CN105761777B - A kind of vehicle glass fine rule silver paste and preparation method thereof - Google Patents
A kind of vehicle glass fine rule silver paste and preparation method thereof Download PDFInfo
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Abstract
The present invention relates to a kind of vehicle glass fine rule silver paste and preparation method thereof, raw material uses following components and weight percent content：Silver powder 60 80%；Glass dust 3 7%；Macromolecule resin 1 8%；Organic additive 1 3%；Organic solvent 10 25%, vehicle glass fine rule silver paste is prepared by steps such as stock, the preparation of carrier, the preparation of silver paste, the productions of silver paste.Compared with prior art, the product that is prepared of the present invention solves the problems such as printing fineness of silver paste, electric conductivity, compactness.
Description
Technical field
The present invention relates to a kind of vehicle glass silver paste and preparation method thereof, more particularly, to a kind of vehicle glass fine rule silver
Slurry and preparation method thereof.
Background technology
With the continuous development of China's economy, auto industry also obtains quick vigorous growth, and auto output also carries year by year
Rise.Meanwhile vehicle glass is also continuously increased with silver paste and the demand of black glaze, and quality requirements are also more and more higher.
White in order to quickly eliminate mist, shelves glass typically can all be furnished with demisting frost heater wire after automobile.Heater wire typically passes through
Silver paste is imprinted on the surface of vehicle glass and black glaze by screen printing technique, handles 3-5min through annealing furnace tempering, adheres to silver paste
Silver layer is formed in the surface of vehicle glass and black glaze.The resistance of heater wire is typically in 0.5-1.2 Ω after sintering, in vehicle glass two
Source of welding current circuit on the silver face of side, after leading to upper 12-13V voltage, whole heater wire starts to generate heat, so as to reach the effect of demisting
Fruit.Due to heater wire with automobile be likely to be exposed at it is damp and hot wait environment in, therefore the acid resistance to vehicle glass silver paste, wearability,
Adhesive force, inoxidizability etc. propose very high technical requirements.Meanwhile in view of silver paste be actually be printed in above black glaze, therefore
Silver paste and the matching of black glaze it is also proposed very high technical requirements.
At present, most of silver paste of domestic automobile glass factory is domestic silver paste, and small part is using Du Pont, Fu Lu and village letter
Ten thousand rich grade external products, are primarily present problems with：The line width of silver paste silk-screen printing is generally 0.6-0.9mm, is not suitable for line width
For 0.3mm or so fine rule product, the frequency to break is higher.
Chinese patent CN101613186A discloses lead-free silver slurry for high-temperature sintered automobile glass heating wire and its preparation side
Method, the lead-free silver slurry include following components and content (weight)：Silver powder 50%~85%；Unleaded silver glass powder 3%~7%；It is high
Molecular adhesion agent 3%~12%；Organic solvent 7%~23%；Superfine metal compound 1%~5%；Additive 0.5%~
3%, component is blended, dissolves, grinds, being filtrated to get lead-free silver slurry for high-temperature sintered automobile glass heating wire.The application is with being somebody's turn to do
Difference between patent essentially consists in the control of glass dust and silver powder to particle size, and the big silver paste of particle diameter is not suitable for
0.3mm or so fine rule product.
The content of the invention
The purpose of the present invention is exactly to solve the printing fineness of silver paste, electric conductivity, fine and close sex chromosome mosaicism and the vapour provided
Car glass fine rule silver paste and preparation method thereof.
The purpose of the present invention can be achieved through the following technical solutions：
A kind of vehicle glass fine rule silver paste, raw material use following components and weight percent content：Silver powder 60-
80%；Glass dust 3-7%；Macromolecule resin 1-8%；Organic additive 1-3%；Organic solvent 10-25%.
Described silver powder is the compound that spherical silver powder and flake silver powder are formed, and the particle diameter of spherical silver powder is 0.3-
3.0 μm, tap density 2.0-4.0g/ml；The particle diameter of flake silver powder is 1-7 μm, tap density 1.0-3.0g/ml.
As preferred embodiment, for the particle diameter of spherical silver powder preferably with 1.0-3.0 μm, the particle diameter of flake silver powder is 5-
6μm。
Described glass dust is the mixture that glass dust-L and glass dust-H is formed,
Glass dust-the L is lead-free glass powder, and particle diameter is 0.5-2 μm, and sintering temperature is 550-650 DEG C, including with the following group
Point and weight percentage：Bi2O355-75、B2O310-30、ZnO 5-15、SiO23-10、Al2O30-3、Na2O 0-3、
Fe2O30-1、ZrO20-1,
Glass dust-the H is lead-free glass powder, and particle diameter is 0.5-2 μm, and sintering temperature is 650-750 DEG C, including with the following group
Point and weight percentage：Bi2O350-70、B2O310-30、ZnO 5-15、SiO23-10、Sb2O33-10、Al2O30-3、Na2O
0-3、Cr2O30-2、Fe2O30-1、ZrO20-1、NiO 0-1、Ag2O 0-1。
Described macromolecule resin is one in ethyl cellulose, NC Nitroncellulose, ethylhydroxyethylcellulose, wood rosin
Kind or several, preferred, ethyl.Described organic additive includes plasticizer, levelling agent, coupling agent,
The plasticizer is that dibutyl phthalate, ATBC, dioctyl phthalate, citric acid three are pungent
One or more in ester；
The levelling agent be organic siliconresin, rilanit special, polyvinyl butyral resin, one kind in polyacrylate or
It is several；
The coupling agent is the one or more in Silane coupling agent KH550, KH560, KH570.
Described organic solvent is terpineol, turpentine oil, butyl, dibutyl ethylene glycol ether, butyl carbitol
One or more of mixtures in acetate, dipropylene glycol monomethyl ether, Tripropylene glycol monomethyl Ether.
Vehicle glass uses following steps with the preparation method of fine rule silver paste：
(1) stocked up according to following components and weight percentage：
(2) preparation of carrier：Macromolecule resin and organic solvent are weighed, is then heated and is warming up to 80 DEG C and constant temperature,
After macromolecule resin is completely dissolved, the filtering and impurity removing on the screen cloth of 400-500 mesh, that is, carrier is obtained；
(3) preparation of silver paste：After weighing silver powder, glass dust, organic additive, filled with carrier in batch mixer
Divide mixing, reuse high speed dispersion agent and disperse at a high speed, that is, obtain uniform slurry；
(4) production of silver paste：Above-mentioned slurry is ground in three-high mill, the thin of silver paste is made by the fine setting of roller
Below 8 μm viscosity 20-30PaS, that is, vehicle glass fine rule silver paste is made in degree control.
Compared with prior art, due in silver paste the particle size of glass dust and silver powder for vehicle glass fine rule product
Silk-screen printing plays conclusive effect, and when particle diameter is bigger than normal, the problem of often occurring to break after silver wire sinters, the present invention passes through
The selection collocation of ultra-fine ball powder and piece powder, to solve printing fineness, electric conductivity, the compactness of silver paste；Pass through the choosing of glass dust
Collocation is selected, to solve the adhesive force between silver paste and glass, and the shade in glass tin face；Pass through the choosing of organic additive
Select, to solve the processing performance of silver paste printing.
Embodiment
With reference to specific embodiment, the present invention is described in detail.
Embodiment 1
(1) stock up 1000g, is stocked up according to following components and quality：
The particle diameter of spherical silver powder used is 1.0 μm, tap density 2.2g/ml；The particle diameter of flake silver powder is 6.2 μm, is shaken
Real density is 2.5g/ml；
In glass dust used, glass dust-L is 10g, and particle diameter is 1.35 μm, and its component and percentage composition are：Bi2O365、
B2O318、ZnO 9、SiO24、Al2O32、Na2O 1、Fe2O30.5、ZrO20.5；Glass dust-H is 20g, and particle diameter is 1.50 μm, its
Component and percentage composition are：Bi2O360、B2O319、ZnO 8、SiO25、Sb2O34、Al2O31、Na2O 1、Cr2O30.5、
Fe2O30.4、ZrO20.4、NiO 0.3、Ag2O 0.5；
Organic additive used is 5g dibutyl phthalates, 2.5g organic siliconresins and 2.5g silane couplers
KH550。
(2) preparation of carrier：10g ethyl celluloses and 150g terpineols are weighed, is then heated and is warming up to 80 DEG C simultaneously
Constant temperature, after ethyl cellulose is completely dissolved, the filtering and impurity removing on the screen cloth of 400-500 mesh, that is, obtain carrier；
(3) preparation of silver paste：Weigh the spherical silver powder of 700g, 100g flake silver powders, 30g glass dust, 10g organic additives
Afterwards, it is sufficiently mixed with organic carrier in batch mixer, reuses high speed dispersion agent and disperse at a high speed, that is, obtain uniform
Slurry；
(4) production of silver paste：Above-mentioned slurry is ground 6 times in three-high mill, silver paste is made by the fine setting of roller
Fineness control less than 8 μm, viscosity 20-30PaS, i.e., the fine rule silver paste of obtained vehicle glass.
Embodiment 2
(1) stock up 1000g, is stocked up according to following components and quality：
The particle diameter of spherical silver powder used is 1.0 μm, tap density 2.2g/ml；The particle diameter of flake silver powder is 7.6 μm, is shaken
Real density is 2.1g/ml；
In glass dust used, glass dust-L is 15g, and particle diameter is 1.65 μm, and its component and percentage composition are：Bi2O370、
B2O316、ZnO 8、SiO23.5、Al2O31.5、Na2O 1.0、Fe2O30、ZrO20；Glass dust-H is 25g, and particle diameter is 1.50 μm,
Its component and percentage composition are：Bi2O360、B2O319、ZnO 8、SiO25、Sb2O34、Al2O31、Na2O 1、Cr2O30.5、
Fe2O30.4、ZrO20.4、NiO 0.3、Ag2O 0.5；
Organic additive used is 6g dioctyl phthalates, 2g organic siliconresins and 2g silane couplers KH560.
(2) preparation of carrier：30g NC Nitroncelluloses and 170g butyls are weighed, is then heated and is warming up to
80 DEG C and constant temperature, after NC Nitroncellulose is completely dissolved, the filtering and impurity removing on the screen cloth of 400-500 mesh, that is, obtain carrier；
(3) preparation of silver paste：Weigh the spherical silver powder of 650g, 100g flake silver powders, 40g glass dust, 10g organic additives
Afterwards, it is sufficiently mixed with organic carrier in batch mixer, reuses high speed dispersion agent and disperse at a high speed, that is, obtain uniform
Slurry；
(4) production of silver paste：Above-mentioned slurry is ground 7 times in three-high mill, silver paste is made by the fine setting of roller
Fineness control less than 8 μm, viscosity 20-30PaS, i.e., the fine rule silver paste of obtained vehicle glass.
Embodiment 3
(1) stock up 1000g, is stocked up according to following components and quality：
The particle diameter of spherical silver powder used is 1.8 μm, tap density 2.6g/ml；The particle diameter of flake silver powder is 8.2 μm, is shaken
Real density is 2.5g/ml；
In glass dust used, glass dust-L is 20g, and particle diameter is 1.65 μm, and its component and percentage composition are：Bi2O370、
B2O316、ZnO 8、SiO23.5、Al2O31.5、Na2O 1.0、Fe2O30、ZrO20；Glass dust-H is 30g, and particle diameter is 1.80 μm,
Its component and percentage composition are：Bi2O362、B2O316、ZnO 10、SiO24、Sb2O35、Al2O31、Na2O 1、Cr2O30.5、
Fe2O30、ZrO20、NiO0、Ag2O 0.5；
Organic additive used is 10g ATBCs, 5g rilanit specials and 5g silane couplers
KH570。
(2) preparation of carrier：50g ethylhydroxyethylcelluloses, 90g terpineols and 90g butyl carbitol acetates are weighed,
Then it is heated and is warming up to 80 DEG C and constant temperature, after ethylhydroxyethylcellulose is completely dissolved, on the screen cloth of 400-500 mesh
Filtering and impurity removing, that is, obtain carrier；
(3) preparation of silver paste：Weigh the spherical silver powder of 600g, 100g flake silver powders, 50g glass dust, 20g organic additives
Afterwards, it is sufficiently mixed with organic carrier in batch mixer, reuses high speed dispersion agent and disperse at a high speed, that is, obtain uniform
Slurry；
(4) production of silver paste：Above-mentioned slurry is ground 6 times in three-high mill, silver paste is made by the fine setting of roller
Fineness control less than 8 μm, viscosity 20-30PaS, i.e., the fine rule silver paste of obtained vehicle glass.
Embodiment 4
(1) stock up 1000g, is stocked up according to following components and quality：
The particle diameter of spherical silver powder used is 1.8 μm, tap density 2.6g/ml；The particle diameter of flake silver powder is 8.6 μm, is shaken
Real density is 2.1g/ml；
In glass dust used, glass dust-L is 25g, and particle diameter is 1.35 μm, and its component and percentage composition are：Bi2O365、
B2O318、ZnO 9、SiO24、Al2O32、Na2O 1、Fe2O30.5、ZrO20.5；Glass dust-H is 35g, and particle diameter is 1.80 μm, its
Component and percentage composition are：Bi2O362、B2O316、ZnO 10、SiO24、Sb2O35、Al2O31、Na2O 1、Cr2O30.5、Fe2O30、
ZrO20、NiO0、Ag2O 0.5；
Organic additive used is 15g trioctyl lemon acids, 10g polyvinyl butyral resins and 5g silane couplers KH560.
(2) preparation of carrier：Weigh 35g ethyl celluloses, 35g NC Nitroncelluloses, 100g Tripropylene glycol monomethyl Ethers and 100
Turpentine oil, then it is heated and is warming up to 80 DEG C and constant temperature, after ethyl cellulose and NC Nitroncellulose are completely dissolved, in 400-
Filtering and impurity removing on the screen cloth of 500 mesh, that is, obtain carrier；
(3) preparation of silver paste：Weigh the spherical silver powder of 550g, 100g flake silver powders, 60g glass dust, 20g organic additives
Afterwards, it is sufficiently mixed with organic carrier in batch mixer, reuses high speed dispersion agent and disperse at a high speed, that is, obtain uniform
Slurry；
(4) production of silver paste：Above-mentioned slurry is ground 7 times in three-high mill, silver paste is made by the fine setting of roller
Fineness control less than 8 μm, viscosity 20-30PaS, i.e., the fine rule silver paste of obtained vehicle glass.
Embodiment 5
(1) stock up 1000g, is stocked up according to following components and quality：
The particle diameter of spherical silver powder used is 2.3 μm, tap density 3.2g/ml；The particle diameter of flake silver powder is 7.2 μm, is shaken
Real density is 2.5g/ml；
In glass dust used, glass dust-L is 25g, and particle diameter is 1.35 μm, and its component and percentage composition are：Bi2O365、
B2O318、ZnO 9、SiO24、Al2O32、Na2O 1、Fe2O30.5、ZrO20.5；Glass dust-H is 45g, and particle diameter is 1.50 μm, its
Component and percentage composition are：Bi2O360、B2O319、ZnO 8、SiO25、Sb2O34、Al2O31、Na2O 1、Cr2O30.5、
Fe2O30.4、ZrO20.4、NiO 0.3、Ag2O 0.5；
Organic additive used is 15g dibutyl phthalates, 7.5g polyacrylate and 7.5g silane couplers
KH560。
(2) preparation of carrier：Weigh 40g ethyl celluloses, 40g wood rosins, 110g Tripropylene glycol monomethyl Ethers and 110g bis-
Butyl cellosolve, then it is heated and is warming up to 80 DEG C and constant temperature, after ethyl cellulose and wood rosin are completely dissolved,
Filtering and impurity removing on the screen cloth of 400-500 mesh, that is, obtain carrier；
(3) preparation of silver paste：Weigh the spherical silver powder of 500g, 100g flake silver powders, 70g glass dust, 30g organic additives
Afterwards, it is sufficiently mixed with organic carrier in batch mixer, reuses high speed dispersion agent and disperse at a high speed, that is, obtain uniform
Slurry；
(4) production of silver paste：Above-mentioned slurry is ground 7 times in three-high mill, silver paste is made by the fine setting of roller
Fineness control less than 8 μm, viscosity 20-30PaS, i.e., the fine rule silver paste of obtained vehicle glass.
Embodiment 6
A kind of vehicle glass fine rule silver paste, the formula and synthesis technique of raw material are same as Example 5, and difference exists
In for the particle diameter of the spherical silver powder used for 1.0 μm, the particle diameter of flake silver powder is 5 μm, by strictly controlling the particle diameter of silver powder, is led to
The selection collocation of ultra-fine ball powder and piece powder is crossed, substantially increases the adhesive force certainly between silver paste and glass, and be prepared
Silver paste also has good electric conductivity and compactness, can be with a width of 0.3mm of prepares line or so fine rule product.
Claims (7)
1. a kind of vehicle glass fine rule silver paste, it is characterised in that raw material uses following components and weight percent content：Metal
Silver powder 60-80%；Glass dust 3-7%；Macromolecule resin 1-8%；Organic additive 1-3%；Organic solvent 10-25%；
Described glass dust is the mixture that glass dust-L and glass dust-H is formed,
Glass dust-the L is lead-free glass powder, and particle diameter is 0.5-2 μm, and sintering temperature is 550-650 DEG C, including following components and
Weight percentage：Bi2O3 55-75、B2O3 10-30、ZnO 5-15、SiO2 3-10、Al2O3 0-3、Na2O 0-3、Fe2O3
0-1、ZrO20-1,
Glass dust-the H is lead-free glass powder, and particle diameter is 0.5-2 μm, and sintering temperature is 650-750 DEG C, including following components and
Weight percentage：Bi2O3 50-70、B2O3 10-30、ZnO 5-15、SiO2 3-10、Sb2O3 3-10、Al2O3 0-3、Na2O
0-3、Cr2O3 0-2、Fe2O3 0-1、ZrO2 0-1、NiO 0-1、Ag2O 0-1。
2. a kind of vehicle glass fine rule silver paste according to claim 1, it is characterised in that described silver powder is ball
The compound that shape silver powder and flake silver powder are formed, the particle diameter of spherical silver powder is 0.3-3.0 μm, tap density 2.0-4.0g/ml；
The particle diameter of flake silver powder is 1-7 μm, tap density 1.0-3.0g/ml.
3. a kind of vehicle glass fine rule silver paste according to claim 1, it is characterised in that described macromolecule resin is
One or more in ethyl cellulose, NC Nitroncellulose, ethylhydroxyethylcellulose, wood rosin.
4. a kind of vehicle glass fine rule silver paste according to claim 1, it is characterised in that described macromolecule resin is
Ethyl cellulose.
A kind of 5. vehicle glass fine rule silver paste according to claim 1, it is characterised in that described organic additive bag
Plasticizer, levelling agent, coupling agent are included,
The plasticizer is in dibutyl phthalate, ATBC, dioctyl phthalate, trioctyl lemon acid
One or more；
The levelling agent is organic siliconresin, rilanit special, polyvinyl butyral resin, one kind in polyacrylate or several
Kind；
The coupling agent is the one or more in Silane coupling agent KH550, KH560, KH570.
6. a kind of vehicle glass fine rule silver paste according to claim 1, it is characterised in that described organic solvent is terpene
Product alcohol, turpentine oil, butyl, dibutyl ethylene glycol ether, butyl carbitol acetate, dipropylene glycol monomethyl ether, 3 third
One or more of mixtures in glycol monomethyl ether.
7. the preparation method of the vehicle glass fine rule silver paste as any one of claim 1-6, it is characterised in that use
Following steps：
(1) stocked up according to following components and weight percentage：
(2) preparation of carrier：Macromolecule resin and organic solvent are weighed, is then heated and is warming up to 80 DEG C and constant temperature, treat height
After molecule resin is completely dissolved, the filtering and impurity removing on the screen cloth of 400-500 mesh, that is, carrier is obtained；
(3) preparation of silver paste：After weighing silver powder, glass dust, organic additive, fully mixed in batch mixer with carrier
Close, reuse high speed dispersion agent and disperse at a high speed, that is, obtain uniform slurry；
(4) production of silver paste：Above-mentioned slurry is ground in three-high mill, the fineness control of silver paste is made by the fine setting of roller
System is below 8 μm, viscosity 20-30PaS, that is, vehicle glass fine rule silver paste is made.
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| CN107393629B (en) * | 2017-09-13 | 2020-01-17 | 福建阿石创新材料股份有限公司 | Conductive silver paste and preparation method and application thereof |
| CN109785992A (en) * | 2017-11-10 | 2019-05-21 | 上海宝银电子材料有限公司 | A kind of vehicle glass high temperature-proof diffusion silver paste and preparation method thereof |
| CN110078377A (en) * | 2018-01-26 | 2019-08-02 | 上海宝银电子材料有限公司 | A kind of car windshield silver paste low-temperature lead-free glass powder and preparation method thereof |
| CN111627590A (en) * | 2020-02-29 | 2020-09-04 | 上海宝银电子材料有限公司 | Conductive silver paste for chip inductor and preparation method thereof |
| CN111370158A (en) * | 2020-02-29 | 2020-07-03 | 上海宝银电子材料有限公司 | Fine wire silver paste for passenger car glass and preparation method thereof |
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