CN104282356A - Low-silver-content composite conductive silver paste and preparation method thereof - Google Patents
Low-silver-content composite conductive silver paste and preparation method thereof Download PDFInfo
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- CN104282356A CN104282356A CN201310294279.4A CN201310294279A CN104282356A CN 104282356 A CN104282356 A CN 104282356A CN 201310294279 A CN201310294279 A CN 201310294279A CN 104282356 A CN104282356 A CN 104282356A
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Abstract
The invention relates to a low-silver-content composite conductive silver paste and a preparation method thereof, and belongs to the technical field of electroconductive slurry. The low-silver-content composite conductive silver paste can be used for screen printing. At present, the conductive silver paste preparation technology in China is high in production cost, complex in preparation technology and the like. According to the low-silver-content composite conductive silver paste, silver-plated copper powder and silver-plated glass powder are adopted to replace pure silver powder, so that the production cost of the silver paste is effectively reduced; the mode that spherical particles and platy particles are combined is selected, so that the conductivity of the silver paste is improved; the silver-plated glass powder with the low specific density is adopted, so that the stability of the conductive silver paste is improved, and the storage life of the silver paste is prolonged. The problems existing in silver paste production at present in China are well solved, the sliver paste preparation technology is simple, the silver paste is good in conductivity and impressionability (including automatic and semi-automatic screen printing and the like), and high in adhesion capacity with various substrates such as a PET film, and has significant application value.
Description
Technical field
The invention belongs to electrocondution slurry technical field, relate to a kind of low silver content composite conducting silver slurry that can be used for silk screen printing and preparation method thereof.
Background technology
In electrocondution slurry field, silver system slurry has that conductance is high, stable performance, impressionability are good, with the feature such as substrate bond strength is large, be widely used in the production of various electronic devices and components, as integrated circuit, thin film switch, electric heating diaphragm etc.Conductive silver paste is generally made up of silver powder, organic carrier and other additives etc., and in order to reach the conductance that application requires, the part by weight of usual silver powder in whole slurry must reach 60-85%, and this part cost accounts for more than 90% of whole conductive silver paste cost.In the Electronic Components Manufacturing of many application conductive silver pastes, as electric heating diaphragm, the cost of silver slurry has accounted for more than 80% of the whole cost of raw material, therefore, reduces the cost of conductive silver paste, for the whole product cost of reduction, has decisive meaning.
Reducing the silver content of conductive silver paste, keep its high conductivity simultaneously, is the effective way reducing silver slurry cost.As Chinese invention patent publication number CN1437200A, disclosed " low-content nanometer conducting silver paste and preparation method thereof ", a microemulsion method is adopted to prepare the narrower nano silver particles of domain size distribution, conductive silver paste prepared by this nano silver particles, while maintenance satisfactory electrical conductivity, silver content has dropped to 20%.In addition, Chinese invention patent publication number CN102831954A, disclosed " crystal silicon solar battery back field silver slurry and preparation method thereof ", by the conductive silver paste that mixing contains silver paste and prepares containing copper slurry two kinds of slurries, while its satisfactory electrical conductivity of maintenance, due to the interpolation of copper powder, effectively reduce the production cost of silver slurry.The standby conductive silver paste of above-mentioned two patent systems all employ nano particle, comprises nano silver particles and nanometer copper particle, preparation technology's more complicated of these nano particles, and the production cost of itself is also higher, is obviously unfavorable for wide popularization and application.
Summary of the invention
The object of the present invention is to provide a kind of low silver content composite conducting silver slurry and preparation method thereof, preparation technology is simple for this silver slurry, under very low silver content (being less than 25% weight ratio), show good conductivity, and there is good impressionability (automatically, semi-automatic screen printing etc.) and the very strong ability as bonding in PET film with various substrate, considerably reduce the production cost of conductive silver paste, there is important using value.
Object of the present invention can be achieved through the following technical solutions:
A low silver content composite conducting silver slurry, is characterized in that, this silver slurry is made up of the raw material comprising following component and content (percentage by weight):
Described silver-plated copper powder is spherical particle, and particle size is 1-3 μm, and electroplate content is 5-15% (weight ratio), and tap density is 3-4g/mL.
Described silvered glass powder is sheet-like particle, and particle size is 2-8 μm, and electroplate content is 20-60% (weight ratio), and tap density is 0.5-1.5g/mL.
Described macromolecule resin is selected from modified poly ethylene or polyester resin.
Described organic solvent is selected from high boiling lipid, ketone or aromatic hydrocarbon solvent.
Other described additives comprise levelling agent and defoamer, and the weight ratio of the two is respectively 1-4 and 0.1-1.5.
Described levelling agent is selected from one or more in cyclohexanone, turpentine oil, castor oil, tributyl phosphate; Described defoamer is selected from one or more in terpinol, methyl-silicone oil, n-hexyl alcohol.
A preparation method for low silver content composite conducting silver slurry, comprises the following steps:
(1) preparation of organic carrier
According to percentage by weight, 1 part of macromolecule resin (modified poly ethylene or polyester) is joined in 5 parts of organic solvents (lipid or ketone or arene), being heated to 60-90 DEG C is stirred well to after resin dissolves completely, and then keep stirring 8 hours in the thermostat water bath being placed on 80 DEG C, finally obtain the organic carrier that viscosity at ambient temperature is 8000-10000 centipoise.
(2) configuration of substrate silver slurry
According to percentage by weight, the silvered glass powder of the silver-plated copper powder of 5-15%, 30-50%, the organic carrier of 10-30%, the additive of 1-5% are fully mixed under mechanical stirring, re-uses high-speed stirred high speed dispersion, obtain uniform slurry.This slurry transfers to rolling repeatedly on three-roller, disperses, is ground to by Hegman grind gage mensuration fineness below 5 μm.
(3) production of terminal silver slurry
The substrate silver obtained in (2) is starched in high speed dispersor, the viscosity, electric conductivity etc. of silver slurry is regulated by adding solvent or carrier (5-20% weight ratio) on a small quantity, finally obtain the slurry that can be directly used in silk screen printing, its viscosity at ambient temperature is 30000-50000 centipoise.
Compared with prior art, the present invention has following useful technique effect:
The present invention adopts silver-plated copper powder and silvered glass powder to replace fine silver powder, while ensureing that conductive silver paste has excellent conductive performance, greatly reduce actual silver content (being less than 25% weight ratio) in silver slurry, thus effectively reduce the production cost of silver slurry.
The mode that the present invention has selected spherical particle (silver-plated copper powder) to combine with sheet-like particle (silvered glass powder) in silver slurry, effectively reduce the gap between conductive particle, thus improve the bulk density of conductive film layer, increase interparticle contact area, reduce the convergent force of rete, improve the conductive capability of silver slurry.
The present invention adopts low-gravity silvered glass powder, and its proportion only has the 30-50% of fine silver powder, and this light silvered glass powder is not easy sedimentation in organic carrier, thus improves the stability of conductive silver paste, extends the storage life of silver slurry.
Embodiment
Be described in further details the present invention below in conjunction with instantiation, the explanation of the invention is not limited.
The concrete preparation process of low silver content composite conducting silver slurry of the present invention is as follows:
(1) preparation of organic carrier
1 is added in three mouthfuls of round-bottomed flasks, 4-dimethylnaphthalene 80 grams, heating water bath to 60 DEG C, measuring polyvinyl acetate particle 20 grams slowly joins in above-mentioned solution, keep stirring always, after resin adds, bath temperature is elevated to 80 DEG C of constant temperature 8 hours, obtains pale yellow transparent viscous resin solution.
(2) preparation of substrate silver slurry
Get the organic carrier solution of preparation in 30 grams (1), add in 200 ml beakers, keep slowly stirring, measure 2 grams of turpentine oil successively and 0.3 gram of methyl-silicone oil adds in carrier solution, high-speed stirred is to mixing, weigh 10 grams of silver-plated copper powders (silver-plated weight ratio is 10%) again, slowly add, keep stirring, after adding, high-speed stirred is in the carrier dispersed to silver-plated copper powder, then 60 grams of silvered glass powder (silver-plated weight ratio is 40%) are measured, successively slowly add, keep stirring, after adding, high-speed stirred is in the carrier dispersed to silvered glass powder, obtain silvery white slurry.This slurry transfers to rolling repeatedly on three-roller, disperses, is ground to by Hegman grind gage mensuration fineness below 5 μm, finally collects about 100 grams of Granular composite uniform substrate silver slurries.
(3) preparation (embodiment 1-4) of terminal silver slurry
Embodiment 1
Get the substrate silver slurry of preparation in 20 grams (2), add 1 gram of Isosorbide-5-Nitrae-dimethylnaphthalene, in high speed dispersor, mixed at high speed is even to slurry, after being cooled to room temperature, measuring its viscosity and is about 50000 centipoises.This silver slurry is printed onto in PET film by the mode (220 order silk screen) of silk screen printing, and in 120 DEG C of constant temperature ovens, drying 10 minutes, obtains the conductive film that thickness is about 25 μm, measure the conductance of this conductive film subsequently.The various performance datas of silver slurry and conductive film are summed up in Table 1.
Embodiment 2
Get the substrate silver slurry of preparation in 20 grams (2), add 2 grams of Isosorbide-5-Nitrae-dimethylnaphthalenes, in high speed dispersor, mixed at high speed is even to slurry, after being cooled to room temperature, measuring its viscosity and is about 40000 centipoises.This silver slurry is printed onto in PET film by the mode (220 order silk screen) of silk screen printing, and in 120 DEG C of constant temperature ovens, drying 10 minutes, obtains the conductive film that thickness is about 25 μm, measure the conductance of this conductive film subsequently.The various performance datas of silver slurry and conductive film are summed up in Table 1.
Embodiment 3
Get the substrate silver slurry of preparation in 20 grams (2), add 3 grams of Isosorbide-5-Nitrae-dimethylnaphthalenes, in high speed dispersor, mixed at high speed is even to slurry, after being cooled to room temperature, measuring its viscosity and is about 35000 centipoises.This silver slurry is printed onto in PET film by the mode (220 order silk screen) of silk screen printing, and in 120 DEG C of constant temperature ovens, drying 10 minutes, obtains the conductive film that thickness is about 25 μm, measure the conductance of this conductive film subsequently.The various performance datas of silver slurry and conductive film are summed up in Table 1.
Embodiment 4
Get the substrate silver slurry of preparation in 20 grams (2), add 4 grams of Isosorbide-5-Nitrae-dimethylnaphthalenes, in high speed dispersor, mixed at high speed is even to slurry, after being cooled to room temperature, measuring its viscosity and is about 30000 centipoises.This silver slurry is printed onto in PET film by the mode (220 order silk screen) of silk screen printing, and in 120 DEG C of constant temperature ovens, drying 10 minutes, obtains the conductive film that thickness is about 25 μm, measure the conductance of this conductive film subsequently.The various performance datas of silver slurry and conductive film are summed up in Table 1.
Table 1 embodiment 1-4 Data Summary compares
Remarks: silver-plated copper powder and silvered glass powder content be its whole silver slurry in weight ratio content.
Data as can be seen from table 1, composite conducting silver slurry of the present invention is under silver content only has the condition of about 20%, show the silver content of the common silver slurry of good conductivity (0.05-0.11 Ω/◇, 25 μm) close electric conductivity more than 60%.In addition, composite silver pulp density of the present invention is low, only has about 1.50g/mL, and common silver-colored pulp density is usual all at more than 2.0g/mL, therefore, and the theoretical coverage area (30-40m of composite silver slurry of the present invention
2/ L/mil) large, be common silver slurry (10-20m
2/ L/mil) 2-3 doubly.In sum, composite silver slurry of the present invention is starched with common silver and is contrasted, not only the production cost of silver-colored slurry own reduces (low silver content), and its actual application cost also reduces (theoretical coverage area is large) greatly, has important market using value.
Claims (7)
1. a low silver content composite conducting silver slurry, is characterized in that, with weight parts, comprise 5-15 part silver-plated copper powder, 30-50 part silvered glass powder, 5-15 part macromolecule resin, 20-40 part organic solvent, other additives of 1-5 part.
2. low silver content composite conducting silver slurry according to claim 1, it is characterized in that, described silver-plated copper powder is spherical particle, and particle size is 1-3 μm, and electroplate content is 5-15% (weight ratio), and tap density is 3-4g/mL.
3. low silver content composite conducting silver slurry according to claim 1, it is characterized in that, described silvered glass powder is sheet-like particle, and particle size is 2-8 μm, and electroplate content is 20-60% (weight ratio), and tap density is 0.5-1.5g/mL.
4. low silver content composite conducting silver slurry according to claim 1, it is characterized in that, described macromolecule resin is selected from modified poly ethylene or polyester resin.
5. low silver content composite conducting silver slurry according to claim 1, it is characterized in that, described organic solvent is selected from high boiling lipid, ketone or aromatic hydrocarbon solvent.
6. low silver content composite conducting silver slurry according to claim 1, it is characterized in that, other described additives comprise levelling agent and defoamer, and the weight ratio of the two is respectively 1-4 and 0.1-1.5.Described levelling agent is selected from one or more in cyclohexanone, turpentine oil, castor oil, tributyl phosphate; Described defoamer is selected from one or more in terpinol, methyl-silicone oil, n-hexyl alcohol.
7. a preparation method for low silver content composite conducting silver slurry, it is characterized in that, the method comprises following processing step:
(1) preparation of organic carrier
According to percentage by weight, 1 part of macromolecule resin (modified poly ethylene or polyester) is joined in 5 parts of organic solvents (lipid or ketone or arene), being heated to 60-90 DEG C is stirred well to after resin dissolves completely, and then keep stirring 8 hours in the thermostat water bath being placed on 80 DEG C, finally obtain the organic carrier that viscosity at ambient temperature is 8000-10000 centipoise.
(2) configuration of substrate silver slurry
According to percentage by weight, the silvered glass powder of the silver-plated copper powder of 5-15%, 30-50%, the organic carrier of 10-30%, the additive of 1-5% are fully mixed under mechanical stirring, re-uses high-speed stirred high speed dispersion, obtain uniform slurry.This slurry transfers to rolling repeatedly on three-roller, disperses, is ground to by Hegman grind gage mensuration fineness below 5 μm.
(3) production of terminal silver slurry
The substrate silver obtained in (2) is starched in high speed dispersor, the viscosity, electric conductivity etc. of silver slurry is regulated by adding solvent or carrier (5-20% weight ratio) on a small quantity, finally obtain the slurry that can be directly used in silk screen printing, its viscosity at ambient temperature is 30000-50000 centipoise.
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Cited By (7)
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| CN104752006A (en) * | 2015-02-13 | 2015-07-01 | 佛山市中彩科技有限公司 | Preparation method of conductive silver paste |
| CN106710716A (en) * | 2016-12-19 | 2017-05-24 | 东莞珂洛赫慕电子材料科技有限公司 | Method for preparing nano electronic paste |
| CN106782884A (en) * | 2016-12-19 | 2017-05-31 | 东莞珂洛赫慕电子材料科技有限公司 | A kind of preparation method of nano-powder base electric slurry |
| CN109461515A (en) * | 2018-11-07 | 2019-03-12 | 刘紫嫣 | A kind of high temperature sintering conductive silver paste and preparation method thereof |
| CN110520485A (en) * | 2017-03-09 | 2019-11-29 | 皮尔金顿集团有限公司 | Electric conductivity ink composition |
| WO2021063149A1 (en) * | 2019-09-30 | 2021-04-08 | 无锡帝科电子材料股份有限公司 | Conductive paste, preparation method therefor, application thereof, solar cell electrode having same, and solar cell |
| CN115348743A (en) * | 2022-09-19 | 2022-11-15 | 广东绿展科技有限公司 | Method for printing circuit on curved carrier and curved printed circuit |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104752006A (en) * | 2015-02-13 | 2015-07-01 | 佛山市中彩科技有限公司 | Preparation method of conductive silver paste |
| CN106710716A (en) * | 2016-12-19 | 2017-05-24 | 东莞珂洛赫慕电子材料科技有限公司 | Method for preparing nano electronic paste |
| CN106782884A (en) * | 2016-12-19 | 2017-05-31 | 东莞珂洛赫慕电子材料科技有限公司 | A kind of preparation method of nano-powder base electric slurry |
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| CN110520485A (en) * | 2017-03-09 | 2019-11-29 | 皮尔金顿集团有限公司 | Electric conductivity ink composition |
| JP2020514502A (en) * | 2017-03-09 | 2020-05-21 | ピルキントン グループ リミテッド | Conductive ink composition |
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| CN109461515A (en) * | 2018-11-07 | 2019-03-12 | 刘紫嫣 | A kind of high temperature sintering conductive silver paste and preparation method thereof |
| WO2021063149A1 (en) * | 2019-09-30 | 2021-04-08 | 无锡帝科电子材料股份有限公司 | Conductive paste, preparation method therefor, application thereof, solar cell electrode having same, and solar cell |
| CN115348743A (en) * | 2022-09-19 | 2022-11-15 | 广东绿展科技有限公司 | Method for printing circuit on curved carrier and curved printed circuit |
| CN115348743B (en) * | 2022-09-19 | 2024-05-10 | 广东绿展科技有限公司 | Method for printing circuit on curved carrier and curved printed circuit |
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