CN107403657A - A kind of UV conductive silver pastes formula and preparation method thereof - Google Patents
A kind of UV conductive silver pastes formula and preparation method thereof Download PDFInfo
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- H—ELECTRICITY
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- 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
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- H—ELECTRICITY
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- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
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Abstract
The invention provides a kind of UV conductive silver pastes formula and preparation method thereof, it is related to electronic chemical technical field of coatings.The UV conductive silver pastes of the present invention are major ingredient by organic carrier solvent, modified silver powder, modified glass powder, other auxiliary agents are prepared for auxiliary material, with with carrier adhesive force is strong, electric conductivity is superior, pliability is good, the feature of environmental protection is good, the characteristics of rheological property is good, it can be widely applied to the printed circuits such as chip, touch-screen, tablet personal computer, digital camera.
Description
Technical field
The present invention relates to electronic chemical technical field of coatings, more particularly to a kind of UV conductive silver pastes formula and its preparation side
Method.
Background technology
With the fast development of electronic information technology, electronic equipment is constantly towards miniaturization, intelligent, environmental protection and low cost
Direction stride forward, promote people constantly to study, develop and using the system such as more advanced inexpensive electronic circuit board, electronic component
Make technology.Full printed electronics technology is a kind of novel electronic product manufacturing technology, and it utilizes the advantage of the art of printing, by electronic equipment
The organic combinations such as the encapsulation of component are fabricated into from element manufacture, circuit, so as to more efficient, more environmentally friendly produce high property
The electronic product of energy, low cost, has very wide application prospect.And conductive silver paste is as in full printed electronics technical field
One of the most key material, cause the highest attention of industrial quarters and academia.The curing mode that conventional conductive silver paste is taken
It is heat cure, hardening time is long, high energy consumption, reduces the efficiency of industrialized production, and UV-curing technology has economic, section
Can, solidification rate is fast and advantages of environment protection, UV-curing technology is applied into conductive silver paste can not only accelerate solidification speed
Degree, and the resolution ratio of printed conductor can be improved.Therefore, ultraviolet light solidification conductive silver paste is silver paste most with prospects at present
One of, become the development new direction of conductive silver paste.
In general, the boiling characteristics of the organic carrier of conductive silver paste directly affect electrocondution slurry performance it is important because
Element, if volatilization is too fast, slurry viscosity in printing, which will gradually increase, easily to be caused slurry to be trembled to be difficult to print, and blocks silk screen,
It is not easy to dry after silk-screen printing if evaporating too slowly in slurry sintering process, and volatilizees when concentrating on certain temperature section, easily
Substantial amounts of hole defect is formed in film surface, electrocondution slurry is ultimately resulted in and is come off from carrier, scrap conducting wire.
The content of the invention
Present invention aims at a kind of UV conductive silver pastes formula and preparation method thereof is provided, waved with solving organic carrier solvent
Send out uneven, ultimately result in electrocondution slurry and come off from carrier, the technical problem for scrapping conducting wire.
To achieve the above object, the invention provides a kind of UV conductive silver pastes formula and preparation method thereof.
A kind of UV conductive silver pastes formula, include the raw material of following parts by weight：Diethylene glycol ether acetate 5-7 parts, Buddhist nun
Imperial dimethyl phthalate 8-10 parts, white slurry 3-5 parts, polyethylene glycol 1.2-2.2 parts, citric acid 5.5-6.5 parts, ethyl cellulose 1.1-
2.3 parts, vinyl neodecanoate 8.8-10.5 parts, epoxy resin 9-11 parts, polyester acrylate 10-15 parts, modified polyorganosiloxane
3-5 parts, polyethylene glycol oxide 2-3 parts, light trigger 0.5-1.5 parts, modified silver powder 30-40 parts；
Described modification silver powder, in parts by weight, 1.2-2.4 part KH-560 are taken, the water stirring for adding 1.2 times of its weight is equal
Even, it is 4-5 to add concentrated hydrochloric acid and adjust pH value, adds 30-40 part nano-silver powders and is well mixed, by mixed solution at 40-45 DEG C
Ultrasonic disperse 15-20min, while mechanical agitation are carried out in water bath with thermostatic control, adds 1-1.5 part titanium dioxide, stirs 15min,
Filtering, is then washed reactant, is dried in vacuo 18-20h at 70 DEG C, is produced modified silver powder；
The modified polyorganosiloxane, in parts by weight, 10-15 parts both-end epoxy radicals polysiloxanes is taken to be removed water with 5-10 parts
Diethylenetriamine and 3-5 part n-butanols be placed in reactor, be then passed through nitrogen in a kettle, keep nitrogen in reactor
It is 3 with the ratio between oxygen:1,75 DEG C of reaction 2-3h of temperature of reaction kettle are kept, is then evaporated under reduced pressure and removes solvent, produce modified poly- silicon
Oxygen alkane；
The modified glass powder, in parts by weight, the quality that 2.2-3.1 parts KH-550 is dissolved in 1.5 times of its weight are dense
Spend in the ethanol for 50%, stir 5min, add 5-10 part lead-free glass powders stir process 40- in 60-70 DEG C of thermostat
60min, taking-up are placed in agate mortar grinding 10-15min, then will be put into 80-100 DEG C of baking oven after glass dust solution natural air drying
Middle drying is placed in resistance furnace to constant weight, then by the glass dust, and sintering temperature controls 1000-1200 DEG C, is incubated 40-60min, cold
But 400 mesh sieves are crossed afterwards, produce modified glass powder.
Described UV conductive silver paste preparation methods, specifically include following steps：
1. pressing the parts by weight, diethylene glycol ether acetate, nylon acid dimethyl ester, the mixing of citric acid mechanical agitation are taken
It is put into and 10min is heated and stirred in 50 DEG C of thermostat water bath, add ethyl cellulose, treats that ethyl cellulose is completely dissolved,
Add vinyl neodecanoate, epoxy resin, polyester acrylate to mix and be placed in homogenizer, rotating speed 1000-
2000r/min, white slurry, polyethylene glycol are then sequentially added, bath temperature is then increased to 70 DEG C of heated at constant temperature stirring 20-
30min, the removal of impurity is filtered off, produce organic carrier；
2. the modification silver powder, organic carrier, modified glass powder of preparation are compared into 1-3 according to weight:3-5：The mixing of 2-4 ratios is put
In mortar, slurry is ground into pasty state, then pasty slurry is placed in ball mill, adds a diameter of 1cm abrading-ball, is being turned
Speed is 120-150r/min, first roughly grinds 10min, then changes abrading-ball into a diameter of 0.2cm, continues to grind 15min, then presses institute again
State parts by weight and sequentially add modified polyorganosiloxane, polyethylene glycol oxide, light trigger continues to grind 30min, then is ground using three rollers
Grinding machine grinding distribution 5min, then carries out vacuum defoamation, and the vacuum of vacuum defoamation is 0.08MPa-0.12MPa, inclined heated plate
For 5min, UV conductive silver pastes are produced.
Further, described step 4. middle modified silver powder, organic carrier, modified glass powder by weight 2:4:3 ratios are mixed
Close.
The invention has the advantages that：
1st, UV conductive silver pastes of the invention are major ingredient by organic carrier solvent, modified silver powder, modified glass powder, other auxiliary agents
Be prepared for auxiliary material, have with carrier adhesive force is strong, electric conductivity is superior, pliability is good, the feature of environmental protection is good, and rheological property is good
The characteristics of, it can be widely applied to the printed circuits such as chip, touch-screen, tablet personal computer, digital camera.
2nd, the present invention mixes low toxicity, the diethylene glycol ether acetate of environmental protection, nylon acid dimethyl ester as organic solvent,
Being equipped with the organic carrier solvent that other auxiliary agents are prepared again has level volatility, this hair in slurry printing and sintering process
The organic carrier solvent volatilization of bright preparation is uniform, effectively solves because organic carrier solvent volatilization is uneven and causes conduction
Slurry adhesive force on carrier reduces, easily causes the technical problem to come off.In terms of auxiliary agent, the neodecanoic acid of the invention added
Vinyl acetate has good compatibility, anti-corrosive properties, plasticity, the feature of environmental protection, than miscible, can arbitrarily ensure that with other auxiliary agents
The uniformity and level volatility of the mixing of organic carrier solvent, and citric acid is also added into, both can adjust in organic cooperation
With the viscosity of organic carrier solvent, the rheological property of slurry is improved so that in slurry printing process, can add at low temperature
The formation of fast cured film, and slurry can be made preferably to be attached to carrier.In sintering, conducting particles can form good lead
Current source, the silver conductive film of continuous densification is obtained, enhance the electric conductivity of slurry.
3rd, because nano-silver powder specific surface area is big, surface atom number is more, surface energy height has substantial amounts of surface defect and outstanding
Key is hung, is easily reunited between particle, the bad dispersibility in organic matrix, therefore, the present invention use silane coupler KH-560
Surface modification is carried out to nano-silver powder so that generate chemical bond between nano-silver powder surface and KH-560 so that nano-silver powder
Surrounding forms one layer of integument, improves the dispersiveness between nano-silver powder and organic carrier solvent, adds also in modifying process
Enter titanium dioxide, while silver powder dosage is substantially reduced, the electric conductivity of strengthening slurry, and enhance the antibacterial of slurry
Performance, while also significantly increase the dispersiveness and stability of nano-silver powder.
4th, with the continuous enhancing of people's environmental consciousness, replacement of the lead-free glass powder as glass dust in terms of electronic material
Product, usually matter be added in organic polymer resin, form various electronic media electrocondution slurries with macromolecule resin, but due to
The general more sticky glass powder of macromolecule resin easily gathers, it is difficult to be uniformly dispersed in macromolecule resin, influences crown glass
Powder plays efficiency, therefore the present invention is modified using silane resin acceptor kh-550 to its powder surface so that modified nothing
Lead glass powder is greatly improved in macromolecule dispersive property and stability in macromolecule resin, enhances electrocondution slurry
Mobile phase and equal uniformity, and lead-free glass powder dosage is reduced, reduce production cost.
In addition to objects, features and advantages described above, the present invention also has other objects, features and advantages.
The present invention is further detailed explanation below.
Embodiment
Embodiments of the invention are described in detail below, but the present invention can be limited and covered according to claim
Multitude of different ways implement.
Embodiment 1
A kind of UV conductive silver pastes formula, include the raw material of following parts by weight：5 parts of diethylene glycol ether acetate, nylon
8 parts of dimethyl phthalate, in vain slurry 3,1.2 parts of polyethylene glycol, 5.5 parts of citric acid, 1.1 parts of ethyl cellulose, vinyl neodecanoate 8.8
Part, 9 parts of epoxy resin, 10 parts of polyester acrylate, 3 parts of modified polyorganosiloxane, 2 parts of polyethylene glycol oxide, 0.5 part of light trigger,
Modified 30 parts of silver powder；
Described modification silver powder, in parts by weight, 1.2 parts of KH-560 being taken, the water for adding 1.2 times of its weight stirs,
It is 4 to add concentrated hydrochloric acid and adjust pH value, adds 30 parts of nano-silver powders and is well mixed, mixed solution is entered in 40 DEG C of waters bath with thermostatic control
Row ultrasonic disperse 15min, while mechanical agitation, 1 part of titanium dioxide is added, stir 15min, filtering, then enter reactant
Row washing, 18h is dried in vacuo at 70 DEG C, produces modified silver powder；
The modified polyorganosiloxane, in parts by weight, take 10 parts of both-end epoxy radicals polysiloxanes and 5 parts of diethyls removed water
Alkene triamine and 3 parts of n-butanols are placed in reactor, are then passed through nitrogen in a kettle, keep in reactor nitrogen and oxygen it
Than for 3:1,75 DEG C of reaction 2h of temperature of reaction kettle are kept, is then evaporated under reduced pressure and removes solvent, produce modified polyorganosiloxane；
The modified glass powder, in parts by weight, the mass concentration that 2.2 parts of KH-550 are dissolved in 1.5 times of its weight is
In 50% ethanol, 5min is stirred, 5 parts of lead-free glass powders stir process 40-60min, taking-up in 60 DEG C of thermostats is added and puts
10min is ground in agate mortar, then will be put into 80 DEG C of baking ovens and dried to constant weight after glass dust solution natural air drying, then should
Glass dust is placed in resistance furnace, and sintering temperature controls 1000 DEG C, is incubated 40-60min, and 400 mesh sieves are crossed after cooling, produce modified glass
Glass powder.
Described UV conductive silver paste preparation methods, specifically include following steps：
1. pressing the parts by weight, diethylene glycol ether acetate, nylon acid dimethyl ester, the mixing of citric acid mechanical agitation are taken
It is put into and 10min is heated and stirred in 50 DEG C of thermostat water bath, add ethyl cellulose, treats that ethyl cellulose is completely dissolved,
Add vinyl neodecanoate, epoxy resin, polyester acrylate to mix and be placed in homogenizer, rotating speed 1000r/min,
Then white slurry, polyethylene glycol are sequentially added, bath temperature is then increased to 70 DEG C of heated at constant temperature stirring 20min, filters off and removes
Impurity, produce organic carrier；
2. by the modification silver powder, organic carrier, modified glass powder of preparation according to weight than 1:3:The mixing of 2 ratios is placed in mortar
In, slurry is ground into pasty state, and then pasty slurry is placed in ball mill, adds a diameter of 1cm abrading-ball, is in rotating speed
120r/min, 10min is first roughly ground, then change abrading-ball into a diameter of 0.2cm, continued to grind 15min, then press the parts by weight again
Number sequentially adds modified polyorganosiloxane, polyethylene glycol oxide, and light trigger continues to grind 30min, then is ground using three-roll grinder
Scattered 5min, then carries out vacuum defoamation, and the vacuum of vacuum defoamation is 0.08MPa, inclined heated plate 5min, produces UV conductions
Silver paste.
Embodiment 2
A kind of UV conductive silver pastes formula, include the raw material of following parts by weight：7 parts of diethylene glycol ether acetate, nylon
10 parts of dimethyl phthalate, white 5 parts of slurry, 2.2 parts of polyethylene glycol, 6.5 parts of citric acid, 2.3 parts of ethyl cellulose, vinyl neodecanoate
10.5 parts, 11 parts of epoxy resin, 15 parts of polyester acrylate, 5 parts of modified polyorganosiloxane, 3 parts of polyethylene glycol oxide, light trigger
1.5 parts, modified 40 parts of silver powder；
Described modification silver powder, in parts by weight, 2.4 parts of KH-560 being taken, the water for adding 1.2 times of its weight stirs,
It is 5 to add concentrated hydrochloric acid and adjust pH value, adds 40 parts of nano-silver powders and is well mixed, mixed solution is entered in 45 DEG C of waters bath with thermostatic control
Row ultrasonic disperse 15-20min, while mechanical agitation, 1.5 parts of titanium dioxide are added, stir 15min, filtering then will reaction
Thing is washed, and is dried in vacuo 20h at 70 DEG C, is produced modified silver powder；
The modified polyorganosiloxane, in parts by weight, take 15 parts of both-end epoxy radicals polysiloxanes and 10 parts of two removed water
Ethene triamine and 5 parts of n-butanols are placed in reactor, are then passed through nitrogen in a kettle, keep nitrogen and oxygen in reactor
The ratio between be 3:1,75 DEG C of reaction 3h of temperature of reaction kettle are kept, is then evaporated under reduced pressure and removes solvent, produce modified polyorganosiloxane；
The modified glass powder, in parts by weight, the mass concentration that 3.1 parts of KH-550 are dissolved in 1.5 times of its weight is
In 50% ethanol, 5min is stirred, 10 parts of lead-free glass powders stir process 60min, taking-up in 70 DEG C of thermostats is added and is placed in
Agate mortar grinds 15min, then will be put into 100 DEG C of baking ovens and is dried to constant weight after glass dust solution natural air drying, then should
Glass dust is placed in resistance furnace, and sintering temperature controls 1200 DEG C, is incubated 60min, and 400 mesh sieves are crossed after cooling, produce modified glass
Powder.
Described UV conductive silver paste preparation methods, specifically include following steps：
1. pressing the parts by weight, diethylene glycol ether acetate, nylon acid dimethyl ester, the mixing of citric acid mechanical agitation are taken
It is put into and 10min is heated and stirred in 50 DEG C of thermostat water bath, add ethyl cellulose, treats that ethyl cellulose is completely dissolved,
Add vinyl neodecanoate, epoxy resin, polyester acrylate to mix and be placed in homogenizer, rotating speed 2000r/min,
Then white slurry, polyethylene glycol are sequentially added, bath temperature is then increased to 70 DEG C of heated at constant temperature stirring 30min, filters off and removes
Impurity, produce organic carrier；
2. by the modification silver powder, organic carrier, modified glass powder of preparation according to weight than 3:5:The mixing of 4 ratios is placed in mortar
In, slurry is ground into pasty state, and then pasty slurry is placed in ball mill, adds a diameter of 1cm abrading-ball, is in rotating speed
150r/min, 10min is first roughly ground, then change abrading-ball into a diameter of 0.2cm, continued to grind 15min, then press the parts by weight again
Number sequentially adds modified polyorganosiloxane, polyethylene glycol oxide, and light trigger continues to grind 30min, then is ground using three-roll grinder
Scattered 5min, then carries out vacuum defoamation, and the vacuum of vacuum defoamation is 0.12MPa, inclined heated plate 5min, produces UV conductions
Silver paste.
Embodiment 3
A kind of UV conductive silver pastes formula, include the raw material of following parts by weight：6 parts of diethylene glycol ether acetate, nylon
9 parts of dimethyl phthalate, white 4 parts of slurry, 1.7 parts of polyethylene glycol, 6 parts of citric acid, 1.8 parts of ethyl cellulose, vinyl neodecanoate 9.5
Part, 10 parts of epoxy resin, 13 parts of polyester acrylate, 4 parts of modified polyorganosiloxane, 2.5 parts of polyethylene glycol oxide, 1 part of light trigger,
Modified 35 parts of silver powder；
Described modification silver powder, in parts by weight, 1.8 parts of KH-560 being taken, the water for adding 1.2 times of its weight stirs,
It is 4.5 to add concentrated hydrochloric acid and adjust pH value, adds 35 parts of nano-silver powders and is well mixed, by mixed solution in 42 DEG C of waters bath with thermostatic control
Ultrasonic disperse 18min, while mechanical agitation are carried out, adds 1.3 parts of titanium dioxide, stirs 15min, filtering then will reaction
Thing is washed, and is dried in vacuo 19h at 70 DEG C, is produced modified silver powder；
The modified polyorganosiloxane, in parts by weight, take 13 parts of both-end epoxy radicals polysiloxanes and 8 parts of diethyls removed water
Alkene triamine and 4 parts of n-butanols are placed in reactor, are then passed through nitrogen in a kettle, keep in reactor nitrogen and oxygen it
Than for 3:1,75 DEG C of reaction 2.5h of temperature of reaction kettle are kept, is then evaporated under reduced pressure and removes solvent, produce modified polyorganosiloxane；
The modified glass powder, in parts by weight, the mass concentration that 2.5 parts of KH-550 are dissolved in 1.5 times of its weight is
In 50% ethanol, 5min is stirred, adds 8 parts of lead-free glass powders stir process 50min in 65 DEG C of thermostats, taking-up is placed in agate
Nao mortar grinder 13min, it then will be put into 90 DEG C of baking ovens and dried to constant weight after glass dust solution natural air drying, then by the glass
Powder is placed in resistance furnace, and sintering temperature controls 1100 DEG C, is incubated 50min, and 400 mesh sieves are crossed after cooling, produce modified glass powder.
Described UV conductive silver paste preparation methods, specifically include following steps：
1. pressing the parts by weight, diethylene glycol ether acetate, nylon acid dimethyl ester, the mixing of citric acid mechanical agitation are taken
It is put into and 10min is heated and stirred in 50 DEG C of thermostat water bath, add ethyl cellulose, treats that ethyl cellulose is completely dissolved,
Add vinyl neodecanoate, epoxy resin, polyester acrylate to mix and be placed in homogenizer, rotating speed 1500r/min,
Then white slurry, polyethylene glycol are sequentially added, bath temperature is then increased to 70 DEG C of heated at constant temperature stirring 25min, filters off and removes
Impurity, produce organic carrier；
2. by the modification silver powder, organic carrier, modified glass powder of preparation according to weight than 2:4:The mixing of 3 ratios is placed in mortar
In, slurry is ground into pasty state, and then pasty slurry is placed in ball mill, adds a diameter of 1cm abrading-ball, is in rotating speed
130r/min, 10min is first roughly ground, then change abrading-ball into a diameter of 0.2cm, continued to grind 15min, then press the parts by weight again
Number sequentially adds modified polyorganosiloxane, polyethylene glycol oxide, and light trigger continues to grind 30min, then is ground using three-roll grinder
Scattered 5min, then carries out vacuum defoamation, and the vacuum of vacuum defoamation is 0.1MPa, inclined heated plate 5min, produces UV conductions
Silver paste.
Test example
UV conductive silver paste performance tests prepared by the present invention
1st, UV solidifies the preparation of silver paste cured film
It is 2016105830629 preparations by the embodiment of the present invention 1, embodiment 2 and embodiment 3 and number of patent application
UV conductive silver pastes are respectively adopted screen process press and silver paste are printed onto into polyethylene terephthalate (PET) film (thickness is
50 μm, wiped and dried with absolute ethyl alcohol before printing) on, then by uv cure machine, uviol lamp power is 4000W, ripple
A length of 365nm solidifies 30s, and silver paste thickness is 10 μm -15 μm after solidification, and cured film 1, cured film 2 and cured film 3 and solidification is made
Film 4.
Electrical conductivity, bending resistance and the adhesive force of cured film 1, cured film 2 and cured film 3, measure side are determined respectively
Method is as follows：
1. electrical conductivity is tested：The resistance value of printed conductor is tested out using digital multi-purpose electric meter, then passes through formula κ=L/
RWH, calculate electrical conductivity；Wherein κ is electrical conductivity (S/m), and L is printed conductor length (m), and R is test resistance (Ω), and W is print
Conductor width (m) processed, H are printed conductor thickness (m).
2. bending resistance is tested：Printed conductor is bent 180 ° to external symmetry, and is pressed in using counterweight in silver paste, pressure
About 5.5kPa, keep 1min；Again by 180 ° of the reverse doubling of printed conductor, it is pressed in using same counterweight in silver paste, keeps 1min,
Carry out the electrical conductivity test of silver paste.Above step is considered as 1 bending, repeats to operate above, bends 10 times, determine conductance.
3. adhesive force is tested：The grade tested by hundred lattice characterizes silver paste and PET adhesive force size, the test of hundred lattice according to
GB9286-98 is measured.Wherein, 5B is that optimal hundred lattice test grade, and 0B then tests grade for worst hundred lattice.
Measurement result is as shown in table 1
The comparison of the performance of 14 kinds of cured films of table
| Electrical conductivity S/m | Bending resistance S/m | Adhesive force | |
| Cured film 1 | 45.8 | 10.5 | 5 |
| Cured film 2 | 46.7 | 10.8 | 5 |
| Cured film 3 | 47.1 | 10.9 | 5 |
| Cured film 4 | 38.8 | 5.9 | 3 |
As shown in Table 1, it is the cured film phase of the 2016105830629 UV conductive silver pastes preparations prepared with number of patent application
Than, using UV conductive silver pastes of the present invention prepare solidification membrane conductivity it is significantly raised, flexibility more preferably, adhesive force it is stronger.
Test example 2
The influence of different modified silver powder, organic carrier, the mixing ratio of modified glass powder of the invention to UV conductive silver paste performances
2 are shown in Table, assay method is consistent with test example 1.
The different proportion of table 2 mixes the influence to UV conductive silver paste performances
| Modified silver powder | Organic carrier | Modified glass powder | Electrical conductivity | Bending resistance | Adhesive force |
| 1 | 3 | 2 | 41.5S/m | 7.1S/m | 4 |
| 3 | 5 | 4 | 41.7S/m | 7.3S/m | 4 |
| 2 | 4 | 3 | 47.8S/m | 11.2S/m | 5 |
| 1.5 | 3.5 | 2.5 | 40.5S/m | 5.8S/m | 3 |
| 2.5 | 4.5 | 3.5 | 40.8S/m | 6.2S/m | 3 |
As shown in Table 2, modified silver powder, modified glass powder are different from organic carrier mixed proportion, then the property of UV conductive silver pastes
Can be also dramatically different, when mixing ratio is 2 between modified silver powder, organic carrier and modified glass powder:4:The UV conductive silvers prepared when 3
The electrical conductivity of slurry is higher, pliability is more preferable, adhesive force more preferably.
Test example 3
Temperature is volatile on organic carrier to influence test
Using the volatility of 5X-5-12 type Muffle furnace combinations electronic analytical balance measurement organic carrier.The present invention is implemented
Organic carrier prepared by example 1, embodiment 2 and embodiment 3 is as test group 1, test group 2 and test group 3 and number of patent application
Organic carrier solvent (control group) sample to be prepared in a kind of high temperature resistant conductive silver paste disclosed in 2015100078373 takes 20g
It is individually placed in Muffle furnace, initial temperature is arranged to 250 DEG C, often raises 20 DEG C and takes out weighing once, record weight, until temperature
Height is to 350 DEG C.
Measurement result is as shown in table 3
The weight of organic carrier compares under the different temperatures of table 3
As shown in Table 3, as temperature constantly raises, organic carrier weight in 4 groups is also reduced in continuous volatilization, temperature from
250 DEG C rise to during 350 DEG C, and the organic carrier solvent of test group 1, test group 2 and test group 3 volatilizees respectively
13.6g13.9g and 11.8g, the 16.6g and control group has volatilized, will become apparent from test group volatile quantity substantially than control group volatile quantity
It is few, and test group is more compared with control group with the rise of temperature, volatilization distribution, and control group from 290 DEG C of temperature-
During 350 DEG C, drastically volatilize, volatilize skewness.
The preferred embodiments of the present invention are the foregoing is only, are not intended to limit the invention, for the skill of this area
For art personnel, the present invention can have various modifications and variations.Within the spirit and principles of the invention, that is made any repaiies
Change, equivalent substitution, improvement etc., should be included in the scope of the protection.
Claims (4)
1. a kind of UV conductive silver pastes formula, it is characterised in that include the raw material of following parts by weight：Diethylene glycol ether acetate
5-7 parts, nylon acid dimethyl ester 8-10 parts, white slurry 3-5 parts, polyethylene glycol 1.2-2.2 parts, citric acid 5.5-6.5 parts, ethyl cellulose
Plain 1.1-2.3 parts, vinyl neodecanoate 8.8-10.5 parts, epoxy resin 9-11 parts, polyester acrylate 10-15 parts, modification are poly-
Siloxanes 3-5 parts, polyethylene glycol oxide 2-3 parts, light trigger 0.5-1.5 parts, modified silver powder 30-40 parts；
Described modification silver powder, in parts by weight, 1.2-2.4 part KH-560 being taken, the water for adding 1.2 times of its weight stirs,
It is 4-5 to add concentrated hydrochloric acid and adjust pH value, adds 30-40 part nano-silver powders and is well mixed, by mixed solution in 40-45 DEG C of constant temperature
Ultrasonic disperse 15-20min, while mechanical agitation are carried out in water-bath, adds 1-1.5 part titanium dioxide, stirs 15min, is filtered,
Then reactant is washed, is dried in vacuo 18-20h at 70 DEG C, produces modified silver powder；
The modified polyorganosiloxane, in parts by weight, take that 10-15 parts both-end epoxy radicals polysiloxanes and 5-10 parts have removed water two
Ethene triamine and 3-5 part n-butanols are placed in reactor, are then passed through nitrogen in a kettle, keep nitrogen and oxygen in reactor
The ratio between gas is 3:1,75 DEG C of reaction 2-3h of temperature of reaction kettle are kept, is then evaporated under reduced pressure and removes solvent, produce modified polyorganosiloxane；
The modified glass powder, in parts by weight, the mass concentration that 2.2-3.1 parts KH-550 is dissolved in 1.5 times of its weight is
In 50% ethanol, 5min is stirred, adds 5-10 part lead-free glass powder stir process 40-60min in 60-70 DEG C of thermostat,
Taking-up is placed in agate mortar grinding 10-15min, then will be put into 80-100 DEG C of baking oven and dries after glass dust solution natural air drying
It is placed in constant weight, then by the glass dust in resistance furnace, sintering temperature controls 1000-1200 DEG C, is incubated 40-60min, mistake after cooling
400 mesh sieves, produce modified glass powder.
2. a kind of UV conductive silver pastes formula according to claim 1, it is characterised in that include the original of following parts by weight
Material：6 parts of diethylene glycol ether acetate, 9 parts of nylon acid dimethyl ester, white 4 parts of slurry, 1.7 parts of polyethylene glycol, 6 parts of citric acid, ethyl
1.8 parts of cellulose, 9.5 parts of vinyl neodecanoate, 10 parts of epoxy resin, 13 parts of polyester acrylate, 4 parts of modified polyorganosiloxane,
2.5 parts of polyethylene glycol oxide, 1 part of light trigger, modified 35 parts of silver powder；
Described modification silver powder, in parts by weight, 1.8 parts of KH-560 are taken, the water for adding 1.2 times of its weight stirs, then adds
It is 4.5 to enter concentrated hydrochloric acid to adjust pH value, adds 35 parts of nano-silver powders and is well mixed, mixed solution is carried out in 42 DEG C of waters bath with thermostatic control
Ultrasonic disperse 18min, while mechanical agitation, 1.3 parts of titanium dioxide are added, stir 15min, filtering, then enter reactant
Row washing, 19h is dried in vacuo at 70 DEG C, produces modified silver powder；
The modified polyorganosiloxane, in parts by weight, take 13 parts of both-end epoxy radicals polysiloxanes and 8 parts of divinyls three removed water
Amine and 4 parts of n-butanols are placed in reactor, are then passed through nitrogen in a kettle, and the ratio between nitrogen and oxygen are in holding reactor
3:1,75 DEG C of reaction 2.5h of temperature of reaction kettle are kept, is then evaporated under reduced pressure and removes solvent, produce modified polyorganosiloxane；
The modified glass powder, it is 50% by the mass concentration that 2.5 parts of KH-550 are dissolved in 1.5 times of its weight in parts by weight
Ethanol in, stir 5min, add 8 parts of lead-free glass powders stir process 50min in 65 DEG C of thermostats, taking-up is placed in agate and ground
Alms bowl grinds 13min, and drying in 90 DEG C of baking ovens then will be put into after glass dust solution natural air drying and is put to constant weight, then by the glass dust
In in resistance furnace, sintering temperature controls 1100 DEG C, is incubated 50min, and 400 mesh sieves are crossed after cooling, produce modified glass powder.
3. a kind of UV conductive silver pastes preparation method according to claim 1 or 2, it is characterised in that comprise the following steps：
1. pressing the parts by weight, diethylene glycol ether acetate, nylon acid dimethyl ester, the mixing of citric acid mechanical agitation is taken to be put into
Heated in 50 DEG C of thermostat water bath and stir 10min, add ethyl cellulose, treat that ethyl cellulose is completely dissolved, then added
Enter vinyl neodecanoate, epoxy resin, polyester acrylate to mix and be placed in homogenizer, rotating speed 1000-2000r/
Min, white slurry, polyethylene glycol are then sequentially added, bath temperature is then increased to 70 DEG C of heated at constant temperature stirring 20-30min, mistake
The removal of impurity is filtered off, produces organic carrier；
2. the modification silver powder, organic carrier, modified glass powder of preparation are compared into 1-3 according to weight:3-5：The mixing of 2-4 ratios, which is placed in, grinds
In alms bowl, slurry is ground into pasty state, then pasty slurry is placed in ball mill, adds a diameter of 1cm abrading-ball, is in rotating speed
120-150r/min, 10min is first roughly ground, then change abrading-ball into a diameter of 0.2cm, continue to grind 15min, then again by described heavy
Amount number sequentially adds modified polyorganosiloxane, polyethylene glycol oxide, and light trigger continues to grind 30min, then using three-roll grinder
Grinding distribution 5min, vacuum defoamation is then carried out, the vacuum of vacuum defoamation is 0.08MPa-0.12MPa, and inclined heated plate is
5min, produce UV conductive silver pastes.
A kind of 4. UV conductive silver pastes preparation method according to claim 3, it is characterised in that described step 4. middle modification
Silver powder, organic carrier, modified glass powder are by weight 2:4:3 ratios mix.
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| CN108735342A (en) * | 2018-06-27 | 2018-11-02 | 合肥同佑电子科技有限公司 | A kind of conductive silver paste and preparation method thereof of flash lamp tube high conductivity |
| CN109256234A (en) * | 2018-11-14 | 2019-01-22 | 轻工业部南京电光源材料科学研究所 | A kind of high-performance conductive silver paste and preparation method thereof |
| CN110335724A (en) * | 2019-07-25 | 2019-10-15 | 西安宏星电子浆料科技股份有限公司 | A kind of preparation method suitable for hetero-junctions high performance solar batteries silver paste |
| CN118430894A (en) * | 2024-07-03 | 2024-08-02 | 天津立进电子材料有限公司 | High-thixotropy conductive silver paste and preparation method thereof |
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| CN108735342A (en) * | 2018-06-27 | 2018-11-02 | 合肥同佑电子科技有限公司 | A kind of conductive silver paste and preparation method thereof of flash lamp tube high conductivity |
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