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.