CN109686498A - A kind of preparation method of photoactive electrode slurry - Google Patents
A kind of preparation method of photoactive electrode slurry Download PDFInfo
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- CN109686498A CN109686498A CN201811587553.6A CN201811587553A CN109686498A CN 109686498 A CN109686498 A CN 109686498A CN 201811587553 A CN201811587553 A CN 201811587553A CN 109686498 A CN109686498 A CN 109686498A
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- electrode slurry
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B13/00—Apparatus or processes specially adapted for manufacturing conductors or cables
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/20—Conductive material dispersed in non-conductive organic material
- H01B1/22—Conductive material dispersed in non-conductive organic material the conductive material comprising metals or alloys
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Abstract
The present invention provides a kind of preparation methods of photoactive electrode slurry, and steps are as follows: the own alditol lactone aqueous solution of L-3- oxo Soviet Union being heated, polyethylene glycol 200 aqueous solution is added, stirs to obtain mixed liquor；Cicada's wings is taken, is impregnated in silver nitrate solution；Mixed liquor stirring is added, stands；Completely reacted cicada's wings is taken out, is dried in vacuo；It is placed in vacuum tube furnace, vacuumizes, heat up, heat preservation；It is cooled to room temperature, is ground into the silver powder with special construction；Acrylic resin, polyvinyl acetate, hydroxypropyl PASELLI EASYGEL and 1,3 butylene glycol are mixed；Add photosensitive monomer, photoinitiator, is placed in ball milling in planetary ball mill；Add glass powder, silver powder and turkey red oil, the ball milling in planetary ball mill；It is put on three-roll grinder and is rolled to obtain the final product.The photoactive electrode slurry Light-Curing Efficiency of the method for the present invention preparation is high, and curing time is shorter, while its sheet resistance is very low, and electric conductivity is good, has very strong adhesive force, good with interface attachment.
Description
Technical field
The present invention relates to a kind of preparation methods of photoactive electrode slurry.
Background technique
Basic material of the electric slurry as electronics and information industry has different classification methods according to property difference.And it is thick
Film electric slurry is then the electric slurry most common kind on the market, always along with the development of electronics and information industry and
It constantly updates.Thick-film electronic slurry mainly includes mainly monomer slurry, alloy pulp, You Jijin based on metallic conductor slurry
Belong to slurry and photoactive electrode slurry.Wherein, photosensitive paste is one kind using silver powder as conductive phase, with vector resin, organic solvent, light
The slurry of curing system, glass powder and organic additive by high degree of dispersion made of three-roller rolling.Photoactive electrode slurry phase
Advantage more maximum than traditional electric slurry is that it can not only printed by screen printing technique large area, but also can pass through
Photoetching technique produces accurate electrode line, and the electrode line width as made from photoactive electrode slurry method can achieve 30-50 μ
M, even and traditional silk-screen printing technique under conditions of most harsh, the electrode line width produced is minimum also to be can only achieve
80 μm, therefore in current electronics and information industry develops to the direction of integrated, precise treatment, miniaturization, photoactive electrode slurry
Development, which seems, to be even more important.
Summary of the invention
Technical problems to be solved:
A kind of preparation method of photoactive electrode slurry is provided, the slurry Light-Curing Efficiency is high, and curing time is shorter, while its
Sheet resistance is very low, and electric conductivity is good, has very strong adhesive force, good with interface attachment.
Technical solution:
The present invention provides a kind of preparation methods of photoactive electrode slurry, and ingredient is by weight, comprising the following steps:
(1) the own alditol lactone aqueous solution of L-3- oxo Soviet Union that compound concentration is 25-30g/L, compound concentration 10-15mL/L
Polyethylene glycol 200 aqueous solution；
(2) the own alditol lactone aqueous solution of L-3- oxo Soviet Union is heated to 40-45 DEG C, is added at revolving speed 400-600rpm poly-
200 aqueous solution of ethylene glycol, stirring 10-20min obtain mixed liquor；
(3) cicada's wings is taken, is impregnated in silver nitrate solution, and is 3-4 with the pH of hydrochloric acid conditioning solution, is soaked at 30-35 DEG C
Stain 3-4d；
(4) mixed liquor is added and stirs 5-10min, stand 30-40min；
(5) completely reacted cicada's wings is taken out, is put into vacuum oven, vacuum drying；
(6) it is placed in vacuum tube furnace, vacuumizes, be warming up to 400-500 DEG C, keep the temperature 2h；
(7) cooled to room temperature is ground into the silver powder with special construction；
(8) by 1-3 parts of acrylic resins, 1-3 parts of polyvinyl acetate, 2-4 parts of hydroxypropyl PASELLI EASYGELs and 50-80
Part 1,3-BDO mixing, stirs 30-40min under 90-95 DEG C of temperature, revolving speed 300-400rpm with magnetic stirrer；
(9) 10-20 parts of photosensitive monomers, 1-3 parts of photoinitiators are added, are placed in planetary ball mill in revolving speed 200-300rpm
Lower ball milling 1-3h；
(10) 4-8 parts of glass powders, 10-20 parts of silver powder and 2-4 parts of turkey red oils are added, with revolving speed in planetary ball mill
250-280rpm ball milling 10-12h；
(11) it is put on three-roll grinder and is rolled, until 3 μm of slurry fineness < is to get photoactive electrode slurry.Into one
Step, the photosensitive monomer is trimethylolpropane trimethacrylate, pentaerythritol triacrylate or dipentaerythritol 5 third
Olefin(e) acid ester.
Further, the photoinitiator is 2- methyl-1-(4- methyl mercapto phenyl)-2- morpholinyl-1- acetone or isopropyl
One or both of base thioxanthone.
Further, heating rate is 3 DEG C/min in the step (6).
Further, 2 μm of partial size < of silver powder in the step (7).
The utility model has the advantages that
It is face or line contact each other when 1. silver powder is as filler conduction, so that network structure is formed, it is prepared by the present invention
Silver powder has special structure, and resistance is much lower far beyond spherical point contact, or even compared with low silver content and relatively thin printed coating
When still there is very high conductivity.
2. be added turkey red oil after, silver conductive film surface distribution can more uniform densification, sheet resistance also therefore and reduce.
3. photoactive electrode slurry of the present invention, the exposure intensity needed when film layer pencil hardness reaches 6H are only 311mJ/
cm2, exposure intensity is lower, then its Light-Curing Efficiency is high, and curing time is shorter, while its sheet resistance is very low, and minimum only 3.97 Ω/
, electric conductivity is good, while its adhesive force is up to 0.94kgf/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 photoactive electrode slurry, ingredient is by weight, comprising the following steps:
(1) the own alditol lactone aqueous solution of L-3- oxo Soviet Union that compound concentration is 25g/L, compound concentration is the poly- second of 10mL/L
200 aqueous solution of glycol；
(2) the own alditol lactone aqueous solution of L-3- oxo Soviet Union is heated to 40 DEG C, polyethylene glycol is added at revolving speed 400rpm
200 aqueous solutions, stirring 10min obtain mixed liquor；
(3) cicada's wings is taken, is impregnated in silver nitrate solution, and is 3 with the pH of hydrochloric acid conditioning solution, impregnates 3d at 30 DEG C；
(4) mixed liquor is added and stirs 5min, stand 30min；
(5) completely reacted cicada's wings is taken out, is put into vacuum oven, vacuum drying；
(6) it is placed in vacuum tube furnace, vacuumizes, be warming up to 400 DEG C with the heating rate of 3 DEG C/min, keep the temperature 2h；
(7) cooled to room temperature is ground into the silver powder with 2 μm of special construction partial size <；
(8) by 1 part of acrylic resin, 1 part of polyvinyl acetate, 2 parts of hydroxypropyl PASELLI EASYGELs and 50 parts of 1,3- fourths
Glycol mixing, stirs 30min under 90 DEG C of temperature, revolving speed 300rpm with magnetic stirrer；
(9) 10 parts of trimethylolpropane trimethacrylates, 1 part of 2- methyl-1-(4- methyl mercapto phenyl)-2- morpholine are added
Base -1- acetone is placed in planetary ball mill the ball milling 1h at revolving speed 200rpm；
(10) 4 parts of glass powders, 10 parts of silver powder and 2 parts of turkey red oils are added, with revolving speed 250rpm in planetary ball mill
Ball milling 10h；
(11) it is put on three-roll grinder and is rolled, until 3 μm of slurry fineness < is to get photoactive electrode slurry.
Embodiment 2
A kind of preparation method of photoactive electrode slurry, ingredient is by weight, comprising the following steps:
(1) the own alditol lactone aqueous solution of L-3- oxo Soviet Union that compound concentration is 27g/L, compound concentration is the poly- second of 12mL/L
200 aqueous solution of glycol；
(2) the own alditol lactone aqueous solution of L-3- oxo Soviet Union is heated to 42 DEG C, polyethylene glycol is added at revolving speed 450rpm
200 aqueous solutions, stirring 15min obtain mixed liquor；
(3) cicada's wings is taken, is impregnated in silver nitrate solution, and is 3.5 with the pH of hydrochloric acid conditioning solution, is impregnated at 32 DEG C
3.5d；
(4) mixed liquor is added and stirs 7min, stand 35min；
(5) completely reacted cicada's wings is taken out, is put into vacuum oven, vacuum drying；
(6) it is placed in vacuum tube furnace, vacuumizes, be warming up to 450 DEG C with the heating rate of 3 DEG C/min, keep the temperature 2h；
(7) cooled to room temperature is ground into the silver powder with 2 μm of special construction partial size <；
(8) by 1.5 parts of acrylic resins, 1.5 parts of polyvinyl acetate, 2.5 parts of hydroxypropyl PASELLI EASYGELs and 60 parts
1,3-BDO mixing, stirs 35min under 92 DEG C of temperature, revolving speed 350rpm with magnetic stirrer；
(9) 13 parts of pentaerythritol triacrylates, 1.5 parts of isopropyl thioxanthones are added, are placed in planetary ball mill
Ball milling 1.5h under revolving speed 250rpm；
(10) 5 parts of glass powders, 12 parts of silver powder and 2.5 parts of turkey red oils are added, with revolving speed in planetary ball mill
260rpm ball milling 10.5h；
(11) it is put on three-roll grinder and is rolled, until 3 μm of slurry fineness < is to get photoactive electrode slurry.
Embodiment 3
A kind of preparation method of photoactive electrode slurry, ingredient is by weight, comprising the following steps:
(1) the own alditol lactone aqueous solution of L-3- oxo Soviet Union that compound concentration is 28g/L, compound concentration is the poly- second of 13mL/L
200 aqueous solution of glycol；
(2) the own alditol lactone aqueous solution of L-3- oxo Soviet Union is heated to 43 DEG C, polyethylene glycol is added at revolving speed 500rpm
200 aqueous solutions, stirring 15min obtain mixed liquor；
(3) cicada's wings is taken, is impregnated in silver nitrate solution, and is 3.5 with the pH of hydrochloric acid conditioning solution, is impregnated at 33 DEG C
3.5d；
(4) mixed liquor is added and stirs 8min, stand 35min；
(5) completely reacted cicada's wings is taken out, is put into vacuum oven, vacuum drying；
(6) it is placed in vacuum tube furnace, vacuumizes, be warming up to 450 DEG C with the heating rate of 3 DEG C/min, keep the temperature 2h；
(7) cooled to room temperature is ground into the silver powder with 2 μm of special construction partial size <；
(8) by 2 parts of acrylic resins, 2 parts of polyvinyl acetate, 3 parts of hydroxypropyl PASELLI EASYGELs and 65 parts of 1,3- fourths
Glycol mixing, stirs 35min under 93 DEG C of temperature, revolving speed 350rpm with magnetic stirrer；
(9) 15 parts of double pentaerythritol C5 methacrylates, 1.5 parts of 2- methyl-1s-(4- methyl mercapto phenyl) -2- morpholine are added
Base -1- acetone, 0.5 part of isopropyl thioxanthone, are placed in planetary ball mill the ball milling 2h at revolving speed 250rpm；
(10) 6 parts of glass powders, 15 parts of silver powder and 3 parts of turkey red oils are added, with revolving speed 265rpm in planetary ball mill
Ball milling 11h；
(11) it is put on three-roll grinder and is rolled, until 3 μm of slurry fineness < is to get photoactive electrode slurry.
Embodiment 4
A kind of preparation method of photoactive electrode slurry, ingredient is by weight, comprising the following steps:
(1) the own alditol lactone aqueous solution of L-3- oxo Soviet Union that compound concentration is 29g/L, compound concentration is the poly- second of 14mL/L
200 aqueous solution of glycol；
(2) the own alditol lactone aqueous solution of L-3- oxo Soviet Union is heated to 44 DEG C, polyethylene glycol is added at revolving speed 550rpm
200 aqueous solutions, stirring 15min obtain mixed liquor；
(3) cicada's wings is taken, is impregnated in silver nitrate solution, and is 3.5 with the pH of hydrochloric acid conditioning solution, is impregnated at 34 DEG C
3.5d；
(4) mixed liquor is added and stirs 9min, stand 35min；
(5) completely reacted cicada's wings is taken out, is put into vacuum oven, vacuum drying；
(6) it is placed in vacuum tube furnace, vacuumizes, be warming up to 450 DEG C with the heating rate of 3 DEG C/min, keep the temperature 2h；
(7) cooled to room temperature is ground into the silver powder with 2 μm of special construction partial size <；
(8) by 2.5 parts of acrylic resins, 2.5 parts of polyvinyl acetate, 3.5 parts of hydroxypropyl PASELLI EASYGELs and 70 parts
1,3-BDO mixing, stirs 35min under 94 DEG C of temperature, revolving speed 350rpm with magnetic stirrer；
(9) 19 parts of trimethylolpropane trimethacrylates, 2.5 parts of isopropyl thioxanthones are added, are placed in planetary ball mill
In at revolving speed 250rpm ball milling 2.5h；
(10) 7 parts of glass powders, 18 parts of silver powder and 3.5 parts of turkey red oils are added, with revolving speed in planetary ball mill
270rpm ball milling 11h；
(11) it is put on three-roll grinder and is rolled, until 3 μm of slurry fineness < is to get photoactive electrode slurry.
Embodiment 5
A kind of preparation method of photoactive electrode slurry, ingredient is by weight, comprising the following steps:
(1) the own alditol lactone aqueous solution of L-3- oxo Soviet Union that compound concentration is 30g/L, compound concentration is the poly- second of 15mL/L
200 aqueous solution of glycol；
(2) the own alditol lactone aqueous solution of L-3- oxo Soviet Union is heated to 45 DEG C, polyethylene glycol is added at revolving speed 600rpm
200 aqueous solutions, stirring 20min obtain mixed liquor；
(3) cicada's wings is taken, is impregnated in silver nitrate solution, and is 4 with the pH of hydrochloric acid conditioning solution, impregnates 4d at 35 DEG C；
(4) mixed liquor is added and stirs 10min, stand 40min；
(5) completely reacted cicada's wings is taken out, is put into vacuum oven, vacuum drying；
(6) it is placed in vacuum tube furnace, vacuumizes, be warming up to 500 DEG C with the heating rate of 3 DEG C/min, keep the temperature 2h；
(7) cooled to room temperature is ground into the silver powder with 2 μm of special construction partial size <；
(8) by 3 parts of acrylic resins, 3 parts of polyvinyl acetate, 4 parts of hydroxypropyl PASELLI EASYGELs and 80 parts of 1,3- fourths
Glycol mixing, stirs 40min under 95 DEG C of temperature, revolving speed 400rpm with magnetic stirrer；
(9) 20 parts of pentaerythritol triacrylates, 3 parts of isopropyl thioxanthones are added, is placed in planetary ball mill and is turning
Ball milling 3h under fast 300rpm；
(10) 8 parts of glass powders, 20 parts of silver powder and 4 parts of turkey red oils are added, with revolving speed 280rpm in planetary ball mill
Ball milling 12h；
(11) it is put on three-roll grinder and is rolled, until 3 μm of slurry fineness < is to get photoactive electrode slurry.
Photoactive electrode slurry of the present invention is uniformly coated on the glass sheet, exposure mask is not covered in photocuring, according to GB/
T6739-2006 national standard measures the hardness of cured film with pencil, and measurement film layer pencil hardness reaches the exposure needed when 6H
Intensity.
The measurement of sheet resistance is measured according to GB/T 17473.3-2008 using resistance meter.
The partial properties index of 1 photoactive electrode slurry of table
Photoactive electrode slurry of the present invention, the exposure intensity needed when film layer pencil hardness reaches 6H are only 311mJ/cm2,
Exposure intensity is lower, then its Light-Curing Efficiency is high, and curing time is shorter, while its sheet resistance is very low, and minimum is only 3.97 Ω/,
Electric conductivity is good, while its adhesive force is up to 0.94kgf/mm2, there is very strong adhesive force, it is good with interface attachment.
Claims (5)
1. a kind of preparation method of photoactive electrode slurry, it is characterised in that: ingredient is by weight, comprising the following steps:
(1) the own alditol lactone aqueous solution of L-3- oxo Soviet Union that compound concentration is 25-30g/L, compound concentration are the poly- of 10-15mL/L
200 aqueous solution of ethylene glycol；
(2) the own alditol lactone aqueous solution of L-3- oxo Soviet Union is heated to 40-45 DEG C, poly- second two is added at revolving speed 400-600rpm
200 aqueous solution of alcohol, stirring 10-20min obtain mixed liquor；
(3) cicada's wings is taken, is impregnated in silver nitrate solution, and is 3-4 with the pH of hydrochloric acid conditioning solution, impregnates 3- at 30-35 DEG C
4d；
(4) mixed liquor is added and stirs 5-10min, stand 30-40min；
(5) completely reacted cicada's wings is taken out, is put into vacuum oven, vacuum drying；
(6) it is placed in vacuum tube furnace, vacuumizes, be warming up to 400-500 DEG C, keep the temperature 2h；
(7) cooled to room temperature is ground into the silver powder with special construction；
(8) acrylic resin, polyvinyl acetate, hydroxypropyl PASELLI EASYGEL and 1,3-BDO are mixed, is stirred with magnetic force
It mixes machine and stirs 30-40min under 90-95 DEG C of temperature, revolving speed 300-400rpm；
(9) photosensitive monomer, photoinitiator is added, is placed in ball milling 1-3h in planetary ball mill；
(10) 4-8 parts of glass powders, 10-20 parts of silver powder and 2-4 parts of turkey red oils are added, with revolving speed 250- in planetary ball mill
280rpm ball milling 10-12h；
(11) it is put on three-roll grinder and is rolled, until 3 μm of slurry fineness < is to get photoactive electrode slurry.
2. a kind of preparation method of photoactive electrode slurry according to claim 1, it is characterised in that: the photosensitive monomer is
Trimethylolpropane trimethacrylate, pentaerythritol triacrylate or double pentaerythritol C5 methacrylate.
3. a kind of preparation method of photoactive electrode slurry according to claim 1, it is characterised in that: the photoinitiator is
2- methyl-1-(4- methyl mercapto phenyl) one or both of-2- morpholinyl-1- acetone or isopropyl thioxanthone.
4. a kind of preparation method of photoactive electrode slurry according to claim 1, it is characterised in that: in the step (6)
Heating rate is 3 DEG C/min.
5. a kind of preparation method of photoactive electrode slurry according to claim 1, it is characterised in that: in the step (7)
2 μm of the partial size < of silver powder.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201811587553.6A CN109686498A (en) | 2018-12-25 | 2018-12-25 | A kind of preparation method of photoactive electrode slurry |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201811587553.6A CN109686498A (en) | 2018-12-25 | 2018-12-25 | A kind of preparation method of photoactive electrode slurry |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2006193795A (en) * | 2005-01-14 | 2006-07-27 | Dowa Mining Co Ltd | Spherical silver powder and its production method |
| CN102974839A (en) * | 2012-12-04 | 2013-03-20 | 中山大学 | Method for preparing nanometer flake silver powder through chemical deposition |
| CN104538084A (en) * | 2015-01-08 | 2015-04-22 | 安徽凤阳德诚科技有限公司 | High-temperature-resistant electric conducting silver paste |
| CN105313391A (en) * | 2014-07-29 | 2016-02-10 | 大日本印刷株式会社 | Laminate, conductive laminate, and touch panel |
| CN106057278A (en) * | 2016-08-05 | 2016-10-26 | 代长华 | Photosensitive electrode slurry and preparation method thereof |
| CN107130231A (en) * | 2017-07-03 | 2017-09-05 | 汕头市三宝云母科技股份有限公司 | Nanometer metallic silver coats the preparation method of synthetic fluoromica powder |
-
2018
- 2018-12-25 CN CN201811587553.6A patent/CN109686498A/en not_active Withdrawn
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2006193795A (en) * | 2005-01-14 | 2006-07-27 | Dowa Mining Co Ltd | Spherical silver powder and its production method |
| CN102974839A (en) * | 2012-12-04 | 2013-03-20 | 中山大学 | Method for preparing nanometer flake silver powder through chemical deposition |
| CN105313391A (en) * | 2014-07-29 | 2016-02-10 | 大日本印刷株式会社 | Laminate, conductive laminate, and touch panel |
| CN104538084A (en) * | 2015-01-08 | 2015-04-22 | 安徽凤阳德诚科技有限公司 | High-temperature-resistant electric conducting silver paste |
| CN106057278A (en) * | 2016-08-05 | 2016-10-26 | 代长华 | Photosensitive electrode slurry and preparation method thereof |
| CN107130231A (en) * | 2017-07-03 | 2017-09-05 | 汕头市三宝云母科技股份有限公司 | Nanometer metallic silver coats the preparation method of synthetic fluoromica powder |
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Application publication date: 20190426 |