CN103366858A - Silver paste for LED (Light-Emitting Diode) lamp aluminum oxide base and application thereof - Google Patents

Silver paste for LED (Light-Emitting Diode) lamp aluminum oxide base and application thereof Download PDF

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Publication number
CN103366858A
CN103366858A CN2013102856712A CN201310285671A CN103366858A CN 103366858 A CN103366858 A CN 103366858A CN 2013102856712 A CN2013102856712 A CN 2013102856712A CN 201310285671 A CN201310285671 A CN 201310285671A CN 103366858 A CN103366858 A CN 103366858A
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China
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silver
aluminium oxide
led lamp
powder
oxide pedestal
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CN2013102856712A
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CN103366858B (en
Inventor
谭汝泉
宋先刚
王惠敏
娄红涛
黄道君
彭梅志
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GUANGDONG LINGGUANG NEW MATERIAL CO Ltd
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GUANGDONG LINGGUANG NEW MATERIAL CO Ltd
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Abstract

The invention discloses silver paste for an LED (Light-Emitting Diode) lamp aluminum oxide base and an application thereof. The silver paste consists of the following components in percentage by weight: 50-80 percent of ultrafine silver powder, 2-10 percent of silver alloy powder, 2-10 percent of glass powder, 1-10 percent of inorganic additive, 2-15 percent of macromolecule resin, 10-40 percent of solvent and 1-10 percent of organic additive. The silver paste for the LED aluminum oxide base disclosed by the invention is used for preparing an aluminum oxide base circuit board, has the advantages of high printing performance and continuous and bright silver surface after sintering, and has high adhesion force, excellent electric performance and high-temperature welding resistance after being sintered.

Description

A kind of LED lamp aluminium oxide pedestal is starched and is used with silver
Technical field
The present invention relates to field of electronic materials, particularly a kind of LED lamp aluminium oxide pedestal is starched and is used with silver.
Background technology
The electronic silver slurry is to be a kind of electric conducting material that dip-coating and silk screen process use in the electronics industry, is set electron, chemical industry, metallurgical Trinitarian high-tech product, is one of main foundation material in the electronics industry.The present invention is the basic material of LED lamp aluminium oxide pedestal wiring board, and the silver slurry is through techniques such as silk screen printing, levelling, oven dry, sintering, and sintering forms conducting film on alumina substrate, makes the wiring board of LED lamp.The wiring board that present LED lamp adopts mostly is the PCB wiring board, the radiating effect of this wiring board is relatively poor, reduced widely the useful life of LED lamp, and adopt the wiring board of aluminium oxide ceramics pedestal printing can solve well heat dissipation problem, electric conductivity is also very excellent, and then improves the useful life of LED lamp.
Along with the wiring board of LED lamp gradually to the development of aluminium oxide pedestal wiring board, market can be increasing with the demand of silver slurry to LED lamp aluminium oxide pedestal, has good market prospects therefore LED lamp aluminium oxide pedestal is starched with silver.And LED lamp aluminium oxide pedestal requires the silver slurry to have good electrical property, high temperature soldering resistance, high adhesion force behind sintering with silver slurry, and this is several technological difficulties of LED silver slurry exploitation, and at present domestic also do not have enterprise can produce LED aluminium oxide pedestal with the silver slurry.
Summary of the invention
For overcoming shortcoming of the prior art, the invention provides a kind of LED lamp aluminium oxide pedestal and starch with silver, it has good electrical property, high temperature soldering resistance and high adhesion force.
Another object of the present invention provides the application that above-mentioned LED lamp aluminium oxide pedestal is starched with silver.
In order to solve the problems of the technologies described above, the present invention is achieved by the following technical solutions: a kind of LED lamp aluminium oxide pedestal is starched with silver, count by weight percentage, prescription forms and comprises following component: super fine silver powder 50~80%, alloy for dental amalgam 2~10%, glass dust 2~10%, inorganic additive 1~10%, macromolecule resin 2~15%, solvent 10~40%, organic additive 1~10%.
Described super fine silver powder be purity greater than 99.95%, granularity is less than the powder of the spherical of 10 μ m or nearly ball-type.
Described alloy for dental amalgam is selected from one or more in silver-bearing copper powder, silver-colored palladium powder, silver-colored nickel powder, the silver-colored titanium valve.
Described glass dust is B 2O 3-SiO 2-Bi 2O 3-Al 2O 3-Mn 2O 3Glass system; Preferably, described B 2O 3-SiO 2-Bi 2O 3-Al 2O 3-Mn 2O 3In the glass system: B 2O 35~30Wt%, SiO 25~25Wt%, Bi 2O 340~85Wt%, Al 2O 32~20Wt%, Mn 2O 35~15Wt%, glass transition temperature is 650~700 ℃.
Described inorganic additive is selected from Fe 2O 3, ZrO, TiO 2, Nb 2O 5, V 2O 5In one or more.
Described macromolecule resin is selected from one or more in ethyl cellulose, acrylic resin, the polyvinyl alcohol resin.
Described solvent is the ester class, and in the ethers, alcohols, hydrocarbon compound at least a kind.
Described organic additive is selected from one or both mixing in organosilicon-modified acrylate or the polyacrylate.
Above-mentioned LED lamp aluminium oxide pedestal is starched in the application for preparing on the aluminium oxide pedestal wiring board with silver.
Above-mentioned application is characterized in that: LED lamp aluminium oxide pedestal descended dry 1-6 minute at 200-250 ℃ after being printed on the aluminium oxide pedestal with the silver slurry, carried out sintering, 800 ℃~830 ℃ of the highest sintering temperatures again.
Silver slurry of the present invention has good printing performance in the high solids content situation, silver-colored face continuously behind the sintering, bright, adhesive force is high, have good electrical property and high temperature soldering resistance.
Embodiment
The present invention is that a kind of LED lamp aluminium oxide pedestal is starched with silver, count by weight percentage, prescription forms and comprises following component: super fine silver powder 50~80%, alloy for dental amalgam 2~10%, glass dust 2~10%, inorganic additive 1~10%, macromolecule resin 2~15%, solvent 10~40%, organic additive 1~10%.
Described super fine silver powder is that commercially available purity is greater than 99.95%, granularity is less than the powder of the spherical or nearly ball-type of 10 μ m, have good dispersion, high-tap density, can make slurry that good rheological property is arranged, effective control electrode bed thickness is thin, raising electrode surface evenness, and there are good compactness and glossiness in dry rear electrode surface, and sintering shrinkage is little, have good conductivity, guarantee that silver-colored face is continuous, bright, adhesive force is high, electrical property is excellent.In the prescription, super fine silver powder 50~80%, preferred 60~80%, more preferably 65~75%.
Described alloy for dental amalgam is selected from one or more in commercially available silver-bearing copper powder, silver-colored palladium powder, silver-colored nickel powder, the silver-colored titanium valve.Alloyed powder requires good dispersion, granularity less than the powder of the spherical or nearly ball-type below the 10 μ m.The present invention forms on the basis of (silver powder, glass dust, organic carrier) at the conventional silver slurry formula, added innovatively alloy for dental amalgam, regulate silver slurry high temperature soldering resistance and electrical property by it, making behind the silver slurry sintering can be 480 ℃ of welding, and has extremely low resistance.Described glass dust is the inorganic bond phase, preferred B 2O 3-SiO 2-Bi 2O 3-Al 2O 3-Mn 2O 3Glass system, preferred, B 2O 3-SiO 2-Bi 2O 3-Al 2O 3-Mn 2O 3In the glass system: B 2O 35~30Wt%, SiO 25~25Wt%, Bi 2O 340~85Wt%, Al 2O 32~20Wt%, Mn 2O 35~15Wt%, glass transition temperature is 650~700 ℃.During preparation, each component is mixed with jar mill in proportion, 430-470 ℃ of preheating 20-40min, 1150-1250 ℃ of melting 50-70min quenches, ball milling to granularity less than 5 μ m, filtering drying gets final product.The used glass powder of the present invention is not leaded, cadmium and compound thereof, meets the environmental requirement of the RoHS of European Union.In the prescription, glass dust 2~10%, preferred 3~8%, more preferably 3~6%.
Described inorganic additive is selected from Fe 2O 3, ZrO, TiO 2, Nb 2O 5, V 2O 5In one or more, improved mechanical strength and the chemical stability of glass, also guaranteed electrical property and the chemical property of glass, be convenient to rete and be attached on the substrate securely at silver layer behind the sintering.Have high adhesion force behind the present invention's silver slurry sintering, adhesive force is greater than 50N.
The organic carrier that macromolecule resin, organic solvent and organic additive etc. form can satisfy the silk-screen printing technique requirement of slurry in LED lamp aluminium oxide pedestal.Behind the organic carrier drying sintering, can be completely decomposed of volatile, can not have residue, bring negative effect to product.Wherein:
Described macromolecule resin is selected from one or more in ethyl cellulose, acrylic resin, the polyvinyl alcohol resin, selects according to the powder body material that reality is used.
Described solvent is the lower ester class of toxicity, and in the ethers, alcohols, hydrocarbon compound at least a kind, make it have difficult volatilization under the low temperature, volatile characteristic under the high temperature, can conveniently in printing process, keep good printing performance like this, after guaranteeing silver slurry sintering, the smooth gloss of silver layer surface, pore-free.Wherein lipid is for must add class, and it can give the silver slurry good lubrification, guarantees the printing performance of silver slurry; More than at least a kind, be used for adjusting silver slurry sintering character in ethers, alcohols, the hydrocarbon compound, behind the assurance silver slurry sintering, the smooth gloss of silver layer surface, pore-free.Applicable ester class, ethers, alcohols, hydrocarbon compound can be selected from fat hydrocarbon solvent, tasteless gasoline, mixed type dibasic acid dimethyl ester such as DBE, terpinol, ethyl oleate, diethylene glycol butyl ether, repefral, diethylene glycol ether amyl acetate, diethylene glycol butyl ether amyl acetate etc.
Described organic additive is selected from one or both mixing in organosilicon-modified acrylate or the polyacrylate.The present invention has added organosilicon-modified acrylate, polyacrylate surfactant in organic carrier, allow organic carrier abundant wetting parcel inoganic solids in rolling the slurry process, make silver powder and glass dust reach sufficient dispersion, improve the dispersiveness of solid powder, the flowability of slurry, whole fineness with the silver slurry is controlled at below the 10 μ m simultaneously, guarantee that the silver slurry in the high solids content situation, has good printing performance, form required figure on the substrate so that slurry is transferred to.
Below the present invention is further elaborated by concrete example, but the present invention is not limited to this specific examples.
Embodiment 1
1, the preparation of glass dust
B by mass percentage 2O 315Wt%, SiO 215Wt%, Bi 2O 360Wt%, Al 2O 33.5Wt%, Mn 2O 35Wt%, ZrO1.5%.Mix with jar mill, 450 ° of C preheating 30min, 1200 ° of C melting 60min quench, ball milling to granularity less than 5 μ m, filtering drying.
2, the preparation of organic carrier
Ethyl cellulose 20%, terpinol 30%, diethylene glycol butyl ether 30%, ethyl oleate 10%, organosilicon-modified acrylate 10% after above each thing mixes, 80 ~ 100 ° of C heating for dissolving, gets transparent glue.
3, mix 73% super fine silver powder, 2% palladium-silver alloy powder, 4% glass dust, 1%TiO 2, be made into powder, after stirring, add 20% organic carrier, after the high speed dispersion, through three-high mill be rolled to fineness less than 10 μ m below, add diluent, adjust viscosity.
Embodiment 2
1, the preparation of glass dust
B by mass percentage 2O 310Wt%, SiO 220Wt%, Bi 2O 355Wt%, Al 2O 35Wt%, Mn 2O 38Wt%, ZrO2%.Mix with jar mill, 450 ° of C preheating 30min, 1200 ° of C melting 60min quench, ball milling to granularity less than 5 μ m, filtering drying.
2, the preparation of organic carrier
Ethyl cellulose 25%, terpinol 45%, diethylene glycol butyl ether amyl acetate 20%, polyacrylate 10% after above each thing mixes, 80~100 ° of C heating for dissolving, gets transparent glue.
3, mix 69% super fine silver powder, 9% yellow gold powder, 4% glass dust, 1%Nb 2O 5, be made into powder, after stirring, add 17% organic carrier, after the high speed dispersion, through three-high mill be rolled to fineness less than 10 μ m below, add diluent, adjust viscosity.
Embodiment 3
1, the preparation of glass dust
B by mass percentage 2O 310Wt%, SiO 215Wt%, Bi 2O 365Wt%, Al 2O 32Wt%, Mn 2O 36Wt%, ZrO2%.Mix with jar mill, 450 ° of C preheating 30min, 1200 ° of C melting 60min quench, ball milling to granularity less than 5 μ m, filtering drying.
3, the preparation of organic carrier
Ethyl cellulose 15%, diethylene glycol ether amyl acetate 22%, diethylene glycol butyl ether 43%, repefral 10%, organosilicon-modified acrylate 10% after above each thing mixes, 80 ~ 100 ° of C heating for dissolving, gets transparent glue.
4, mix 75% super fine silver powder, 5% silver-nickel powder, 5% glass dust, 1%Nb 2O 5, be made into powder, after stirring, add 14% organic carrier, after the high speed dispersion, through three-high mill be rolled to fineness less than 10 μ m below, add diluent, adjust viscosity.
Experimental example
The silver slurry using method of embodiment 1-3:
1. silk screen printing (is annotated: standard printing condition: mesh: 250 orders) on alumina substrate
2.. drying condition: 230 ℃ 3 minutes
3.. sintering condition: sintering temperature: 800 ℃ ~ 830 ℃
Sintering condition in this experimental example: the highest 810 ℃, kept 10 minutes the high-temperature region, 60 minutes altogether.
4.. carry out performance test behind the sintering, corresponding product is randomly drawed 10, and the soldering resistance method of testing is pressed GB/T17473.7-2008 and implemented, and the adhesive force test is pressed GB/T17473.4-2008 and implemented, and the sheet resistance test is pressed GB/T17473.3-2008 and implemented.Data such as table 1.
Table 1.

Claims (10)

1. a LED lamp aluminium oxide pedestal is starched with silver, count by weight percentage, prescription forms and comprises following component: super fine silver powder 50~80%, alloy for dental amalgam 2~10%, glass dust 2~10%, inorganic additive 1~10%, macromolecule resin 2~15%, solvent 10~40%, organic additive 1~10%.
2. LED lamp aluminium oxide pedestal according to claim 1 is characterized in that with the silver slurry: described super fine silver powder be purity greater than 99.95%, granularity is less than the powder of the spherical or nearly ball-type of 10 μ m.
3. LED lamp aluminium oxide pedestal according to claim 1 is starched with silver, and it is characterized in that: described alloy for dental amalgam is selected from one or more in silver-bearing copper powder, silver-colored palladium powder, silver-colored nickel powder, the silver-colored titanium valve.
4. LED lamp aluminium oxide pedestal according to claim 1 is starched with silver, and it is characterized in that: described glass dust is B 2O 3-SiO 2-Bi 2O 3-Al 2O 3-Mn 2O 3Glass system; Preferably, described B 2O 3-SiO 2-Bi 2O 3-Al 2O 3-Mn 2O 3In the glass system: B 2O 35~30Wt%, SiO 25~25Wt%, Bi 2O 340~85Wt%, Al 2O 32~20Wt%, Mn 2O 35~15Wt%, glass transition temperature is 650~700 ℃.
5. LED lamp aluminium oxide pedestal according to claim 1 is starched with silver, and it is characterized in that: described inorganic additive is selected from Fe 2O 3, ZrO, TiO 2, Nb 2O 5, V 2O 5In one or more.
6. LED lamp aluminium oxide pedestal according to claim 1 is starched with silver, and it is characterized in that: described macromolecule resin is selected from one or more in ethyl cellulose, acrylic resin, the polyvinyl alcohol resin.
7. LED lamp aluminium oxide pedestal according to claim 1 is with the silver slurry, and it is characterized in that: described solvent is the ester class, and in the ethers, alcohols, hydrocarbon compound at least a kind.
8. LED lamp aluminium oxide pedestal according to claim 1 is starched with silver, and it is characterized in that: described organic additive is selected from one or both mixing in organosilicon-modified acrylate or the polyacrylate.
9. the described LED lamp of arbitrary claim aluminium oxide pedestal is starched in the application for preparing on the aluminium oxide pedestal wiring board with silver among the claim 1-8.
10. application according to claim 9 is characterized in that: LED lamp aluminium oxide pedestal descended dry 1-6 minute at 200-250 ℃ after being printed on the aluminium oxide pedestal with the silver slurry, carried out sintering, 800 ℃~830 ℃ of the highest sintering temperatures again.
CN201310285671.2A 2013-07-08 2013-07-08 A kind of LED aluminium oxide pedestal silver slurry and application thereof Active CN103366858B (en)

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Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1049675A (en) * 1990-03-06 1991-03-06 北京市印刷技术研究所 Conductive printing ink of copper series
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
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
CN102222536A (en) * 2011-03-28 2011-10-19 彩虹集团公司 Environment-friendly silver conductive paste for surface mounting of semiconductor chips and preparation method of environment-friendly silver conductive paste
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
CN102569603A (en) * 2012-01-13 2012-07-11 张家港市金港镇东南电子厂 Light emitting diode (LED) ceramic substrate and production method thereof
JP2013041683A (en) * 2011-08-11 2013-02-28 Tamura Seisakusho Co Ltd Conductive material

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1049675A (en) * 1990-03-06 1991-03-06 北京市印刷技术研究所 Conductive printing ink of copper series
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
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
CN102222536A (en) * 2011-03-28 2011-10-19 彩虹集团公司 Environment-friendly silver conductive paste for surface mounting of semiconductor chips and preparation method of environment-friendly silver conductive paste
JP2013041683A (en) * 2011-08-11 2013-02-28 Tamura Seisakusho Co Ltd Conductive material
CN102569603A (en) * 2012-01-13 2012-07-11 张家港市金港镇东南电子厂 Light emitting diode (LED) ceramic substrate and production 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

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Denomination of invention: Silver paste for LED (Light-Emitting Diode) lamp aluminum oxide base and application thereof

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