 50 respectively
Part filtrate is stirred, and staticly settles 2h, filters and collect filter cake, and 5h is dried at 80 DEG C, is prepared into dry calcium tartrate；Most
Afterwards in mass ratio 1:8, calcium tartrate will be dried and deionized water is stirred and is placed in beaker, then the sonic oscillation under 300W
15min is handled, then to the sulfuric acid of mass concentration 98% is added dropwise in beaker, after being added dropwise to and being produced without precipitation, stands 2h, filtering is simultaneously
Filtrate is collected, the rotary evaporated to dryness at 80 DEG C, collects drying crystalline；Count in parts by weight afterwards, respectively weigh 50 parts go from
Sub- water, 15 parts of polyethylene glycol, 5 parts of cetyl trimethylammonium bromides, 8 parts of Tea Polyphenols and the drying crystalline of 15 parts of above-mentioned preparations are put
In three-necked flask, it is stirred and is placed in heating water bath 2h at 70 DEG C；After the completion of finally treating heating water bath, three-necked flask is added
Add the silver nitrate solution of deionized water quality 1/2, it is 15% to control silver nitrate solution mass concentration, time for adding 15min, is treated
After being added dropwise to complete, then 2h is stirred under 800r/min, 15min is then centrifuged under 9000r/min, collected lower floor and sink
Form sediment, washed respectively 5 times with absolute ethyl alcohol and deionized water, then 8h is dried at 45 DEG C, standing is milled after being cooled to room temperature, you can
It is prepared into a kind of conductive silver paste strong adhesive force conductive silver powder.
This example operation is easy, in use, in mass ratio 9: 1, water and polyvinyl alcohol are placed in container, stirred,
15% conductive silver powder produced by the present invention of mixed liquor quality is added into container again, is again stirring for being well mixed, with rotary coating
Mode, which is coated on PU substrates, forms a film, is placed at 150 DEG C and heats 15min, surveys its resistance, and obtaining average resistivity is
5.4 Ω .cm, enhance the stability and electric conductivity of conductive silver paste.
Claims (1)
1. a kind of conductive silver paste preparation method of strong adhesive force conductive silver powder, it is characterised in that specifically preparation process is：
（1）In mass ratio 1:5, the treaster after wine brewing and the sulfuric acid of mass concentration 10% are stirred, extracted at 35~40 DEG C
2~3h is handled, then filters and collects filtrate, count in parts by weight, weighs 10~15 parts of sodium hydroxides, 20~25 parts of carbon respectively
Sour calcium and 45~50 parts of filtrates are stirred, and staticly settle 1~2h, filter and collect filter cake, dry 3 at 65~80 DEG C~
5h, it is prepared into dry calcium tartrate；
（2）In mass ratio 1:8, calcium tartrate will be dried and deionized water is stirred and is placed in beaker, then in 200~300W
Lower sonic oscillation handles 10~15min, then to the sulfuric acid of mass concentration 98% is added dropwise in beaker, after being added dropwise to and being produced without precipitation,
1~2h is stood, filters and collects filtrate, the rotary evaporated to dryness at 65~80 DEG C, collects drying crystalline；
（3）Count in parts by weight, weigh 45~50 parts of deionized waters, 10~15 parts of polyethylene glycol, 3~5 parts of cetyls respectively
The drying crystalline of trimethylammonium bromide, 5~8 parts of Tea Polyphenols and 10~15 parts of above-mentioned preparations is placed in three-necked flask, is stirred
It is placed in 1~2h of heating water bath at 65~70 DEG C；
（4）After the completion for the treatment of heating water bath, the silver nitrate solution of deionized water quality 1/2 is added to three-necked flask, controls silver nitrate
Concentration of polymer solution is 15%, and time for adding is 10~15min, after being added dropwise to complete, then stirs and mixes under 600~800r/min
1~2h is closed, 10~15min is then centrifuged under 6800~9000r/min, collects lower sediment, with absolute ethyl alcohol and is gone
Ionized water is washed 3~5 times respectively, then 6~8h is dried at 40~45 DEG C, and standing is milled after being cooled to room temperature, you can is prepared into
A kind of conductive silver paste strong adhesive force conductive silver powder.
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| CN201610484288.3A CN106112004B (en) | 2016-06-28 | 2016-06-28 | A kind of preparation method of conductive silver paste strong adhesive force conductive silver powder |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1718699A (en) * | 2005-04-06 | 2006-01-11 | 尹小林 | Catalytic combustion adjuvant for coal |
| CN104152317A (en) * | 2014-06-24 | 2014-11-19 | 高耸 | Method for brewing wine by using peel residue |
| CN104658700A (en) * | 2015-01-23 | 2015-05-27 | 华南师范大学 | Preparation method for transparent silver nanowire conducting electrode |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| US20120276030A1 (en) * | 2011-04-29 | 2012-11-01 | Garden Art Innovations, Llc | Cosmetic composition |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1718699A (en) * | 2005-04-06 | 2006-01-11 | 尹小林 | Catalytic combustion adjuvant for coal |
| CN104152317A (en) * | 2014-06-24 | 2014-11-19 | 高耸 | Method for brewing wine by using peel residue |
| CN104658700A (en) * | 2015-01-23 | 2015-05-27 | 华南师范大学 | Preparation method for transparent silver nanowire conducting electrode |
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Inventor after: Liu Shunzhao Inventor after: Liang Shuang Inventor after: Wang Chengxin Inventor after: Jian Zhuangli Inventor after: Liu Sha Inventor after: Fan Min Inventor before: Guo Yingqing Inventor before: Zhang Ming Inventor before: Gao Yugang |
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