CN105097069A - High-resolution and high-conductivity curved type silver paste and preparation method thereof - Google Patents
High-resolution and high-conductivity curved type silver paste and preparation method thereof Download PDFInfo
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- CN105097069A CN105097069A CN201510400609.2A CN201510400609A CN105097069A CN 105097069 A CN105097069 A CN 105097069A CN 201510400609 A CN201510400609 A CN 201510400609A CN 105097069 A CN105097069 A CN 105097069A
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Abstract
The invention relates to a high-resolution and high-conductivity curved type silver paste which comprises the following constituents: micro-sized silver powder, polyurethane resin, an organic solvent and an additive, wherein the micro-sized silver powder comprises two powder pieces having different radius-thickness rates, and the additive comprises a rheological agent and a curing agent. The silver paste is a low-temperature curved type silver paste suitable for a silk-screen printing process, has high printing resolution under the printing process and has low resistance after low-temperature curving. The product disclosed by the invention also has high universality, can be directly used for printed wiring, and also can serve as a laser silver paste for use.
Description
Technical field
The present invention relates to a kind of ink class field of material technology, be specifically related to a kind of high-resolution, high connductivity curing type silver slurry, the invention still further relates to the preparation method of this high-resolution, high connductivity curing type silver slurry.
Background technology
Conductive silver paste is one of key foundation material of printing thick-film electronic components and parts, and be widely used in electronic information field, for it provides conducting wiring, consumption is very huge.At present, electronic information field is to the miniaturization of product and integratedly have higher requirement, and this forces conducting wiring must possess less live width and distance between centers of tracks, and lower impedance.Therefore, develop the conductive silver paste taking into account high-resolution printing capability and low square resistance and will bring wide utilization prospect.
For conductive silver paste, often conflicting between high-resolution and high connductivity, possess larger difference in the selecting party face of raw material.Silver powder aspect, in general, flake silver powder is conducive to the high conduction performance of rete, and the larger impedance of radius-thickness ratio is less; But excessive radius-thickness ratio can cause again slurry wire drawing characteristic significantly thus reduce printed resolution.Resin aspect, less molecular weight is conducive to higher printed resolution, and less molecular weight can make the conductive capability of rete and mechanical property decline to some extent, so must search out suitable solution route.
Silk screen printing is very ripe thick film preparation, is widely used in the large area of printed electronic product, low cost manufacture.At present, the method adopting silk-screen printing technique to prepare fine wire mainly contains two kinds, a kind of direct wiring, another kind of employing laser ablation, and the versatility silver slurry possessing these two kinds of performances can expand its engineering application field.For versatility silver slurry, its uniformity is very important, and uneven composition in system (such as soft-agglomerated, bubble etc.) will have influence on the quality of forming film of two kinds of wiring methods simultaneously.Therefore, need to select suitable formula and preparation technology to realize good uniformity.
Summary of the invention
The object of the invention is to overcome above-mentioned the deficiencies in the prior art, a kind of high-resolution, high connductivity curing type silver slurry and preparation method thereof is provided.This silver slurry is applicable to silk-screen printing technique, and possesses higher printed resolution, has lower resistance, namely have high-resolution and high conductivity simultaneously after low-temperature setting.Meanwhile, product of the present invention also possesses good versatility, can be directly used in printed wiring, also can be used as laser silver slurry and uses.
For solving the problems of the technologies described above, the present invention proposes following technical scheme:
High-resolution, a high connductivity curing type silver slurry, it is characterized in that, described conductive silver paste comprises following component and content (Wt%):
Micron order silver powder 60% ~ 75%,
Polyurethane based resin 6% ~ 12%,
Organic solvent 16% ~ 25%,
Additive 1 ~ 5%;
Described micron order silver powder obtains the sheet powder A of Different Diameter thickness rate and sheet powder B by one species ball powder through different spheroidal graphite technique and forms, can modulation ratio, wherein class ball powder as required between A and B: apparent density is 2.5g/cm
3~ 3.6g/cm
3, its domain size distribution D
50it is 0.8 μm ~ 1.2 μm; Sheet powder A: apparent density is 1.8g/cm
3~ 2.5g/cm
3, its domain size distribution D
50it is 1.8 μm ~ 2.1 μm; Sheet powder B: apparent density is 0.8g/cm
3~ 1.5g/cm
3, its domain size distribution D
50it is 2.5 μm ~ 3.5 μm.
Described polyurethane based resin, its number-average molecular weight is between 10000 ~ 20000, and vitrification point is 50 DEG C ~ 80 DEG C.
The high boiling solvents such as described organic solvent cyclohexanone, isophorone, ethylene glycol ether acetate (CAC), 1-Methoxy-2-propyl acetate (PMA), ethylene glycol monobutyl ether (BCS), dibasic acid ester (DBE), 1-METHYLPYRROLIDONE (NMP).
Described additive comprises auxiliary rheological agents and curing agent, wherein auxiliary rheological agents 0% ~ 1%, curing agent 1% ~ 5%.Auxiliary rheological agents is at least one in conductive black and polyamide wax, and conductive black is nanometer spherical particle, its particle diameter D
50be less than 30nm.Curing agent is the latent curing agent of difunctional or trifunctional, activation temperature 80 DEG C ~ 130 DEG C.
A preparation method for high-resolution, high connductivity curing type silver slurry, it is characterized in that, the method includes the steps of:
Step one, prepared by resin solution carrier
First described organic solvent is mixed with toner, after heating for dissolving obtained solid content 25% ~ 40% polyurethane resin solution;
Step 2, silver slurry is pre-dispersed
Planetary stirring machine is adopted the resin solution prepared and electrically conductive particles to be mixed, mixing point three steps are carried out, 40s ~ 60s is stirred, obtained electrically conductive ink mixture under stirring 100s ~ 150s, 800r/min ~ 900r/min revolution speed under successively stirring 15s ~ 35s, 1200r/min ~ 1550r/min revolution speed under 850r/min ~ 1050r/min revolution speed; Add described additive again, and mix according to aforementioned three-step approach;
Step 3, three-roll rolling silver slurry
The slurry obtained by step 2 is put into three-high mill grind, concrete technology parameter is: successively according to 90/60,60/30,30/20,20/10(gap, μm) each three times, speed 150 ~ 300 revolutions per seconds, obtained slurry fineness should control below 5 μm.
Step 4, vacuum defoamation
The slurry obtained by step 3 is put into vacuum defoamation machine and carries out vacuum defoamation.
From above technical scheme, sheet powder A and the sheet powder B of the Different Diameter thickness rate that described electrically conductive particles is obtained through different spheroidal graphite technique by one species ball powder form, and wherein the radius-thickness ratio of sheet powder A is less than B.Mentioned the high conduction performance that flake silver powder is conducive to rete above, and the larger impedance of radius-thickness ratio is less, and excessive radius-thickness ratio can cause slurry wire drawing characteristic significantly thus reduce printed resolution.That is, sheet powder A is beneficial to the high-resolution printing capability of silver slurry, and sheet powder B is beneficial to the high conduction performance of rete, can take into account high-resolution and high connductivity problem by ratio between modulation A and B.Meanwhile, sheet powder A and B is micron powder, and particle diameter is little, favorable dispersibility, can improve the uniformity of silver slurry further, reduce final fineness.
Above-mentioned conductive silver paste, select low-molecular-weight, low Tg, the polyurethane of end-blocking is not matrix resin completely, the polyurethane of this class feature makes slurry possess good printed resolution (being beneficial to forming fine wiring), but rete conductive capability and mechanical property deficiency.Here select suitable curing agent, when rete is by hot curing, polyurethane molecular increases and forming section is cross-linked, and can effectively optimize rete conductive capability and mechanical property.
Silver slurry product in the present invention, using at least one in conductive black and polyamide wax as auxiliary rheological agents, these two kinds elite auxiliary agents, improve printing except improving rheological behavior; The dispersiveness can also improving system reduces the soft-agglomerated of system.Meanwhile, above-mentioned silver slurry preparation method, also effectively can improve the dispersed silver that reduces and starch fineness; Step 4 also can reduce the bubble in silver slurry.
Based on above-mentioned characteristic, the conductive silver paste in the present invention can be widely used in the fields such as touch-screen, Flexible Displays, illumination, thin film switch, for it provides the conducting wiring of high accuracy, low resistance.
Embodiment
Below by specific embodiment, the present invention is described in further detail, but protection range not thereby limiting the invention.
Embodiment 1 ~ 3:
Embodiment 1 ~ 3 is the content of fixing micron order silver powder, polyurethane based resin, organic solvent, additive, changes the relative amount of sheet powder A and sheet powder B.Wherein the mass ratio of embodiment 1, A and B is 10:0; The mass ratio of embodiment 2, A and B is 9:1; The mass ratio of embodiment 3, A and B is 7:3.
The component of embodiment 1 ~ 3 and content (Wt%) as shown in table 1.
Described micron order silver powder obtains the sheet powder A of Different Diameter thickness rate and sheet powder B by one species ball powder through different spheroidal graphite technique and forms, wherein class ball powder: apparent density is 2.5g/cm
3~ 3.6g/cm
3, its domain size distribution D
50it is 0.8 μm ~ 1.2 μm; Sheet powder A: apparent density is 1.8g/cm
3~ 2.5g/cm
3, its domain size distribution D
50it is 1.8 μm ~ 2.1 μm; Sheet powder B: apparent density is 0.8g/cm
3~ 1.5g/cm
3, its domain size distribution D
50it is 2.5 μm ~ 3.5 μm.
Described polyurethane based resin, its number-average molecular weight 1 ~ 20,000, vitrification point 50 DEG C ~ about 80 DEG C.Described organic solvent is dibasic acid ester (DBE).Described additive comprises auxiliary rheological agents and curing agent, wherein auxiliary rheological agents 0.5%, curing agent 3.5%.Auxiliary rheological agents is conductive black, and curing agent is the latent curing agent of trifunctional, activation temperature 120 DEG C.
The preparation method of above-mentioned conductive silver paste, comprises following steps:
Step one, prepared by resin solution carrier
First described organic solvent is mixed with toner, the polyurethane resin solution of obtained solid content 26.9% after heating for dissolving;
Step 2, silver slurry is pre-dispersed
Planetary stirring machine is adopted the resin solution prepared and electrically conductive particles to be mixed, mixing point three steps are carried out, 40s ~ 60s is stirred, obtained electrically conductive ink mixture under stirring 100s ~ 150s, 800r/min ~ 900r/min revolution speed under successively stirring 15s ~ 35s, 1200r/min ~ 1550r/min revolution speed under 850r/min ~ 1050r/min revolution speed; Add conductive black and curing agent successively again, and mix according to aforementioned three-step approach;
Step 3, three-roll rolling silver slurry
The slurry obtained by step 2 is put into three-high mill grind, concrete technology parameter is: successively according to 90/60,60/30,30/20,20/10(gap, μm) each three times, speed 150 ~ 300 revolutions per seconds, obtained slurry fineness should control below 5 μm;
Step 4, vacuum defoamation
The slurry obtained by step 3 is put into vacuum defoamation machine and carries out vacuum defoamation.
Adopt silk-screen printing technique, the silver slurry in embodiment 1 ~ 3 is carried out direct wiring and laser ablation respectively on glass, and technique is as shown in table 2, and the performance test results of each embodiment is as shown in table 3.
Embodiment 4 ~ 6:
Embodiment 4 ~ 6 is the relative amount of sheet powder A and sheet powder B in fixing micron order silver powder, and wherein the mass ratio of A and B is fixed as 9:1.Change the content of other components.
The component of embodiment 4 ~ 6 and content (Wt%) as shown in table 4.
Described micron order silver powder obtains the sheet powder A of Different Diameter thickness rate and sheet powder B by one species ball powder through different spheroidal graphite technique and forms, and the mass ratio of A and B is 9:1, wherein class ball powder: apparent density is 2.5g/cm
3~ 3.6g/cm
3, its domain size distribution D
50it is 0.8 μm ~ 1.2 μm; Sheet powder A: apparent density is 1.8g/cm
3~ 2.5g/cm
3, its domain size distribution D
50it is 1.8 μm ~ 2.1 μm; Sheet powder B: apparent density is 0.8g/cm
3~ 1.5g/cm
3, its domain size distribution D
50it is 2.5 μm ~ 3.5 μm.
Described polyurethane based resin, its number-average molecular weight 1 ~ 20,000, vitrification point 50 DEG C ~ about 80 DEG C.Described organic solvent is dibasic acid ester (DBE).Described additive is polyamide wax and conductive black.Curing agent is the latent curing agent of trifunctional, activation temperature 120 DEG C.
The preparation method of above-mentioned conductive silver paste, comprises following steps:
Step one, prepared by resin solution carrier
First described organic solvent is mixed with toner, obtained polyurethane resin solution after heating for dissolving;
Step 2, silver slurry is pre-dispersed
Planetary stirring machine is adopted the resin solution prepared and electrically conductive particles to be mixed, mixing point three steps are carried out, 40s ~ 60s is stirred, obtained electrically conductive ink mixture under stirring 100s ~ 150s, 800r/min ~ 900r/min revolution speed under successively stirring 15s ~ 35s, 1200r/min ~ 1550r/min revolution speed under 850r/min ~ 1050r/min revolution speed; Add polyamide wax (or conductive black) and curing agent more successively, and mix according to aforementioned three-step approach;
Step 3, three-roll rolling silver slurry
The slurry obtained by step 2 is put into three-high mill grind, concrete technology parameter is: successively according to 90/60,60/30,30/20,20/10(gap, μm) each three times, speed 150 ~ 300 revolutions per seconds, obtained slurry fineness should control below 5 μm;
Step 4, vacuum defoamation
The slurry obtained by step 3 is put into vacuum defoamation machine and carries out vacuum defoamation.
Adopt silk-screen printing technique, the silver slurry in embodiment 4 ~ 6 is carried out direct wiring and laser engraving respectively on glass, and technique is as shown in table 2, and the performance test results of each embodiment is as shown in table 5.
Contrasted can be found by embodiment 2 and 4, after polyamide wax being changed into conductive black, the resolution of direct wiring improves, and laser ablation resolution reduces.Embodiment 5 illustrates can modulate sheet resistance by the relative amount of suitable change silver powder and resin.Add while embodiment 6 illustrates polyamide wax and conductive black and can finely tune printed resolution.
There are above-mentioned table 3 and table 5 to find out, conductive silver paste that the present invention is made and preparation method thereof, while effectively can improving printed resolution, improve the electric conductivity of rete; And the rete optimized also has embodied good electric conductivity and mechanical property simultaneously; Described silver slurry preparation method also effectively can improve dispersiveness, reduces the fineness of silver slurry, reduces the bubble in silver slurry.
Claims (8)
1. a high-resolution, high connductivity curing type silver slurry, it is characterized in that, described conductive silver paste comprises following component and content (Wt%):
Micron order silver powder 60% ~ 75%,
Polyurethane based resin 6% ~ 12%,
Organic solvent 16% ~ 25%,
Additive 1 ~ 5%.
2. high-resolution according to claim 1, high connductivity curing type silver slurry, it is characterized in that, described micron order silver powder obtains the sheet powder A of Different Diameter thickness rate and sheet powder B by one species ball powder through different spheroidal graphite technique and forms, can modulation ratio, wherein class ball powder as required between A and B: apparent density is 2.5g/cm
3~ 3.6g/cm
3, its domain size distribution D
50it is 0.8 μm ~ 1.2 μm; Sheet powder A: apparent density is 1.8g/cm
3~ 2.5g/cm
3, its domain size distribution D
50it is 1.8 μm ~ 2.1 μm; Sheet powder B: apparent density is 0.8g/cm
3~ 1.5g/cm
3, its domain size distribution D
50it is 2.5 μm ~ 3.5 μm.
3. high-resolution according to claim 1, high connductivity curing type silver slurry, it is characterized in that, described polyurethane based resin, its number-average molecular weight is between 10000 ~ 20000, and vitrification point is 50 DEG C ~ 80 DEG C.
4. high-resolution according to claim 1, high connductivity curing type silver slurry, it is characterized in that, described organic solvent is the high boiling solvents such as cyclohexanone, isophorone, ethylene glycol ether acetate, 1-Methoxy-2-propyl acetate, ethylene glycol monobutyl ether, dibasic acid ester, 1-METHYLPYRROLIDONE.
5. high-resolution according to claim 1, high connductivity curing type silver slurry, it is characterized in that, described additive comprises auxiliary rheological agents and curing agent, wherein auxiliary rheological agents 0% ~ 1%, curing agent 1% ~ 5%.
6. high-resolution according to claim 5, high connductivity curing type silver slurry, it is characterized in that, described auxiliary rheological agents is at least one in conductive black and polyamide wax, and conductive black is nanometer spherical particle, its particle diameter D
50be less than 30nm.
7. high-resolution according to claim 5, high connductivity curing type silver slurry, it is characterized in that, described curing agent is the latent curing agent of difunctional or trifunctional, activation temperature 80 DEG C ~ 130 DEG C.
8. a preparation method for high-resolution, high connductivity curing type silver slurry, it is characterized in that, the method includes the steps of:
Step one, prepared by resin solution carrier
First described organic solvent is mixed with toner, after heating for dissolving obtained solid content 25% ~ 40% polyurethane resin solution;
Step 2, silver slurry is pre-dispersed
Planetary stirring machine is adopted the resin solution prepared and electrically conductive particles to be mixed, mixing point three steps are carried out, 40s ~ 60s is stirred, obtained electrically conductive ink mixture under stirring 100s ~ 150s, 800r/min ~ 900r/min revolution speed under successively stirring 15s ~ 35s, 1200r/min ~ 1550r/min revolution speed under 850r/min ~ 1050r/min revolution speed; Add described additive again, and mix according to aforementioned three-step approach;
Step 3, three-roll rolling silver slurry
The slurry obtained by step 2 is put into three-high mill grind, concrete technology parameter is: successively according to 90/60,60/30,30/20,20/10(gap, μm) each three times, speed 200 revolutions per seconds, obtained slurry fineness should control below 5 μm;
Step 4, vacuum defoamation
The slurry obtained by step 3 is put into vacuum defoamation machine and carries out vacuum defoamation.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105632588A (en) * | 2016-02-22 | 2016-06-01 | 昆山海斯电子有限公司 | High-conductivity silver paste and preparation method thereof |
| CN105679407A (en) * | 2016-01-05 | 2016-06-15 | 苏州纳英科纳米材料有限公司 | Low-temperature solidified conductive silver paste and preparation method thereof and prepared film |
| CN106504815A (en) * | 2016-10-21 | 2017-03-15 | 常州亚环环保科技有限公司 | A kind of preparation method of low temperature polyurethane-base conductive silver paste |
| CN106847369A (en) * | 2016-12-15 | 2017-06-13 | 西北稀有金属材料研究院 | A kind of printed form capacitive touch screen low-temperature cured conductive silver paste and preparation method |
| CN106898411A (en) * | 2017-03-20 | 2017-06-27 | 北京市合众创能光电技术有限公司 | A kind of low-temperature setting touch-screen conductive silver paste of suitable laser ablation processing |
| CN107863175A (en) * | 2017-11-22 | 2018-03-30 | 青岛纳印新材料科技有限公司 | A kind of conductive silver paste for high temperature-resistant printing circuit |
| CN108133768A (en) * | 2017-12-25 | 2018-06-08 | 深圳市百柔新材料技术有限公司 | A kind of high conductivity low temperature curing type electrocondution slurry and preparation method thereof |
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| CN101645318A (en) * | 2008-08-07 | 2010-02-10 | 上海昌银电子材料科技有限公司 | Conductive silver paste special for circuit of laptop keyboard and preparation method thereof |
| CN104332214A (en) * | 2014-10-28 | 2015-02-04 | 深圳市思迈科新材料有限公司 | Low-temperature curing conductive silver paste and preparation method thereof |
| CN104464881A (en) * | 2014-11-17 | 2015-03-25 | 昆明贵金属研究所 | Dual-function electric conduction silver paste for touch screen and preparation method and application thereof |
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| JP2004111057A (en) * | 2002-09-13 | 2004-04-08 | Nippon Perunotsukusu Kk | Conductive paste composition |
| CN101645318A (en) * | 2008-08-07 | 2010-02-10 | 上海昌银电子材料科技有限公司 | Conductive silver paste special for circuit of laptop keyboard and preparation method thereof |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105679407A (en) * | 2016-01-05 | 2016-06-15 | 苏州纳英科纳米材料有限公司 | Low-temperature solidified conductive silver paste and preparation method thereof and prepared film |
| CN105632588A (en) * | 2016-02-22 | 2016-06-01 | 昆山海斯电子有限公司 | High-conductivity silver paste and preparation method thereof |
| CN105632588B (en) * | 2016-02-22 | 2018-03-27 | 昆山海斯电子有限公司 | A kind of high conductivity silver paste and preparation method thereof |
| CN106504815A (en) * | 2016-10-21 | 2017-03-15 | 常州亚环环保科技有限公司 | A kind of preparation method of low temperature polyurethane-base conductive silver paste |
| CN106847369A (en) * | 2016-12-15 | 2017-06-13 | 西北稀有金属材料研究院 | A kind of printed form capacitive touch screen low-temperature cured conductive silver paste and preparation method |
| CN106898411A (en) * | 2017-03-20 | 2017-06-27 | 北京市合众创能光电技术有限公司 | A kind of low-temperature setting touch-screen conductive silver paste of suitable laser ablation processing |
| CN107863175A (en) * | 2017-11-22 | 2018-03-30 | 青岛纳印新材料科技有限公司 | A kind of conductive silver paste for high temperature-resistant printing circuit |
| CN108133768A (en) * | 2017-12-25 | 2018-06-08 | 深圳市百柔新材料技术有限公司 | A kind of high conductivity low temperature curing type electrocondution slurry and preparation method thereof |
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Denomination of invention: A high-resolution, high conductivity solidified silver paste and its preparation method Effective date of registration: 20220621 Granted publication date: 20170125 Pledgee: Rizhao Donggang Rural Commercial Bank Co.,Ltd. Pledgor: RIZHAO ZHONGBANG ELECTRONIC Co.,Ltd. Registration number: Y2022980008408 |
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