CN102157221A - Method for preparing electrode silver paste for environment-friendly semiconductor capacitor - Google Patents
Method for preparing electrode silver paste for environment-friendly semiconductor capacitor Download PDFInfo
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- CN102157221A CN102157221A CN 201110075889 CN201110075889A CN102157221A CN 102157221 A CN102157221 A CN 102157221A CN 201110075889 CN201110075889 CN 201110075889 CN 201110075889 A CN201110075889 A CN 201110075889A CN 102157221 A CN102157221 A CN 102157221A
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Abstract
The invention discloses a method for preparing environment-friendly electrode silver paste for a semiconductor capacitor. The electrode silver paste is used for screen printing and is prepared from superfine silver powder, environment-friendly glass powder, an organic carrier and a solvent. The method has the following beneficial effects: the environment-friendly electrode silver paste prepared by the method is mainly applied to the semiconductor capacitor, is coated on the surface of a dielectric substrate of the semiconductor capacitor through screen printing and then is sintered into an electrode; the electrode silver paste is an important material for the semiconductor capacitor and has the characteristics of low loss, high capacitance, strong adhesion and welding resistance; and the silver paste prepared by the method absolutely meets the environmental requirements (free of Pb, Cd, Hg, Cr(VI), poly brominated biphenyl (PBB) and poly brominated diphenyl ether (PBDE) and conforming to the directive 2005/84/EC of European union RoHS on phthalates) of European union RoHS (restriction of hazardous substances) and is an ideal substitute for the non-environment-friendly silver paste which is commonly used at present.
Description
Technical field
The invention belongs to technical field of electronic materials, be specifically related to the preparation method of a kind of semiconductor capacitor with electrode silver plasm.
Background technology
Semiconductor capacitor is to adopt the semi-conducting material of high-ks such as barium titanate, strontium titanates, manganese oxide, strontium oxide strontia and zinc oxide as dielectric; at dielectric surface printing electrode slurry; through high temperature sintering and welding lead, re-using epoxy resin is that insulating protective layer is made.The profile of semiconductor capacitor is in the majority with chip.The fissipation factor of semiconductor capacitor is very little, and the resonance frequency height has semi-conductive characteristic again concurrently.Semiconductor capacitor is widely used in TV as basic device at present, computer, various electronic applications such as electronic instrument.Along with popularizing of household electrical appliance in recent years, electronic product is to miniaturization, microminiaturized developmentization development, and the demand of semiconductor capacitor increases year by year, as the also progressively increase of conductive silver paste demand of semiconductor capacitor electrode.
Semiconductor capacitor, mostly is and uses the flint glass powder more than 100 tons with present domestic year use amount of electrode silver plasm.Since 2005, the environmental protection standard of electronic material industry is all followed the RoHS instruction (not containing Pb, Cd, Hg, Cr (VI), Polybrominated biphenyl PBB, Poly Brominated Diphenyl Ethers PBDE) of European Union, and purpose is to satisfy the needs of outlet European Union electronic product.Original leaded silver-colored slurry can not satisfy industry requirement.
Summary of the invention
The purpose of this invention is to provide a kind of preparation method who can be used for the environment-friendly type semiconductor capacitor of silk screen printing with electrode silver plasm, using the silver of this method preparation to starch the environmental requirement (not containing Pb, Cd, Hg, Cr (VI), Polybrominated biphenyl PBB, Poly Brominated Diphenyl Ethers PBDE and the RoHS of the European Union instruction 2005/84/EC about phthalic acid ester) that meets the RoHS of European Union fully, is the desirable substituent of the present non-environmental protection silver slurry that generally uses.
For achieving the above object, the present invention takes following technical scheme:
A kind of environment-friendly type semiconductor capacitor preparation method of electrode silver plasm comprises following basic step:
Steps A: preparation environmental protection glass dust
Raw material composition and mass percent thereof according to environmental protection glass dust are weighed:
Bi
2O
3?70-76％；SiO
2?11-15％；SrO?2-6％；ZnO?6-10％；TiO
2?1-3％；
Load weighted above-mentioned raw materials mixed be placed on high temperature furnace heating, temperature controlling range: 900-1200 ℃, temperature retention time: 30-60 minute, after the quenching of the use of the glass powder particle after fusing deionized water, ball milling is to 0.5-2um, and the 200-400 order sieves, dry for standby; Add SrO and TiO
2Glass dust and matrix easier congruent melting when sintering of capacitor, form the phase of new homogeneous;
Step B: preparation silver powder
The silver powder of getting surface-treated average grain diameter 0.2-1um places vacuum drying chamber, and oven dry is 2-3 hour in 80-120 ℃ of drying box, and the secluding air sealing is preserved, and waits until standby;
Step C: preparation organic bond
According to the mass fraction, get 0.2 part of ethyl cellulose, 0.05 part in phenolic resins adds 0.75 part of solvent and is heated to 90-120 ℃, makes faint yellow transparent organic bond after being stirred well to complete solvent;
Step D: according to the mass fraction, get silver powder 50-70 part after the oven dry among the step B, the glass dust 1-3 part that makes in the steps A, average grain diameter 0.5-5um bismuth oxide powder 1-4 part and average grain diameter 0.5-4um nickel powder 2-5 part are stirred to abundant mixing; In well-mixed powder, add the organic bond of 15-30 part step C preparation, use three-roller or miscellaneous equipment fully to grind; Be ground to the outward appearance exquisiteness, when evenly not having particle, add the organic bond of 1-7 part step C preparation again, 2-9 part diluent stirs, and promptly can be made into environment-friendly type semiconductor capacitor electrode silver plasm.
Solvent among the described step C comprises one or more mixtures with arbitrary proportion in butyl carbitol, 1-Methoxy-2-propyl acetate, ethylene glycol ethyl ether, ethylene glycol monomethyl ether acetate, benzinum, turpentine oil, the terpinol.
Diluent in the described step F comprises one or more mixtures with arbitrary proportion in butyl carbitol, 1-Methoxy-2-propyl acetate, ethylene glycol ethyl ether, ethylene glycol monomethyl ether acetate, benzinum, turpentine oil, terpinol, castor oil, the cyclohexanone.
Adopt the environment-friendly type semiconductor capacitor of the present invention's preparation to be mainly used in semiconductor capacitor with electrode silver plasm, method by silk screen printing is coated in semiconductor capacitor dielectric substrate surface, behind the sintering as electrode, be the important materials of semiconductor capacitor, have the characteristics of low-loss, high-capacitance, strong adhesion and soldering resistance; The silver slurry material therefor of this method preparation meets the environmental requirement (not containing Pb, Cd, Hg, Cr (VI), Polybrominated biphenyl PBB, Poly Brominated Diphenyl Ethers PBDE and the RoHS of the European Union instruction 2005/84/EC about phthalic acid ester) of the RoHS of European Union fully,, be the silver-colored desirable substituent of starching of non-environmental protection that generally uses at present not in the RoHS of European Union instruction banned substance scope.
Embodiment
The present invention will be further described below by specific embodiment.
The environment-friendly type semiconductor capacitor of the present invention preparation method of electrode silver plasm comprises following basic step:
Steps A: preparation environmental protection glass dust
Raw material composition and mass percent thereof according to environmental protection glass dust are weighed:
Bi
2O
3?70-76％；SiO
2?11-15％；SrO?2-6％；ZnO?6-10％；TiO
2?1-3％；
Load weighted above-mentioned raw materials mixed be placed on high temperature furnace heating, temperature controlling range: 900-1200 ℃, temperature retention time: 30-60 minute, after the quenching of the use of the glass powder particle after fusing deionized water, ball milling is to 0.5-2um, and the 200-400 order sieves, dry for standby; Add SrO and the glass dust of TiO2 and matrix easier congruent melting when sintering of capacitor, form the phase of new homogeneous;
Step B: preparation silver powder
The silver powder of getting surface-treated average grain diameter 0.2-1um places vacuum drying chamber, and oven dry is 2-3 hour in 80-120 ℃ of drying box, and the secluding air sealing is preserved, and waits until standby;
Step C: preparation organic bond
According to the mass fraction, get 0.2 part of ethyl cellulose, 0.05 part in phenolic resins, add 0.75 part of solvent and be heated to 90-120 ℃, make faint yellow transparent organic bond after being stirred well to complete solvent, described solvent comprises one or more mixtures with arbitrary proportion in butyl carbitol, 1-Methoxy-2-propyl acetate, ethylene glycol ethyl ether, ethylene glycol monomethyl ether acetate, benzinum, turpentine oil, the terpinol;
Step D: according to the mass fraction, get silver powder 50-70 part after the oven dry among the step B, the glass dust 1-3 part that makes in the steps A, average grain diameter 0.5-5um bismuth oxide powder 1-4 part and average grain diameter 0.5-4um nickel powder 2-5 part are stirred to abundant mixing; In well-mixed powder, add the organic bond of 15-30 part step C preparation, use three-roller or miscellaneous equipment fully to grind; Be ground to the outward appearance exquisiteness, during evenly no particle, the organic bond that adds 1-7 part step C preparation again, 2-9 part diluent stirs, described diluent comprises one or more mixtures with arbitrary proportion in butyl carbitol, 1-Methoxy-2-propyl acetate, ethylene glycol ethyl ether, ethylene glycol monomethyl ether acetate, benzinum, turpentine oil, terpinol, castor oil, the cyclohexanone, promptly can be made into environment-friendly type semiconductor capacitor electrode silver plasm.
Specific embodiment proportioning (mass fraction) sees the following form:
The silver slurry that uses the inventive method to make, appearance luster is bright, (the rich power of the U.S. flies viscosimeter BRF DV-II+14# to viscosity at 60-150kcps, 10RPM), mobile splendid, after the silk screen printing of use 200-300 order, figure is clear, complete, no curtain coating phenomenon, 120-150 ℃ of aeration-drying bone dry after 3 minutes.
With the semiconductor capacitor ceramics high temperature sintering that prints, sintering temperature curve is step curve (total cycle is 48-75 minute, heats up, lowers the temperature each 20-30 minute, and 750-850 ℃ of high temperature section is 8-15 minute).
Ceramics after burning till can carry out welding lead according to the normal process of present industry, insulation such as seals at technological operation, makes the semiconductor capacitor finished product.Its performance reaches the identical level of the semiconductor capacitor that uses leaded silver slurry fully.
Though the present invention has made detailed description with above-mentioned preferred embodiment to the present invention, the foregoing description also is not used in qualification the present invention.Under the situation that does not break away from given technical characterictic of technical solution of the present invention and range of structures, the increase that technical characterictic is done, distortion or with the replacement of the same content in this area all should belong to protection scope of the present invention.
Claims (3)
1. the preparation method of an environment-friendly type semiconductor capacitor usefulness electrode silver plasm is characterized in that, comprises following basic step:
Steps A: preparation glass dust
Raw material composition and mass percent thereof according to glass dust are weighed:
Bi
2O
3?70-76％；SiO
2?11-15％；SrO?2-6％；ZnO?6-10％；TiO
2?1-3％；
Load weighted above-mentioned raw materials mixed be placed on high temperature furnace heating, control temperature: 900-1200 ℃, be incubated 30-60 minute; After the quenching of the use of the glass powder particle after fusing deionized water, ball milling is to 0.5-2um, and the 200-400 order sieves, dry for standby;
Step B: preparation silver powder
The silver powder of getting surface-treated average grain diameter 0.2-1um places vacuum drying chamber, and oven dry is 2-3 hour in 80-120 ℃ of drying box, and the secluding air sealing is preserved, and waits until standby;
Step C: preparation organic bond
According to the mass fraction, get 0.2 part of ethyl cellulose, 0.05 part in phenolic resins is stirred well to fully dissolving with 0.75 part of solvent, be heated to 90-120 ℃ after, make faint yellow transparent organic bond;
Step D: according to the mass fraction, get among the step B silver powder 50-70 part after the oven dry, the glass dust 1-3 part that makes in the steps A is that 0.5-5um bismuth oxide powder 1-4 part and average grain diameter 0.5-4um nickel powder 2-5 part are stirred to fully and mix with average grain diameter; In well-mixed powder, add the organic bond of 15-30 part step C preparation, use three-roller fully to grind; When being ground to even no particle, add the organic bond of 1-7 part step C preparation again, 2-9 part diluent stirs, and promptly can be made into environment-friendly type semiconductor capacitor electrode silver plasm.
2. the environment-friendly type semiconductor capacitor according to claim 1 preparation method of electrode silver plasm, it is characterized in that the solvent among the described step C comprises one or more mixtures with arbitrary proportion in butyl carbitol, 1-Methoxy-2-propyl acetate, ethylene glycol ethyl ether, ethylene glycol monomethyl ether acetate, benzinum, turpentine oil, the terpinol.
3. the environment-friendly type semiconductor capacitor according to claim 1 preparation method of electrode silver plasm, it is characterized in that the diluent among the described step D comprises one or more mixtures with arbitrary proportion in butyl carbitol, 1-Methoxy-2-propyl acetate, ethylene glycol ethyl ether, ethylene glycol monomethyl ether acetate, benzinum, turpentine oil, terpinol, castor oil, the cyclohexanone.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102903422A (en) * | 2012-10-23 | 2013-01-30 | 广东风华高新科技股份有限公司 | Silk print full-silver-end electrode slurry for capacitor |
| CN103165217A (en) * | 2011-12-14 | 2013-06-19 | 上海宝银电子材料有限公司 | Electric conduction silver paste for mica plate capacitor and preparation method thereof |
| CN103390443A (en) * | 2013-06-25 | 2013-11-13 | 彩虹集团电子股份有限公司 | Lead-free electrode silver paste for semiconductive ceramic capacitors and preparation method of lead-free electrode silver paste |
| CN107545945A (en) * | 2017-07-03 | 2018-01-05 | 杭州正祺新材料有限公司 | A kind of capacitor electrode film encapsulation electrocondution slurry and its manufacture method |
| CN111362690A (en) * | 2020-03-17 | 2020-07-03 | 东北大学秦皇岛分校 | Preparation method of bismuth ferrite-barium titanate composite piezoelectric ceramic |
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| SU494369A1 (en) * | 1973-07-30 | 1975-12-05 | Предприятие П/Я М-5457 | Ceramic material |
| CN101094818A (en) * | 2004-05-29 | 2007-12-26 | 肖特股份公司 | Nano glass powder and use thereof, particularly multicomponent glass powder with a mean particle size of less than 1 [mu]m |
| CN101720311A (en) * | 2007-06-29 | 2010-06-02 | E.I.内穆尔杜邦公司 | Conductor paste for ceramic substrate and electric circuit |
| CN101777423A (en) * | 2010-03-16 | 2010-07-14 | 彩虹集团公司 | Preparation method of electrode paste for environment protective ceramic capacitor |
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2011
- 2011-03-28 CN CN 201110075889 patent/CN102157221A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| SU494369A1 (en) * | 1973-07-30 | 1975-12-05 | Предприятие П/Я М-5457 | Ceramic material |
| CN101094818A (en) * | 2004-05-29 | 2007-12-26 | 肖特股份公司 | Nano glass powder and use thereof, particularly multicomponent glass powder with a mean particle size of less than 1 [mu]m |
| CN101720311A (en) * | 2007-06-29 | 2010-06-02 | E.I.内穆尔杜邦公司 | Conductor paste for ceramic substrate and electric circuit |
| CN101777423A (en) * | 2010-03-16 | 2010-07-14 | 彩虹集团公司 | Preparation method of electrode paste for environment protective ceramic capacitor |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103165217A (en) * | 2011-12-14 | 2013-06-19 | 上海宝银电子材料有限公司 | Electric conduction silver paste for mica plate capacitor and preparation method thereof |
| CN102903422A (en) * | 2012-10-23 | 2013-01-30 | 广东风华高新科技股份有限公司 | Silk print full-silver-end electrode slurry for capacitor |
| CN102903422B (en) * | 2012-10-23 | 2015-06-17 | 广东风华高新科技股份有限公司 | Silk print full-silver-end electrode slurry for capacitor |
| CN103390443A (en) * | 2013-06-25 | 2013-11-13 | 彩虹集团电子股份有限公司 | Lead-free electrode silver paste for semiconductive ceramic capacitors and preparation method of lead-free electrode silver paste |
| CN107545945A (en) * | 2017-07-03 | 2018-01-05 | 杭州正祺新材料有限公司 | A kind of capacitor electrode film encapsulation electrocondution slurry and its manufacture method |
| CN111362690A (en) * | 2020-03-17 | 2020-07-03 | 东北大学秦皇岛分校 | Preparation method of bismuth ferrite-barium titanate composite piezoelectric ceramic |
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Application publication date: 20110817 |