CN109493994A - Critical superconduction silver paste based on linear silver nano-grain and preparation method thereof - Google Patents
Critical superconduction silver paste based on linear silver nano-grain and preparation method thereof Download PDFInfo
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- CN109493994A CN109493994A CN201811624534.6A CN201811624534A CN109493994A CN 109493994 A CN109493994 A CN 109493994A CN 201811624534 A CN201811624534 A CN 201811624534A CN 109493994 A CN109493994 A CN 109493994A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/20—Conductive material dispersed in non-conductive organic material
- H01B1/22—Conductive material dispersed in non-conductive organic material the conductive material comprising metals or alloys
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/20—Conductive material dispersed in non-conductive organic material
- H01B1/24—Conductive material dispersed in non-conductive organic material the conductive material comprising carbon-silicon compounds, carbon or silicon
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B13/00—Apparatus or processes specially adapted for manufacturing conductors or cables
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- G—PHYSICS
- G06—COMPUTING; CALCULATING OR COUNTING
- G06F—ELECTRIC DIGITAL DATA PROCESSING
- G06F3/00—Input arrangements for transferring data to be processed into a form capable of being handled by the computer; Output arrangements for transferring data from processing unit to output unit, e.g. interface arrangements
- G06F3/01—Input arrangements or combined input and output arrangements for interaction between user and computer
- G06F3/03—Arrangements for converting the position or the displacement of a member into a coded form
- G06F3/041—Digitisers, e.g. for touch screens or touch pads, characterised by the transducing means
- G06F3/044—Digitisers, e.g. for touch screens or touch pads, characterised by the transducing means by capacitive means
Abstract
A kind of critical superconduction silver paste provided by the invention, including (weight ratio): linear silver nano-grain 75-85%, dispersing agent 0.1-4%, levelling agent 0-2%, organic resin 2.5-8%, conductive nano carbon particle 1.3-3.8%, solvent 8-20%, the linear nano silver particle length is 1-5 μm, width 10-15nm.The critical superconduction silver paste resistivity that the present invention is prepared is almost 0, and sheet resistance is only 1.5-2.9 Ω/, has very excellent electric conductivity.
Description
Technical field
The present invention relates to a kind of critical superconduction silver pastes and preparation method thereof, more particularly to one kind is based on linear silver nano-grain
Critical superconduction laser-induced thermal etching silver paste and preparation method thereof.
Background technique
With the rapid development of economy, people's lives quality is also with improve, either for the purpose amused and diverted oneself,
Connection between kith and kin still works, and mobile phone already becomes essential tool in everyone life, with smart phone
Fast development, handset touch panel quality largely determine user experience.It is conductive in capacitive touch screen
Silver paste is primarily used to do the electrode material of four edges or four pins, plays conclusive work to the reaction rate of capacitance plate
With.
The Chinese invention patent of Publication No. CN107123459A, which discloses, has carried out a kind of conductive silver paste, including airborne body and table
The Argent grain of organic compound is modified in face, and the Argent grain includes submicron order Argent grain and Silver Nanoparticles, the sub-micro
The partial size of meter level Argent grain is 100-1000nm, and the partial size of the Silver Nanoparticles is 2-50nm, institute in the conductive silver paste
The mass fraction for stating submicron order Argent grain is 73%-89%, the quality point of Silver Nanoparticles described in the conductive silver paste
Number is 1%-17%.The conductive silver paste reaches low-resistance purpose by being surface modified to nano-Ag particles, however its
Sheet resistance at 40 DEG C but reaches 24.5 Ω/, still in very high level, is unable to satisfy requirement of the capacitance plate to conductive silver paste.
The Chinese invention patent of Publication No. CNCN104464887A, which discloses, has carried out a kind of conductive silver paste, weighs 28- respectively
32wt% conductive silver wire, the resin of 25-40wt%, 20-30wt% organic solvent, 1-10wt% glass powder and 1-10wt% add
Add agent.Above components content summation is 100%.Weighed resin is dissolved in organic solvent 60 DEG C of stirrings in water-bath to add
Nano-silver thread, glass powder and additive are added into organic carrier and stirs evenly 30 for hot 30 minutes formation organic carriers
Minute.Nano-silver thread described in the conductive silver wire is by the reducing agent glycerine of 10 parts by weight, the polyvinylpyrrolidine of 2 parts by weight
Ketone, the ammonium chloride of the silver nitrate of 1 parts by weight and 1 parts by weight or ammonium fluoride are in 200 DEG C of agitating and heatings 20-30 minutes and to product
Using obtained by 400 mesh filter screen separating and filterings.However, conductive silver paste made from the above method, resistivity is at 3.1-3.3 Ω m, place
In higher level, it is equally unable to satisfy requirement of the capacitance plate to conductive silver paste.
Summary of the invention
In view of the deficiencies of the prior art, it is an object of the present invention to provide a kind of, resistivity small with sheet resistance is almost 0 to face
Boundary's superconduction silver paste, to achieve the purpose that good conductivity.
To achieve the above object, a kind of critical superconduction silver paste provided by the invention, including (weight ratio): linear silver nanoparticle
Grain 75-85%, dispersing agent 0.1-4%, levelling agent 0-2%, organic resin 2.5-8%, conductive nano carbon particle 1.3-3.8%,
Solvent 8-20%, the linear nano silver particle length is 1-5 μm, width 10-15nm.
Preferably, the dispersing agent is sodium tripolyphosphate, in calgon, sodium pyrophosphate, lauryl sodium sulfate
More than one.
Preferably, the levelling agent is crosslinked polysiloxane acrylate, acroleic acid esterification polysiloxanes, the soft phosphatide of ovum
Dimethyl siloxane, one or more of polymethylphenylsiloxane.
Preferably, the partial size of the conductive nano carbon particle is between 8-12nm.
Preferably, the solvent is one or more of isophorone, 2-Butoxyethyl acetate, butyl.
Preferably, the organic resin is one or more of bisphenol A epoxide resin, saturation copolymer resins, polyurethane.
The present invention also provides a kind of preparation methods of above-mentioned critical superconduction silver paste, the specific steps are as follows:
1) preparation of linear silver nano-grain: 20-50ml ethylene glycol or polyethylene glycol are placed in conical flask, to flask
Middle addition 45-60mg polyethylene glycol pyrrolidones is configured to reducing solution, states addition 30-45mg nitric acid in reducing solution then up
Above-mentioned reaction solution is placed in 60-85 DEG C of water-bath and reacts by silver, and it is same during which to apply the electromagnetic agitation that frequency is 120-200Hz
When into above-mentioned reaction solution be added dropwise 5-8mg NaCl, reaction 5 minutes more than after carry out natural cooling, then pass through centrifugal analysis,
Up to linear silver nano-grain after washing, baking step；
2) it is 100% metering according to silver paste total content, the electrically conductive carbon particle of the solvent of 4-10% and 1.3-3.8% is mixed
It closes, the linear silver nano-grain that the step 1) of 75-85% is prepared is added in stirring after so that electrically conductive carbon particle is uniformly dispersed, then
0.1-4% dispersing agent and 0-2% levelling agent is added, after mixing evenly for use；
3) 2.5-8% organic resin and remaining solvent are added into said mixture, heating dissolves it sufficiently, so
After carry out filtering removal impurity and insoluble substance；
4) said mixture is ground to 1-8 μm in three-roller, obtains critical superconduction silver paste.
Preferably, the dispersing agent is sodium tripolyphosphate, in calgon, sodium pyrophosphate, lauryl sodium sulfate
More than one.
Preferably, the levelling agent is crosslinked polysiloxane acrylate, acroleic acid esterification polysiloxanes, the soft phosphatide of ovum
Dimethyl siloxane, one or more of polymethylphenylsiloxane.
Preferably, the partial size of the conductive nano carbon particle is between 8-12nm.
Preferably, the solvent is one or more of isophorone, 2-Butoxyethyl acetate, butyl.
Preferably, the organic resin is one or more of bisphenol A epoxide resin, saturation copolymer resins, polyurethane.
The dispersibility of system on the one hand is enhanced by adding a small amount of electrically conductive carbon particle, further reduced volume resistance
Rate, another aspect electrically conductive carbon particle be adsorbed on be conducive on linear silver nano-grain improve silver powder in having technology in compatibility
Volume resistivity is further decreased, research shows that the size controlling when electrically conductive carbon particle can be such that silver paste shows between 8-12nm
Superior electric conductivity works as content in addition, its electric conductivity facilitation effect is bad when the content of electrically conductive carbon particle is lower than 1.3%
The resistivity for being enriched with and increasing silver paste can be generated when higher than 3.3% in silver paste.
The structure of nano silver has decisive impact the electric conductivity of silver paste, research shows that when linear silver nano-grain
Length control can make silver paste show excellent electric conductivity at 1-5 μm, effective due to that can not be formed when length is less than 1 μm
Conductive network and so that the electric conductivity of silver paste is deteriorated, when length is greater than 5 μm due to linear silver nano-grain too long generations winding with
Reunite, the electric conductivity of silver paste thus can also be greatly reduced, in addition, the content of linear nano-Ag particles is higher, the conductive mesh of silver paste
The formation of network is more intensive, therefore the conductivity of silver paste can decline to a great extent.
Dispersing agent is added in the present invention can be such that linear silver nano-grain and electrically conductive carbon particle dispersibility and uniformity enhances；
The addition of levelling agent realizes film densification and planarization of the conductive silver paste under quick print.
Compared with the existing technology, the critical superconduction silver paste resistivity that the present invention is prepared is almost 0, and sheet resistance is only 1.5-
2.9 Ω/ have very excellent electric conductivity, and furthermore the silver paste has excellent flexibility, can be arbitrarily curved with substrate after printing
Folding.
Detailed description of the invention
Fig. 1 critical superconduction silver paste prepared by the present invention
Fig. 2 critical superconduction silver paste products application prepared by the present invention is in flexible circuit effect
Specific embodiment
Embodiment 1
A kind of critical superconduction silver paste, including (weight ratio): linear silver nano-grain 75%, dispersing agent 4%, levelling agent
1.2%, organic resin 2.5%, conductive nano carbon particle 1.3%, solvent 16%, the linear nano silver particle average length are
1 μm, mean breadth 15nm.
The preparation method of above-mentioned critical superconduction silver paste, the specific steps are as follows:
1) preparation of linear silver nano-grain: 50ml ethylene glycol or polyethylene glycol are placed in conical flask, into flask
60mg polyethylene glycol pyrrolidones is added and is configured to reducing solution, states addition 45mg silver nitrate in reducing solution then up, it will be above-mentioned
Reaction solution, which is placed in 75 DEG C of water-baths, to be reacted, and during which applying frequency is the electromagnetic agitation of 120-200Hz simultaneously to above-mentioned reaction
The NaCl of 5mg is added dropwise in liquid, reaction carries out natural cooling after five minutes, then after centrifugal analysis, washing, baking step i.e.
Obtain linear silver nano-grain；
It 2) is 100% metering according to silver paste total content, the average grain diameter by 5% solvent and 1.3% is 8.6nm conductive
The linear silver nanoparticle that 75% step 1) is prepared is added in carbon particle mixing, stirring after so that electrically conductive carbon particle is uniformly dispersed
Grain, is then added 4% dispersing agent and 1.2% levelling agent, after mixing evenly for use；
3) 2.5% organic resin and remaining solvent are added into said mixture, heating dissolves it sufficiently, then
It is filtered removal impurity and insoluble substance；
4) said mixture is ground to 8 μm in three-roller, obtains critical superconduction silver paste.
After tested, the sheet resistance of critical superconduction silver paste is 1.52 Ω/.
Embodiment 2
A kind of critical superconduction silver paste, including (weight ratio): linear silver nano-grain 85%, dispersing agent 0.9%, levelling agent
0.6%, organic resin 3%, conductive nano carbon particle 1.5%, solvent 9%, the linear nano silver particle average length are 3 μ
M, mean breadth is 10nm.
The preparation method of above-mentioned critical superconduction silver paste, the specific steps are as follows:
1) preparation of linear silver nano-grain: 45ml ethylene glycol or polyethylene glycol are placed in conical flask, into flask
45mg polyethylene glycol pyrrolidones is added and is configured to reducing solution, states addition 42mg silver nitrate in reducing solution then up, it will be above-mentioned
Reaction solution, which is placed in 60 DEG C of water-baths, to be reacted, and during which applies the electromagnetic agitation that frequency is 180Hz while into above-mentioned reaction solution
The NaCl of 7mg is added dropwise, carries out natural cooling after reaction 5 minutes or more, then after centrifugal analysis, washing, baking step i.e.
Obtain linear silver nano-grain；
2) average grain diameter of 5% solvent and 1.5% is mixed for 9.4nm electrically conductive carbon particle, stirring makes conductive carbon granules
The 85% linear silver nano-grain that is prepared of step 1) is added in son after being uniformly dispersed, be then added 0.9% dispersing agent and
0.6% levelling agent, after mixing evenly for use；
3) be added 3% organic resin and remaining solvent into said mixture, heating dissolves it sufficiently, then into
Row filtering removal impurity and insoluble substance；
4) said mixture is ground to 6 μm in three-roller, obtains critical superconduction silver paste.
After tested, the sheet resistance of critical superconduction silver paste is 2.21 Ω/.
Embodiment 3
A kind of critical superconduction silver paste, including (weight ratio): linear silver nano-grain 78%, dispersing agent 1.3%, levelling agent
2%, organic resin 4%, conductive nano carbon particle 2.7%, solvent 12%, the linear nano silver particle average length be 5 μm,
Mean breadth is 10nm.
The preparation method of above-mentioned critical superconduction silver paste, the specific steps are as follows:
1) preparation of linear silver nano-grain: 20ml ethylene glycol or polyethylene glycol are placed in conical flask, into flask
45mg polyethylene glycol pyrrolidones is added and is configured to reducing solution, states addition 30mg silver nitrate in reducing solution then up, it will be above-mentioned
Reaction solution, which is placed in 75 DEG C of water-baths, to be reacted, and during which applying frequency is the electromagnetic agitation of 120-200Hz simultaneously to above-mentioned reaction
The NaCl of 8mg is added dropwise in liquid, carries out natural cooling after reaction 5 minutes or more, then passes through centrifugal analysis, washing, baking step
Afterwards up to linear silver nano-grain；
2) average grain diameter of 6% solvent and 2.7% is mixed for 8nm electrically conductive carbon particle, stirring makes electrically conductive carbon particle
The linear silver nano-grain that 78% step 1) is prepared is added after being uniformly dispersed, 1.3% dispersing agent and 2% stream is then added
Flat agent, after mixing evenly for use；
3) be added 4% organic resin and remaining solvent into said mixture, heating dissolves it sufficiently, then into
Row filtering removal impurity and insoluble substance；
4) said mixture is ground to 4 μm in three-roller, obtains critical superconduction silver paste.
After tested, the sheet resistance of critical superconduction silver paste is 2.48 Ω/.
Embodiment 4
A kind of critical superconduction silver paste, including (weight ratio): linear silver nano-grain 75%, dispersing agent 1.1%, organic resin
6%, conductive nano carbon particle 3.8%, solvent 14.3%, the linear nano silver particle average length is 2 μm, mean breadth is
14nm。
The preparation method of above-mentioned critical superconduction silver paste, the specific steps are as follows:
1) preparation of linear silver nano-grain: 45ml ethylene glycol or polyethylene glycol are placed in conical flask, into flask
56mg polyethylene glycol pyrrolidones is added and is configured to reducing solution, states addition 40mg silver nitrate in reducing solution then up, it will be above-mentioned
Reaction solution, which is placed in 75 DEG C of water-baths, to be reacted, and during which applies the electromagnetic agitation that frequency is 200Hz while into above-mentioned reaction solution
The NaCl of 6mg is added dropwise, reaction carried out natural cooling after 8 minutes, then up to line after centrifugal analysis, washing, baking step
Shape silver nano-grain；
2) average grain diameter of 7% solvent and 3.8% is mixed for 10nm electrically conductive carbon particle, stirring makes electrically conductive carbon particle
Then plus 1.1% dispersing agent the 75% linear silver nano-grain that is prepared of step 1) is added after being uniformly dispersed, stirs evenly
It is stand-by afterwards；
3) be added 6% organic resin and remaining solvent into said mixture, heating dissolves it sufficiently, then into
Row filtering removal impurity and insoluble substance；
4) said mixture is ground to 5 μm in three-roller, obtains critical superconduction silver paste.
After tested, the sheet resistance of critical superconduction silver paste is 2.88 Ω/.
The above embodiment is a preferred embodiment of the present invention, but embodiments of the present invention are not by above-described embodiment
Limitation, other any changes, modifications, substitutions, combinations, simplifications made without departing from the spirit and principles of the present invention,
It should be equivalent substitute mode, be included within the scope of the present invention.
Claims (10)
1. a kind of critical superconduction silver paste, which is characterized in that including (weight ratio): linear silver nano-grain 75-85%, dispersing agent
0.1-4%, levelling agent 0-2%, organic resin 2.5-8%, conductive nano carbon particle 1.3-3.8%, solvent 8-20%, the line
Shape nano-Ag particles average length is 1-5 μm, mean breadth 10-15nm.
2. a kind of silver paste as described in claim 1, which is characterized in that the dispersing agent is sodium tripolyphosphate, hexa metaphosphoric acid
One or more of sodium, sodium pyrophosphate, lauryl sodium sulfate, the levelling agent are crosslinked polysiloxane acrylate, third
Olefin(e) acid is esterified polysiloxanes, the soft phosphatide dimethyl siloxane of ovum, one or more of polymethylphenylsiloxane.
3. a kind of silver paste as described in claim 1, which is characterized in that the average grain diameter of the conductive nano carbon particle is in 8-
Between 12nm.
4. a kind of silver paste as described in claim 1, which is characterized in that the solvent is isophorone, butyl glycol ether acetic acid
One or more of ester, butyl, the organic resin are bisphenol A epoxide resin, in saturation copolymer resins, polyurethane
More than one.
5. the preparation method of critical superconduction silver paste described in a kind of claim 1, the specific steps are as follows:
1) preparation of linear silver nano-grain: 20-50ml ethylene glycol or polyethylene glycol are placed in conical flask, added into flask
Enter 45-60mg polyethylene glycol pyrrolidones and be configured to reducing solution, states addition 30-45mg silver nitrate in reducing solution then up, it will
Above-mentioned reaction solution, which is placed in 60-85 DEG C of water-bath, to be reacted, and it is upward simultaneously during which to apply the electromagnetic agitation that frequency is 120-200Hz
State in reaction solution be added dropwise 5-8mg NaCl, reaction 5 minutes more than after carry out natural cooling, then pass through centrifugal analysis, washing,
Up to linear silver nano-grain after baking step；
2) electrically conductive carbon particle of the solvent of 4-10% and 1.3-3.8% are mixed, after stirring makes electrically conductive carbon particle be uniformly dispersed
The linear silver nano-grain that the step 1) of 75-85% is prepared is added, 0.1-4% dispersing agent and 0-2% levelling is then added
Agent, after mixing evenly for use；
3) 2.5-8% organic resin and remaining solvent are added into said mixture, heating dissolves it sufficiently, then into
Row filtering removal impurity and insoluble substance；
4) said mixture is ground to 1-8 μm in three-roller, obtains critical superconduction silver paste.
6. a kind of method as claimed in claim 5, which is characterized in that the dispersing agent is sodium tripolyphosphate, hexa metaphosphoric acid
One or more of sodium, sodium pyrophosphate, lauryl sodium sulfate.
7. a kind of such as method described in claim 5 or 6, which is characterized in that the levelling agent is crosslinked polysiloxane propylene
The soft phosphatide dimethyl siloxane of acid esters, acroleic acid esterification polysiloxanes, ovum, one or more of polymethylphenylsiloxane.
8. a kind of method as claimed in claim 5, which is characterized in that the partial size of the conductive nano carbon particle 8-12nm it
Between.
9. a kind of such as method described in claim 5 or 6, which is characterized in that the solvent is isophorone, butyl glycol ether vinegar
One or more of acid esters, butyl.
10. a kind of such as method described in claim 5 or 6, which is characterized in that the organic resin is bisphenol A epoxide resin, satisfies
With one or more of copolymer resins, polyurethane.
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| CN201811624534.6A CN109493994B (en) | 2018-12-28 | 2018-12-28 | Critical superconducting silver paste based on linear silver nanoparticles and preparation method thereof |
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| CN201811624534.6A CN109493994B (en) | 2018-12-28 | 2018-12-28 | Critical superconducting silver paste based on linear silver nanoparticles and preparation method thereof |
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|---|---|---|---|---|
| US7566360B2 (en) * | 2002-06-13 | 2009-07-28 | Cima Nanotech Israel Ltd. | Nano-powder-based coating and ink compositions |
| CN104916344A (en) * | 2014-03-13 | 2015-09-16 | 艾登株式会社 | Transparent conductor using silver nanowires to improve haze and electrical conductivity |
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