CN101613186A - Lead-free silver slurry for high-temperature sintered automobile glass heating wire and preparation method thereof - Google Patents
Lead-free silver slurry for high-temperature sintered automobile glass heating wire and preparation method thereof Download PDFInfo
- Publication number
- CN101613186A CN101613186A CN200810039730A CN200810039730A CN101613186A CN 101613186 A CN101613186 A CN 101613186A CN 200810039730 A CN200810039730 A CN 200810039730A CN 200810039730 A CN200810039730 A CN 200810039730A CN 101613186 A CN101613186 A CN 101613186A
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- lead
- heating wire
- free silver
- temperature sintered
- powder
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Abstract
The present invention relates to a kind of lead-free silver slurry for high-temperature sintered automobile glass heating wire and preparation method thereof, this lead-free silver slurry comprises following component and content (weight): silver powder 50%～85%; Lead-free silver glass powder 3%～7%; Polymer binder 3%～12%; Organic solvent 7%～23%; Superfine metal compound 1%～5%; Additive 0.5%～3%, described component obtains lead-free silver slurry for high-temperature sintered automobile glass heating wire through mixing, dissolve, grind, filtering.Compared with prior art, lead-free silver slurry for high-temperature sintered automobile glass heating wire of the present invention has the following advantages: resistance to acids and bases and good weatherability, the technology printing is good, firing temperature is wide, good with the automobile glass printing ink matching, production cost is low, and electroconductibility, the weldability of the metal conduction band film behind the sintering are good, strong adhesion, metallic membrane back side color setting range is big, environmental protection.
Description
Technical field
The present invention relates to the employed silver slurry of automotive safety glass, relate in particular to lead-free silver slurry for high-temperature sintered automobile glass heating wire and preparation method thereof.
Background technology
Automotive safety glass all is toughened glass usually; toughened glass is to make glass have safety performance by physical toughened method; be about to glass at the process furnace internal heating near the softening temperature of glass; in cooling apparatus, cool off rapidly then with heat-eliminating mediums such as air; form stress on its surface; the inner tension stress that forms; stretch-proof performance, intensity and the thermotolerance of glass have been improved; when glass breakage; under outer field protection; glass is kept together or be covered with fissured aggregate, form the particle of no sharp corner angle about 10mm.
Automobile glass printing ink is mainly used in the surperficial glazing of float glass, the effect of playing protection and decorating reticulate pattern.The production technique of automotive safety glass: cutting---edging---printing (printing ink, silver slurry)---tempering---moulding cooling (hot bending)---weldering tongue piece---packing.
Environment is polluted in making use for reducing electronic product, European Union is in the formal ROHS decree of implementing on July 1st, 2006, wherein the content of lead, mercury, sexavalent chrome, Polybrominated biphenyl and Poly Brominated Diphenyl Ethers must not surpass 0.1% in the ROHS instruction regulation electronic product, the content of cadmium must not surpass 0.01%, and China Ministry of Information Industry has issued " electronics and IT products pollution control management way " on March 1st, 2006.
At present, the employed silver slurry of automotive safety glass is the product of BASF and Zhuan Chen Wan Feng, mainly have following problem: the resistance to acids and bases of metal level and weathering resistance are poor behind the sintering, weldability is good inadequately, and the sticking power between glass substrate is little, and the silver slurry is not suitable for the high ultra-fine line pattern of printed resolution, great majority all are leaded non-environmentfriendly products, the cost height, not good with the automobile glass printing ink matching, metallic membrane back side color tunable scope is little.
Summary of the invention
Purpose of the present invention is exactly to provide lead-free silver slurry for high-temperature sintered automobile glass heating wire of a kind of environmental protection, resistance to acids and bases and good weatherability and preparation method thereof for the defective that overcomes above-mentioned prior art existence.
Purpose of the present invention can be achieved through the following technical solutions:
Lead-free silver slurry for high-temperature sintered automobile glass heating wire is characterized in that, comprises following component and content (weight):
Silver powder 50%～85%;
Lead-free silver glass powder 3%～7%;
Polymer binder 3%～12%;
Organic solvent 7%～23%;
Superfine metal compound 1%～5%;
Additive 0.5%～3%.
Described silver powder is to mix silver powder by what spherical and flake silver powder were formed, and the median size of this mixing silver powder is 0.5～3 μ m, and tap density is 1.8～2.4g/ml.
Described lead-free silver glass powder is by Bi
2O
3, SiO
2, B
2O
3, ZnO, Al
2O
3, TiO
2, composition such as Ag, the content of described Ag is 0.05wt%～1wt%.
Described polymer binder is selected from one or more in ethyl cellulose, the Nitrocellulose; Described organic solvent is selected from one or more in Terpineol 350, Diethylene Glycol butyl ether, the turps.
Described superfine metal compound is selected from SnO
2, CuO, ZrO
2In one or more, the grain diameter of described superfine metal compound is less than 0.5 μ m; Described additive is selected from one or more in dibutyl phthalate, the Yelkin TTS.
The preparation method of lead-free silver slurry for high-temperature sintered automobile glass heating wire is characterized in that, this method may further comprise the steps:
(1) get the raw materials ready by following component and content (weight):
Silver powder 50%～85%
Lead-free silver glass powder 3%～7%
Polymer binder 3%～12%
Organic solvent 7%～23%
Superfine metal compound 1%～5%
Additive 0.5%～3%;
(2) organic solvent of adding meltage in additive makes its dissolving, and is standby;
(3) polymer binder and remaining organic solvent are put into water-bath and mix, be heated to dissolving fully, add the dissolved additive then, stir and make organic carrier;
(4) silver powder, lead-free silver glass powder, superfine metal compound are mixed with organic carrier stir evenly, by the three-roll grinder dispersion grinding until fineness less than 5 μ m, the slurry that obtains filters on 350 order screen cloths and promptly gets lead-free silver slurry for high-temperature sintered automobile glass heating wire.
Described silver powder is to mix silver powder by what spherical and flake silver powder were formed, and the median size of this mixing silver powder is 0.5～3 μ m, and tap density is 1.8～2.4g/ml.
Described lead-free silver glass powder is by Bi
2O
3, SiO
2, B
2O
3, ZnO, Al
2O
3, TiO
2, composition such as Ag, the content of described Ag is 0.05wt%～1wt%.
Described polymer binder is selected from one or more in ethyl cellulose, the Nitrocellulose; Described organic solvent is selected from one or more in Terpineol 350, Diethylene Glycol butyl ether, the turps.
Described superfine metal compound is selected from SnO
2, CuO, ZrO
2In one or more, the grain diameter of described superfine metal compound is less than 0.5 μ m; Described additive is selected from one or more in dibutyl phthalate, the Yelkin TTS.
The present invention improves the printing of slurry by adding spherical silver powder and additive, can obtain smooth, the circuit clearly of conduction band edge when the high ultra-fine line pattern of printed resolution; By selecting the suitable glass powder solution and the problem of printing ink matching; By to the selection of glass powder with mix resistance to acids and bases and the weathering resistance that the superfine metal compound improves slurry; Improve weldability and sticking power by the selection that adds an amount of sheet powder, superfine metal compound and glass powder; By the selection of glass powder and the addition of adjusting superfine metal compound are realized that the variable range of metal level back side color is big; By in glass powder, adding Ag, can significantly improve the electroconductibility of slurry, reduce production costs; Objectionable impuritiess such as not leaded in the slurry, cadmium are environmentfriendly products.
Compared with prior art, lead-free silver slurry for high-temperature sintered automobile glass heating wire of the present invention has the following advantages: resistance to acids and bases and good weatherability, the technology printing is good, firing temperature is wide, good with the automobile glass printing ink matching, production cost is low, and electroconductibility, the weldability of the metal conduction band film behind the sintering are good, strong adhesion, metallic membrane back side color setting range is big, environmental protection.
Embodiment
The invention will be further described below in conjunction with specific embodiment.
Embodiment 1～5
A kind of preparation method of lead-free silver slurry for high-temperature sintered automobile glass heating wire, this method may further comprise the steps:
(1) embodiment 1～5 gets the raw materials ready by following component and content (weight) respectively:
In the foregoing description 1: described silver powder is formed (the two weight ratio is 1: 2) by spherical with flake silver powder, and the median size of this mixing silver powder is 0.5 μ m, and tap density is 2.4g/ml, and described lead-free silver glass powder is by Bi
2O
3, SiO
2, B
2O
3, ZnO, Al
2O
3, TiO
2, composition such as Ag, the content of Ag is 0.05wt%, described polymer binder is an ethyl cellulose, described organic solvent is a Terpineol 350, described superfine metal compound is SnO
2, grain diameter is less than 0.5 μ m, and described additive is a dibutyl phthalate;
In the foregoing description 2: described silver powder is formed (weight ratio is 1: 5) by spherical with flake silver powder, and the median size of this mixing silver powder is 1 μ m, and tap density is 2.2g/ml, and described lead-free silver glass powder is by Bi
2O
3, SiO
2, B
2O
3, ZnO, Al
2O
3, TiO
2, composition such as Ag, the content of Ag is 0.2wt%, described polymer binder is a Nitrocellulose, described organic solvent is the Diethylene Glycol butyl ether, described superfine metal compound is SnO
2And CuO (weight ratio is 1: 1), grain diameter is less than 0.5 μ m, and described additive is a Yelkin TTS;
In the foregoing description 3: described silver powder is formed (weight ratio is 1: 8) by spherical with flake silver powder, and the median size of this mixing silver powder is 2 μ m, and tap density is 2g/ml, and described lead-free silver glass powder is by Bi
2O
3, SiO
2, B
2O
3, ZnO, Al
2O
3, TiO
2, composition such as Ag, the content of Ag is 0.5wt%, described polymer binder is ethyl cellulose and Nitrocellulose (weight ratio is 1: 1), and described organic solvent is Diethylene Glycol butyl ether and turps (weight ratio is 1: 1), and described superfine metal compound is SnO
2, CuO and ZrO (weight ratio is 1: 1: 2), grain diameter is less than 0.5 μ m, described additive is dibutyl phthalate and Yelkin TTS (weight ratio is 1: 1);
In the foregoing description 4: described silver powder is formed (weight ratio is 1: 10) by spherical with flake silver powder, and the median size of this mixing silver powder is 3 μ m, and tap density is 1.8g/ml, and described lead-free silver glass powder is by Bi
2O
3, SiO
2, B
2O
3, ZnO, Al
2O
3, TiO
2, composition such as Ag, the content of Ag is 0.8wt%, described polymer binder is ethyl cellulose and Nitrocellulose (weight ratio is 2: 1), described organic solvent is Terpineol 350 and turps (weight ratio is 1: 2), described superfine metal compound is SnO
2, CuO and ZrO (weight ratio is 2: 1: 4), grain diameter is less than 0.5 μ m, described additive is dibutyl phthalate and Yelkin TTS (weight ratio is 1: 2);
In the foregoing description 5: described silver powder is formed (weight ratio is 1: 12) by spherical (particle diameter is less than 1 μ m) with flake silver powder, and the median size of this mixing silver powder is 3 μ m, and tap density is 1.8g/mi, and described lead-free silver glass powder is by Bi
2O
3, SiO
2, B
2O
3, ZnO, Al
2O
3, TiO
2, composition such as Ag, the content of Ag is 1wt%, described polymer binder is ethyl cellulose and Nitrocellulose (weight ratio is 1: 2), described organic solvent is Terpineol 350 and turps (weight ratio is 2: 1), described superfine metal compound is SnO
2, CuO and ZrO (weight ratio is 1: 1: 1), grain diameter is less than 0.5 μ m, described additive is dibutyl phthalate and Yelkin TTS (weight ratio is 2: 1);
After getting material ready, carry out following operation:
(2) organic solvent of adding meltage in additive makes its dissolving, and is standby;
(3) polymer binder and remaining organic solvent are put into water-bath and mix, be heated to dissolving fully, add the dissolved additive then, stir and make organic carrier;
(4) silver powder, lead-free silver glass powder, superfine metal compound are mixed with organic carrier stir evenly, by the three-roll grinder dispersion grinding until fineness less than 5 μ m, the slurry that obtains filters on 350 order screen cloths and promptly gets lead-free silver slurry for high-temperature sintered automobile glass heating wire.
Claims (10)
1. lead-free silver slurry for high-temperature sintered automobile glass heating wire is characterized in that, comprises following component and content (weight):
Silver powder 50%～85%;
Lead-free silver glass powder 3%～7%;
Polymer binder 3%～12%;
Organic solvent 7%～23%;
Superfine metal compound 1%～5%;
Additive 0.5%～3%.
2. lead-free silver slurry for high-temperature sintered automobile glass heating wire according to claim 1, it is characterized in that, described silver powder is to mix silver powder by what spherical and flake silver powder were formed, and the median size of this mixing silver powder is 0.5～3 μ m, and tap density is 1.8～2.4g/ml.
3. lead-free silver slurry for high-temperature sintered automobile glass heating wire according to claim 1 is characterized in that, described lead-free silver glass powder is by Bi
2O
3, SiO
2, B
2O
3, ZnO, Al
2O
3, TiO
2, composition such as Ag, the content of described Ag is 0.05wt%～1wt%.
4. lead-free silver slurry for high-temperature sintered automobile glass heating wire according to claim 1 is characterized in that described polymer binder is selected from one or more in ethyl cellulose, the Nitrocellulose; Described organic solvent is selected from one or more in Terpineol 350, Diethylene Glycol butyl ether, the turps.
5. lead-free silver slurry for high-temperature sintered automobile glass heating wire according to claim 1 is characterized in that, described superfine metal compound is selected from SnO
2, CuO, ZrO
2In one or more, the grain diameter of described superfine metal compound is less than 0.5 μ m; Described additive is selected from one or more in dibutyl phthalate, the Yelkin TTS.
6. the preparation method of lead-free silver slurry for high-temperature sintered automobile glass heating wire is characterized in that, this method may further comprise the steps:
(1) get the raw materials ready by following component and content (weight):
Silver powder 50%～85%
Lead-free silver glass powder 3%～7%
Polymer binder 3%～12%
Organic solvent 7%～23%
Superfine metal compound 1%～5%
Additive 0.5%～3%;
(2) organic solvent of adding meltage in additive makes its dissolving, and is standby;
(3) polymer binder and remaining organic solvent are put into water-bath and mix, be heated to dissolving fully, add the dissolved additive then, stir and make organic carrier;
(4) silver powder, lead-free silver glass powder, superfine metal compound are mixed with organic carrier stir evenly, by the three-roll grinder dispersion grinding until fineness less than 5 μ m, the slurry that obtains filters on 350 order screen cloths and promptly gets lead-free silver slurry for high-temperature sintered automobile glass heating wire.
7. the preparation method of lead-free silver slurry for high-temperature sintered automobile glass heating wire according to claim 6, it is characterized in that, described silver powder is to mix silver powder by what spherical and flake silver powder were formed, and the median size of this mixing silver powder is 0.5～3 μ m, and tap density is 1.8～2.4g/ml.
8. the preparation method of lead-free silver slurry for high-temperature sintered automobile glass heating wire according to claim 6 is characterized in that, described lead-free silver glass powder is by Bi
2O
3, SiO
2, B
2O
3, ZnO, Al
2O
3, TiO
2, composition such as Ag, the content of described Ag is 0.05wt%～1wt%.
9. the preparation method of lead-free silver slurry for high-temperature sintered automobile glass heating wire according to claim 6 is characterized in that, described polymer binder is selected from one or more in ethyl cellulose, the Nitrocellulose; Described organic solvent is selected from one or more in Terpineol 350, Diethylene Glycol butyl ether, the turps.
10. the preparation method of lead-free silver slurry for high-temperature sintered automobile glass heating wire according to claim 6 is characterized in that, described superfine metal compound is selected from SnO
2, CuO, ZrO
2In one or more, the grain diameter of described superfine metal compound is less than 0.5 μ m; Described additive is selected from one or more in dibutyl phthalate, the Yelkin TTS.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200810039730A CN101613186A (en) | 2008-06-27 | 2008-06-27 | Lead-free silver slurry for high-temperature sintered automobile glass heating wire and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200810039730A CN101613186A (en) | 2008-06-27 | 2008-06-27 | Lead-free silver slurry for high-temperature sintered automobile glass heating wire and preparation method thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN101613186A true CN101613186A (en) | 2009-12-30 |
Family
ID=41493095
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN200810039730A Pending CN101613186A (en) | 2008-06-27 | 2008-06-27 | Lead-free silver slurry for high-temperature sintered automobile glass heating wire and preparation method thereof |
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|---|---|
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| CN101964219A (en) * | 2010-08-10 | 2011-02-02 | 上海九晶电子材料股份有限公司 | Silver paste for positive of crystalline silicon solar cell and preparation method thereof |
| CN101986390A (en) * | 2010-11-23 | 2011-03-16 | 肇庆市羚光电子化学品材料科技有限公司 | Silver paste for disk capacitor electrode |
| CN102013282A (en) * | 2010-12-21 | 2011-04-13 | 昆明理工大学 | Silver paste special for glass defogging heater wires and preparation method thereof |
| CN102360628A (en) * | 2011-09-22 | 2012-02-22 | 山东省科学院新材料研究所 | Method for preparing silver paste used for back electrode of photovoltaic cell |
| CN102543260A (en) * | 2012-02-27 | 2012-07-04 | 江苏科技大学 | Silver paste for electrode of solar cell and method for preparing silver paste |
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| CN103606394A (en) * | 2013-11-08 | 2014-02-26 | 四川大学 | Silver slurry containing multiple-hydrogen bond supermolecule self assembly system, and application thereof |
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| CN110856298A (en) * | 2019-11-22 | 2020-02-28 | 湖南嘉业达电子有限公司 | Electromagnetic induction heating film capable of controlling temperature automatically 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 |
-
2008
- 2008-06-27 CN CN200810039730A patent/CN101613186A/en active Pending
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| CN101986390A (en) * | 2010-11-23 | 2011-03-16 | 肇庆市羚光电子化学品材料科技有限公司 | Silver paste for disk capacitor electrode |
| CN101986390B (en) * | 2010-11-23 | 2013-04-03 | 广东羚光新材料股份有限公司 | Silver paste for disk capacitor electrode |
| CN102013282A (en) * | 2010-12-21 | 2011-04-13 | 昆明理工大学 | Silver paste special for glass defogging heater wires and preparation method thereof |
| CN102360628A (en) * | 2011-09-22 | 2012-02-22 | 山东省科学院新材料研究所 | Method for preparing silver paste used for back electrode of photovoltaic cell |
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| CN103165220A (en) * | 2011-12-15 | 2013-06-19 | 上海宝银电子材料有限公司 | Lead-free soldering-resistant electric conduction silver paste for electro-thermal film quartz glass tube electric heating piece and preparation method |
| CN103165213B (en) * | 2011-12-15 | 2016-01-06 | 上海宝银电子材料有限公司 | A kind of passenger vehicle windshield conductive silver paste and preparation method thereof |
| CN102543260A (en) * | 2012-02-27 | 2012-07-04 | 江苏科技大学 | Silver paste for electrode of solar cell and method for preparing silver paste |
| CN102779566A (en) * | 2012-05-14 | 2012-11-14 | 乐凯胶片股份有限公司 | Lead-free conductive silver paste for front faces of crystalline silicon solar cells |
| CN103000251A (en) * | 2012-11-10 | 2013-03-27 | 江苏瑞德新能源科技有限公司 | Solar cell silver-backed slurry with wide sintering process window |
| CN103000251B (en) * | 2012-11-10 | 2015-05-20 | 江苏瑞德新能源科技有限公司 | Solar cell silver-backed slurry with wide sintering process window |
| CN103606394A (en) * | 2013-11-08 | 2014-02-26 | 四川大学 | Silver slurry containing multiple-hydrogen bond supermolecule self assembly system, and application thereof |
| CN105764168A (en) * | 2016-01-12 | 2016-07-13 | 昆明理工大学 | Car rear windshield heating wire silver paste and preparation method thereof |
| CN107393629A (en) * | 2017-09-13 | 2017-11-24 | 福建阿石创新材料股份有限公司 | A kind of conductive silver paste and its preparation method and application |
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| 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 |
| CN110856298A (en) * | 2019-11-22 | 2020-02-28 | 湖南嘉业达电子有限公司 | Electromagnetic induction heating film capable of controlling temperature automatically and preparation method thereof |
| CN110856298B (en) * | 2019-11-22 | 2022-05-13 | 湖南嘉业达电子有限公司 | Electromagnetic induction heating film capable of controlling temperature automatically 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 |
| 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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Open date: 20091230 |