CN103310868B - A kind of electronic devices and components silver slurry and preparation method thereof - Google Patents
A kind of electronic devices and components silver slurry and preparation method thereof Download PDFInfo
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- CN103310868B CN103310868B CN201210062470.1A CN201210062470A CN103310868B CN 103310868 B CN103310868 B CN 103310868B CN 201210062470 A CN201210062470 A CN 201210062470A CN 103310868 B CN103310868 B CN 103310868B
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Abstract
The present patent application provides a kind of electronic devices and components silver slurry, by containing oxidation silver powder, the mixed-powder of glass dust and wetting agent and containing solvent, adhesive, the organic carrier of levelling agent and defoamer is made, wherein mixed-powder accounts for the 65%-90% of the percentage by weight of slurry, organic carrier accounts for the 10%-35% of the percentage by weight of slurry, silver oxide powder comprises the spherical powder A of average grain diameter at 2-3 micron, average grain diameter is at the spherical powder B of 0.5-1.5 micron and the average grain diameter spherical powder C at 0.1-0.3 micron, the present patent application additionally provides the preparation method of above-mentioned slurry.The sintering temperature that described silver slurry reduces slurry is low to moderate 400 DEG C most, improves the electrical property after slurry sintering and solderability, improves the sintering outward appearance of rete.
Description
Technical field
The present patent application relates to a kind of electrocondution slurry, specifically relates to the preparation method of a kind of electronic devices and components silver slurry and this slurry.
Background technology
Electric slurry product be logging material, metallurgy, chemical industry, electronic technology in the electronic functional material of one, be hybrid integrated circuit, senser, surface installation technique, resistor network, display, and the basic material of various electronic discrete elements etc.Through techniques such as silk screen printing, levelling, oven dry, sintering, electric slurry can solidify to form conducting film on the substrates such as pottery, can be made into thick film integrated circuit, resistor, resistor network, capacitor, multilayer ceramic capacitor (MLCC), conductor ink, electrode of solar battery, LED cold light source, organic light emitting display (OLED), printing and high-resolution electric conductor, thin film switch/flexible circuit, conducting resinl, sensitive components and other electronic devices and components.
Electric slurry is primarily of function phase, Binder Phase, organic carrier three part composition, and silver slurry is current most widely used electrocondution slurry, and its function is the silver powder of excellent electric conductivity, moderate difformity and size mutually.But because silver point is 961.8 DEG C, so the sintering temperature of silver slurry is generally higher, super fine silver powder generally just has reasonable sintering effect at 600 DEG C-800 DEG C, which limits its range of application.
Summary of the invention
Namely the present patent application is the above-mentioned defect for existing in current electric slurry technology, provides a kind of electronic devices and components silver slurry and preparation method thereof.
The thinking of the present patent application is as described below: adopt silver oxide powder body to substitute silver powder as function phase, because silver oxide will resolve into silver and oxygen completely at 300 DEG C, first ensure that its conductivity, and the silver just having transformed generation inherently has certain adhesive force and its sintering activity is good, this will reduce the sintering temperature of slurry greatly, just has good sintering effect at 400-500 DEG C; And the oxygen that silver oxide decomposition generates can react with the organic substance in slurry, makes its Thorough combustion, reduce the residual of impurity, and then improve its solderability and electrical property, improve the sintering outward appearance of rete.
An object of the present patent application is to provide a kind of electronic devices and components silver slurry, and this object is realized by following technical scheme:
Specifically, described electronic devices and components silver slurry, by the mixed-powder containing oxidation silver powder, glass dust and wetting agent and make containing the organic carrier of solvent, adhesive, levelling agent and defoamer, the 10%-35% that wherein mixed-powder accounts for the 65%-90% of the percentage by weight of slurry, organic carrier accounts for the percentage by weight of slurry.
Further, the percentage by weight that described mixed-powder accounts for slurry is 84%, and the percentage by weight that organic carrier accounts for slurry is 16%.
Further, described silver oxide powder comprises average grain diameter in the spherical powder A of 2-3 micron, average grain diameter at the spherical powder B of 0.5-1.5 micron and the average grain diameter spherical powder C at 0.1-0.3 micron, and the percetage by weight accounting for the wetting mixed-powder mixed respectively is 30%-65%, 20-40% and 5%-30%.
Further, the average grain diameter of described glass dust is at 0.2-2.5 micron, and melt temperature is 400 DEG C-500 DEG C, and the percetage by weight accounting for the wetting mixed-powder mixed is 5%-10%.
Further, described wetting agent is one or more the mixture in terpinol, n-butanol, n-octyl alcohol, castor oil, and the percetage by weight accounting for the wetting mixed-powder mixed is 0.8%-5%.
Preferably, in the described powder soaked, the percentage by weight shared by each composition is respectively: silver oxide powder A:61.2%, silver oxide powder B:22.7%, silver oxide powder C:9.5%, glass dust: 5.6%, wetting agent: 1.0%.
Further, in described organic carrier, solvent is one or more mixture of terpinol, turpentine oil, isoamyl acetate, butyl, occupies the 75%-90% of airborne body weight percentage.
In addition, binding agent is cellulose ethers, cellulose esters, dibutyl phthalate, one or more mixture stearic, occupies the 5%-20% of airborne body weight percentage.
In addition, defoamer is one or more the mixture in palmityl alcohol, dimethicone, BYK-141, BYK-A530, occupies the 1%-2.5% of airborne body weight percentage.
In addition, levelling agent is one or more the mixture in SKR-A450, BYK-306, BYK-346, GSK-533, occupies the 1%-4% of airborne body weight percentage.
Another object of the present patent application is to provide the preparation method of above-mentioned electronic devices and components silver slurry, and this object is realized by following technical scheme:
The preparation method of described electronic devices and components silver slurry, has following operation:
1, the preparation of mixed-powder: in proportion different types of oxidation silver powder and glass dust are mixed 0.5-2h in batch mixer, then add wetting agent mixing 2-4h, formation mixes, the powder of moistened surface;
2, the preparation of organic carrier: in proportion solvent, adhesive, levelling agent and defoamer are mixed, heating water bath, to 60-80 DEG C, fully stirs 4-10h, until form even, transparent jelly;
3, the preparation of slurry: by the powder mixed and the organic carrier ground and mixed prepared, form the paste with certain viscosity and printing.
The sintering temperature that silver slurry described in the present patent application reduces slurry is low to moderate 400 DEG C most, improves the electrical property after slurry sintering and solderability, improves the sintering outward appearance of rete.
Specific embodiment
Below in conjunction with concrete formula and preparation method; electronic devices and components silver slurry described in the present patent application and preparation method thereof is described; object is in order to the public better understands described technology contents; instead of the restriction to described technology contents; in fact; in the improvement carried out the process conditions in described electric slurry formula and preparation process thereof with identical or approximate principle; to realize identical or approximate technique effect, then all within the present patent application technical scheme required for protection.
embodiment 1
First the silver oxide powder A514 gram of average grain diameter at 2-3 micron is taken, average grain diameter is at the silver oxide powder B190.7 gram of 0.5-1.5 micron, average grain diameter is at the silver oxide powder C79.8 gram of 0.1-0.3 micron, average grain diameter is at 47 grams, the lead and cadmium free glass dust of 0.2-2.5 micron, 1 hour is mixed in batch mixer, then add 8.4 grams of terpinols, then continue mixing 3 hours, formed mix, the powder of moistened surface; Then take the butyl of 123.2 grams, the ethyl cellulose of 28.8 grams, the dimethicone of 3.2 grams, the SKR-A450 of 4.8 grams, mixing, heating water bath, to 60 DEG C, fully stirs 6h, until form even, transparent jelly, and cooling; Then with three-high mill by the powder mixed and the abundant ground and mixed of organic carrier for preparing, form the paste with certain viscosity and printing.
embodiment 2
First the silver oxide powder A400 gram of average grain diameter at 2-3 micron is taken, average grain diameter is at the silver oxide powder B240 gram of 0.5-1.5 micron, average grain diameter is at the silver oxide powder C88 gram of 0.1-0.3 micron, average grain diameter is at 60 grams, the lead and cadmium free glass dust of 0.2-2.5 micron, 0.5 hour is mixed in batch mixer, then add 12 grams of n-octyl alcohols, then continue mixing 2 hours, package spare; Take the terpinol of 160 grams, the stearic acid of 32 grams, the BYK-A530 of 4 grams, the GSK-533 of 4 grams, mixing, heating water bath, to 70 DEG C, fully stirs 4h, until form even, transparent jelly, and cooling; Then with three-high mill by the powder mixed and the abundant ground and mixed of organic carrier for preparing, form the paste with certain viscosity and printing.
embodiment 3
First the silver oxide powder A452 gram of average grain diameter at 2-3 micron is taken, average grain diameter is at the silver oxide powder B202 gram of 0.5-1.5 micron, average grain diameter is at the silver oxide powder C80.5 gram of 0.1-0.3 micron, average grain diameter is at 52 grams, the lead and cadmium free glass dust of 0.2-2.5 micron, 2 hours are mixed in batch mixer, then add 10.5 grams of castor oil, then continue mixing 4 hours, package spare; Take the terpinol of 143 grams, the stearic acid of 30.4 grams, the palmityl alcohol of 3.8 grams, the BYK-306 of 4.2 grams, mixing, heating water bath, to 80 DEG C, fully stirs 10h, until form even, transparent jelly, and cooling; Then with three-high mill by the powder mixed and the abundant ground and mixed of organic carrier for preparing, form the paste with certain viscosity and printing.
Take the electronic devices and components silver slurry that technique described in the present patent application prepares, the sintering temperature of slurry can be reduced, and the electrical property that improve after slurry sintering and solderability, improve the sintering outward appearance of rete.
Claims (9)
1. an electronic devices and components silver slurry, it is characterized in that: described slurry is by the mixed-powder containing oxidation silver powder, glass dust and wetting agent and make containing the organic carrier of solvent, adhesive, levelling agent and defoamer, the 10%-35% that wherein mixed-powder accounts for the 65%-90% of the percentage by weight of slurry, organic carrier accounts for the percentage by weight of slurry; Described oxidation silver powder comprises average grain diameter in the spherical powder A of 2-3 micron, average grain diameter at the spherical powder B of 0.5-1.5 micron and the average grain diameter spherical powder C at 0.1-0.3 micron, and the percetage by weight accounting for the wetting mixed-powder mixed respectively is 30%-65%, 20-40% and 5%-30%.
2. slurry according to claim 1, is characterized in that: the percentage by weight that described mixed-powder accounts for slurry is 84%, and the percentage by weight that organic carrier accounts for slurry is 16%.
3. slurry according to claim 1 and 2, is characterized in that: the average grain diameter of described glass dust is at 0.2-2.5 micron, and melt temperature is 400 DEG C-500 DEG C, and the percetage by weight accounting for the wetting mixed-powder mixed is 5%-10%.
4. slurry according to claim 1 and 2, is characterized in that: described wetting agent is one or more the mixture in terpinol, n-butanol, n-octyl alcohol, castor oil, and the percetage by weight accounting for mixed-powder is 0.8%-5%.
5. slurry according to claim 1, is characterized in that: in described mixed-powder, and the percentage by weight shared by each composition is respectively: oxidation silver powder A:61.2%, oxidation silver powder B:22.7%, oxidation silver powder C:9.5%, glass dust: 5.6%, wetting agent: 1.0%.
6. slurry according to claim 1 and 2, it is characterized in that: in described organic carrier, solvent is one or more mixture of terpinol, turpentine oil, isoamyl acetate, butyl, occupies the 75%-90% of airborne body weight percentage.
7. slurry according to claim 1 and 2, it is characterized in that: in described organic carrier, adhesive is cellulose ethers, cellulose esters, dibutyl phthalate, one or more mixture stearic, occupies the 5%-20% of airborne body weight percentage.
8. slurry according to claim 1 and 2, it is characterized in that: in described organic carrier, defoamer is one or more the mixture in palmityl alcohol, dimethicone, BYK-141, BYK-A530, occupies the 1%-2.5% of airborne body weight percentage; Levelling agent is one or more the mixture in SKR-A450, BYK-306, BYK-346, GSK-533, occupies the 1%-4% of airborne body weight percentage.
9. the preparation method of the electronic devices and components silver slurry described in claim 1-8, is characterized in that, comprises following step:
1) preparation of mixed-powder: in proportion different types of oxidation silver powder and glass dust are mixed 0.5-2h in batch mixer, then add wetting agent mixing 2-4h, formation mixes, the powder of moistened surface;
2) preparation of organic carrier: in proportion solvent, adhesive, levelling agent and defoamer are mixed, heating water bath, to 60-80 DEG C, fully stirs 4-10h, until form even, transparent jelly;
3) preparation of slurry: by the powder mixed and the organic carrier ground and mixed prepared, form the paste with certain viscosity and printing.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201210062470.1A CN103310868B (en) | 2012-03-12 | 2012-03-12 | A kind of electronic devices and components silver slurry and preparation method thereof |
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| CN201210062470.1A CN103310868B (en) | 2012-03-12 | 2012-03-12 | A kind of electronic devices and components silver slurry and preparation method thereof |
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| CN103310868A CN103310868A (en) | 2013-09-18 |
| CN103310868B true CN103310868B (en) | 2015-12-02 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105599360A (en) * | 2014-11-14 | 2016-05-25 | 贺利氏德国有限责任两合公司 | Layered complex used for producing electric induction heating elements |
| CN105611660A (en) * | 2014-11-14 | 2016-05-25 | 贺利氏德国有限责任两合公司 | Method of manufacturing electric induction heating component |
| CN104464882B (en) * | 2014-12-05 | 2016-08-17 | 清华大学 | A kind of photovoltaic cell silver slurry and sintering method thereof |
| CN107731341A (en) * | 2017-09-25 | 2018-02-23 | 江苏时瑞电子科技有限公司 | A kind of negative tempperature coefficient thermistor compound copper electrode paste and preparation method thereof |
| CN112712913A (en) * | 2020-12-15 | 2021-04-27 | 陕西彩虹新材料有限公司 | Silver oxide slurry for electronic component and preparation method thereof |
| CN112750552A (en) * | 2020-12-25 | 2021-05-04 | 邯郸学院 | Sintered silver paste and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101604557A (en) * | 2008-06-11 | 2009-12-16 | 四川虹欧显示器件有限公司 | The plasma display of electrocondution slurry and this slurry of use |
| CN101609849A (en) * | 2009-07-13 | 2009-12-23 | 中南大学 | Silver conductive paste used for positive electrode of solar battery and preparation technology thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| US7226573B2 (en) * | 2003-09-10 | 2007-06-05 | Dowa Mining Co., Ltd. | Fine-grain silver oxide powder |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101604557A (en) * | 2008-06-11 | 2009-12-16 | 四川虹欧显示器件有限公司 | The plasma display of electrocondution slurry and this slurry of use |
| CN101609849A (en) * | 2009-07-13 | 2009-12-23 | 中南大学 | Silver conductive paste used for positive electrode of solar battery and preparation technology thereof |
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