CN105097069B - 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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- CN105097069B CN105097069B CN201510400609.2A CN201510400609A CN105097069B CN 105097069 B CN105097069 B CN 105097069B CN 201510400609 A CN201510400609 A CN 201510400609A CN 105097069 B CN105097069 B CN 105097069B
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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 is and in particular to a kind of high-resolution, high connductivity curing type silver paste,
The invention still further relates to the preparation method of this high-resolution, high connductivity curing type silver paste.
Background technology
Conductive silver paste is one of key foundation material of printing thick-film electronic components and parts, is widely used in electronic information neck
Domain, provides conducting wiring for it, and consumption is very huge.At present, electronic information field is to the miniaturization of product and integrated proposition
Higher requirement, this forces conducting wiring must possess less live width and distance between centers of tracks, and relatively low impedance.Therefore, open
Send out and take into account high-resolution printing capability and the conductive silver paste of low square resistance will bring wide utilization prospect.
For conductive silver paste, often conflicting between high-resolution and high connductivity, possess larger in the selecting party face of raw material
Difference.Argentum powder aspect, in general, flake silver powder is conducive to the high conduction performance of film layer, and the bigger impedance of radius-thickness ratio is less;
But, excessive radius-thickness ratio can cause slurry wire drawing characteristic notable thus reducing printed resolution again.Resin aspect, less point
Son amount is conducive to higher printed resolution, and less molecular weight can make the conductive capability of film layer and mechanical property
Decline, so having to look for suitable solution route.
Silk screen printing is very ripe thick film preparation, be widely used in printed electronic product large area,
Low cost manufactures.At present, mainly there are two kinds using the method that silk-screen printing technique prepares fine wire, a kind of direct wiring, separately
One kind adopts laser ablation, and the versatility silver paste possessing both performances can expand its engineering application field.For versatility
Silver paste, its uniformity is particularly significant, and the uneven composition (such as soft-agglomerated, bubble etc.) in system will have influence on two kinds of cloth simultaneously
The quality of forming film of line method.Accordingly, it would be desirable to select suitable formula and preparation technology to realize good uniformity.
Content of the invention
The invention aims to overcoming above-mentioned the deficiencies in the prior art, provide a kind of high-resolution, high connductivity curing type
Silver paste and preparation method thereof.This silver paste is applied to silk-screen printing technique, and possesses higher printed resolution, after low-temperature setting
There is relatively low resistance, there is high-resolution and high conductivity simultaneously.Meanwhile, the product of the present invention be also equipped with good general
Property, can be directly used for printed wiring, also can use as laser silver paste.
For solving above-mentioned technical problem, present invention proposition technical scheme below:
A kind of high-resolution, high connductivity curing type silver paste are it is characterised in that described conductive silver paste includes following components and content
(wt%):
Micron order argentum powder 69.5%~75%,
Polyurethane based resin 6%~12%,
Organic solvent 16%~25%,
Additive 1~4.5%;
Described micron order argentum powder is obtained piece powder a and the piece powder of different radius-thickness ratios by one species ball powder through different ball-milling technologies
B forms, can modulation ratio, wherein class ball powder as needed between a and b: apparent density is 2.5g/cm3~3.6g/cm3, its grain
Footpath is distributed d50For 0.8 μm~1.2 μm;Piece powder a: apparent density is 1.8g/cm3~2.5g/cm3, its particle diameter distribution d50For 1.8 μm
~2.1 μm;Piece powder b: apparent density is 0.8g/cm3~1.5g/cm3, its particle diameter distribution d50For 2.5 μm~3.5 μm.
Described polyurethane based resin, between 10000~20000, vitrification point is 50 DEG C~80 to its number-average molecular weight
℃.
Described organic solvent Ketohexamethylene, isophorone, ethylene glycol ether acetate (cac), propylene glycol methyl ether acetate
(pma), the high boiling solvent such as ethylene glycol monobutyl ether (bcs), dibasic acid ester (dbe), n- methyl pyrrolidone (nmp).
Described additive includes auxiliary rheological agents and firming agent, wherein auxiliary rheological agents 0%~1%, firming agent 1%~4.5%.Rheology
Auxiliary agent is at least one in conductive black and polyamide wax, and conductive black is nanometer spherical granule, its particle diameter d50Less than 30nm.
Firming agent is the latent curing agent of difunctional or trifunctional, 80 DEG C~130 DEG C of activation temperature.
A kind of high-resolution, the preparation method of high connductivity curing type silver paste are it is characterised in that the method includes the steps of:
Step one, prepared by resin solution carrier
First described organic solvent is mixed with toner, poly- ammonia that solid content 25%~40% after heated dissolving, is obtained
Ester resin solution;
Step 2, silver paste is pre-dispersed
Using planetary stirring machine, the resin solution preparing and electrically conductive particles are mixed, mixing is carried out in three steps, successively
Under 850r/min~1050r/min revolution speed stirring 15s~35s, stir under 1200 r/min~1550r/min revolution speed
Mix 100s~150s, stir 40s~60s, prepared electrically conductive ink mixture under 800r/min~900r/min revolution speed;Add again
Plus described additive, and according to the mixing of aforementioned three-step approach;
Step 3, three-roll rolling silver paste
The slurry being obtained by step 2 is put into three-high mill be ground, specific process parameter is: successively according to 90/
60th, 60/30,30/20,20/10(gap, μm) each three times, 150~300 revolutions per seconds of speed, prepared slurry fineness should control in 5 μ
Below m.
Step 4, vacuum defoamation
The slurry being obtained by step 3 is put into vacuum degasing machine and carries out vacuum defoamation.
The difference being obtained through different ball-milling technologies by one species ball powder from above technical scheme, described electrically conductive particles
The piece powder a of radius-thickness ratio and piece powder b composition, the wherein radius-thickness ratio of piece powder a are less than b.It is previously mentioned that flake silver powder is conducive to film
The high conduction performance of layer, and the bigger impedance of radius-thickness ratio is less, and excessive radius-thickness ratio can cause slurry wire drawing characteristic notable
Thus reducing printed resolution.That is, piece powder a is beneficial to the high-resolution printing capability of silver paste, and piece powder b is beneficial to the high conductivity of film layer
Can, high-resolution and high connductivity problem can be taken into account by modulating ratio between a and b.Meanwhile, piece powder a and b is micron order powder
End, particle diameter is little, favorable dispersibility, can improve the uniformity of silver paste further, reduces final fineness.
Above-mentioned conductive silver paste, from low-molecular-weight, low Tg, not the polyurethane of end-blocking completely be main body tree
Fat, the polyurethane of this class feature makes slurry possess good printed resolution (beneficial to forming fine wiring), but film layer conductive capability
Not enough with mechanical property.Here select suitable firming agent, when film layer is subject to heat cure, polyurethane molecular increases and forming part
Crosslinking, can effectively optimize film layer conductive capability and mechanical property.
Silver paste product in the present invention, using at least one in conductive black and polyamide wax as auxiliary rheological agents, this two
Plant elite auxiliary agent, improve printing except rheological behavior can be improved;The dispersibility that system can also be improved reduces system
Soft-agglomerated.Meanwhile, above-mentioned silver paste preparation method reduces silver paste fineness it is also possible to effectively improve dispersibility;Step 4 also can subtract
Bubble in few silver paste.
Based on above-mentioned characteristic, the conductive silver paste in the present invention can be widely used in touch screen, Flexible Displays, illumination, thin film
The fields such as switch, provide the conducting wiring of high accuracy, low resistance for it.
Specific embodiment
Below by specific embodiment, the present invention is described in further detail, but guarantor not thereby limiting the invention
Shield scope.
Embodiment 1~3:
Embodiment 1~3 is fixing micron order argentum powder, polyurethane based resin, organic solvent, the content of additive, changes piece
Powder a and the relative amount of piece powder b.Wherein embodiment 1, the mass ratio of a and b is 10:0;Embodiment 2, the mass ratio of a and b is 9:
1;Embodiment 3, the mass ratio of a and b is 7:3.
The component of embodiment 1~3 and content (wt%) are as shown in table 1.
Described micron order argentum powder is obtained piece powder a and the piece powder of different radius-thickness ratios by one species ball powder through different ball-milling technologies
B forms, wherein class ball powder: apparent density is 2.5g/cm3~3.6g/cm3, its particle diameter distribution d50For 0.8 μm~1.2 μm;Piece powder
A: apparent density is 1.8g/cm3~2.5g/cm3, its particle diameter distribution d50For 1.8 μm~2.1 μm;Piece powder b: apparent density is
0.8g/cm3~1.5g/cm3, its particle diameter distribution d50For 2.5 μm~3.5 μm.
Described polyurethane based resin, its number-average molecular weight 1~20,000,50 DEG C~80 DEG C about of vitrification point.Described organic
Solvent is dibasic acid ester (dbe).Described additive includes auxiliary rheological agents and firming agent, wherein auxiliary rheological agents 0.5%, firming agent
3.5%.Auxiliary rheological agents are conductive black, and firming agent is the latent curing agent of trifunctional, 120 DEG C of activation temperature.
The preparation method of above-mentioned conductive silver paste, comprises the steps of
Step one, prepared by resin solution carrier
First described organic solvent is mixed with toner, the polyurethane tree of solid content 26.9% after heated dissolving, is obtained
Lipoprotein solution;
Step 2, silver paste is pre-dispersed
Using planetary stirring machine, the resin solution preparing and electrically conductive particles are mixed, mixing is carried out in three steps, successively
Under 850r/min~1050r/min revolution speed stirring 15s~35s, stir under 1200 r/min~1550r/min revolution speed
Mix 100s~150s, stir 40s~60s, prepared electrically conductive ink mixture under 800r/min~900r/min revolution speed;Again according to
Secondary interpolation conductive black and firming agent, and according to the mixing of aforementioned three-step approach;
Step 3, three-roll rolling silver paste
The slurry being obtained by step 2 is put into three-high mill be ground, specific process parameter is: successively according to 90/
60th, 60/30,30/20,20/10(gap, μm) each three times, 150~300 revolutions per seconds of speed, prepared slurry fineness should control in 5 μ
Below m;
Step 4, vacuum defoamation
The slurry being obtained by step 3 is put into vacuum degasing machine and carries out vacuum defoamation.
Using silk-screen printing technique, the silver paste in embodiment 1~3 is carried out on glass respectively direct wiring and laser incising
Erosion, as shown in table 2, the performance test results of each embodiment are as shown in table 3 for technique.
Embodiment 4~6:
Embodiment 4~6 is the relative amount of piece powder a and piece powder b in fixing micron order argentum powder, and the mass ratio of wherein a and b is solid
It is set to 9:1.Change the content of other components.
The component of embodiment 4~6 and content (wt%) are as shown in table 4.
Described micron order argentum powder is obtained piece powder a and the piece powder of different radius-thickness ratios by one species ball powder through different ball-milling technologies
B forms, and the mass ratio of a and b is 9:1, wherein class ball powder: apparent density is 2.5g/cm3~3.6g/cm3, its particle diameter distribution d50
For 0.8 μm~1.2 μm;Piece powder a: apparent density is 1.8g/cm3~2.5g/cm3, its particle diameter distribution d50For 1.8 μm~2.1 μm;
Piece powder b: apparent density is 0.8g/cm3~1.5g/cm3, its particle diameter distribution d50For 2.5 μm~3.5 μm.
Described polyurethane based resin, its number-average molecular weight 1~20,000,50 DEG C~80 DEG C about of vitrification point.Described organic
Solvent is dibasic acid ester (dbe).Described additive is polyamide wax and conductive black.Firming agent is that the latency of trifunctional is solid
Agent, 120 DEG C of activation temperature.
The preparation method of above-mentioned conductive silver paste, comprises the steps of
Step one, prepared by resin solution carrier
First described organic solvent is mixed with toner, after heated dissolving, polyurethane resin solution is obtained;
Step 2, silver paste is pre-dispersed
Using planetary stirring machine, the resin solution preparing and electrically conductive particles are mixed, mixing is carried out in three steps, successively
Under 850r/min~1050r/min revolution speed stirring 15s~35s, stir under 1200 r/min~1550r/min revolution speed
Mix 100s~150s, stir 40s~60s, prepared electrically conductive ink mixture under 800r/min~900r/min revolution speed;Again according to
Secondary interpolation polyamide wax (or conductive black) and firming agent, and according to the mixing of aforementioned three-step approach;
Step 3, three-roll rolling silver paste
The slurry being obtained by step 2 is put into three-high mill be ground, specific process parameter is: successively according to 90/
60th, 60/30,30/20,20/10(gap, μm) each three times, 150~300 revolutions per seconds of speed, prepared slurry fineness should control in 5 μ
Below m;
Step 4, vacuum defoamation
The slurry being obtained by step 3 is put into vacuum degasing machine and carries out vacuum defoamation.
Using silk-screen printing technique, the silver paste in embodiment 4~6 is carried out on glass respectively direct wiring and laser carving
Carve, as shown in table 2, the performance test results of each embodiment are as shown in table 5 for technique.
By embodiment 2 with 4 contrasts it is found that the resolution changing polyamide wax into after conductive black direct wiring carries
Height, and laser ablation resolution reduces.Embodiment 5 explanation can be adjusted by the relative amount of suitable change argentum powder and resin
Sheet resistance processed.Add while embodiment 6 explanation polyamide wax and conductive black and can finely tune printed resolution.
There are above-mentioned table 3 and table 5 as can be seen that made conductive silver paste of the present invention and preparation method thereof, can effectively carry
While high printed resolution, improve the electric conductivity of film layer;And the film layer optimizing also has embodied good conduction simultaneously
Performance and mechanical property;Described silver paste preparation method can also effectively improve dispersibility, reduces the fineness of silver paste, reduces silver
Bubble in slurry.
Claims (5)
1. a kind of high-resolution, high connductivity curing type silver paste are it is characterised in that described conductive silver paste includes following components and content
(wt%):
Micron order argentum powder 69.5%~75%,
Polyurethane based resin 6%~12%,
Organic solvent 16%~25%,
Additive 1~5%,
Described micron order argentum powder is obtained piece powder a and the piece powder b group of different radius-thickness ratios by one species ball powder through different ball-milling technologies
Become, can modulation ratio, wherein class ball powder as needed between a and b: apparent density is 2.5g/cm3~3.6g/cm3, its particle diameter divides
Cloth d50For 0.8 μm~1.2 μm;Piece powder a: apparent density is 1.8g/cm3~2.5g/cm3, its particle diameter distribution d50For 1.8 μm~
2.1μm;Piece powder b: apparent density is 0.8g/cm3~1.5g/cm3, its particle diameter distribution d50For 2.5 μm~3.5 μm.
2. high-resolution according to claim 1, high connductivity curing type silver paste be it is characterised in that described polyurethane based resin,
Between 10000~20000, vitrification point is 50 DEG C~80 DEG C to its number-average molecular weight.
3. high-resolution according to claim 1, high connductivity curing type silver paste are it is characterised in that described organic solvent is ring
Hexanone, isophorone, ethylene glycol ether acetate (cac), propylene glycol methyl ether acetate (pma), ethylene glycol monobutyl ether (bcs),
Dibasic acid ester (dbe), n- methyl pyrrolidone (nmp) high boiling solvent.
4. high-resolution according to claim 1, high connductivity curing type silver paste are it is characterised in that described additive includes flowing
Become auxiliary agent and firming agent, wherein auxiliary rheological agents 0%~1%, firming agent 1%~5%, described auxiliary rheological agents are conductive black and polyamide
At least one in wax, described conductive black is nanometer spherical granule, its particle diameter d50Less than 30nm, described firming agent is difunctionality
Group or the latent curing agent of trifunctional, 80 DEG C~130 DEG C of activation temperature.
5. the preparation method of a kind of high-resolution as claimed in claim 1, high connductivity curing type silver paste is it is characterised in that the party
Method comprises the steps of
Step one, prepared by resin solution carrier
First described organic solvent is mixed with toner, polyurethane tree that solid content 25%~40% after heated dissolving, is obtained
Lipoprotein solution;
Step 2, silver paste is pre-dispersed
Using planetary stirring machine, the resin solution preparing and electrically conductive particles are mixed, mixing is carried out in three steps, and successively exists
Stirring 15s~35s under 850r/min~1050r/min revolution speed, stir under 1200 r/min~1550r/min revolution speed
40s~60s, prepared electrically conductive ink mixture is stirred under 100s~150s, 800r/min~900r/min revolution speed;Add again
Described additive, and according to the mixing of aforementioned three-step approach;
Step 3, three-roll rolling silver paste
The slurry being obtained by step 2 is put into three-high mill be ground, specific process parameter is: successively according to running roller gap
For 90 μm/60 μm, 60 μm/30 μm, 30 μm/20 μm, each operation of 20 μm/10 μm of parameter three times, 200 revolutions per seconds of speed, prepared
Slurry fineness should control below 5 μm;
Step 4, vacuum defoamation
The slurry being obtained by step 3 is put into vacuum degasing machine and carries out vacuum defoamation.
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CN105679407B (en) * | 2016-01-05 | 2018-05-04 | 张跃 | A kind of low-temperature cured conductive silver paste and preparation method thereof and institute's made membrane |
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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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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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 |