CN103366858B - A kind of LED aluminium oxide pedestal silver slurry and application thereof - Google Patents

A kind of LED aluminium oxide pedestal silver slurry and application thereof Download PDF

Info

Publication number
CN103366858B
CN103366858B CN201310285671.2A CN201310285671A CN103366858B CN 103366858 B CN103366858 B CN 103366858B CN 201310285671 A CN201310285671 A CN 201310285671A CN 103366858 B CN103366858 B CN 103366858B
Authority
CN
China
Prior art keywords
silver
aluminium oxide
oxide pedestal
silver slurry
powder
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Active
Application number
CN201310285671.2A
Other languages
Chinese (zh)
Other versions
CN103366858A (en
Inventor
谭汝泉
宋先刚
王惠敏
娄红涛
黄道君
彭梅志
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
GUANGDONG LINGGUANG NEW MATERIAL CO Ltd
Original Assignee
GUANGDONG LINGGUANG NEW MATERIAL CO Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by GUANGDONG LINGGUANG NEW MATERIAL CO Ltd filed Critical GUANGDONG LINGGUANG NEW MATERIAL CO Ltd
Priority to CN201310285671.2A priority Critical patent/CN103366858B/en
Publication of CN103366858A publication Critical patent/CN103366858A/en
Application granted granted Critical
Publication of CN103366858B publication Critical patent/CN103366858B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Abstract

The invention discloses a kind of LED aluminium oxide pedestal silver slurry and application thereof, count by weight percentage, silver-colored slurry formula composition 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%.LED aluminium oxide pedestal silver slurry of the present invention is applied in prepares aluminium oxide pedestal wiring board, has good printing performance, after sintering, silver-colored face is continuous, light, adhesive force are high, has excellent electrical property and high temperature soldering resistance.

Description

A kind of LED aluminium oxide pedestal silver slurry and application thereof
Technical field
The present invention relates to field of electronic materials, particularly a kind of LED aluminium oxide pedestal silver slurry and application thereof.
Background technology
Electronic silver slurry is a kind of electric conducting material for dip-coating and silk screen process use in electronics industry, and being set electron, chemical industry, metallurgical Trinitarian high-tech product, is one of primary base material in electronics industry.The present invention is the basic material of LED aluminium oxide pedestal wiring board, and silver slurry is through techniques such as silk screen printing, levelling, oven dry, sintering, and on alumina substrate, sintering forms conducting film, makes the wiring board of LED.The wiring board that current LED adopts mostly is PCB, the radiating effect of this wiring board is poor, greatly reduce the useful life of LED, and adopt the wiring board of aluminium oxide ceramics pedestal printing can solve heat dissipation problem well, electric conductivity is also very excellent, and then improves the useful life of LED.
Along with the wiring board of LED is gradually to the development of aluminium oxide pedestal wiring board, the demand of market to LED aluminium oxide pedestal silver slurry can be increasing, therefore LED aluminium oxide pedestal silver slurry has good market prospects.And LED aluminium oxide pedestal silver slurry requires that silver slurry has good electrical property, high temperature soldering resistance, high adhesion force after sintering, this is several technological difficulties of LED silver slurry exploitation, and domestic at present also do not have enterprise can produce LED aluminium oxide pedestal silver slurry.
Summary of the invention
For overcoming shortcoming of the prior art, the invention provides a kind of LED aluminium oxide pedestal silver slurry, it has excellent electrical property, high temperature soldering resistance and high adhesion force.
Another object of the present invention is to provide the application of above-mentioned LED aluminium oxide pedestal silver slurry.
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 aluminium oxide pedestal silver slurry, count by weight percentage, formula composition 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 purity is greater than 99.95%, and granularity is less than the powder of the spherical or nearly ball-type of 10 μm.
Described alloy for dental amalgam be selected from silver-bearing copper powder, silver-colored palladium powder, silver-colored nickel powder, silver-colored titanium valve one or more.
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 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 DEG C.
Described inorganic additive is selected from Fe 2o 3, ZrO, TiO 2, Nb 2o 5, V 2o 5in one or more.
Described macromolecule resin be selected from ethyl cellulose, acrylic resin, polyvinyl alcohol resin one or more.
Described solvent is ester class, and ethers, alcohols, in hydrocarbon compound at least a kind.
Described organic additive is selected from one or both mixing in organosilicon-modified acrylate or polyacrylate.
The application on aluminium oxide pedestal wiring board prepared by above-mentioned LED aluminium oxide pedestal silver slurry.
Above-mentioned application, is characterized in that: after LED aluminium oxide pedestal silver slurry is printed on aluminium oxide pedestal, dry 1-6 minute at 200-250 DEG C, then sinter, most high sintering temperature 800 DEG C ~ 830 DEG C.
Silver slurry of the present invention, in high solids content situation, has good printing performance, and after sintering, silver-colored face is continuous, light, adhesive force are high, have excellent electrical property and high temperature soldering resistance.
Embodiment
The present invention is a kind of LED aluminium oxide pedestal silver slurry, count by weight percentage, formula composition 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 μm, there is good dispersion, high-tap density, slurry can be made to have good rheological property, effective control electrode thickness, raising electrode surface evenness, there are excellent compactness and glossiness in dry rear electrode surface, and sintering shrinkage is little, there is good conductivity, ensure that silver-colored face is continuous, light, adhesive force are high, excellent electrical property.In formula, super fine silver powder 50 ~ 80%, preferably 60 ~ 80%, more preferably 65 ~ 75%.
Described alloy for dental amalgam be selected from commercially available silver-bearing copper powder, silver-colored palladium powder, silver-colored nickel powder, silver-colored titanium valve one or more.The powder that alloyed powder requires good dispersion, granularity is less than the spherical or nearly ball-type of less than 10 μm.The present invention is on the basis of conventional silver slurry formula composition (silver powder, glass dust, organic carrier), add alloy for dental amalgam innovatively, regulate silver slurry high temperature soldering resistance and electrical property by it, after making silver slurry sintering, 480 DEG C of welding, and extremely low resistance can be had.Described glass dust is 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 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 DEG C.During preparation, each component mixed with jar mill in proportion, 430-470 DEG C of preheating 20-40min, 1150-1250 DEG C of melting 50-70min, quenching, is milled to granularity and is less than 5 μm, filtering drying.The present invention's glass powder used is not leaded, cadmium and compound thereof, meets the environmental requirement of European Union RoHS.In formula, glass dust 2 ~ 10%, preferably 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, improve mechanical strength and the chemical stability of glass, also assures that electrical property and the chemical property of glass, be convenient to rete after sintering silver layer be attached to securely on substrate.Have high adhesion force after the present invention's silver slurry sintering, adhesive force is greater than 50N.
The organic carrier of the composition such as macromolecule resin, organic solvent and organic additive, can meet the silk-screen printing technique requirement of slurry in LED aluminium oxide pedestal.After organic carrier drying sintering, can be completely decomposed of volatile, can not residue be there is, bring negative effect to product.Wherein:
Described macromolecule resin be selected from ethyl cellulose, acrylic resin, polyvinyl alcohol resin one or more, select according to the powder body material that reality uses.
Described solvent is the ester class that toxicity is lower, and ethers, alcohols, in hydrocarbon compound at least a kind, difficult volatilization under making it have low temperature, volatile characteristic under high temperature, conveniently can keep good printing performance in printing process like this, after ensureing silver slurry sintering, the smooth gloss of silver layer surface, pore-free.Wherein lipid is for must add class, and it can give silver slurry good lubrification, ensures the printing performance of silver slurry; In ethers, alcohols, hydrocarbon compound more than at least a kind, for adjusting silver slurry sintering character, after ensureing silver slurry sintering, the smooth gloss of silver layer surface, pore-free.The ester class be suitable for, ethers, alcohols, hydrocarbon compound can be selected from fat hydrocarbon solvent, tasteless gasoline, mixed type dibasic acid dimethyl ester as DBE, terpinol, ethyl oleate, butyl, repefral, diethylene glycol ether amyl acetate, butyl amyl acetate etc.
Described organic additive is selected from one or both mixing in organosilicon-modified acrylate or polyacrylate.The present invention adds organosilicon-modified acrylate, polyacrylate surfactant in organic carrier, organic carrier is allowed to roll fully wetting parcel inoganic solids in slurry process, silver powder and glass dust is made to reach sufficient dispersion, improve the dispersiveness of solid powder, the mobility of slurry, the overall fineness that silver is starched is controlled below 10 μm simultaneously, ensure that silver slurry is in high solids content situation, has good printing performance, so that slurry is transferred on substrate form required figure.
Below by way of concrete example, the present invention is further elaborated, 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, quenching, is milled to granularity and is less than 5 μm, filtering drying.
2, the preparation of organic carrier
Ethyl cellulose 20%, terpinol 30%, butyl 30%, ethyl oleate 10%, organosilicon-modified acrylate 10%, after above each thing mixing, 80 ~ 100 ° of C heating for dissolving, obtains 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 high speed dispersion, be rolled to fineness through three-high mill and be less than less than 10 μm, add diluent, adjustment 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, quenching, is milled to granularity and is less than 5 μm, filtering drying.
2, the preparation of organic carrier
Ethyl cellulose 25%, terpinol 45%, butyl amyl acetate 20%, polyacrylate 10%, after above each thing mixing, 80 ~ 100 ° of C heating for dissolving, obtains transparent glue.
3,69% super fine silver powder, 9% yellow gold powder, 4% glass dust, 1%Nb is mixed 2o 5, be made into powder, after stirring, add 17% organic carrier, after high speed dispersion, be rolled to fineness through three-high mill and be less than less than 10 μm, add diluent, adjustment 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, quenching, is milled to granularity and is less than 5 μm, filtering drying.
3, the preparation of organic carrier
Ethyl cellulose 15%, diethylene glycol ether amyl acetate 22%, butyl 43%, repefral 10%, organosilicon-modified acrylate 10%, after above each thing mixing, 80 ~ 100 ° of C heating for dissolving, obtains transparent glue.
4,75% super fine silver powder, 5% silver-nickel powder, 5% glass dust, 1%Nb is mixed 2o 5, be made into powder, after stirring, add 14% organic carrier, after high speed dispersion, be rolled to fineness through three-high mill and be less than less than 10 μm, add diluent, adjustment viscosity.
Experimental example
The silver slurry using method of embodiment 1-3:
1. silk screen printing (note: standard printing condition: mesh: 250 orders) on alumina substrate
2.. drying condition: 230 DEG C 3 minutes
3.. sintering condition: sintering temperature: 800 DEG C ~ 830 DEG C
Sintering condition in this experimental example: the highest 810 DEG C, high-temperature region maintains 10 minutes, 60 minutes altogether.
4.. carry out performance test after sintering, corresponding product randomly draws 10, and soldering resistance method of testing is pressed GB/T17473.7-2008 and implemented, and adhesive force test is pressed GB/T17473.4-2008 and implemented, and sheet resistance test is pressed GB/T17473.3-2008 and implemented.Data are as table 1.
Table 1.

Claims (7)

1. a LED aluminium oxide pedestal silver slurry, count by weight percentage, formula composition 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%; Wherein, glass dust is B 2o 3-SiO 2-Bi 2o 3-Al 2o 3-Mn 2o 3glass system; Inorganic additive is selected from Fe 2o 3, ZrO, TiO 2, Nb 2o 5, V 2o 5in one or more; Macromolecule resin be selected from ethyl cellulose, acrylic resin, polyvinyl alcohol resin one or more; Described organic additive is selected from one or both mixing in organosilicon-modified acrylate or polyacrylate.
2. LED aluminium oxide pedestal silver slurry according to claim 1, it is characterized in that: described super fine silver powder is that purity is greater than 99.95%, granularity is less than the powder of the spherical or nearly ball-type of 10 μm.
3. LED aluminium oxide pedestal according to claim 1 silver slurry, is characterized in that: described alloy for dental amalgam be selected from silver-bearing copper powder, silver-colored palladium powder, silver-colored nickel powder, silver-colored titanium valve one or more.
4. LED aluminium oxide pedestal silver slurry according to claim 1, is characterized in that: described B 2o 3-SiO 2-Bi 2o 3-Al 2o 3-Mn 2o 3in 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 DEG C.
5. LED aluminium oxide pedestal according to claim 1 silver slurry, is characterized in that: described solvent is ester class, and ethers, alcohols, in hydrocarbon compound at least a kind.
6. the application on aluminium oxide pedestal wiring board prepared by the LED aluminium oxide pedestal silver slurry in claim 1-5 described in arbitrary claim.
7. application according to claim 6, is characterized in that: after LED aluminium oxide pedestal silver slurry is printed on aluminium oxide pedestal, dry 1-6 minute at 200-250 DEG C, then sinter, most high sintering temperature 800 DEG C ~ 830 DEG C.
CN201310285671.2A 2013-07-08 2013-07-08 A kind of LED aluminium oxide pedestal silver slurry and application thereof Active CN103366858B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201310285671.2A CN103366858B (en) 2013-07-08 2013-07-08 A kind of LED aluminium oxide pedestal silver slurry and application thereof

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201310285671.2A CN103366858B (en) 2013-07-08 2013-07-08 A kind of LED aluminium oxide pedestal silver slurry and application thereof

Publications (2)

Publication Number Publication Date
CN103366858A CN103366858A (en) 2013-10-23
CN103366858B true CN103366858B (en) 2015-10-14

Family

ID=49368015

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201310285671.2A Active CN103366858B (en) 2013-07-08 2013-07-08 A kind of LED aluminium oxide pedestal silver slurry and application thereof

Country Status (1)

Country Link
CN (1) CN103366858B (en)

Citations (6)

* 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

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP5887086B2 (en) * 2011-08-11 2016-03-16 株式会社タムラ製作所 Conductive material

Patent Citations (6)

* 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
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

Also Published As

Publication number Publication date
CN103366858A (en) 2013-10-23

Similar Documents

Publication Publication Date Title
CN101986390B (en) Silver paste for disk capacitor electrode
CN102568704B (en) Environment-friendly lead-free semiconductor ceramic capacitive electrode silver paste and preparation method thereof
CN101377966B (en) Method for preparing leadless silver electrode slurry for glass substrates
CN1329926C (en) Electrode thick liquid without lead and silver and mfg. method thereof
CN102354544B (en) Silver conductive paste for front electrode of crystalline silicon solar cell and preparation method thereof
CN101820002B (en) Conductive paste for solar cell and preparation method thereof
CN105873248B (en) A kind of heating film low-temperature sintering slurry and preparation method thereof
CN103177791B (en) A kind of aluminum conductive electric slurry used for solar batteries and preparation method thereof
CN101710509B (en) Preparation method of leadless nickel electrode slurry for thick-film resistor
CN103985431B (en) A kind of high intensity printed circuit board (PCB) conductive silver paste and preparation method thereof
CN110217998B (en) Lead-free conductive silver paste capable of being sintered at low temperature and preparation method and application thereof
CN111564234B (en) Titanate-based lead-free silver electrode slurry and preparation and use methods thereof
CN102610326B (en) Conductive silver paste for ferrite core inductance and method for producing same
CN1216380C (en) Resistance sizing agent and its producing process for high-power thick-film circuit based on stainless steel substrate
CN106851872A (en) A kind of aluminium alloy base plate large power thick film circuit intermediate sintering temperature silver palladium resistance slurry and preparation method thereof
CN104021838A (en) Polythiophene/ mixed valence metal oxide collaborative conductive slurry and preparation method thereof
CN104078096A (en) Low-cost printed circuit board silver paste and preparation method thereof
CN101354926B (en) Method for preparing conductor slurry containing carbon and silver
CN106653145A (en) Medium-and-high temperature thick film circuit conductor paste and preparation method thereof
CN111116239A (en) Electronic paste suitable for PZT atomized sheet co-firing process and co-firing method
CN103366858B (en) A kind of LED aluminium oxide pedestal silver slurry and application thereof
CN104143377A (en) PCB conductive silver paste and preparing method thereof
CN110942842A (en) Conductor paste and conductor material
CN114783652B (en) Gold conductor wiring slurry co-fired with microwave dielectric ceramic at low temperature and preparation method thereof
CN116564578A (en) Silver paste for preparing ceramic dielectric capacitor and preparation method and application thereof

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
C10 Entry into substantive examination
SE01 Entry into force of request for substantive examination
C14 Grant of patent or utility model
GR01 Patent grant
PE01 Entry into force of the registration of the contract for pledge of patent right
PE01 Entry into force of the registration of the contract for pledge of patent right

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

Effective date of registration: 20200426

Granted publication date: 20151014

Pledgee: China Co. truction Bank Corp Zhaoqing branch

Pledgor: GUANGDONG LINGGUANG NEW MATERIAL Co.,Ltd.

Registration number: Y2020440000098

PC01 Cancellation of the registration of the contract for pledge of patent right
PC01 Cancellation of the registration of the contract for pledge of patent right

Granted publication date: 20151014

Pledgee: China Co. truction Bank Corp Zhaoqing branch

Pledgor: GUANGDONG LINGGUANG NEW MATERIAL Co.,Ltd.

Registration number: Y2020440000098