CN101719395B - Macromolecular solution dispersing medium with complete combustion and volatilization for dispensing organic powder - Google Patents
Macromolecular solution dispersing medium with complete combustion and volatilization for dispensing organic powder Download PDFInfo
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- CN101719395B CN101719395B CN 200810167514 CN200810167514A CN101719395B CN 101719395 B CN101719395 B CN 101719395B CN 200810167514 CN200810167514 CN 200810167514 CN 200810167514 A CN200810167514 A CN 200810167514A CN 101719395 B CN101719395 B CN 101719395B
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- dispersing medium
- butyl carbitol
- ethyl acetate
- decentralized medium
- volatilization
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Abstract
The invention relates to a macromolecular solution dispersing medium with complete combustion and volatilization for dispensing organic powder. The dispersing medium has the composition characteristic that nitrocellulose or ethylcellulose is dissolved in single solvent or mixing solvent of ethyl acetate, terpilenol, butyl carbitol, butyl carbitol acetate and the like; auxiliaries of organic silicon block copolymer hyper-dispersant, defoamer and the like are added, and then a macromolecular solution is formed and used as the dispersing medium of the organic powder to prepare electronic slurry. The dispersing medium has the property characteristic that the electronic slurry has good uniform dispersing stability and rheology for easy forming, and the temperature can be reduced to 290 D during high-temperature sintering for manufacturing electronic components; after the temperature is held for 10 minutes in air, the dispersing medium can combust and volatize more than 99.99% of the original weight.
Description
Technical field
But the present invention relates to a kind of organic toughness Polymer Solution decentralized medium of the completing combustion volatilization for disperseing inorganic particle.Be used for making the paste electric slurry, this electric slurry is being made in the electronic devices and components process through high temperature sintering, can be low to moderate 290 ℃, insulation is after 10 minutes in the air, and the organic polymer solution decentralized medium can burn its initial quality mark of volatilization more than 99.99%.Stop behind the electric slurry sintering residual carbon to the impact of electronic devices and components performance.Belong to the electronic devices and components field of electronic materials.
Background technology
The inorganic particle that often needs to have the functions such as light, heat, electricity, magnetic in various electronic devices and components, sensitive function components and parts (photosensitive, wet sensitive, air-sensitive) and the various photoelectric display device manufacturing process is made into slurry, be convenient to adopt silk screen printing or painting method to be shaped to the needed shape of device, then solidify preparation function electronic devices and components through high-temperature sintering process.In making the slurry process, various inorganic functional powders need to be dispersed in organic toughness Polymer Solution.Organic toughness Polymer Solution is usually by macromolecule and the solvent composition of thickening.Different according to adopting high molecular kind, molecular weight, usually after the high temperature sintering cooling, macromolecule can not the completing combustion volatilization, and it is that 1% to 10% residual carbon exists that mass fraction is arranged, and residual carbon will make the electronic devices and components performance degradation.Polymer Solution decentralized medium disclosed by the invention can be low to moderate 290 ℃, and insulation is after 10 minutes in the air, and the organic polymer solution decentralized medium can burn its initial quality of volatilization more than 99.99%.Substantially solved behind the slurry sintering residual carbon to the problem of components and parts performance impact.
University Of Tianjin's publication number be CN1870310 patent disclosure a kind of with particle diameter less than the 100nm nano silver particles, under ultrasonic water bath is assisted, evenly be mixed with the nano mattisolda that forms with dispersant fish oil, binding agent alpha-terpineol and solvent acetone.Do not have macromolecule or polymer in its used decentralized medium, the silver paste that will cause making is difficult to stablize in a long time, and its printability has no evaluation.
Advantage of the present invention is: adopt nitrocellulose and ethyl cellulose as thickener, both guaranteed that slurry had good dispersion stabilization and silk screen printing adaptive, can stop again the residual of carbon behind the slurry sintering, guarantee the performance of prepared electronic devices and components.
Summary of the invention
Be that 1% to 15% nitrocellulose is dissolved in the mixed solvent of independent ethyl acetate or ethyl acetate and terpinol, butyl carbitol, turpentine oil, butyl carbitol acetate, repefral, dibutyl phthalate etc. with mass percent, adding the auxiliary agents such as organic silicon block copolymer class hyper-dispersant and defoamer, namely is the decentralized medium that can be used for disperseing inorganic particle of indication among the present invention.
Be that 1% to 15% ethyl cellulose is dissolved in the mixed solvents such as independent terpinol or terpinol and ethyl acetate, butyl carbitol, turpentine oil, butyl carbitol acetate, repefral, dibutyl phthalate with mass percent, adding the auxiliary agents such as organic silicon block copolymer class hyper-dispersant and defoamer, namely is the decentralized medium that can be used for disperseing inorganic particle of indication among the present invention.
The invention has the beneficial effects as follows: (1) is compared with the decentralized medium that without macromolecule is thickener take macromolecule nitrocellulose or ethyl cellulose as the thickener of solution.When being used for dispersing nanometer or micron inorganic particle, have better Uniform Dispersion stability and the rheological characteristic of being convenient to moulding.(2) compare as the decentralized medium of the thickener of solution with adopting other macromolecule, it has the almost nil characteristics of residual carbon behind the high temperature sintering, has stopped the impact of residual carbon on the electronic devices and components performance.
Embodiment
The invention will be further described by following specific embodiment.
Embodiment 1
Make the transparent dielectric paste of plasma scope prebasal plate.The plasma scope prebasal plate need to be made the visible transparent glassy layer that a layer thickness is the 10-20 micron thickness, requires the film surface evenness high, and visible light transmissivity is more high better.
With satisfactory medium glass powder levigate to average grain diameter be 3 microns, the largest particles particle diameter is less than 10 microns.
Be that 5% nitrocellulose is dissolved in the mixed solvent of ethyl acetate or ethyl acetate and butyl carbitol, dibutyl phthalate (mass ratio is 50:25:25) with mass percent.Adding accounts for the organic silicon block copolymer hyper-dispersant of solvent quality 2% and 2% defoamer is mixed with homogeneous solution, is indication decentralized medium of the present invention.With mass fraction be 75% medium glass powder to be dispersed in mass fraction be in 25% the decentralized medium, being uniformly dispersed with three-roll grinder is prepared into dielectric paste.The typical shear shinning body of the rheological behavior of slurry has good silk screen printing adaptive.To glass substrate, be under 580 ℃ at peak temperature with the slurry silk screen printing then, 15 minutes sintering of insulation in the air after the cooling, are measured the visible light mean transmissivity of glass greater than 87%, and evenness meets the demands behind the dielectric layer sintering of printing.Contain mass percent less than 0.001% with residual carbon in ICP-AES (inductively coupled plasma-atomic emission spectrum) the analysis glass medium layer.
Another example is to be that 4% ethyl cellulose is dissolved in the mixed solvent of terpinol or terpinol and butyl carbitol acetate, repefral (mass ratio is 50:25:25) with mass percent.Adding accounts for the organic silicon block copolymer hyper-dispersant of solvent quality 4% and 2% defoamer is mixed with homogeneous solution, also is indication decentralized medium of the present invention.With mass fraction be 78% medium glass powder to be dispersed in mass fraction be in 22% the decentralized medium, being uniformly dispersed with three-roll grinder is prepared into dielectric paste.The typical shear shinning body of the rheological behavior of slurry has good silk screen printing adaptive.To glass substrate, be under 585 ℃ at peak temperature with the slurry silk screen printing then, 10 minutes sintering of insulation in the air after the cooling, are measured the visible light mean transmissivity of broken glass greater than 87%, and evenness meets the demands behind the dielectric layer sintering of printing.Contain mass percent less than 0.001% with residual carbon in ICP-AES (inductively coupled plasma-atomic emission spectrum) the analysis glass medium layer.
The present invention's advantage in the present embodiment is: (1) slurry has the evenness that fine rheological characteristic has guaranteed the transparent dielectric layer of made.(2) residual carbon is almost nil behind the sintering has guaranteed very high visible light transmissivity.
Embodiment 2
Make nano-silver conductive slurry.
Inorganic particle be the particle maximum particle diameter less than 100 nanometers, average grain diameter is the silver powder of 60 nanometers.
Be that 5% nitrocellulose is dissolved in the mixed solvent of ethyl acetate or ethyl acetate and butyl carbitol acetate, repefral (mass ratio is 50:25:25) with mass percent.Adding accounts for the organic silicon block copolymer hyper-dispersant of solvent quality 6% and 2% defoamer is mixed with homogeneous solution, is indication decentralized medium of the present invention.With mass fraction be 75% nano-silver powder to be dispersed in mass fraction be in 25% the decentralized medium, being uniformly dispersed with three-roll grinder is prepared into nano-silver conductive slurry.The typical shear shinning body of the rheological behavior of slurry has good silk screen printing adaptive.Slurry silk screen printing to surface is had on the monocrystalline silicon substrate of Gold plated Layer, is under 290 ℃ at peak temperature then, 10 minutes sintering of insulation in the air, the organic polymer solution decentralized medium volatilizees substantially fully, after the cooling, the pure white densification of silver-colored sintered membrane is adhered to well with Gold plated Layer.Contain mass percent less than 0.01% with residual carbon in ICP-AES (inductively coupled plasma-atomic emission spectrum) the analysis silver layer.
Another example is to be that 6% ethyl cellulose is dissolved in (mass ratio is 75:25) in terpinol or terpinol and the butyl carbitol mixed solvent with mass percent.Adding accounts for the organic silicon block copolymer hyper-dispersant of solvent quality 5% and 2% defoamer is mixed with homogeneous solution, also is indication decentralized medium of the present invention.With mass fraction be 76% nano-silver powder to be dispersed in mass fraction be in 24% the decentralized medium, being uniformly dispersed with three-roll grinder is prepared into dielectric paste.The typical shear shinning body of the rheological behavior of slurry has good silk screen printing adaptive.Slurry silk screen printing to surface is had on the monocrystalline silicon substrate of Gold plated Layer, is under 300 ℃ at peak temperature then, 10 minutes sintering of insulation in the air, the organic polymer solution decentralized medium volatilizees substantially fully, after the cooling, the pure white densification of silver-colored sintered membrane is adhered to well with Gold plated Layer.Contain mass percent less than 0.01% with residual carbon in ICP-AES (inductively coupled plasma-atomic emission spectrum) the analysis silver layer.
In the present embodiment, advantage of the present invention is:
Different according to the binding agent that adheres to silver powder, the silver slurry can be divided into two large classes: a class is with the at high temperature melting of low-melting-point glass powder silver powder to be sticked on the base material; Another kind of is at a lower temperature silver powder to be sticked on the base material with macromolecule generation hot curing cross-linking reactions such as epoxy or polyester.
In the present embodiment, because requirement on devices, can not residual any non-silver components in the silver layer of made, and element manufacturing should not adopt evaporation or various gas-phase deposition to make silver film, can only make of thick-film technique, sintering temperature can not be higher than 300 ℃, in case other parts high temperature that completes first in the device technology is impaired.Although silver point is about 960 ℃, according to bibliographical information, the fusing point of nano-silver powder can be low to moderate about 100 ℃.Present embodiment is exactly nano-silver powder to be dispersed in the decentralized medium of indication of the present invention be prepared into slurry, by silk screen printing, is being lower than 290 ℃, in the air behind 10 minutes sintering of insulation, organic dispersion medium volatilizees substantially fully, and residual carbon is almost nil in the silver-colored sintered body, has guaranteed performance of devices.If adopting other macromolecule is the decentralized medium of thickener, at 300 ℃, behind 10 minutes sintering of insulation, higher carbon is residual with having in the air, thus affect silver-colored sinter layer compactness and with the adhesive strength of Gold plated Layer, affect performance of devices.
Above embodiment only is illustrative rather than definitive thereof technical scheme of the present invention, it will be appreciated by those skilled in the art that, technical scheme of the present invention is carried out various changes and equivalence replacement, and do not deviate from principle and the scope of technical solution of the present invention, all should be encompassed among the scope of claim of the present invention.
Claims (3)
1. but the Polymer Solution decentralized medium of completing combustion volatilization, be used for disperseing inorganic particle to make the paste electric slurry, its composition is (mass percent): nitrocellulose, 1-15, all the other are organic silicon block copolymer class hyper-dispersant, the mixed solvent of defoamer and independent ethyl acetate or ethyl acetate and terpinol, butyl carbitol, turpentine oil, butyl carbitol acetate, repefral, dibutyl phthalate.
2. described Polymer Solution decentralized medium according to claim 1, it is characterized in that: nitrocellulose is dissolved in the toughness solution that organic solvent forms, and organic solvent is the mixed solvent of independent ethyl acetate or ethyl acetate and terpinol, butyl carbitol, turpentine oil, butyl carbitol acetate, repefral, dibutyl phthalate.
3. Polymer Solution decentralized medium according to claim 1 is characterized in that: be incubated 10 minutes and namely volatilize its initial quality mark more than 99.99% in being low to moderate 290 ℃ of lower air.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200810167514 CN101719395B (en) | 2008-10-09 | 2008-10-09 | Macromolecular solution dispersing medium with complete combustion and volatilization for dispensing organic powder |
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| Application Number | Priority Date | Filing Date | Title |
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| CN 200810167514 CN101719395B (en) | 2008-10-09 | 2008-10-09 | Macromolecular solution dispersing medium with complete combustion and volatilization for dispensing organic powder |
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| Publication Number | Publication Date |
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| CN101719395A CN101719395A (en) | 2010-06-02 |
| CN101719395B true CN101719395B (en) | 2013-04-24 |
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| CN 200810167514 Expired - Fee Related CN101719395B (en) | 2008-10-09 | 2008-10-09 | Macromolecular solution dispersing medium with complete combustion and volatilization for dispensing organic powder |
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Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102646459A (en) * | 2012-05-23 | 2012-08-22 | 湖南利德电子浆料有限公司 | Silver paste for front face of mixed silver powder crystalline silicon based solar battery and preparation method thereof |
| WO2015015833A1 (en) * | 2013-07-29 | 2015-02-05 | 株式会社村田製作所 | Internal electrode paste |
| CN104183335A (en) * | 2014-09-17 | 2014-12-03 | 北京印刷学院 | Method for fast sintering printing nano-silver paste at low temperature through laser to form pure-silver conductive image and text |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1182941A (en) * | 1996-06-25 | 1998-05-27 | 纳幕尔杜邦公司 | Conducting composition used as end electrode of sheet resistance |
| CN1285599A (en) * | 1999-06-30 | 2001-02-28 | 太阳诱电株式会社 | Method for making packed ceramic electronic element |
| CN1518007A (en) * | 2003-01-24 | 2004-08-04 | E.I.���¶��Ű˾ | Terminal electrod composition for multilayer ceramic capacitor |
| CN1710668A (en) * | 2005-07-22 | 2005-12-21 | 张振中 | Metal NiCr function thick-film electronic slurry |
| EP1468766B1 (en) * | 2001-06-14 | 2006-08-23 | Toho Titanium Co., Ltd. | Method for producing metal powder |
| US7128870B2 (en) * | 1999-06-30 | 2006-10-31 | Taiyo Yuden Co., Ltd. | Method for the manufacture of multilayer ceramic electronic component |
-
2008
- 2008-10-09 CN CN 200810167514 patent/CN101719395B/en not_active Expired - Fee Related
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1182941A (en) * | 1996-06-25 | 1998-05-27 | 纳幕尔杜邦公司 | Conducting composition used as end electrode of sheet resistance |
| CN1285599A (en) * | 1999-06-30 | 2001-02-28 | 太阳诱电株式会社 | Method for making packed ceramic electronic element |
| US7128870B2 (en) * | 1999-06-30 | 2006-10-31 | Taiyo Yuden Co., Ltd. | Method for the manufacture of multilayer ceramic electronic component |
| EP1468766B1 (en) * | 2001-06-14 | 2006-08-23 | Toho Titanium Co., Ltd. | Method for producing metal powder |
| CN1518007A (en) * | 2003-01-24 | 2004-08-04 | E.I.���¶��Ű˾ | Terminal electrod composition for multilayer ceramic capacitor |
| CN1710668A (en) * | 2005-07-22 | 2005-12-21 | 张振中 | Metal NiCr function thick-film electronic slurry |
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