CN109785991A - A kind of anti-oxidant silver paste of car windshield and preparation method thereof - Google Patents
A kind of anti-oxidant silver paste of car windshield and preparation method thereof Download PDFInfo
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Abstract
The present invention relates to anti-oxidant silver paste of a kind of car windshield and preparation method thereof, raw material uses following components and weight percent content: silver powder 60-80%；Glass powder 3-6%；Macromolecule resin 2-8%；Organic additive 0.5-1.5%；Inorganic additive 0.5-4.5%；Organic solvent 10-30%, by stock, the preparation of carrier, the preparation of silver paste, the production of silver paste and etc. the anti-oxidant silver paste of car windshield is prepared.Compared with prior art, the product that the present invention is prepared not only be able to satisfy the electric conductivity of existing car windshield, adhesive force, tin face color, with the technical requirements such as the matching of black glaze, while also having the advantages that antioxygenic property.
Description
Technical field
The present invention relates to car windshield silver pastes and preparation method thereof, use more particularly, to a kind of car windshield
Anti-oxidant silver paste and preparation method thereof.
Background technique
With the continuous development of China's economy, auto industry also obtains quick vigorous growth, and bus and coach yield also mentions year by year
It rises.Meanwhile car windshield silver paste and the demand of black glaze are also continuously increased, and quality requirements are also higher and higher.
In order to quickly eliminate mist frost, car windshield side generally can all be furnished with demisting frost heater wire.Heater wire is general
Silver paste is imprinted on to the surface of car glass and black glaze by screen printing technique, through 600 DEG C of heating 30-45min of bending furnace high temperature,
Silver paste is set to be attached to the surface formation silver layer of car windshield and black glaze.It is welded on the silver face of car windshield two sides after sintering
Power circuit is connect, is powered after pressure, entire heater wire starts to generate heat, to achieve the effect that demisting.Since car glass is being installed
Preceding storage environment, or may be exposed to car after installing in damp and hot equal environment, therefore to car glass silver paste
Inoxidizability, adhesive force, wearability etc. propose very high technical requirements.Meanwhile black glaze is actually printed in view of silver paste
Above, therefore silver paste and the matching of black glaze also proposed very high technical requirements.
Currently, most of the silver paste of domestic car glass station-service is domestic silver paste, small part is using Du Pont, Fu Lu and village letter
Ten thousand rich equal external products, be primarily present following problems: the antioxygenic property of silver paste is bad, and silver wire is easy discoloration, before leading to car
Keeping off the glass product resting period cannot be too long, influences the quality of car windshield product.
Chinese patent 201410806068.9 discloses acidproof anti-oxidant silver paste and its preparation side of a kind of vehicle glass
Method, raw material use following components and weight percent content: silver powder 55-75%；Glass powder 5-15%；Macromolecule resin 2-
10%；Organic additive 1-3%；Organic solvent 10-30% passes through stock, the preparation of carrier, the preparation of silver paste, the life of silver paste
Produce and etc. the acidproof anti-oxidant silver paste of vehicle glass is prepared.Difference between the application and the patent essentially consists in this
Patent is mainly anti-to improve jointly in terms of the selection of silver powder type collocation, the selection of glass powder type and the raising of its content two
Oxidation susceptibility, and the application is mainly from selection collocation, the selection of inorganic additive of silver powder type, Lai Youhua antioxygenic property.
Chinese patent 201110421404.4 discloses a kind of car windshield conductive silver paste and preparation method thereof, should
Conductive silver paste includes following components and weight percentage: silver powder 60-80；Glass powder 2-9；Organic carrier 10-30；Solvent
5-10；Additive 0.2-0.5.Macromolecule resin and organic solvent are weighed, is then heated and is warming up to 80 DEG C and constant temperature, until
Resin constant temperature is dissolved to 15000-35000cps, then by resin on the screen cloth of 300-400 mesh filtering and impurity removing, obtained airborne
Body；Silver powder, glass powder are weighed, it is sufficiently mixed in batch mixer with organic carrier, solvent and additive, is being used
High speed disperser carries out high speed dispersion, obtains uniform slurry；Above-mentioned slurry is ground in the grinding of three rollers, front is made
The dedicated conductive silver paste of glass.Difference between the application and the patent essentially consists in the selection of inorganic additive, silver powder type
Selection collocation leads to the patent some shortcomings in terms of antioxygenic property.
Summary of the invention
It is an object of the present invention to overcome the above-mentioned drawbacks of the prior art and provide one kind to be not only able to satisfy visitor
The electric conductivity of front windshield, adhesive force, tin face color, with the technical requirements such as the matching of black glaze, while also having anti-
Anti-oxidant silver paste of car windshield of oxidation susceptibility and preparation method thereof.
The purpose of the present invention can be achieved through the following technical solutions:
A kind of anti-oxidant silver paste of car windshield, raw material use following components and weight percent content:
Silver powder 60-80%；Glass powder 3-6%；Macromolecule resin 2-8%；Organic additive 0.5-1.5%；It is inorganic
Additive 0.5-4.5%；Organic solvent 10-30%.
The silver powder is the compound that spherical silver powder and flake silver powder are constituted,
Preferably, the partial size of spherical silver powder is 0.5-6.0 μm, tap density 2.0-4.0g/ml；The partial size of flake silver powder
It is 1-12 μm, tap density 1.0-3.0g/ml.
The glass powder is lead-free glass powder (glass powder-L), and partial size is 0.5-3 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；
The macromolecule resin is ethyl cellulose, NC Nitroncellulose, ethylhydroxyethylcellulose, one in wood rosin
Kind is several.
Preferably, macromolecule resin is ethyl cellulose.It is preferred that softening point is 135~155 DEG C, fusing point is 165~185 DEG C
Ethyl cellulose.
The organic additive includes one or more of plasticizer, levelling agent, coupling agent,
Preferably, plasticizer is dibutyl phthalate, tributyl citrate, dioctyl phthalate, citric acid
One or more of three monooctyl esters,
Preferably, levelling agent is organic siliconresin, rilanit special, polyvinyl butyral, one in polyacrylate
Kind is several,
Preferably, coupling agent is one or more of Silane coupling agent KH550, KH560, KH570.
The inorganic additive is metal oxide, including titanium dioxide, molybdenum trioxide, cobaltosic oxide, five oxidations
One or more of two vanadium.
Preferably, inorganic additive is molybdenum trioxide, and when solid-state, anhydrous molybdenum trioxide is rhombic system, contains deformation eight
Face body MoO6The layer structure of composition.Octahedra chaining, between have an oxygen atom crosslinking, a Mo-O (non-crosslinked oxygen) in octahedron
Bond distance is shorter, in substrate surface without preferred orientation；Crystal particle scale range is between 0.5~1 μm.
The organic solvent is terpineol, turpentine oil, butyl, dibutyl ethylene glycol ether, butyl carbitol
The mixture of one or more of acetate, dipropylene glycol monomethyl ether or Tripropylene glycol monomethyl Ether, preferably terpineol and diethyl
The glycol butyl ether mixed solvent that 1:4 is mixed by volume.
For from sorting, the present invention selects metal oxide to improve as additive to silver paste, especially has
The molybdenum trioxide of special construction and characteristic, being used in mixed way to use with silver powder has synergistic effect, and in the work of macromolecule resin
Under, while increasing its antioxygenic property, the ethyl cellulose that thermal stability, thermoplasticity, the especially present invention select is improved
Under the action of above-mentioned mixed solvent, degree of etherification falling is improved, and softening point and hygroscopicity reduce, and 13.7~54.9Mpa of intensity, body are stretched in drawing
Product resistivity 10*e12~10*e14ω cm, be not only able to satisfy the electric conductivity of car windshield, adhesive force, tin face color, with
The technical requirements such as the matching of black glaze, and antioxygenic property has obtained larger raising.
The preparation method of the anti-oxidant silver paste of car windshield uses following steps:
(1) it stocks up according to following components and weight percent content:
Silver powder 60-80%；Glass powder 3-6%；Macromolecule resin 2-8%；Organic additive 0.5-1.5%；It is inorganic
Additive 0.5-4.5%；Organic solvent 10-30%；
(2) preparation of carrier: weighing macromolecule resin and organic solvent, is then heated and is warming up to 80 DEG C and constant temperature,
After macromolecule resin is completely dissolved, on the screen cloth of 300-400 mesh filtering and impurity removing to get arrive carrier；
(3) preparation of silver paste: after weighing silver powder, glass powder, organic additive, inorganic additive, with carrier mixed
It is sufficiently mixed in material machine, reuses high speed dispersion agent and carry out high speed dispersion to get uniform slurry is arrived；
(4) production of silver paste: above-mentioned slurry is ground in three-high mill, and the fineness of silver paste is made by idler wheel fine tuning
Control at 15 μm hereinafter, viscosity be 20-30PaS, that is, the anti-oxidant silver paste of car windshield is prepared.
Compared with prior art, the present invention is arranged in pairs or groups by the selection of inorganic additive, the selection of silver powder type, common to improve
The antioxygenic property of silver paste, the silver paste being prepared not only are able to satisfy the electric conductivity of car windshield, adhesive force, tin face
The technical requirements such as the matching of color and black glaze, while also having the advantages that antioxygenic property.
After high temperature sintering, cracking volatilization can occur for the organic substance in silver paste, and silver powder and glass powder are attached to glass
Glass substrate surface plays heating conduction.Wherein, glass powder plays viscous mainly between glass baseplate and silver powder
The effect of agent is tied, the performance of glass powder determines the acid resistance of silver paste, adhesive force；Silver powder is in glass powder, and phase
There are gap of different sizes between mutually, the selection collocation of silver powder determines the surface topography of silver paste, affects silver layer surface
Oxidation resistance；The relative scale of glass powder and silver powder also has a certain impact to the adhesive force of silver paste, inoxidizability.Metal
Oxide, mainly includes titanium dioxide, molybdenum trioxide, cobaltosic oxide and vanadic anhydride, can significant less silver layer surface from
The content of son, plays the role of inoxidizability apparent.
Specific embodiment
The present invention is described in detail combined with specific embodiments below.
Embodiment 1
(1) stock up 100g, stocks up according to following components and quality:
The partial size of spherical silver powder used is 2.3 μm, tap density 3.2g/ml；The partial size of flake silver powder is 6 μm, jolt ramming
Density is 2.4g/ml；
The component and percentage composition of glass powder-L used are as follows: Bi2O3 65、B2O3 18、ZnO 9、SiO2 4、Al2O3 2、
Na2O 1、Fe2O3 0.5、ZrO20.5；
Organic additive used is 0.25g dibutyl phthalate and 0.25g Silane coupling agent KH550.
Titanium dioxide used is to analyze pure grade.Organic solvent be terpineol and butyl by volume 1:4 into
Row mixing.
(2) preparation of carrier: weighing ethyl cellulose and organic solvent, is then heated and is warming up to 80 DEG C and constant temperature,
After ethyl cellulose is completely dissolved, on the screen cloth of 300-400 mesh filtering and impurity removing to get arrive carrier；
(3) preparation of silver paste: after weighing spherical silver powder, flake silver powder, glass powder-L, organic additive, titanium dioxide, with
Carrier, solvent are sufficiently mixed in batch mixer, are reused high speed dispersion agent and are carried out high speed dispersion to get uniform slurry is arrived
Body；
(4) production of silver paste: above-mentioned slurry is carried out to grinding 5 times in three-high mill, silver paste is made by the fine tuning of idler wheel
Fineness control at 15 μm hereinafter, viscosity be 20-30PaS, obtain the anti-oxidant silver paste of car windshield.
Embodiment 2
(1) stock up 100g, stocks up according to following components and quality:
The partial size of spherical silver powder used is 2.8 μm, tap density 3.8g/ml；The partial size of flake silver powder is 6 μm, jolt ramming
Density is 2.4g/ml；
The component and percentage composition of glass powder-L used are as follows: Bi2O3 70、B2O3 16、ZnO 8、SiO2 3.5、Al2O3
1.5、Na2O 1.0、Fe2O3 0、ZrO20；
Organic additive used is 0.5g dioctyl phthalate and 0.5g organic siliconresin.
Molybdenum trioxide used is to analyze pure grade.
(2) preparation of carrier: weighing NC Nitroncellulose and terpineol, is then heated and is warming up to 80 DEG C and constant temperature, to
After NC Nitroncellulose is completely dissolved, on the screen cloth of 300-400 mesh filtering and impurity removing to get arrive carrier；
(3) preparation of silver paste: after weighing spherical silver powder, flake silver powder, glass powder-L, organic additive, molybdenum trioxide, with
Carrier, solvent are sufficiently mixed in batch mixer, are reused high speed dispersion agent and are carried out high speed dispersion to get uniform slurry is arrived
Body；
(4) production of silver paste: above-mentioned slurry is carried out to grinding 7 times in three-high mill, silver paste is made by the fine tuning of idler wheel
Fineness control at 15 μm hereinafter, viscosity be 20-30PaS, obtain the anti-oxidant silver paste of car windshield.
Embodiment 3
(1) stock up 100g, stocks up according to following components and quality:
The partial size of spherical silver powder used is 1.8 μm, tap density 2.6g/ml；The partial size of flake silver powder is 7.5 μm, vibration
Real density is 1.9g/ml；
The component and percentage composition of glass powder-L used are as follows: Bi2O3 70、B2O3 16、ZnO 8、SiO2 3.5、Al2O3
1.5、Na2O 1.0、Fe2O3 0、ZrO20；
Organic additive used is 0.6g tributyl citrate, 0.2g rilanit special and 0.20g silane coupling agent
KH570。
Cobaltosic oxide used, vanadic anhydride are the pure grade of analysis.
(2) preparation of carrier: ethylhydroxyethylcellulose, terpineol and butyl carbitol acetate are weighed, then by it
It is heated to 80 DEG C and constant temperature, after ethylhydroxyethylcellulose is completely dissolved, crosses and filters out on the screen cloth of 300-400 mesh
It is miscellaneous to get arrive carrier；
(3) spherical silver powder, flake silver powder, glass powder-L, organic additive, cobaltosic oxide, five preparation of silver paste: are weighed
It after V 2 O, is sufficiently mixed in batch mixer with carrier, solvent, reuses high speed dispersion agent and carry out high speed dispersion, i.e.,
Obtain uniform slurry；
(4) production of silver paste: above-mentioned slurry is carried out to grinding 6 times in three-high mill, silver paste is made by the fine tuning of idler wheel
Fineness control at 15 μm hereinafter, viscosity be 20-30PaS, obtain the anti-oxidant silver paste of car windshield.
Embodiment 4
(1) stock up 100g, stocks up according to following components and quality:
The partial size of spherical silver powder used is 4.5 μm, tap density 3.5g/ml；The partial size of flake silver powder is 8.0 μm, vibration
Real density is 2.2g/ml；
The component and percentage composition of glass powder-L used is Bi2O3 65、B2O3 18、ZnO 9、SiO2 4、Al2O3 2、Na2O
1、Fe2O3 0.5、ZrO20.5；
Organic additive used is 1g trioctyl lemon acid, 0.25g organic siliconresin and 0.25g silane coupling agent KH560.
Vanadic anhydride used is the pure grade of analysis.
(2) preparation of carrier: weighing ethyl cellulose, NC Nitroncellulose, Tripropylene glycol monomethyl Ether and terpineol, then will
It is heated to 80 DEG C and constant temperature, after ethyl cellulose and NC Nitroncellulose are completely dissolved, on the screen cloth of 300-400 mesh
Filtering and impurity removing to get arrive carrier；
(3) preparation of silver paste: after weighing spherical silver powder, flake silver powder, glass powder-L, organic additive, with carrier, five oxygen
Change two vanadium, solvent is sufficiently mixed in batch mixer, reuse high speed dispersion agent and carry out high speed dispersion to get to uniform slurry
Body；
(4) production of silver paste: above-mentioned slurry is carried out to grinding 7 times in three-high mill, silver paste is made by the fine tuning of idler wheel
Fineness control at 15 μm hereinafter, viscosity be 20-30PaS, obtain the anti-oxidant silver paste of car windshield.
The embodiment 1-4 performance that acidproof anti-oxidant silver paste is prepared is detected, the results are shown in Table 1.
Table 1
From above-mentioned test result can be seen that silver paste that this method is prepared electric conductivity, adhesive force, tin face color,
With it is very outstanding in the matching of black glaze, and antioxygenic property is increased substantially.
Claims (8)
1. a kind of anti-oxidant silver paste of car windshield, which is characterized in that raw material includes following components and weight percent
Content: silver powder 60-80%；Glass powder 3-6%；Macromolecule resin 2-8%；Organic additive 0.5-1.5%；Inorganic addition
Agent 0.5-4.5%；Organic solvent 10-30%.
2. a kind of anti-oxidant silver paste of car windshield according to claim 1, which is characterized in that described is inorganic
Additive is metal oxide, and the metal oxide is titanium dioxide, in molybdenum trioxide, cobaltosic oxide, vanadic anhydride
One or more, preferred molybdenum trioxide.
3. a kind of anti-oxidant silver paste of car windshield according to claim 1, which is characterized in that the glass
Powder is L-type lead-free glass powder, and partial size is 0.5-3 μm, and sintering temperature is 550-650 DEG C, including following components and weight percent contain
Amount: Bi2O3 55-75、B2O3 10-30、ZnO 5-15、SiO2 3-10、Al2O3 0-3、Na2O 0-3、Fe2O3 0-1、ZrO2 0-
1。
4. a kind of anti-oxidant silver paste of car windshield according to claim 1, which is characterized in that the high score
Subtree rouge is one or more of ethyl cellulose, NC Nitroncellulose, ethylhydroxyethylcellulose, wood rosin, is preferably softened
Point is 135~155 DEG C, the ethyl cellulose that fusing point is 165~185 DEG C.
5. a kind of anti-oxidant silver paste of car windshield according to claim 1, which is characterized in that described is organic
Additive includes one or more of plasticizer, levelling agent, coupling agent；
The plasticizer is dibutyl phthalate, in tributyl citrate, dioctyl phthalate, trioctyl lemon acid
One or more；
The levelling agent is one of organic siliconresin, rilanit special, polyvinyl butyral, polyacrylate or several
Kind；
The coupling agent is one or more of Silane coupling agent KH550, KH560, KH570.
6. a kind of anti-oxidant silver paste of car windshield according to claim 1, which is characterized in that the metal
Silver powder is the compound that spherical silver powder and flake silver powder are constituted, and the partial size of spherical silver powder is 0.5-6.0 μm, tap density 2.0-
4.0g/ml；The partial size of flake silver powder is 1-12 μm, tap density 1.0-3.0g/ml.
7. a kind of anti-oxidant silver paste of car windshield according to claim 1, which is characterized in that described is organic
Solvent is terpineol, turpentine oil, butyl, dibutyl ethylene glycol ether, butyl carbitol acetate, dipropylene glycol list first
The mixture of one or more of ether or Tripropylene glycol monomethyl Ether, preferably terpineol and butyl 1:4 by volume
Mixed mixture.
8. the preparation method of the anti-oxidant silver paste such as car windshield of any of claims 1-7, feature
It is, using following steps:
(1) it stocks up according to following components and weight percent content:
Silver powder 60-80%；Glass powder 3-6%；Macromolecule resin 2-8%；Organic additive 0.5-1.5%；Inorganic addition
Agent 0.5-4.5%；Organic solvent 10-30%；
(2) preparation of carrier: weighing macromolecule resin and organic solvent, is then heated and is warming up to 80 DEG C and constant temperature, to height
After molecule resin is completely dissolved, on the screen cloth of 300-400 mesh filtering and impurity removing to get arrive carrier；
(3) preparation of silver paste: after weighing silver powder, glass powder, organic additive, inorganic additive, with carrier in batch mixer
In be sufficiently mixed, reuse high speed dispersion agent and carry out high speed dispersion to get to uniform slurry；
(4) production of silver paste: above-mentioned slurry is ground in three-high mill, controls the fineness of silver paste by idler wheel fine tuning
At 15 μm hereinafter, viscosity is 20-30PaS, that is, the anti-oxidant silver paste of car windshield is prepared.
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| CN201711104822.4A CN109785991B (en) | 2017-11-10 | 2017-11-10 | Antioxidant silver paste for front windshield of passenger car and preparation method thereof |
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| CN109785991B CN109785991B (en) | 2020-07-31 |
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| 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 |
| CN113539545A (en) * | 2020-04-21 | 2021-10-22 | 上海宝银电子材料有限公司 | Gray conductive silver paste for automobile glass and preparation method thereof |
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| CN114171237A (en) * | 2021-12-23 | 2022-03-11 | 上海宝银电子材料有限公司 | Conductive paste for vacuum glass and preparation method thereof |
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| 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 |
| CN111477378B (en) * | 2020-04-13 | 2021-08-13 | 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 |
| CN113539545A (en) * | 2020-04-21 | 2021-10-22 | 上海宝银电子材料有限公司 | Gray conductive silver paste for automobile glass and preparation method thereof |
| CN113539546A (en) * | 2020-04-21 | 2021-10-22 | 上海宝银电子材料有限公司 | Conductive silver paste for electronic cigarette lighter and preparation method thereof |
| WO2021213189A1 (en) * | 2020-04-21 | 2021-10-28 | 上海宝银电子材料有限公司 | Gray conductive silver paste for automotive glass and preparation method therefor |
| CN114171237A (en) * | 2021-12-23 | 2022-03-11 | 上海宝银电子材料有限公司 | Conductive paste for vacuum glass 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 |
| CN116564576A (en) * | 2023-05-24 | 2023-08-08 | 南通艾盛新能源科技有限公司 | Conductive paste added with inorganic material and preparation method thereof |
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| CN109785991B (en) | 2020-07-31 |
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Denomination of invention: An antioxidant silver paste for front windshield glass of passenger cars and its preparation method Effective date of registration: 20230321 Granted publication date: 20200731 Pledgee: Industrial and Commercial Bank of China Limited Shanghai Jiading Branch Pledgor: Shanghai Baoyin Electronic Materials Ltd. Registration number: Y2023980035524 |