CN109801757A - A kind of preparation method of electronic device electrode slurry - Google Patents
A kind of preparation method of electronic device electrode slurry Download PDFInfo
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- CN109801757A CN109801757A CN201811611567.7A CN201811611567A CN109801757A CN 109801757 A CN109801757 A CN 109801757A CN 201811611567 A CN201811611567 A CN 201811611567A CN 109801757 A CN109801757 A CN 109801757A
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Abstract
The present invention provides a kind of preparation methods of electronic device electrode slurry, and steps are as follows: silver nitrate aqueous solution and polyvinylpyrrolidonesolution solution being uniformly mixed to obtain solution A, glucose solution and polyvinylpyrrolidonesolution solution are uniformly mixed to obtain solution B；Solution B is added in solution A and is reacted；Centrifuge washing, dry nanometer multidimensional silver powder；Prepare modified Nano flake aluminum；By nanometer multidimensional silver powder, modified Nano flake aluminum, bismuth oxide, titanium nitride, surfactant and deionized water mixing and ball milling；Filtering drying；Polyvinylpyrrolidone, ethylene-vinyl acetate copolymer, α-terpineol is added, is placed in ball milling in planetary ball mill；It moves into three-roll grinder and further grinds to obtain the final product.The electronic device electrode slurry of the method for the present invention preparation forms fine and close film layer after sintering, and resistance is low, and electric conductivity is good, while having very strong adhesive force, good with interface attachment.
Description
Technical field
The present invention relates to a kind of preparation methods of electronic device electrode slurry.
Background technique
Electrode slurry occupys an important position in field of electronic materials, 20 th century laters, the information processing technology and electricity
Sub-information digitizing technique, which is combined, has pushed to a unprecedented new height for communication system, and is applied to production communication system
The development of the critical material of the various microwave devices of system plays important restrictive function to modern information technologies.Electrode slurry is just
It is applied to one of the three big electronic materials for playing electric action in electronic component as conductive material, is that manufacture microwave communication is set
The basic material of the core devices of standby, household electrical appliance etc. occupies extremely in every field across electronics and the big field of material two
Consequence.Therefore, research and development electric conductivity is good, and the strong electrode slurry of adhesive force has great importance answers with wide
Use prospect.
Summary of the invention
Technical problems to be solved:
A kind of preparation method of electronic device electrode slurry is provided, slurry forms fine and close film layer, resistance after sintering
Low, electric conductivity is good, while having very strong adhesive force, good with interface attachment.
Technical solution:
The present invention provides a kind of preparation method of electronic device electrode slurry, ingredient by weight, including following step
It is rapid:
(1) silver nitrate aqueous solution of 5-10 parts of 1.5mmol/L is prepared, and adjusting pH value with concentrated nitric acid is 1, prepares 5-10 parts
The glucose solution of 5mmol/L, and adjusting pH value with concentrated nitric acid is 1, prepares the polyvinylpyrrolidone of 20-40 parts of 10wt%
Solution；
(2) silver nitrate aqueous solution and 10-20 parts of polyvinylpyrrolidonesolution solutions are uniformly mixed to obtain solution A, by glucose
Aqueous solution and 10-20 parts of polyvinylpyrrolidonesolution solutions are uniformly mixed to obtain solution B；
(3) at 25-30 DEG C of temperature, mixing speed 300-400r/min, solution B is added rapidly in solution A, is reacted
20-30min；
(4) it is centrifuged, is washed 3-5 times with deionized water and dehydrated alcohol respectively, dry nanometer multidimensional silver powder；
(5) it is coated with one layer of peeling layer resin in PET film, is dried at 120-140 DEG C；
(6) it is put into vacuum coating equipment, vacuumizes, when vacuum degree reaches 10-9When Pa, the aluminium made on evaporation boat is begun to warm up
Silk melts, evaporates, and starts to be deposited, obtains PET aluminizer；
(7) it is put into aluminium film stripping machine, is stripped down aluminium film with solvent, remove solvent with seperator, it is equal to be put into high pressure
It is high-pressure homogeneous at pressure 100-150MPa to be crushed in matter machine；
(8) it is sieved, carboxymethylcellulose sodium solution is added and stirs 10-20min；
(9) 10-15wt% nano zero valence iron is added dropwise, continues to stir 10-20min, not open close nitrogen in reaction；
(10) it filters, is washed 2-3 times with dehydrated alcohol, dry modified Nano flake aluminum；
(11) by 5-10 parts of nanometer multidimensional silver powder, 3-5 parts of modified Nano flake aluminums, 1-3 parts of bismuth oxides, 3-5 parts of nitridations
Titanium, 10-25 part surfactant and 20-30 parts of deionized water mixing, are placed in planetary ball mill in revolving speed 400-600r/min
Lower ball milling 10-12h；
(12) it filters, is put into vacuum oven and dries；
(13) 5-10 parts of polyvinylpyrrolidones, 3-5 parts of ethylene-vinyl acetate copolymers, 30-50 parts of α-terpins are added
Alcohol is placed in ball milling 8-10h in planetary ball mill；
(14) it moves into three-roll grinder and further grinds 30-60min to obtain the final product.
Further, the surfactant is sodium lignin sulfonate, sodium sulfate of polyethenoxy ether of fatty alcohol, modified soybean
One or more of phosphatide or glycerin monostearate.
Further, the partial size of the nanometer multidimensional silver powder is 50-200nm.
Further, the peeling layer resin viscosity is 20-28s.
Further, the aluminium film and the ratio of carboxymethylcellulose sodium solution are 2g:7mL.
The utility model has the advantages that
1. nanometer multidimensional silver powder due to its nanometer of level characteristics, has dispersibility and compatibility well, simultaneously because it is more
The characteristic of dimension, surface area is very big, shows fabulous electric conductivity.
2. nanometer multidimensional silver powder and the mutual intercalation synthesis of modified Nano flake aluminum, merges more evenly, stablize between raw material
Property more preferably, meanwhile, the network-like structure that polyvinylpyrrolidone and ethylene-vinyl acetate copolymer are formed can preferably be stablized
Nanoparticle, formed it is stable align, improve electric conductivity.
3. the slurry of the method for the present invention preparation forms fine and close film layer after sintering, this film layer resistance is low, minimum to be only
1.7 Ω, electric conductivity is good, while its adhesive force is up to 0.99kgf/mm2, there is very strong adhesive force, it is good with interface attachment.
Specific embodiment
The following examples can make those skilled in the art that the present invention be more fully understood, but not limit this in any way
Invention.
Embodiment 1
A kind of preparation method of electronic device electrode slurry, ingredient is by weight, comprising the following steps:
(1) silver nitrate aqueous solution of 5 parts of 1.5mmol/L is prepared, and adjusting pH value with concentrated nitric acid is 1, prepares 5 parts of 5mmol/
The glucose solution of L, and adjusting pH value with concentrated nitric acid is 1, prepares the polyvinylpyrrolidonesolution solution of 20 parts of 10wt%；
(2) silver nitrate aqueous solution and 10 parts of polyvinylpyrrolidonesolution solutions are uniformly mixed to obtain solution A, glucose is water-soluble
Liquid and 10 parts of polyvinylpyrrolidonesolution solutions are uniformly mixed to obtain solution B；
(3) at 25 DEG C of temperature, mixing speed 300r/min, solution B is added rapidly in solution A, reacts 20min；
(4) it is centrifuged, is washed 3 times with deionized water and dehydrated alcohol respectively, dry nanometer multidimensional silver powder；
(5) it is coated with one layer of peeling layer resin in PET film, is dried at 120 DEG C；
(6) it is put into vacuum coating equipment, vacuumizes, when vacuum degree reaches 10-9When Pa, the aluminium made on evaporation boat is begun to warm up
Silk melts, evaporates, and starts to be deposited, obtains PET aluminizer；
(7) it is put into aluminium film stripping machine, is stripped down aluminium film with solvent, remove solvent with seperator, it is equal to be put into high pressure
It is high-pressure homogeneous at pressure 100MPa to be crushed in matter machine；
(8) it is sieved, carboxymethylcellulose sodium solution is added and stirs 10min, wherein aluminium film and carboxymethylcellulose sodium solution
Ratio be 2g:7mL；
(9) 10wt% nano zero valence iron is added dropwise, continues to stir 10min, not open close nitrogen in reaction；
(10) it filters, is washed 2 times with dehydrated alcohol, dry modified Nano flake aluminum；
(11) by 5 parts of nanometer multidimensional silver powder, 3 parts of modified Nano flake aluminums, 1 part of bismuth oxide, 3 parts of titanium nitrides, 10 parts of wood
Quality sodium sulfonate and 20 parts of deionized water mixing, are placed in planetary ball mill the ball milling 10h at revolving speed 400r/min；
(12) it filters, is put into vacuum oven and dries；
(13) 5 parts of polyvinylpyrrolidones, 3 parts of ethylene-vinyl acetate copolymers, 30 parts of α-terpineols are added, are placed in row
Ball milling 8h in celestial body grinding machine；
(14) it moves into three-roll grinder and further grinds 30min to obtain the final product.
Embodiment 2
A kind of preparation method of electronic device electrode slurry, ingredient is by weight, comprising the following steps:
(1) silver nitrate aqueous solution of 7 parts of 1.5mmol/L is prepared, and adjusting pH value with concentrated nitric acid is 1, prepares 7 parts of 5mmol/
The glucose solution of L, and adjusting pH value with concentrated nitric acid is 1, prepares the polyvinylpyrrolidonesolution solution of 25 parts of 10wt%；
(2) silver nitrate aqueous solution and 12 parts of polyvinylpyrrolidonesolution solutions are uniformly mixed to obtain solution A, glucose is water-soluble
Liquid and 12 parts of polyvinylpyrrolidonesolution solutions are uniformly mixed to obtain solution B；
(3) at 27 DEG C of temperature, mixing speed 350r/min, solution B is added rapidly in solution A, reacts 25min；
(4) it is centrifuged, is washed 4 times with deionized water and dehydrated alcohol respectively, dry nanometer multidimensional silver powder；
(5) it is coated with one layer of peeling layer resin in PET film, is dried at 125 DEG C；
(6) it is put into vacuum coating equipment, vacuumizes, when vacuum degree reaches 10-9When Pa, the aluminium made on evaporation boat is begun to warm up
Silk melts, evaporates, and starts to be deposited, obtains PET aluminizer；
(7) it is put into aluminium film stripping machine, is stripped down aluminium film with solvent, remove solvent with seperator, it is equal to be put into high pressure
It is high-pressure homogeneous at pressure 120MPa to be crushed in matter machine；
(8) it is sieved, carboxymethylcellulose sodium solution is added and stirs 15min, wherein aluminium film and carboxymethylcellulose sodium solution
Ratio be 2g:7mL；
(9) 12wt% nano zero valence iron is added dropwise, continues to stir 15min, not open close nitrogen in reaction；
(10) it filters, is washed 2 times with dehydrated alcohol, dry modified Nano flake aluminum；
(11) by 7 parts of nanometer multidimensional silver powder, 3.5 parts of modified Nano flake aluminums, 1.5 parts of bismuth oxides, 3.5 parts of titanium nitrides,
15 parts of sodium sulfate of polyethenoxy ether of fatty alcohol and 25 parts of deionized water mixing, are placed in planetary ball mill at revolving speed 450r/min
Ball milling 11h；
(12) it filters, is put into vacuum oven and dries；
(13) 7 parts of polyvinylpyrrolidones, 3.5 parts of ethylene-vinyl acetate copolymers, 35 parts of α-terpineols are added, are placed in
Ball milling 9h in planetary ball mill；
(14) it moves into three-roll grinder and further grinds 40min to obtain the final product.
Embodiment 3
A kind of preparation method of electronic device electrode slurry, ingredient is by weight, comprising the following steps:
(1) silver nitrate aqueous solution of 8 parts of 1.5mmol/L is prepared, and adjusting pH value with concentrated nitric acid is 1, prepares 8 parts of 5mmol/
The glucose solution of L, and adjusting pH value with concentrated nitric acid is 1, prepares the polyvinylpyrrolidonesolution solution of 30 parts of 10wt%；
(2) silver nitrate aqueous solution and 15 parts of polyvinylpyrrolidonesolution solutions are uniformly mixed to obtain solution A, glucose is water-soluble
Liquid and 15 parts of polyvinylpyrrolidonesolution solutions are uniformly mixed to obtain solution B；
(3) at 28 DEG C of temperature, mixing speed 350r/min, solution B is added rapidly in solution A, reacts 25min；
(4) it is centrifuged, is washed 4 times with deionized water and dehydrated alcohol respectively, dry nanometer multidimensional silver powder；
(5) it is coated with one layer of peeling layer resin in PET film, is dried at 130 DEG C；
(6) it is put into vacuum coating equipment, vacuumizes, when vacuum degree reaches 10-9When Pa, the aluminium made on evaporation boat is begun to warm up
Silk melts, evaporates, and starts to be deposited, obtains PET aluminizer；
(7) it is put into aluminium film stripping machine, is stripped down aluminium film with solvent, remove solvent with seperator, it is equal to be put into high pressure
It is high-pressure homogeneous at pressure 130MPa to be crushed in matter machine；
(8) it is sieved, carboxymethylcellulose sodium solution is added and stirs 15min, wherein aluminium film and carboxymethylcellulose sodium solution
Ratio be 2g:7mL；
(9) 13wt% nano zero valence iron is added dropwise, continues to stir 15min, not open close nitrogen in reaction；
(10) it filters, is washed 3 times with dehydrated alcohol, dry modified Nano flake aluminum；
(11) by 8 parts of nanometer multidimensional silver powder, 4 parts of modified Nano flake aluminums, 2 parts of bismuth oxides, 4 parts of titanium nitrides, 18 parts of rouge
Fat alcohol polyethenoxy ether sodium sulfate and 25 parts of deionized water mixing, are placed in planetary ball mill the ball milling at revolving speed 500r/min
11h；
(12) it filters, is put into vacuum oven and dries；
(13) 8 parts of polyvinylpyrrolidones, 4 parts of ethylene-vinyl acetate copolymers, 40 parts of α-terpineols are added, are placed in row
Ball milling 9h in celestial body grinding machine；
(14) it moves into three-roll grinder and further grinds 45min to obtain the final product.
Embodiment 4
A kind of preparation method of electronic device electrode slurry, ingredient is by weight, comprising the following steps:
(1) silver nitrate aqueous solution of 9 parts of 1.5mmol/L is prepared, and adjusting pH value with concentrated nitric acid is 1, prepares 9 parts of 5mmol/
The glucose solution of L, and adjusting pH value with concentrated nitric acid is 1, prepares the polyvinylpyrrolidonesolution solution of 35 parts of 10wt%；
(2) silver nitrate aqueous solution and 18 parts of polyvinylpyrrolidonesolution solutions are uniformly mixed to obtain solution A, glucose is water-soluble
Liquid and 18 parts of polyvinylpyrrolidonesolution solutions are uniformly mixed to obtain solution B；
(3) at 29 DEG C of temperature, mixing speed 380r/min, solution B is added rapidly in solution A, reacts 25min；
(4) it is centrifuged, is washed 4 times with deionized water and dehydrated alcohol respectively, dry nanometer multidimensional silver powder；
(5) it is coated with one layer of peeling layer resin in PET film, is dried at 135 DEG C；
(6) it is put into vacuum coating equipment, vacuumizes, when vacuum degree reaches 10-9When Pa, the aluminium made on evaporation boat is begun to warm up
Silk melts, evaporates, and starts to be deposited, obtains PET aluminizer；
(7) it is put into aluminium film stripping machine, is stripped down aluminium film with solvent, remove solvent with seperator, it is equal to be put into high pressure
It is high-pressure homogeneous at pressure 140MPa to be crushed in matter machine；
(8) it is sieved, carboxymethylcellulose sodium solution is added and stirs 15min, wherein aluminium film and carboxymethylcellulose sodium solution
Ratio be 2g:7mL；
(9) 14wt% nano zero valence iron is added dropwise, continues to stir 18min, not open close nitrogen in reaction；
(10) it filters, is washed 3 times with dehydrated alcohol, dry modified Nano flake aluminum；
(11) by 9 parts of nanometer multidimensional silver powder, 4.5 parts of modified Nano flake aluminums, 2.5 parts of bismuth oxides, 4.5 parts of titanium nitrides,
20 parts of modified soy bean lipoids and 25 parts of deionized water mixing, are placed in planetary ball mill the ball milling 11h at revolving speed 550r/min；
(12) it filters, is put into vacuum oven and dries；
(13) 9 parts of polyvinylpyrrolidones, 4.5 parts of ethylene-vinyl acetate copolymers, 45 parts of α-terpineols are added, are placed in
Ball milling 9h in planetary ball mill；
(14) it moves into three-roll grinder and further grinds 50min to obtain the final product.
Embodiment 5
A kind of preparation method of electronic device electrode slurry, ingredient is by weight, comprising the following steps:
(1) silver nitrate aqueous solution of 10 parts of 1.5mmol/L is prepared, and adjusting pH value with concentrated nitric acid is 1, prepares 10 parts
The glucose solution of 5mmol/L, and adjusting pH value with concentrated nitric acid is 1, the polyvinylpyrrolidone for preparing 40 parts of 10wt% is molten
Liquid；
(2) silver nitrate aqueous solution and 20 parts of polyvinylpyrrolidonesolution solutions are uniformly mixed to obtain solution A, glucose is water-soluble
Liquid and 20 parts of polyvinylpyrrolidonesolution solutions are uniformly mixed to obtain solution B；
(3) at 30 DEG C of temperature, mixing speed 400r/min, solution B is added rapidly in solution A, reacts 30min；
(4) it is centrifuged, is washed 5 times with deionized water and dehydrated alcohol respectively, dry nanometer multidimensional silver powder；
(5) it is coated with one layer of peeling layer resin in PET film, is dried at 140 DEG C；
(6) it is put into vacuum coating equipment, vacuumizes, when vacuum degree reaches 10-9When Pa, the aluminium made on evaporation boat is begun to warm up
Silk melts, evaporates, and starts to be deposited, obtains PET aluminizer；
(7) it is put into aluminium film stripping machine, is stripped down aluminium film with solvent, remove solvent with seperator, it is equal to be put into high pressure
It is high-pressure homogeneous at pressure 150MPa to be crushed in matter machine；
(8) it is sieved, carboxymethylcellulose sodium solution is added and stirs 20min, wherein aluminium film and carboxymethylcellulose sodium solution
Ratio be 2g:7mL；
(9) 15wt% nano zero valence iron is added dropwise, continues to stir 20min, not open close nitrogen in reaction；
(10) it filters, is washed 3 times with dehydrated alcohol, dry modified Nano flake aluminum；
(11) by 10 parts of nanometer multidimensional silver powder, 5 parts of modified Nano flake aluminums, 3 parts of bismuth oxides, 5 parts of titanium nitrides, 25 parts of lists
Tristerin and 30 parts of deionized water mixing, are placed in planetary ball mill the ball milling 12h at revolving speed 600r/min；
(12) it filters, is put into vacuum oven and dries；
(13) 10 parts of polyvinylpyrrolidones, 5 parts of ethylene-vinyl acetate copolymers, 50 parts of α-terpineols are added, are placed in row
Ball milling 10h in celestial body grinding machine；
(14) it moves into three-roll grinder and further grinds 60min to obtain the final product.
It is sintered after the slurry of the method for the present invention preparation is carried out coating, with a thickness of 8 μm, is sintered at 750 DEG C, according to
National standard measures its electric conductivity and adhesion.
The partial properties index of 1 electronic device electrode slurry of table
The slurry of the method for the present invention preparation forms fine and close film layer after sintering, this film layer resistance is low, and minimum is only 1.7
Ω, electric conductivity is good, while its adhesive force is up to 0.99kgf/mm2, there is very strong adhesive force, it is good with interface attachment.
Claims (5)
1. a kind of preparation method of electronic device electrode slurry, it is characterised in that: ingredient is by weight, comprising the following steps:
(1) silver nitrate aqueous solution of 5-10 parts of 1.5mmol/L is prepared, and adjusting pH value with concentrated nitric acid is 1, prepares 5-10 parts
The glucose solution of 5mmol/L, and adjusting pH value with concentrated nitric acid is 1, prepares the polyvinylpyrrolidone of 20-40 parts of 10wt%
Solution；
(2) silver nitrate aqueous solution and 10-20 parts of polyvinylpyrrolidonesolution solutions are uniformly mixed to obtain solution A, glucose is water-soluble
Liquid and 10-20 parts of polyvinylpyrrolidonesolution solutions are uniformly mixed to obtain solution B；
(3) at 25-30 DEG C of temperature, mixing speed 300-400r/min, solution B is added rapidly in solution A, reacts 20-
30min；
(4) it is centrifuged, is washed 3-5 times with deionized water and dehydrated alcohol respectively, dry nanometer multidimensional silver powder；
(5) it is coated with one layer of peeling layer resin in PET film, is dried at 120-140 DEG C；
(6) it is put into vacuum coating equipment, vacuumizes, when vacuum degree reaches 10-9When Pa, beginning to warm up melts the aluminium wire on evaporation boat
Change, evaporation, starts to be deposited, obtain PET aluminizer；
(7) it is put into aluminium film stripping machine, is stripped down aluminium film with solvent, remove solvent with seperator, be put into high pressure homogenizer
In, it is high-pressure homogeneous at pressure 100-150MPa to be crushed；
(8) it is sieved, carboxymethylcellulose sodium solution is added and stirs 10-20min；
(9) 10-15wt% nano zero valence iron is added dropwise, continues to stir 10-20min, not open close nitrogen in reaction；
(10) it filters, is washed 2-3 times with dehydrated alcohol, dry modified Nano flake aluminum；
(11) by 5-10 parts of nanometer multidimensional silver powder, 3-5 parts of modified Nano flake aluminums, 1-3 parts of bismuth oxides, 3-5 parts of titanium nitrides,
10-25 parts of surfactants and 20-30 parts of deionized water mixing, are placed in planetary ball mill the ball at revolving speed 400-600r/min
Grind 10-12h；
(12) it filters, is put into vacuum oven and dries；
(13) 5-10 parts of polyvinylpyrrolidones, 3-5 parts of ethylene-vinyl acetate copolymers, 30-50 parts of α-terpineols are added, set
The ball milling 8-10h in planetary ball mill；
(14) it moves into three-roll grinder and further grinds 30-60min to obtain the final product.
2. a kind of preparation method of electronic device electrode slurry according to claim 1, it is characterised in that: the surface is living
Property agent be sodium lignin sulfonate, sodium sulfate of polyethenoxy ether of fatty alcohol, modified soy bean lipoid or glycerin monostearate in one
Kind is several.
3. a kind of preparation method of electronic device electrode slurry according to claim 1, it is characterised in that: the nanometer is more
The partial size for tieing up silver powder is 50-200nm.
4. a kind of preparation method of electronic device electrode slurry according to claim 1, it is characterised in that: the peeling layer
Resin viscosity is 20-28s.
5. a kind of preparation method of electronic device electrode slurry according to claim 1, it is characterised in that: the aluminium film with
The ratio of carboxymethylcellulose sodium solution is 2g:7mL.
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| CN113990964A (en) * | 2021-08-27 | 2022-01-28 | 泰州隆基乐叶光伏科技有限公司 | Electrode paste, solar cell and preparation method thereof |
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Application publication date: 20190524 |