CN109785992A - A kind of vehicle glass high temperature-proof diffusion silver paste and preparation method thereof - Google Patents

A kind of vehicle glass high temperature-proof diffusion silver paste and preparation method thereof Download PDF

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CN109785992A
CN109785992A CN201711104343.2A CN201711104343A CN109785992A CN 109785992 A CN109785992 A CN 109785992A CN 201711104343 A CN201711104343 A CN 201711104343A CN 109785992 A CN109785992 A CN 109785992A
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silver paste
powder
silver
glass
glass powder
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朱庆明
江海涵
何利娜
王德龙
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BAOYIN ELECTRONIC MATERIAL Co Ltd SHANGHAI
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BAOYIN ELECTRONIC MATERIAL Co Ltd SHANGHAI
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Abstract

The present invention relates to a kind of vehicle glass high temperature-proof to spread silver paste and preparation method thereof, and raw material uses following components and weight percent content: silver powder 50-80%;Glass powder 3-6%;Macromolecule resin 2-8%;Inorganic additive 1-8%;Organic solvent 10-40%, by stock, the preparation of carrier, the preparation of silver paste, the production of silver paste and etc. be prepared vehicle glass high temperature-proof spread silver paste.Compared with prior art, the product that the present invention is prepared not only is able to satisfy all technical requirement of existing tempered glass of automobile (650-720 DEG C/3min), the demand of the curved glass of depth of higher sintering technological temperature (720-730 DEG C) can also be met simultaneously, there is a phenomenon where silver wires to spread.

Description

A kind of vehicle glass high temperature-proof diffusion silver paste and preparation method thereof
Technical field
The present invention relates to a kind of vehicle glass silver pastes and preparation method thereof, more particularly, to a kind of vehicle glass high temperature-proof Spread silver paste and preparation method thereof.
Background technique
With the continuous development of China's economy, auto industry also obtains quick vigorous growth, and auto output also mentions year by year It rises.Meanwhile vehicle glass 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, shelves glass generally can all be furnished with demisting frost heater wire after automobile.Heater wire generally passes through Silver paste is imprinted on the surface of vehicle glass and black glaze by screen printing technique, is handled 3-5min through annealing furnace tempering, is adhered to silver paste Silver layer is formed in the surface of vehicle glass and black glaze.The resistance of heater wire is generally in 0.5-1.2 Ω after sintering, in vehicle glass two Source of welding current route on the silver face of side, after leading to the voltage of upper 12-13V, entire heater wire starts to generate heat, to reach the effect of demisting Fruit.Since heater wire is likely to be exposed in damp and hot equal environment with automobile, thus the acid resistance to vehicle glass silver paste, wearability, Adhesive force, inoxidizability etc. propose very high technical requirements.Meanwhile being actually printed in above black glaze in view of silver paste, therefore Silver paste and the matching of black glaze also proposed very high technical requirements.
Currently, most of silver paste of domestic automobile 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: conductive silver paste is applied to deeply curved (720-730 DEG C) tempered glass of automobile and produces When product, silver wire is easy to happen diffusion jaundice, influences the product quality of vehicle glass, causes the complaint and feedback of client.
A kind of acidproof anti-oxidant silver paste and preparation method thereof of the vehicle glass of Chinese patent 20140806068.9, China A kind of filament silver paste and preparation method thereof of the vehicle glass of patent 20140804458.2, Chinese patent 200610027668.0 A kind of heat resistant antisticking no-lead black glaze for automobile glass and preparation method thereof, disclosed automobile fiberglass technological temperature are 650- 720 DEG C, time 3min.
Summary of the invention
The object of the invention is to mention to solve conductive silver paste in the diffusion yellowing phenomenon of deep curved tempered glass of automobile For a kind of higher conductive silver paste of tempered glass of automobile sintering temperature, electric conductivity, adhesive force, tin face color, with black glaze It is all met the requirements with technical indicators such as property.
The purpose of the present invention can be achieved through the following technical solutions:
A kind of vehicle glass high temperature-proof diffusion silver paste, raw material use following components and weight percent content: metallic silver Powder 50-80%;Glass powder 3-6%;Macromolecule resin 2-8%;Inorganic additive 1-8%;Organic solvent 10-40%.
The 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.
The glass powder is glass powder-L, glass powder-M and glass powder-H is what 1:1~2:1~2 was constituted in mass ratio Mixture,
Glass powder-the L is lead-free glass powder, and partial size is 0.5-3 μm, and sintering temperature is 550-650 DEG C, including with the following group Point and weight percentage: Bi2O3 55-75、B2O3 10-30、ZnO 5-15、SiO2 3-10、Al2O3 0-3、Na2O 0-3、 Fe2O3 0-1、ZrO2 0-1。
Glass powder-the M is lead-free glass powder, and partial size is 0.5-3 μm, and sintering temperature is 650-750 DEG C, including with the following group Point and weight percentage: Bi2O3 55-75、SiO2 15-35、B2O3 5-15、Sb2O3 1-5、Na2O 0-2、Al2O3 0-1、 ZnO 0-1、CuO 0-1、CaO 0-1、Fe2O3 0-1、ZrO2 0-1。
Glass powder-the H is lead-free glass powder, and partial size is 0.5-3 μm, and sintering temperature is 650-750 DEG C, including with the following group Point 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。
The macromolecule resin is ethyl cellulose, NC Nitroncellulose, ethylhydroxyethylcellulose, one in wood rosin Kind is several, and preferably softening point is 135~155 DEG C, the ethyl cellulose that fusing point is 165~185 DEG C.
The inorganic additive is metal oxide,
The metal oxide is nickel oxide, titanium dioxide, manganese dioxide, molybdenum trioxide, di-iron trioxide, four oxidations three One or more of cobalt, vanadic anhydride, preferably apparent density 0.5-1.5g/cm3, tap density 2.0-3.0g/cm3Four Co 3 O, the cobaltosic oxide have spinel structure.
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, Tripropylene glycol monomethyl Ether.
The preparation method that vehicle glass high temperature-proof spreads silver paste uses following steps:
(1) it stocks up according to following components and weight percentage:
(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) it the preparation of silver paste: after weighing silver powder, glass powder, inorganic additive, is filled in batch mixer with carrier Divide mixing, 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, makes the thin of silver paste by the fine tuning of idler wheel Degree control at 15 μm hereinafter, viscosity be 20-30PaS, obtain vehicle glass high temperature-proof diffusion silver paste.
Compared with prior art, the invention has the following advantages that
1. the selection by inorganic additive is arranged in pairs or groups, to solve the phenomenon that High temperature diffusion of silver paste is turned to be yellow;Pass through silver powder Selection collocation, to solve electric conductivity, the compactness of silver paste;Arranged in pairs or groups by the selection of glass powder, come solve silver paste and glass it Between adhesive force and glass tin face shade;By the selection of organic additive, to solve the craftsmanship of silver paste printing Energy.
It mainly include nickel oxide, titanium dioxide, manganese dioxide, molybdenum trioxide, three 2. inorganic additive is metal oxide Aoxidize one or more of two iron, cobaltosic oxide, vanadic anhydride, preferably cobaltosic oxide.The weight of metal oxide Percentage composition is 1-8%, is most preferably no more than 6%.After adding metal oxide, silver paste can promote during high temperature sintering The generation of silver ion, while with glass tin face redox reaction can occur for a large amount of silver ion, and glass tin face color is caused to add Deep is in dark-brown, and more normal tin face color is significantly deepened.Especially preferred apparent density 0.5-1.5g/cm3, tap density 2.0-3.0g/cm3Cobaltosic oxide, the cobaltosic oxide have spinel structure, combined silver of the present invention can be improved The dispersion of powder and hybrid glass powder makes the combination of glass powder and silver powder can reach the monolayer distribution of ionic level, to promote More fully redox reaction occurs for silver ion and glass tin face, while improving electric conductivity, has widened silver paste High temperature resistance, to solve the phenomenon that High temperature diffusion jaundice of silver paste.
3. having carried out collocation present invention employs three component lead-free glass powders to use, the sheet resistance scope of application of silver paste has been widened And sintering range, while improving the adhesive force of silver paste film layer and silicon substrate;Glass powder size controlling is in highly stable range It is interior, it both ensure that the stability of slurry viscosity system in this way, while ensure that stablizing for performance plays glass powder in the slurry.
4. glass powder of the present invention is all made of the raw material preparation of leadless environment-friendly type, belongs to environmentally friendly material, human body is pacified Atoxic;
5. three component glass powders of the invention can mix according to a certain percentage, there is different proportions different sheet resistances to be applicable in Characteristic, therefore, can arrange in pairs or groups out the very wide sheet resistance scope of application;Simultaneously three groups of glass powders due to softening point height difference and The sintering window for having widened silver paste, improves the high temperature resistance of silver paste;
6. since three kinds of glass powders are more than the metallization processes that can promote silver powder after respective softening temperature, pole Big improves the adhesive force of silver paste and substrate.
Specific embodiment
The present invention is described in detail combined with specific embodiments below.
Embodiment 1
(1) stock up 1000g, stocks up according to following components and quality:
The partial size of spherical silver powder used is 1.0 μm, tap density 2.2g/ml;The partial size of flake silver powder is 6.2 μm, vibration Real density is 2.5g/ml;
In glass powder used, glass powder-L is 10g, component and percentage composition are as follows: Bi2O3 65、B2O318、ZnO 9、 SiO2 4、Al2O3 2、Na2O 1、Fe2O3 0.5、ZrO20.5;Glass powder-M is 15g, component and percentage composition are as follows: Bi2O3 61、SiO2 30、B2O3 5、Sb2O3 1.5、Na2O 1.0、Al2O30.5、ZnO 0.45、CuO 0.30、CaO 0.25、Fe2O3 0、ZrO20;Glass powder-H is 15g, component and percentage composition are as follows: Bi2O3 60、B2O3 19、ZnO 8、SiO2 5、Sb2O3 4、 Al2O3 1、Na2O 1、Cr2O3 0.5、Fe2O3 0.4、ZrO2 0.4、NiO 0.3、Ag2O 0.5;
Cobaltosic oxide used, di-iron trioxide are to analyze pure grade.
(2) preparation of carrier: weighing 80g ethyl cellulose and 310g terpineol, is then heated and is warming up to 80 DEG C simultaneously 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: weigh the spherical silver powder of 450g, 50g flake silver powder, 40g glass powder, 50g cobaltosic oxide, It after 20g di-iron trioxide, is sufficiently mixed in batch mixer with organic carrier, reuses high speed dispersion agent and carry out high speed point It dissipates to get uniform slurry is arrived;
(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 vehicle glass high temperature-proof diffusion silver paste.
Embodiment 2
(1) stock up 1000g, 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;
In glass powder used, glass powder-L is 10g, component and percentage composition are as follows: Bi2O3 65、B2O318、ZnO 9、 SiO2 4、Al2O3 2、Na2O 1、Fe2O3 0.5、ZrO20.5;Glass powder-M is 15g, component and percentage composition are as follows: Bi2O3 61、SiO2 30、B2O3 5、Sb2O3 1.5、Na2O 1.0、Al2O30.5、ZnO 0.45、CuO 0.30、CaO 0.25、Fe2O3 0、ZrO20;Glass powder-H is 15g, component and percentage composition are as follows: Bi2O3 60、B2O3 19、ZnO 8、SiO2 5、Sb2O3 4、 Al2O3 1、Na2O 1、Cr2O3 0.5、Fe2O3 0.4、ZrO2 0.4、NiO 0.3、Ag2O 0.5;
Cobaltosic oxide used, molybdenum trioxide, vanadic anhydride are to analyze pure grade.
(2) preparation of carrier: 70g NC Nitroncellulose and 280g butyl are weighed, is then heated and is warming up to 80 DEG C and constant temperature, after NC Nitroncellulose is completely dissolved, filtering and impurity removing is on the screen cloth of 300-400 mesh to get arriving carrier;
(3) preparation of silver paste: weigh the spherical silver powder of 500g, 50g flake silver powder, 40g glass powder, 20g cobaltosic oxide, After 20g molybdenum trioxide, 20g vanadic anhydride, it is sufficiently mixed in batch mixer with organic carrier, reuses high speed dispersion agent High speed dispersion is carried out to get uniform slurry is arrived;
(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 vehicle glass high temperature-proof diffusion silver paste.
Embodiment 3
(1) stock up 1000g, 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 8.2 μm, vibration Real density is 2.5g/ml;
In glass powder used, glass powder-L is 10g, component and percentage composition are as follows: Bi2O3 65、B2O318、ZnO 9、 SiO2 4、Al2O3 2、Na2O 1、Fe2O3 0.5、ZrO20.5;Glass powder-M is 10g, component and percentage composition are as follows: Bi2O3 61、SiO2 30、B2O3 5、Sb2O3 1.5、Na2O 1.0、Al2O30.5、ZnO 0.45、CuO 0.30、CaO 0.25、Fe2O3 0、ZrO20;Glass powder-H is 10g, component and percentage composition are as follows: Bi2O3 60、B2O3 19、ZnO 8、SiO2 5、Sb2O3 4、 Al2O3 1、Na2O 1、Cr2O3 0.5、Fe2O3 0.4、ZrO2 0.4、NiO 0.3、Ag2O 0.5;
Nickel oxide used is to analyze pure grade.
(2) 60g ethylhydroxyethylcellulose, 130g terpineol and 130g butyl carbitol acetic acid the preparation of carrier: are weighed Then ester is heated and is warming up to 80 DEG C and constant temperature, after ethylhydroxyethylcellulose is completely dissolved, in the net of 300-400 mesh On cloth filtering and impurity removing to get arrive carrier;
(3) preparation of silver paste: after weighing the spherical silver powder of 500g, 100g flake silver powder, 30g glass powder, 50g nickel oxide, with Organic carrier is sufficiently mixed in batch mixer, is reused high speed dispersion agent and is carried out high speed dispersion to get uniform slurry is arrived;
(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 vehicle glass high temperature-proof diffusion silver paste.
Embodiment 4
(1) stock up 1000g, 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;
In glass powder used, glass powder-L is 20g, component and percentage composition are as follows: Bi2O3 65、B2O318、ZnO 9、 SiO2 4、Al2O3 2、Na2O 1、Fe2O3 0.5、ZrO20.5;Glass powder-M is 20g, component and percentage composition are as follows: Bi2O3 61、SiO2 30、B2O3 5、Sb2O3 1.5、Na2O 1.0、Al2O30.5、ZnO 0.45、CuO 0.30、CaO 0.25、Fe2O3 0、ZrO20;Glass powder-H is 20g, component and percentage composition are as follows: Bi2O3 60、B2O3 19、ZnO 8、SiO2 5、Sb2O3 4、 Al2O3 1、Na2O 1、Cr2O3 0.5、Fe2O3 0.4、ZrO2 0.4、NiO 0.3、Ag2O 0.5;
Titanium dioxide used is to analyze pure grade.
(2) 30g ethyl cellulose, 30g NC Nitroncellulose, 120g Tripropylene glycol monomethyl Ether and 120 preparation of carrier: are weighed Then turpentine oil is heated and is warming up to 80 DEG C and constant temperature, after ethyl cellulose and NC Nitroncellulose are completely dissolved, in 300- On the screen cloth of 400 mesh filtering and impurity removing to get arrive carrier;
(3) preparation of silver paste: after weighing the spherical silver powder of 500g, 100g flake silver powder, 60g glass powder, 40g titanium dioxide, It is sufficiently mixed in batch mixer with organic carrier, reuses high speed dispersion agent and carry 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 vehicle glass high temperature-proof diffusion silver paste.
Embodiment 5
(1) stock up 1000g, 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 7.2 μm, vibration Real density is 2.5g/ml;
In glass powder used, glass powder-L is 10g, component and percentage composition are as follows: Bi2O3 65、B2O318、ZnO 9、 SiO2 4、Al2O3 2、Na2O 1、Fe2O3 0.5、ZrO20.5;Glass powder-M is 20g, component and percentage composition are as follows: Bi2O3 61、SiO2 30、B2O3 5、Sb2O3 1.5、Na2O 1.0、Al2O30.5、ZnO 0.45、CuO 0.30、CaO 0.25、Fe2O3 0、ZrO20;Glass powder-H is 20g, component and percentage composition are as follows: Bi2O3 60、B2O3 19、ZnO 8、SiO2 5、Sb2O3 4、 Al2O3 1、Na2O 1、Cr2O3 0.5、Fe2O3 0.4、ZrO2 0.4、NiO 0.3、Ag2O 0.5;
Manganese dioxide used is to analyze pure grade.
(2) 20g ethyl cellulose, 20g wood rosin, 90g Tripropylene glycol monomethyl Ether and 90g diethyl the preparation of carrier: are weighed Then dibutyl ether is heated and is warming up to 80 DEG C and constant temperature, after ethyl cellulose and wood rosin are completely dissolved, in 300- On the screen cloth of 400 mesh filtering and impurity removing to get arrive carrier;
(3) preparation of silver paste: after weighing the spherical silver powder of 600g, 100g flake silver powder, 50g glass powder, 30g manganese dioxide, It is sufficiently mixed in batch mixer with organic carrier, reuses high speed dispersion agent and carry 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 vehicle glass high temperature-proof diffusion silver paste.
Embodiment 6
(1) stock up 1000g, stocks up according to following components and quality:
The partial size of spherical silver powder used is 1.0 μm, tap density 2.2g/ml;The partial size of flake silver powder is 7.6 μm, vibration Real density is 2.1g/ml;
In glass powder used, glass powder-L is 10g, component and percentage composition are as follows: Bi2O3 65、B2O318、ZnO 9、 SiO2 4、Al2O3 2、Na2O 1、Fe2O3 0.5、ZrO20.5;Glass powder-M is 20g, component and percentage composition are as follows: Bi2O3 61、SiO2 30、B2O3 5、Sb2O3 1.5、Na2O 1.0、Al2O30.5、ZnO 0.45、CuO 0.30、CaO 0.25、Fe2O3 0、ZrO20;Glass powder-H is 20g, component and percentage composition are as follows: Bi2O3 60、B2O3 19、ZnO 8、SiO2 5、Sb2O3 4、 Al2O3 1、Na2O 1、Cr2O3 0.5、Fe2O3 0.4、ZrO2 0.4、NiO 0.3、Ag2O 0.5;
Molybdenum trioxide used is to analyze pure grade.
(2) preparation of carrier: 20g wood rosin and 110g Tripropylene glycol monomethyl Ether are weighed, is then heated and is warming up to 80 DEG C and constant temperature, after ethyl cellulose and wood rosin are completely dissolved, on the screen cloth of 300-400 mesh filtering and impurity removing to get to carry Body;
(3) preparation of silver paste: after weighing the spherical silver powder of 700g, 100g flake silver powder, 50g glass powder, 20g molybdenum trioxide, It is sufficiently mixed in batch mixer with organic carrier, reuses high speed dispersion agent and carry 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 vehicle glass high temperature-proof diffusion silver paste.
The embodiment 1-6 performance that silver paste is prepared is detected, the results are shown in Table 1.
Table 1
Can be seen that the silver paste automobile fiberglass technological temperature that this method is prepared from above-mentioned test result is 650- 730 DEG C, time 3-5min.It has been more than existing 650-720 DEG C, time 3min, while it seem that the performance increase is not Very much, but this point this field be very difficult to realize because sintering temperature it is every raising once, silver paste can be substantially speeded up Diffusion reaction plays the role of catalysis, and this point brings very big economic benefit, and conductive silver paste is applied to automobile depth When curved tempered glass product, since its temperature range is generally at 720-730 DEG C, common process, which is difficult to meet this temperature, to be wanted It asks, causes silver wire to be easy to happen diffusion jaundice, inventive formulation extends its temperature range and time, to substantially reduce this Technology controlling and process cost, improves product quality, to bring high economic benefit.
And from upper table data it can also be seen that silver paste electric conductivity of the present invention, adhesive force, tin face color, with black glaze It is all met the requirements with technical indicators such as property.

Claims (7)

1. a kind of vehicle glass high temperature-proof spreads silver paste, which is characterized in that raw material is contained using following components and weight percent Amount: silver powder 50-80%;Glass powder 3-6%;Macromolecule resin 2-8%;Inorganic additive 1-8%;Organic solvent 10- 40%.
2. a kind of vehicle glass according to claim 1 high temperature-proof spreads silver paste, which is characterized in that the metallic 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.
3. a kind of vehicle glass according to claim 1 high temperature-proof spreads silver paste, which is characterized in that the glass powder It is in mass ratio the mixture that 1:1~2:1~2 is constituted for glass powder-L, glass powder-M and glass powder-H;
Glass powder-the L be lead-free glass powder, partial size be 0.5-3 μm, sintering temperature be 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、ZrO2 0-1。
Glass powder-the M be lead-free glass powder, partial size be 0.5-3 μm, sintering temperature be 650-750 DEG C, including following components and Weight percentage: Bi2O3 55-75、SiO2 15-35、B2O3 5-15、Sb2O3 1-5、Na2O 0-2、Al2O3 0-1、ZnO 0-1、CuO 0-1、CaO 0-1、Fe2O3 0-1、ZrO2 0-1。
Glass powder-the H be lead-free glass powder, partial size be 0.5-3 μm, sintering temperature be 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。
4. a kind of vehicle glass according to claim 1 high temperature-proof spreads silver paste, which is characterized in that the macromolecule Resin is one or more of ethyl cellulose, NC Nitroncellulose, ethylhydroxyethylcellulose, wood rosin, preferably softening point It is 135~155 DEG C, the ethyl cellulose that fusing point is 165~185 DEG C.
5. a kind of vehicle glass according to claim 1 high temperature-proof spreads silver paste, which is characterized in that described inorganic to add Adding agent is metal oxide,
The metal oxide be nickel oxide, titanium dioxide, manganese dioxide, molybdenum trioxide, di-iron trioxide, cobaltosic oxide, One or more of vanadic anhydride, preferably cobaltosic oxide.
6. a kind of vehicle glass according to claim 1 high temperature-proof spreads silver paste, which is characterized in that described is organic molten Agent is terpineol, turpentine oil, butyl, dibutyl ethylene glycol ether, butyl carbitol acetate, dipropylene glycol list first The mixture of one or more of ether, Tripropylene glycol monomethyl Ether.
7. such as the vehicle glass of any of claims 1-6 preparation method of high temperature-proof diffusion silver paste, feature exists In using following steps:
(1) it stocks up according to following components and weight percentage:
(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) it the preparation of silver paste: after weighing silver powder, glass powder, inorganic additive, is sufficiently mixed in batch mixer with carrier It closes, 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 control of silver paste is made by the fine tuning of idler wheel System at 15 μm hereinafter, viscosity be 20-30PaS, obtain vehicle glass high temperature-proof diffusion silver paste.
CN201711104343.2A 2017-11-10 2017-11-10 A kind of vehicle glass high temperature-proof diffusion silver paste and preparation method thereof Pending CN109785992A (en)

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CN111243777A (en) * 2020-03-03 2020-06-05 深圳市利红金科技有限公司 Composite conductive powder and preparation method thereof
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
CN111511099A (en) * 2020-03-25 2020-08-07 上海玖银电子科技有限公司 Quick-drying silver paste for large keyboard conductive film circuit and preparation method thereof
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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CN1072940A (en) * 1991-12-03 1993-06-09 E·I·内穆尔杜邦公司 The thick film conductor paste that vehicle glass is used
CN101462832A (en) * 2009-01-12 2009-06-24 付明 Environment protection type automobile wind screen defrosting heater wire silver slurry
CN101613186A (en) * 2008-06-27 2009-12-30 上海昌银电子材料科技有限公司 Lead-free silver slurry for high-temperature sintered automobile glass heating wire and preparation method thereof
CN105761777A (en) * 2014-12-18 2016-07-13 上海宝银电子材料有限公司 Filament silver paste for automobile glass and preparation method of filament silver paste
CN105753335A (en) * 2014-12-18 2016-07-13 上海宝银电子材料有限公司 Acid-resistant and antioxidant silver paste for automotive glass and method for preparing acid-resistant and antioxidant silver paste

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CN1072940A (en) * 1991-12-03 1993-06-09 E·I·内穆尔杜邦公司 The thick film conductor paste that vehicle glass is used
CN101613186A (en) * 2008-06-27 2009-12-30 上海昌银电子材料科技有限公司 Lead-free silver slurry for high-temperature sintered automobile glass heating wire and preparation method thereof
CN101462832A (en) * 2009-01-12 2009-06-24 付明 Environment protection type automobile wind screen defrosting heater wire silver slurry
CN105761777A (en) * 2014-12-18 2016-07-13 上海宝银电子材料有限公司 Filament silver paste for automobile glass and preparation method of filament silver paste
CN105753335A (en) * 2014-12-18 2016-07-13 上海宝银电子材料有限公司 Acid-resistant and antioxidant silver paste for automotive glass and method for preparing acid-resistant and antioxidant silver paste

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111243777A (en) * 2020-03-03 2020-06-05 深圳市利红金科技有限公司 Composite conductive powder and preparation method thereof
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
CN111326849B (en) * 2020-03-09 2021-07-06 广东四维新材料有限公司 Method for preparing signal receiving/transmitting antenna of automatic driving automobile
CN111511099A (en) * 2020-03-25 2020-08-07 上海玖银电子科技有限公司 Quick-drying silver paste for large keyboard conductive film circuit and preparation method thereof
CN111511099B (en) * 2020-03-25 2021-06-08 上海玖银电子科技有限公司 Quick-drying silver paste for large keyboard conductive film circuit and preparation method thereof
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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Application publication date: 20190521