CN101728001A - Lead-free and low-silver photosensitive silver paste and preparation method thereof - Google Patents
Lead-free and low-silver photosensitive silver paste and preparation method thereof Download PDFInfo
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- CN101728001A CN101728001A CN200910212490A CN200910212490A CN101728001A CN 101728001 A CN101728001 A CN 101728001A CN 200910212490 A CN200910212490 A CN 200910212490A CN 200910212490 A CN200910212490 A CN 200910212490A CN 101728001 A CN101728001 A CN 101728001A
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Abstract
The invention relates to lead-free and low-silver photosensitive silver paste and preparation method thereof. The preparation method comprises the following steps of: uniformly mixing a certain proportion of sliver-cladding high-melting point and lead-free inorganic microspheres, superfine silver powder, low-melting point and lead-free glass powder, an organic solvent, cellulosic resins, a photosensitive monomer, a light initiator, other additives and the like, grinding to a certain fineness to obtain silver slurry, and sintering after light curing of the silver slurry. Compared with the prior art, because the paste uses the silver-cladding high-melting point and lead-free inorganic microspheres, not only a large amount of precious metallic silver can be saved, but also the slurry can be sintered at high temperature with favorable conductivity. In addition, the paste has the advantages of no lead, environmental protection, fine electrode manufactured by adopting a light curing method, accurate alignment, simple technology and low cost, thereby having extensive application prospect.
Description
Technical field
The present invention relates to a kind of lead-free and low-silver photosensitive silver paste and preparation method thereof, be mainly used in the bus electrode of making plasma display electrode, particularly prebasal plate and the addressing electrode of metacoxal plate.
Background technology
Photosensitive silver is starched the plasma display electrode of making, and both can guarantee the quality of electrode wires, improves the electrode precision, can reduce technology and equipment cost again, is the main method for preparing PDP bus electrode and addressing electrode at present.
Granted publication number is the patent of invention of CN1290121C, has prepared a kind of photosensitive silver slurry that is used for bus electrode, and glass dust is leaded in its system, does not meet environmental requirement.And use the glass powder with low melting point electroplate, and when the higher temperature sintering, coated glass dust and begin to melt, to block crosslinked conductive network, so can not add too much silver in the system and coat glass dust, addition will be below 20%, otherwise conductivity is descended.Application number is 200510073226.5 patent of invention, has proposed a kind of unleaded silver paste composition of the PDP of being used for addressing electrode, and glass dust is not leaded in its system, but silver content is very high, reaches 60～90%wt.If may cause electrodes conduct performance variation but reduce silver content, electrode is discontinuous, adverse consequencess such as broken string.
Summary of the invention
The objective of the invention is to guarantee under the conductivity good premise, reduce the content of silver as far as possible, the invention provides a kind of lead-free and low-silver photosensitive silver paste and preparation method thereof.
Technical scheme of the present invention is: a kind of lead-free and low-silver photosensitive silver paste, this slurry consists of, in wt%: the high-melting point lead-free inorganic microsphere 30～60% that silver coats, particle diameter is the super fine silver powder 10～35% of 1～5 μ m, low-melting point lead-less glasses powder 3～10%, photosensitive monomer 5～20%, light trigger 0.5～2%, organic carrier surplus.The high-melting point lead-free inorganic microsphere that described silver coats is that fusing point is higher than 600 ℃ crown glass microballoon, SiO
2Microballoon, TiO
2Microballoon, ZrO
2Any one microballoon in the microballoon coats one deck silverskin outward.The high-melting point lead-free inorganic microsphere particle diameter that silver coats is 0.5～5 μ m.Described low-melting point lead-less glasses powder particle diameter is 1～5 μ m, forms and counts with wt%: SiO
24～20%, B
2O
310～30%, ZnO 2～10%, Al
2O
31～3%, BaO 0.1～3%, ZrO
20.1～1%, CeO 0.1～0.5%, Bi
2O
3Surplus.Described photosensitive monomer uses double pentaerythritol C5 methacrylate, double pentaerythritol methacrylate, 1,6 hexanediyl esters, pentaerythritol triacrylate, trimethylolpropane triacrylate, ethoxylated trimethylolpropane triacrylate, any one in the propoxylation trimethylolpropane triacrylate or arbitrarily several arbitrarily than mixture.Described light trigger is 1-to any one or the mixture of several any ratios arbitrarily in morpholinyl phenyl-2-dimethylamino-2-benzyl-1-butanone, Alpha-hydroxy cyclohexyl-phenyl ketone, the styrax dimethyl ether.Described organic carrier consists of by weight percentage: celluosic resin 0.5～5%, thickener 8～15%, additive 1～5%, organic solvent surplus are formed; Wherein, described organic solvent is diethylene glycol monobutyl ether, terpinol, castor oil, phenmethylol, tributyl citrate, 2,2,4-trimethyl-1, the mixture of any one in the 3-pentanediol mono isobutyrate or arbitrarily several any ratio.Described thickener is dioctyl phthalate or butyl carbitol acetate.Described celluosic resin is hydroxyethylcellulose, carboxymethyl cellulose, ethyl cellulose, methyl hydroxyethylcellulose, any one of hydroxypropyl methylcellulose or arbitrarily several arbitrarily than mixture.Described additive is lecithin, ethanol, cyclohexanone, silane coupler.
The preparation method of described lead-free and low-silver photosensitive silver paste utilizes electroless plating method or other method that unleaded inorganic microsphere surface is plated silver layer, unleaded inorganic microsphere, super fine silver powder, lead-free glass powder, photosensitive monomer, light trigger, organic solvent, celluosic resin with the silver coating, additive press the formula rate dispersing and mixing evenly after, carry out three-roll rolling, slurry is lead-free and low-silver photosensitive silver paste after reaching and setting fineness, viscosity.
Principle is: plate one deck silverskin on high-melting point lead-free inorganic microsphere surface, the softening fusion of low-melting point lead-less glasses powder particle during sintering, be bonded between substrate and the silver layer, along with the rising of temperature, the silver layer that unleaded microsphere surface coats, beginning is slowly softening, viscosity and plastic flowing take place, and this moment, sintering temperature did not reach the fusing point of high-melting point lead-free microballoon, so the high-melting point lead-free microballoon melts, therefore conductive network was not exerted an influence.Softening silverskin is connected with the super fine silver powder of fusion and is cross-linked to form network configuration, can carry out electrical conductivity.
Beneficial effect:
1. this method makes silver-colored consumption significantly reduce, and being reduced to present fine silver powder content by the fine silver powder content of 60 general～90%wt is 10～35%wt.
2. owing to utilized the fusing point difference of different materials, make silver be evenly distributed, the resistance that makes is little, and shrinkage is little, and good conductivity does not break.
Description of drawings:
Fig. 1 silver slurry film forming schematic diagram.
Embodiment
Following percentage is all mass percent
Embodiment 1
It is silver-plated that fusing point is higher than 600 ℃ crown glass microsphere surface
Get the AgNO of 10g
3Fully be dissolved in the 125ml distilled water, constantly agitating solution slowly adds ammoniacal liquor, until generating the brown sediment, adds ammoniacal liquor again and dissolves fully to sediment; Add the 25g dissolution of sodium hydroxide in 100ml distilled water, be mixed with sodium hydroxide solution.In the 125ml liquor argenti nitratis ophthalmicus, add the 40ml sodium hydroxide solution, be added dropwise to ammoniacal liquor again, make that solution is transparent promptly to be ended, make silver plating liquid.Glucose 60g, tartaric acid 5g are dissolved in the 1000ml distilled water successively, are cooled to room temperature after boiling 10min, add 25ml absolute ethyl alcohol preparation reducing solution.Silver plating liquid and reducing solution were mixed in 1: 1 by volume, weighing 25g fusing point is higher than 600 ℃, diameter is that the crown glass microballoon of 2 μ m is to solution, with the solution sonicated, ultrasonic power is 50W, and frequency is 40kHz, takes out after 3 hours, left standstill 24 hours, with pressed powder isolate, wash, drying.
The modulation of photosensitive silver slurry
By weight percentage, 600 ℃ crown glass microballoon 50% with the silver coating, super fine silver powder (average grain diameter 3 μ m) 15%, low-melting point lead-less glasses powder (average grain diameter 5 μ m) 5%, ethoxylated trimethylolpropane triacrylate 5%, 1-is to morpholinyl phenyl-2-dimethylamino-2-benzyl-1-butanone 0.5%, and organic carrier 24.5% places container, after dispersing and mixing is even, carry out three-roll rolling.Wherein, low-melting point lead-less glasses powder consists of Bi
2O
378%, SiO
25%, B
2O
310%, ZnO 3%, Al
2O
32%, BaO 1%, ZrO
20.5%, CeO 0.5%.Organic carrier is for taking by weighing hydroxypropyl methylcellulose 3%, terpinol 64%, diethylene glycol monobutyl ether 24% by weight, silane coupler 0.5%, lecithin 0.5%, thickener butyl carbitol acetate 8% are in beaker, 90 ℃ of heating in water-bath, constantly stir, up to resin dissolves.Be incubated 2 hours, use silk screen filter after the cooling.Testing size fineness≤5 μ m, viscosity 150 ± 50Pas.Be evenly coated on the substrate with print process, drying, ultraviolet photoetching, the back sintering that develops forms.The side's of recording resistance≤10m Ω, shrinkage≤20%.
Embodiment 2
SiO
2Microsphere surface is silver-plated
Get the AgNO of 10g
3Fully be dissolved in the 125ml distilled water, constantly stir silvering solution, slowly add ammoniacal liquor,, add ammoniacal liquor again and dissolve fully to sediment until generating the brown sediment; Add the 25g dissolution of sodium hydroxide in 100ml distilled water, be mixed with sodium hydroxide solution.In the 125ml liquor argenti nitratis ophthalmicus, add the 40ml sodium hydroxide solution, be added dropwise to ammoniacal liquor again, make that solution is transparent promptly to be ended, make silver plating liquid.Glucose 60g, tartaric acid 5g are dissolved in the 1000ml distilled water successively, are cooled to room temperature after boiling 10min, add 25ml absolute ethyl alcohol preparation reducing solution.Silver plating liquid and reducing solution were mixed in 1: 1 by volume, and weighing 25g diameter is the SiO of 0.5 μ m
2Microballoon is to solution, and with the solution sonicated, ultrasonic power is 50W, and frequency is 40kHz, takes out after 3 hours, left standstill 24 hours, with pressed powder isolate, wash, drying.
The modulation of photosensitive silver slurry
SiO with the silver coating
2Microballoon 45%, super fine silver powder (average grain diameter 3 μ m) 20%, lead-free glass powder (average grain diameter 5 μ m) 5%, 1,6 hexanediyl ester 5%, Alpha-hydroxy cyclohexyl-phenyl ketone 0.5%, organic carrier 24.5% places container, after dispersing and mixing is even, carries out three-roll rolling.Wherein, low-melting point lead-less glasses powder consists of Bi
2O
366.5%, SiO
210%, B
2O
315%, ZnO 5%, Al
2O
31%, BaO 2%, ZrO
20.2%, CeO 0.3%.Organic carrier is for to take by weighing methyl hydroxyethylcellulose 3%, terpinol 56%, 2 by proportioning, 2,4-trimethyl-1,3-pentanediol mono isobutyrate 15%, tributyl citrate 10%, silane coupler 0.5%, lecithin 0.5%, thickener dioctyl phthalate 15% in beaker, 90 ℃ of heating in water-bath, constantly stir, up to resin dissolves.Be incubated 2 hours, use silk screen filter after the cooling.Testing size fineness≤5 μ m, viscosity 150 ± 30Pas.Be evenly coated on the substrate with print process, drying, ultraviolet photoetching, the back sintering that develops forms.The side's of recording resistance≤10m Ω, shrinkage≤20%.
Embodiment 3
TiO
2Microsphere surface is silver-plated
Get 10gAgNO
3Fully be dissolved in the 125ml distilled water, constantly stir silvering solution, slowly add ammoniacal liquor,, add ammoniacal liquor again and dissolve fully to sediment until generating the brown sediment; Add the 25g dissolution of sodium hydroxide in 100ml distilled water, be mixed with sodium hydroxide solution.In the 125ml liquor argenti nitratis ophthalmicus, add the 40ml sodium hydroxide solution, be added dropwise to ammoniacal liquor again, make that solution is transparent promptly to be ended, make silver plating liquid.Glucose 60g, tartaric acid 5g are dissolved in the 1000ml distilled water successively, are cooled to room temperature after boiling 10min, add 25ml absolute ethyl alcohol preparation reducing solution.Silver plating liquid and reducing solution were mixed in 1: 1 by volume, and weighing 25g diameter is the TiO of 5 μ m
2Microballoon is to solution, and with the solution sonicated, ultrasonic power is 50W, and frequency is 40kHz, takes out after 3 hours, left standstill 24 hours, with pressed powder isolate, wash, drying.
The modulation of photosensitive silver slurry
SiO with the silver coating
2Microballoon 35%, super fine silver powder (average grain diameter 3 μ m) 30%, lead-free glass powder (average grain diameter 5 μ m) 5%, trimethylolpropane triacrylate 5%, styrax dimethyl ether 0.5%, organic carrier 24.5% places container, after dispersing and mixing is even, carry out three-roll rolling.Wherein, low-melting point lead-less glasses powder consists of SiO
215%, B
2O
310%, ZnO 3%, Al
2O
32%, BaO 1%, ZrO
20.5%, CeO 0.5%, Bi
2O
368%, organic carrier is for to take by weighing ethyl cellulose 3%, terpinol 61%, diethylene glycol monobutyl ether 20% by proportioning, phenmethylol 5%, silane coupler 0.5%, lecithin 0.5%, thickener butyl carbitol acetate 10% are in beaker, 90 ℃ of heating in water-bath, constantly stir, up to resin dissolves.Be incubated 2 hours, use silk screen filter after the cooling.Testing size fineness≤6 μ m, viscosity 150 ± 30Pas.Be evenly coated on the substrate with print process, drying, ultraviolet photoetching, the back sintering that develops forms.The side's of recording resistance≤10m Ω, shrinkage≤20%.
Embodiment 4
ZrO
2Microsphere surface is silver-plated
Get 10gAgNO
3Fully be dissolved in the 125ml distilled water, constantly stir silvering solution, slowly add ammoniacal liquor,, add ammoniacal liquor again and dissolve fully to sediment until generating the brown sediment; Add the 25g dissolution of sodium hydroxide in 100ml distilled water, be mixed with sodium hydroxide solution.In the 125ml liquor argenti nitratis ophthalmicus, add the 40ml sodium hydroxide solution, be added dropwise to ammoniacal liquor again, make that solution is transparent promptly to be ended, make silver plating liquid.Glucose 60g, tartaric acid 5g are dissolved in the 1000ml distilled water successively, are cooled to room temperature after boiling 10min, add 25ml absolute ethyl alcohol preparation reducing solution.Silver plating liquid and reducing solution were mixed in 1: 1 by volume, and weighing 25g diameter is the ZrO of 3 μ m
2Microballoon is to solution, and with the solution sonicated, ultrasonic power is 50W, and frequency is 40kHz, takes out after 3 hours, left standstill 24 hours, with pressed powder isolate, wash, drying.The modulation of photosensitive silver slurry
ZrO with the silver coating
2Microballoon 55%, super fine silver powder (average grain diameter 3 μ m) 10%, lead-free glass powder (average grain diameter 5 μ m) 5%, propoxylation trimethylolpropane triacrylate 5%, Alpha-hydroxy cyclohexyl-phenyl ketone 0.5%, organic carrier 24.5% places container, after dispersing and mixing is even, carry out three-roll rolling.Wherein, low-melting point lead-less glasses powder consists of SiO
25%, B
2O
330%, ZnO 3%, Al
2O
33%, BaO1%, ZrO
21%, CeO 0.5%, Bi
2O
356.5%, organic carrier is for to take by weighing CMC 3%, terpinol 58%, 2 by proportioning, 2,4-trimethyl-1,3-pentanediol mono isobutyrate 20%, castor oil 8%, silane coupler 0.5%, lecithin 0.5%, thickener dioctyl phthalate 10% are in beaker, 90 ℃ of heating in water-bath are constantly stirred, up to resin dissolves.Be incubated 2 hours, use silk screen filter after the cooling.Testing size fineness≤5 μ m, viscosity 150 ± 30Pas.Be evenly coated on the substrate with print process, drying, ultraviolet photoetching, the back sintering that develops forms.The side's of recording resistance≤10m Ω, shrinkage≤20%.
The electroplate of described unleaded inorganic microsphere also can adopt alternate manner such as HVAF, gas aggradation method etc.
Claims (10)
1. lead-free and low-silver photosensitive silver paste, it is characterized in that, this slurry consists of, in wt%: the high-melting point lead-free inorganic microsphere 30～60% that silver coats, particle diameter is the super fine silver powder 10～35% of 1～5 μ m, low-melting point lead-less glasses powder 3～10%, photosensitive monomer 5～20%, light trigger 0.5～2%, the organic carrier surplus.
2. lead-free and low-silver photosensitive silver paste according to claim 1 is characterized in that, the high-melting point lead-free inorganic microsphere that described silver coats is that fusing point is higher than 600 ℃ crown glass microballoon, SiO
2Microballoon, TiO
2Microballoon, ZrO
2Any one microballoon in the microballoon coats one deck silverskin outward.
3. lead-free and low-silver photosensitive silver paste according to claim 1 is characterized in that, the high-melting point lead-free inorganic microsphere particle diameter that silver coats is 0.5～5 μ m.
4. lead-free and low-silver photosensitive silver paste according to claim 1 is characterized in that, described low-melting point lead-less glasses powder particle diameter is 1～5 μ m, forms and counts with wt%: SiO
24～20%, B
2O
310～30%, ZnO 2～10%, Al
2O
31～3%, BaO 0.1～3%, ZrO
20.1～1%, CeO 0.1～0.5%, Bi
2O
3Surplus.
5. lead-free and low-silver photosensitive silver paste according to claim 1, it is characterized in that, described photosensitive monomer uses double pentaerythritol C5 methacrylate, double pentaerythritol methacrylate, 1,6 hexanediyl ester, pentaerythritol triacrylate, trimethylolpropane triacrylate, ethoxylated trimethylolpropane triacrylate, any one in the propoxylation trimethylolpropane triacrylate or arbitrarily several arbitrarily than mixture.
6. lead-free and low-silver photosensitive silver paste according to claim 1, it is characterized in that described light trigger is 1-to any one or the mixture of several any ratios arbitrarily in morpholinyl phenyl-2-dimethylamino-2-benzyl-1-butanone, Alpha-hydroxy cyclohexyl-phenyl ketone, the styrax dimethyl ether.
7. lead-free and low-silver photosensitive silver paste according to claim 1 is characterized in that, described organic carrier consists of by weight percentage: celluosic resin 0.5～5%, thickener 8～15%, additive 1～5%, organic solvent surplus are formed;
Wherein, described organic solvent is diethylene glycol monobutyl ether, terpinol, castor oil, phenmethylol, tributyl citrate, 2,2,4-trimethyl-1, and the mixture of any one in the 3-pentanediol mono isobutyrate or arbitrarily several any ratio,
Described thickener is dioctyl phthalate or butyl carbitol acetate.
8. lead-free and low-silver photosensitive silver paste according to claim 1, it is characterized in that, described celluosic resin is hydroxyethylcellulose, carboxymethyl cellulose, ethyl cellulose, methyl hydroxyethylcellulose, any one in the hydroxypropyl methylcellulose or arbitrarily several arbitrarily than mixture.
9. lead-free and low-silver photosensitive silver paste according to claim 1 is characterized in that, described additive is lecithin, ethanol, cyclohexanone, silane coupler.
10. the preparation method of lead-free and low-silver photosensitive silver paste according to claim 1, it is characterized in that, unleaded inorganic microsphere, super fine silver powder, lead-free glass powder, photosensitive monomer, light trigger, organic solvent, celluosic resin, the additive that silver is coated press the formula rate dispersing and mixing even after, carry out three-roll rolling, slurry is lead-free and low-silver photosensitive silver paste after reaching and setting fineness, viscosity.
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