CN107393629A - A kind of conductive silver paste and its preparation method and application - Google Patents
A kind of conductive silver paste and its preparation method and application Download PDFInfo
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- CN107393629A CN107393629A CN201710822738.XA CN201710822738A CN107393629A CN 107393629 A CN107393629 A CN 107393629A CN 201710822738 A CN201710822738 A CN 201710822738A CN 107393629 A CN107393629 A CN 107393629A
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- silver paste
- powder
- conductive silver
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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
- H01B13/00—Apparatus or processes specially adapted for manufacturing conductors or cables
Abstract
The invention discloses a kind of conductive silver paste and its preparation method and application.The present invention utilizes the cooperation of spherical silver powder, glass dust different stage particle diameter, cooperates with the use of additive, has obtained the preferable silver paste of thixotropy, electric conductivity, printing, can be used as automobile wind screen defrosting demisting material.Conductive silver paste preparation method provided by the invention is simply efficient, has preferable market prospects.
Description
Technical field
The invention belongs to technical field of electronic materials, more particularly to a kind of conductive silver paste and its preparation method and application.
Background technology
One kind machinery that conductive silver paste is made up of metal silver particles, adhesive, solvent and the auxiliary agent of high-purity mixes
The thick slurry of thing, available for solar cell, windshield multiple fields.
The principle of defrosting-defogging that conductive silver paste is used for windshield is：Conductive silver paste is printed on vehicle glass and passed through
After tempering processing, glass surface be coated in by sintering so that glass surface has certain resistance, releases heat reality during energization
The removal of existing glass surface frost mist, so as to reach defrosting-defogging effect.Automobile using conductive silver paste is more to the performance requirement of silver paste,
Such as electric conductivity, printing, tensile strength, resistance to acids and bases, weatherability and thixotropy.Wherein, thixotropy refers to liquid viscosity in perseverance
Determine the extension under shearing rate effect over time and reduce, and after shear rate is removed, the property of viscosity rising.Thixotropy pair
The printing performance and stability of silver paste have a direct impact, because when the silver paste with compared with high thixotropic is normally placed, silver
It is larger to starch viscosity, silver powder and glass dust in slurries not free settling, and during by shearing force, viscosity declines, and is easy to print.
At present, automobile using conductive silver paste thixotropic index is about 1.5, conductive silver paste less stable, is brought to printing tired
It is difficult, it is difficult to form uniform and relatively thin serous coat, and then influence glass surface defrosting-defogging effect.
The content of the invention
It is an object of the invention to provide a kind of conductive silver paste and its preparation method and application.Conductive silver provided by the invention
Slurry, has higher thixotropy.
To realize object above, the invention provides a kind of conductive silver paste, count in parts by weight, including following components：
The ball shape silver powder D50 is 1~3 μm.
Preferably, the ball shape silver powder includes raw Ag powder and thin silver powder, and the D50 of the raw Ag powder is 2.0~3 μm, described
The D50 of thin silver powder is 1~1.8 μm.
Preferably, the mass ratio of the raw Ag powder and the thin silver powder is 1：1~2.
Preferably, the apparent density of the ball shape silver powder is 1~3g/mL, and tap density is 2~4g/mL.
Preferably, the D50 of the lead-free glass powder is 3~7 μm.
Preferably, thermal coefficient of expansion of the lead-free glass powder under the conditions of 200~300 DEG C is 6.0 × 10-6~7.0 ×
10-6/℃。
Preferably, the additive includes the one or more in anti-settling agent, coupling agent, surfactant and defoamer.
Present invention also offers the preparation method of the conductive silver paste described in above-mentioned technical proposal, comprise the following steps：To have
Solvent, cellulose and additive mixing, obtain mixed serum；The mixed serum is mixed with ball shape silver powder and lead-free glass powder
Close, obtain conductive silver paste.
Preferably, the ball shape silver powder, lead-free glass powder also include after being mixed with the mixed serum：Mixing to obtaining
Feed liquid is ground, and the grinding is specially：Material in the mixed liquor is ground to granularity less than 20 μm.
Present invention also offers preparation method system described in conductive silver paste described in above-mentioned technical proposal or above-mentioned technical proposal
Application of the standby obtained conductive silver paste in glass defrosting-defogging.
The invention provides a kind of conductive silver paste, count in parts by weight, including 60~80 parts of ball shape silver powder, 3~10 parts
Lead-free glass powder, 10~30 parts of organic solvent, 1~10 part of cellulose and 0.1~3 part of additive；Wherein, spherical silver
Powder D50 is 1~3 μm.The present invention is used as one of raw material using ball shape silver powder, the particle diameter of strict control silver powder, with lead-free glass powder,
Organic solvent, cellulose and additive cooperation, the contact area being effectively increased between silver powder particles, and then improve touching for silver paste
Denaturation.The result of embodiment shows that the thixotropic index of conductive silver paste provided by the present invention reaches more than 2.0, and silver paste is higher
Thixotropy can avoid viscosity it is excessive cause in printing process coat uneven thickness or it is blocked up the problem of, it is ensured that the uniform film of thickness
Ultimately form, improve the defrosting-defogging effect of vehicle glass.
The preparation method of conductive silver paste provided by the invention is simple, easily-controllable, is easy to industrialized production use.
Brief description of the drawings
The SEM figures of silver paste film after Fig. 1 embodiments 2 sinter.
Fig. 2 conductive silver pastes are used for silk-screen printing line map when glass surface coats.
Embodiment
The invention provides a kind of conductive silver paste, count in parts by weight, including following components：
The ball shape silver powder D50 is 1~3 μm.
In the present invention, in addition to being particularly limited to, D50 represents the average grain diameter of particle.
Conductive silver paste provided by the invention, in terms of parts by weight, include 60 parts~80 parts of ball shape silver powder, preferably 65~
78 parts, more preferably 70~77 parts, most preferably 77 parts.In the present invention, the D50 of the ball shape silver powder is preferably 1.2
~2.8 μm, more preferably 1.5~2.5 μm.In the present invention, the apparent density of the ball shape silver powder is preferably 1~3g/
ML, more preferably 1.1~2.8g/mL, more preferably 1.4~2.5g/mL；The tap density of the ball shape silver powder is preferably
2~4g/mL, more preferably 2.2~3.8g/mL, more preferably 2.5~3.5g/mL.The present invention is to the ball shape silver powder
Source does not have particular/special requirement, using commercially available prod well-known to those skilled in the art.
In the present invention, the ball shape silver powder preferably includes raw Ag powder and thin silver powder；The matter of the raw Ag powder and thin silver powder
Measure ratio preferably 1：1~2, more preferably 1：1.2~1.5, more preferably 1:1.3~1.4.In the present invention, the thick silver
The D50 of powder is preferably 2.0~3 μm, more preferably 2.01~2.50 μm；The D50 of the thin silver powder is preferably 1~1.8 μm,
More preferably 1.2~1.7 μm, more preferably 1.5~1.65 μm.In the present invention, the raw Ag powder coordinates with thin silver powder
Use, for single particle size silver powder, can further increase the surface area contacted between silver powder, improve the conduction of silver paste
Property.
In the present invention, the apparent density of the raw Ag powder is preferably 1~3g/mL, more preferably 1.4~2.6g/
ML, more preferably 1.5~2.2g/mL, most preferably 1.58g/mL；The tap density of the raw Ag powder is preferably 2~4g/mL,
More preferably 2.2~3.8g/mL, more preferably 2.5~3.5g/mL, most preferably 3.23g/mL.
In the present invention, the apparent density of the thin silver powder is 1~2g/mL, more preferably 1.2~1.8g/mL；Institute
The tap density for stating thin silver powder is preferably 2~3g/mL, more preferably 2.2~2.8g/mL, more preferably 2.3~2.7g/
ML, most preferably 2.5~2.6g/mL.
Based on the ball shape silver powder of the parts by weight, conductive silver paste provided by the invention includes the nothing of 3~10 parts by weight
Lead glass powder, preferably 4~8 parts, more preferably 5~7 parts, most preferably 5.5~6 parts.
In the present invention, the lead-free glass powder is preferably the non-crystallization type glass dust of low melting point；The lead-free glass powder
Fusing point is preferably 500~800 DEG C, more preferably 600~700 DEG C.In an embodiment of the present invention, the lead-free glass powder
Preferably Na-Bi glass frits.In the present invention, the D50 of the lead-free glass powder is preferably 3~7 μm, more preferably 4
~6 μm, more preferably 5 μm.In the present invention, thermal coefficient of expansion of the lead-free glass powder under the conditions of 200~300 DEG C is preferred
For 6.0 × 10-6~7.0 × 10-6/ DEG C, more preferably 6.5 × 10-6/℃；The glass transition temperature of the lead-free glass powder
Preferably 450~550 DEG C；The sintering temperature of the lead-free glass powder is preferably 560~600 DEG C, the tempering temperature with vehicle glass
Degree is close, is advantageous to the combination of silver paste and vehicle glass, improves adhesive force of the conductive silver paste on vehicle glass, while can also carry
The acid corrosion-resistant performance of highly conductive silver paste.The present invention does not have particular/special requirement to the source of the lead-free glass powder, of the invention real
Apply in example, using commercially available prod well-known to those skilled in the art.
Based on the ball shape silver powder of the parts by weight, conductive silver paste provided by the invention includes having for 10~30 parts by weight
Solvent, preferably 12~27 parts, more preferably 14~25 parts.
In the present invention, the organic solvent is preferably volatile organic solvent, and more preferably freezing point is at -10 DEG C
Below and organic solvent of the boiling point below 250 DEG C, more preferably alcohol organic solvent, based organic solvent or ethers are molten
Agent；The alcohol organic solvent further preferably includes butyl carbitol and/or terpinol；The based organic solvent is further
Preferably include butyl carbitol acetate and/or ATBC；The ether organic solvent is more preferably propane diols
Methyl ether and/or butyl.When the organic solvent is the mixture of many kinds of substance, the present invention is in the mixture
The mass ratio of each component does not have particular/special requirement.In embodiments of the present invention, organic solvent used is preferably butyl carbitol, pine tar
The mixture of alcohol and butyl carbitol acetate；The mixture of the butyl carbitol, terpinol and butyl carbitol acetate
The mass ratio of middle butyl carbitol, terpinol and butyl carbitol acetate is preferably 6.0~12：3~8：2~5, more preferably
6~8：4~6：3~4.
Based on the ball shape silver powder of the parts by weight, conductive silver paste provided by the invention includes the fibre of 1~10 parts by weight
Dimension element, more preferably preferably 1.5~8 parts, 2 parts.
In the present invention, the cellulose is preferably ethyl cellulose or NC Nitroncellulose；In the present invention, cellulose energy
Enough promote the bonding between ball shape silver powder and lead-free glass powder.In embodiments of the present invention, the cellulose is ethyl cellulose,
For the commercially available prod of routine.
Based on the ball shape silver powder of the parts by weight, conductive silver paste provided by the invention includes the outer of 0.1~3 parts by weight
Add agent, preferably 0.2~2 part, more preferably 0.5~1.5 part, more preferably 0.6~1.2 part, most preferably 0.8 part.
In the present invention, the additive preferably includes one kind in anti-settling agent, coupling agent, surfactant and defoamer
It is or a variety of.
In the present invention, the anti-settling agent further preferably include polyolefin-wax, modified hydrogenated castor oil, polyamide wax,
One or more in castor oil derivative；The anti-settling agent effectively can prevent ball shape silver powder from precipitating.The present invention is to described anti-settling
The specific source of agent does not have particular/special requirement, using anti-settling agent well-known to those skilled in the art.In the embodiment of the present invention
In, anti-settling agent used is modified hydrogenated castor oil.
In the present invention, the coupling agent is more preferably silane coupler, more preferably amido functional group silane
Or γ-methacryloxypropyl trimethoxy silane (KH570) (KH550).In the present invention, the coupling agent can have
The dispersiveness of the improvement slurry of effect.The present invention does not have particular/special requirement to the specific source of the coupling agent, using art technology
Commercially available prod known to personnel.
In the present invention, the surfactant further preferably includes lecithin, 1-METHYLPYRROLIDONE, acetone and second
One or more in alcohol.In the present invention, the surfactant can effectively avoid the group of ball shape silver powder, lead-free glass powder
It is poly-, improve the scattered uniformity of ball shape silver powder, crown glass powder particles.The present invention is to the source of the surfactant without spy
It is different to require, using surfactant well known to those skilled in the art.
In the present invention, the defoamer preferably includes organic silicon defoaming agent and/or BYK-A555 defoamer.In the present invention
In, the defoamer can effectively reduce surface tension, reduce bubble formation.
In the present invention, the additive is preferably anti-settling agent and surfactant, more preferably modified castor oil and ovum
Phosphatide；When using anti-settling agent and surfactant as additive, the anti-settling agent is preferably with surfactant qualities ratio：
0.5~3:1, more preferably 1~2:1.In embodiments of the present invention, the modified castor oil and lecithin are conventional
Commercially available prod.
In the present invention, the conductive silver paste D50 preferably≤20 μm, more preferably≤18 μm, more preferably≤15 μ
m。
Present invention also offers the preparation method of conductive silver paste described in above-mentioned technical proposal, including：By the ball shape silver powder,
Lead-free glass powder mixes with the mixed serum including the organic solvent, cellulose and additive, obtains conductive silver paste.
The present invention does not have particular/special requirement to the manner of formulation of the mixed serum of the organic solvent, cellulose and additive,
Using the manner of formulation of mixed material well-known to those skilled in the art.The present invention preferably by the cellulose with it is organic
Mixed again with additive after solvent mixing.In the present invention, the preparation of the mixed serum is preferably entered under condition of water bath heating
OK, the temperature of the heating water bath is preferably 80~90 DEG C.
The mixed serum including organic solvent, cellulose and additive carries out sieving processing described in preferred pair of the present invention, with
The particle diameter of each component in mixed serum is refined, lifts the performance of slurry.In the present invention, the sieve aperture of the sieving processing screen cloth
Preferably 200~400 mesh, extracting screen underflow are standby.
The present invention is by the ball shape silver powder, lead-free glass powder with including the mixed of the organic solvent, cellulose and additive
Slurries mixing is closed, obtains conductive silver paste.In the present invention, the mixing preferably includes：By the ball shape silver powder and crown glass
Powder is mixed to get mixed powder；By the obtained mixed powder and mixing including the organic solvent, cellulose and additive
Close slurries mixing.
The present invention does not have particular/special requirement to the hybrid mode of the ball shape silver powder and lead-free glass powder, using art technology
Hybrid mode known to personnel.In the present invention, the rotating speed of the mixing is preferably 30~50rpm；The mixing when
Between be preferably 60~90min.In an embodiment of the present invention, the mixing of the ball shape silver powder and lead-free glass powder is preferably in three-dimensional
Carried out in mixer；The present invention is improved using the translation of three-dimensional mixer, the integrated operation of three kinds of hybrid modes of rotation and axial direction
The mixability of ball shape silver powder and lead-free glass powder.
The present invention does not have particular/special requirement to the hybrid mode of the mixed powder and mixed serum, using people in the art
Material hybrid mode known to member.In the present invention, the rotating speed of the mixing is preferably 1000~3000rmp；It is described mixed
When the temperature of conjunction is preferably 20~27 DEG C；The time of the mixing is preferably 5~8h.In embodiments of the present invention, the mixing
It is preferred that carried out using mixer；The present invention does not have particular/special requirement to the concrete model of the mixer, using people in the art
Mixer known to member.
After the mixing for completing the mixed powder and mixed serum, the compound obtained described in preferred pair of the present invention is ground
Mill processing, further to improve the thixotropic property of conductive silver paste.In the present invention, the granularity of the compound after the milled processed
Preferably no greater than 20 μm, more preferably granularity is not higher than 15 μm.The present invention does not have to the embodiment of the milled processed
Particular/special requirement, using milled processed mode well-known to those skilled in the art.In the present invention, the speed of the grinding
Preferably slow rollers speed, it is preferably：20~30rmp, milling time are preferably 60~90min.In an embodiment of the present invention, institute
Milled processed is stated preferably to complete by three-roll grinder.
Present invention also offers preparation method system described in the conductive silver paste described in above-mentioned technical proposal or above-mentioned technical proposal
Application of the standby obtained conductive silver paste in glass defrosting-defogging.The present invention is to the conductive silver paste in glass defrosting-defogging
Application mode does not have particular/special requirement, using conductive silver paste well-known to those skilled in the art answering in the defrosting-defogging of glass
With mode.After the conductive silver paste is preferably coated in glass surface by the present invention, it is dried and sinters successively.
In the present invention, the coating processing, the thickness of coat is preferably 20~30 μm, more preferably 22~27
μm.The present invention does not have particular/special requirement to the mode of the coating, using conductive silver paste well-known to those skilled in the art in glass
The coating method on glass surface.In the present invention, the mode of the coating is preferably to print, more preferably screen printing
Brush, the printing of more preferably 200 mesh polyester nets；As shown in Figure 2,1 it is conducting wire measurement point in figure, mainly passes through origin 1
Measurement circuitry resistance；2 are：Line width 1mm conducting wire, it is heatable after energization；3 are：30*35mm rectangle, for testing
The tensile strength of silver paste.
In the present invention, the coating preferably includes following steps：The conductive silver paste is printed on using polyester net
On the glass cleaned up, silver paste coat is obtained.In the present invention, the dosage of the conductive silver paste is preferably 4.5~5.5g,
More preferably 5g；The present invention does not have particular/special requirement to the pattern of silver paste coat, using those skilled in the art institute
The pattern of well known film.
After the coating, processing is dried in coat obtained by preferred pair of the present invention, to remove the solvent composition in silver paste.
In the present invention, the drying temperature is preferably 120~160 DEG C, more preferably 130~155 DEG C, more preferably 140~
150℃；The drying time is 2~6h, more preferably 3~5h, more preferably 3.5~4h.The present invention is to the drying
The mode of processing does not have particular/special requirement, using drying mode well-known to those skilled in the art；In the implementation of the present invention
In example, the drying process is specifically to be carried out in air dry oven.
After completing the drying, the dried coat of preferred pair of the present invention is sintered so that conductive silver paste into
Film.In the present invention, the temperature of the sintering processes is preferably 650~680 DEG C, more preferably 660~670 DEG C, optimal
Elect 670 DEG C as；The maximum temperature soaking time is preferably 2~5min, more preferably 3~4min, most preferably 3min.
The present invention to sintering processes mode without particular determination, using sintering processing well known to those skilled in the art；At this
In the embodiment of invention, the sintering processes are carried out in Muffle furnace.Film forming after sintering can be measured by micrometer,
Compactness is observed by SEM, and the thickness of film forming is 10~15 μm after the sintering, and compactness is preferable.
In order to further illustrate the present invention, with reference to embodiment to conductive silver paste provided by the invention and preparation method thereof
It is described in detail with application, but they can not be interpreted as limiting the scope of the present invention.
Embodiment 1：
A kind of conductive silver paste, including：
The D50 of above-mentioned thin silver powder is 1.63 μm, apparent density 1.22g/ml, tap density 2.55g/ml；Raw Ag powder
D50 be 2.01 μm, apparent density 1.58g/ml, tap density 3.23g/ml.
The D50 of above-mentioned lead-free glass powder is at 5 μm, 300 DEG C, and linear expansion coefficient is 6.5 × 10-6/ DEG C, glass transition temperature
For 450 DEG C, sintering temperature is 560 DEG C.
The conductive silver paste preparation method includes：
Thin silver powder, raw Ag powder and lead-free glass powder are placed in three-dimensional mixer by weight proportion and mixed, must be mixed
Powder is standby.
By butyl carbitol, terpinol, butyl carbitol acetate, ethyl cellulose, modified hydrogenated castor oil and lecithin
Fat is by weight proportion at 90 DEG C, after stirring 30min, crosses 400 mesh sieves, mixed serum obtained by screenings is standby.
Well mixed powder and mixed serum are mixed into 6h at 2000rmp, 25 ± 2 DEG C, obtain mixed slurry.
Mixed slurry is rolling to slurry fineness as 11 μm with three-roll grinder, that is, obtains conductive silver paste.
Conductive silver paste film forming is then completed by following steps：Coated according to the conductive silver paste shown in Fig. 2 for glass surface
When silk-screen printing line map, by 4.5g conductive silver pastes coated in coat of the thickness for 22 μ m-thicks on glass, is formed, 155
3h is dried at DEG C, then the sintered heat insulating 3min film forming at 670 DEG C, obtain defrosting-defogging glass of the cladding thickness for 12 μm of films
Glass.
The compactness of silver paste film after sintering is tested, the bright film compactness of SEM charts is preferable.
The viscosity of conductive silver paste is tested, is 75rpm in rotating speed, temperature is at 25 DEG C using viscotron
Viscosity test is carried out to conductive silver paste, the viscosity for measuring conductive silver paste is 20PaS.
The thixotropic index of conductive silver paste is tested, the method for testing of thixotropic index is：Under the conditions of 25 DEG C, survey respectively
6r/min and 60r/min viscosity is tried, the two ratio is the thixotropic index of conductive silver paste, and the thixotropic index for measuring silver paste is
2.5。
Electric conductivity burns till the electric conductivity of silverskin using four-point probe well known to those skilled in the art test, according to upper
Method test is stated, the sheet resistance that conductive silver paste burns till film is 12.5m Ω/.
Tensile strength burns till the tensile strength of film using welding well known to those skilled in the art test, according to above-mentioned side
Method is tested, and the tensile strength that conductive silver paste burns till film is 278N.
Acid and alkali resistance corrosive nature is carried out to the glass for covering conductive silver paste film, impact resistance and weatherability are carried out
Test, method of testing are as shown in table 1.After the test of resistance to acids and bases, impact resistance and weatherability, silver slurry layer is not fallen off, and
Front and rear resistance variations are respectively less than 10%.
Table 1：The test of conductive silver paste film acid resistance, impact resistance and weatherability
The glass defrosting-defogging performance of covering conductive silver paste film has a direct impact with sheet resistance, and sheet resistance is lower, film
Caloric value it is bigger, defrosting-defogging effect is better, and the sheet resistance that conductive silver paste burns till film is 12.5m Ω/, illustrates to have preferable
Defrosting-defogging effect.
Embodiment 2：
A kind of conductive silver paste, including：
Thin silver powder, the D50 of raw Ag powder, apparent density and tap density, D50, the line of lead-free glass powder are swollen in the present embodiment
Swollen coefficient, glass transition temperature and sintering temperature, performance test methods are same as Example 1, preparation process and the phase of embodiment 1
Together, difference is to obtain conductive silver paste after being ground to 15 μm.Conductive silver paste 5g, prints according to Fig. 2, and coat thickness is 24
μm, 4h is dried at 140 DEG C, 670 DEG C of sintering 3min, obtains defrosting-defogging glass of the cladding thickness for 13 μm of films.After sintering
The compactness of silver paste film is tested, and accompanying drawing 1 is schemed for SEM, understands that silver paste film has preferable compactness according to image；It is right
Conductive silver paste and film carry out performance test, and test result is shown in Table 1.
Embodiment 3：
A kind of conductive silver paste, including：
D50, apparent density and the tap density of thin silver powder in the present embodiment, the D50 of lead-free glass powder, linear expansion coefficient,
Glass transition temperature and sintering temperature, performance test methods are same as Example 1, and preparation method is same as Example 1, different
Part is that being ground to 14 μm obtains conductive silver paste.Conductive silver paste 5.5g, prints according to Fig. 1, coat thickness be 24 μm, 160
2h is dried at DEG C, sinters 2min at 680 DEG C, obtains defrosting-defogging glass of the cladding thickness for 15 μm of films, to conductive silver paste and
Film carries out performance test, and test result is shown in Table 1.
Embodiment 4：
A kind of conductive silver paste, including：
The D50 of raw Ag powder, apparent density and tap density in the present embodiment, the D50 of lead-free glass powder, linear expansion coefficient,
Glass transition temperature and sintering temperature, preparation method and performance test methods are same as Example 1.Conductive silver paste 5g, according to
Fig. 1 prints, and coat thickness is that 3.5h is dried at 22 μm, 140 DEG C, and 3min is sintered at 670 DEG C, and it is 14 μm thin to obtain cladding thickness
The defrosting-defogging glass of film, performance test is carried out to conductive silver paste and film, test result is shown in Table 1.
Embodiment 5：
A kind of conductive silver paste, including：
In the present embodiment the D50 of raw Ag powder be 2.15 μm, apparent density 1.60g/ml, tap density 3.40g/ml,
The D50 of lead-free glass powder is 4 μm, linear expansion coefficient is 7.0 × 10-6/ DEG C, glass transition temperature be 550 DEG C, sintering temperature is
500 DEG C, conductive silver paste preparation method is same as Example 1.Conductive silver paste 5.5g, coat thickness is 24 μm, follow-up to dry temperature
Spend for 120 DEG C, time 5h, sintering temperature is to be incubated 3min at 650 DEG C, 650 DEG C, obtains cladding thickness removing for 13 μm of films
White antifog glass, performance test methods are same as Example 1, and test result is shown in Table 1.
Embodiment 6：
A kind of conductive silver paste, including：
In the present embodiment the D50 of thin silver powder be 1.50 μm, apparent density 1.50g/ml, tap density 2.30g/ml,
The D50 of raw Ag powder is 2.40 μm, apparent density 2.00g/ml, tap density 3.20g/ml, and the D50 of lead-free glass powder is 6 μ
M, linear expansion coefficient, glass transition temperature and sintering temperature be with embodiment 1, and preparation method and performance test methods are and embodiment
1 is identical.The application process and parameter of conductive silver paste are same as Example 1, and test result is shown in Table 1.
The performance test results after the conductive silver paste of table 1 and film forming
As shown in Table 1, conductive silver paste obtained by the embodiment of the present application has higher thixotropic index, modest viscosity, is easy to print
Scopiform is into coat in uniform thickness；And gained film forming after sintering, compactness is preferable, has relatively low sheet resistance, illustrates that film forming is led
Electrically good, glass has excellent defrosting-defogging effect；Tensile strength is higher, illustrates between film forming and glass with stronger
Cohesive force, it is difficult for drop-off；Simultaneously preferable to acid, alkali, weather and the patience of impact, conductive silver paste film forming is not fallen off after test, and
Resistance variations are less than 10% before and after test, illustrate that gained conductive silver paste is used in defrosting-defogging, are suitable for the working environment of complexity,
Extend the service life of film forming, improve the utilization rate of conductive silver paste.
Described above is only the preferred embodiment of the present invention, not makees any formal limitation to the present invention.Should
Point out, for those skilled in the art, under the premise without departing from the principles of the invention, if can also make
Dry improvements and modifications, these improvements and modifications also should be regarded as protection scope of the present invention.
Claims (10)
1. a kind of conductive silver paste, is counted in parts by weight, including following components：
The D50 of the ball shape silver powder is 1~3 μm.
2. conductive silver paste according to claim 1, it is characterised in that the ball shape silver powder includes raw Ag powder and thin silver powder,
The D50 of the raw Ag powder is 2.0~3 μm, and the D50 of the thin silver powder is 1~1.8 μm.
3. conductive silver paste according to claim 2, it is characterised in that the mass ratio of the raw Ag powder and the thin silver powder is
1：1~2.
4. according to the conductive silver paste described in any one of claims 1 to 3, it is characterised in that the apparent density of the ball shape silver powder
For 1~3g/mL, tap density is 2~4g/mL.
5. conductive silver paste according to claim 1, it is characterised in that the D50 of the lead-free glass powder is 3~7 μm.
6. conductive silver paste according to claim 1 or 5, it is characterised in that the lead-free glass powder is in 200~300 DEG C of bars
Thermal coefficient of expansion under part is 6.0 × 10-6~7.0 × 10-6/℃。
7. conductive silver paste according to claim 1, it is characterised in that the additive includes anti-settling agent, coupling agent, surface
One or more in activating agent and defoamer.
8. the preparation method of the conductive silver paste described in any one of claim 1~7, comprises the following steps：
Organic solvent, cellulose and additive are mixed, obtain mixed serum；
The mixed serum is mixed with ball shape silver powder and lead-free glass powder, obtains conductive silver paste.
9. preparation method according to claim 8, it is characterised in that the ball shape silver powder, lead-free glass powder mix with described
Also include after closing slurries mixing：Obtained mixed liquor is ground, the grinding is specially：By thing in the mixed liquor
Abrasive lapping to granularity is less than 20 μm.
What 10. conductive silver paste or claim 8 or 9 preparation method described in any one of claim 1~7 were prepared
Application of the conductive silver paste in glass defrosting-defogging.
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| CN109671516A (en) * | 2019-01-24 | 2019-04-23 | 日照众邦电子有限公司 | A kind of method of preparation and use of electric heating resistance slurry |
| CN111326849A (en) * | 2020-03-09 | 2020-06-23 | 广东四维新材料有限公司 | Method for preparing signal receiving/transmitting antenna of automatic driving automobile |
| CN111477378A (en) * | 2020-04-13 | 2020-07-31 | 湖南省国银新材料有限公司 | Automobile glass hot wire silver paste capable of meeting low sintering temperature and preparation method thereof |
| CN114171238A (en) * | 2021-12-23 | 2022-03-11 | 上海宝银电子材料有限公司 | Low-resistance silver paste for automobile glass and preparation method thereof |
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| CN114171238A (en) * | 2021-12-23 | 2022-03-11 | 上海宝银电子材料有限公司 | Low-resistance silver paste for automobile glass and preparation method thereof |
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| CN107393629B (en) | 2020-01-17 |
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