CN106057278A - Photosensitive electrode slurry and preparation method thereof - Google Patents

Photosensitive electrode slurry and preparation method thereof Download PDF

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Publication number
CN106057278A
CN106057278A CN201610633070.XA CN201610633070A CN106057278A CN 106057278 A CN106057278 A CN 106057278A CN 201610633070 A CN201610633070 A CN 201610633070A CN 106057278 A CN106057278 A CN 106057278A
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electrode slurry
parts
preparation
rotating speed
photoactive electrode
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CN106057278B (en
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代长华
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Nanjing Zhengchun Electronic Technology Co ltd
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    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01BCABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B1/00Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
    • H01B1/20Conductive material dispersed in non-conductive organic material
    • H01B1/22Conductive material dispersed in non-conductive organic material the conductive material comprising metals or alloys
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01BCABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B13/00Apparatus or processes specially adapted for manufacturing conductors or cables

Abstract

The invention provides a photosensitive electrode slurry and a preparation method thereof. The preparation method comprises the following steps that (1) acrylic resin, propylene glycol alginate, cellulose nitrate, polyvinyl acetate, terpilenol and isopropanol are mixed and stirred; (2) trimethylolpropane triacrylate, isopropyl thioxanthone and 1-hydroxycyclohexyl phenyl ketone are added and placed in a planetary ball mill for ball milling; (3) glass powder, silica micropowder and spherical nano silver are added, and ball milling is carried out on the glass powder, silica micropowder and spherical nano silver for 10 to 13 hours at the rotating speed of 250-280r/min in the planetary ball mill; (4) filtering is carried out to remove large particles; (5) lauramidopropyl betaine and epoxy soybean oil are added, and ball milling is continued; and (6) and a three-roller grinder carries out rolling to obtain the photosensitive electrode slurry. The photosensitive electrode slurry is high in the light curing efficiency, short in solidification time, very low in resistivity, and high in conductive performance, has a very high adhesion force, and is adhered to the interface well.

Description

A kind of photoactive electrode slurry and preparation method thereof
Technical field
The present invention relates to field of electronic materials, be specifically related to a kind of photoactive electrode slurry and preparation method thereof.
Background technology
Electronic industrial products is both closely bound up with the life of people, and it is again a kind of embodiment of overall national strength, from military project to Aviation, the application of electronic industrial products is ubiquitous, is that overall national strength develops whether powerful important symbol, builds in national economy Considerable status is occupied during if.And as one of the basic material of electronic industrial products, the development of electric slurry Also receiving increasing attention, it is as the important ingredient of electronic industrial material, and its quality and performance are directly determined Quality and the performance of final products are determined.Electric slurry be sufficiently mixed by conductive phase, organic carrier and inorganic binder after, warp Cross the liquid paste of a kind of high degree of dispersion that three-roller rolling is formed, mainly for the manufacture of integrated circuit, resistor, conductor oil Ink, capacitor, electrode of solar battery, printing and high-resolution electric conductor, conducting resinl, sensitive components and other electronics unit device Part.And photonasty electrode slurry is the one in electric slurry, also known as photosensitive paste, it is a kind of with argentum powder as conductive phase, with load The slurry of the high degree of dispersion that body resin, organic solvent, photocuring system, glass dust and organic additive roll through three-roller Material.Photonasty electrode slurry advantage of maximum compared with traditional electric slurry is that it both can pass through screen printing technique Large area is printed, and can make accurate electrode line by photoetching technique again, for current electronics and information industry to integrated, Precise treatment, miniaturization have great importance.
Summary of the invention
Solving the technical problem that: it is an object of the invention to provide a kind of photoactive electrode slurry, Light-Curing Efficiency is high, solidification Time is the shortest, and resistivity is the lowest, and electric conductivity is good, has the strongest adhesive force simultaneously, good with interface attachment.
Technical scheme: a kind of photoactive electrode slurry, is prepared from weight portion by following component: glass dust 4-8 part, silicon are micro- Powder 1-3 part, spherical nano-silver 10-20 part, acrylic resin 1-3 part, propylene glycol alginate 2-4 part, NC Nitroncellulose 2-5 part, Polyvinyl acetate 1-3 part, trimethylolpropane trimethacrylate 2-5 part, lauroylamidopropyl betaine 3-6 part, isopropyl Thioxanthone 2-5 part, 1-hydroxycyclohexyl phenyl ketone 2-4 part, epoxy soybean oil 1-3 part, terpinol 50-80 part, isopropanol 10-30 part.
It is further preferred that described a kind of photoactive electrode slurry, following component it is prepared from weight portion: glass dust 5-7 part, silicon powder 1.5-2.5 part, spherical nano-silver 12-18 part, acrylic resin 1.5-2.5 part, propylene glycol alginate 2.5- 3.5 parts, NC Nitroncellulose 3-4 part, polyvinyl acetate 1.5-2.5 part, trimethylolpropane trimethacrylate 3-4 part, Laurel Amido propyl betaine 4-5 part, isopropyl thioxanthone 3-4 part, 1-hydroxycyclohexyl phenyl ketone 2.5-3.5 part, epoxy are big Oleum Glycines 1.5-2.5 part, terpinol 60-70 part, isopropanol 15-25 part.
The preparation method of above-mentioned photoactive electrode slurry comprises the following steps:
(1) acrylic resin, propylene glycol alginate, NC Nitroncellulose, polyvinyl acetate, terpinol and isopropanol are mixed, Stir 30-50 minute at temperature 90-95 DEG C, rotating speed 100-130r/min with magnetic stirrer;
(2) add trimethylolpropane trimethacrylate, isopropyl thioxanthone and 1-hydroxycyclohexyl phenyl ketone, be placed in In planetary ball mill under rotating speed 150-200r/min ball milling 1-3 hour;
(3) glass dust, silicon powder and spherical nano-silver are added, with rotating speed 250-280r/min ball milling 10-in planetary ball mill 13 hours;
(4) filter, remove bulky grain;
(5) add lauroylamidopropyl betaine and epoxy soybean oil, continue ball milling 1-2 hour;
(6) put into and carry out rolling 3-4 time on three-roll grinder and get final product.
Further, the preparation method of described a kind of photoactive electrode slurry, in described step (1), temperature is 91-94 DEG C, rotating speed is 110-120r/min, and mixing time is 35-45 minute.
Further, the preparation method of described a kind of photoactive electrode slurry, described step (2) medium speed is 160- 190r/min, Ball-milling Time is 1.5-2.5 hour.
Further, the preparation method of described a kind of photoactive electrode slurry, described step (3) medium speed is 260- 270r/min, Ball-milling Time is 11-12 hour.
Further, the preparation method of described a kind of photoactive electrode slurry, in described step (5), Ball-milling Time is 1.5 hour.
Beneficial effect: the exposure intensity that the film layer pencil hardness of the photoactive electrode slurry of the present invention reaches to need during 6H is only 316mJ/cm2, exposure intensity is the lowest, then its Light-Curing Efficiency is high, and hardening time is the shortest, and its resistivity is the lowest, minimum is only 6.97×10-3Ω cm, electric conductivity is good, and its adhesive force is up to 0.89kgf/mm simultaneously2, there is the strongest adhesive force, with boundary Face attachment is good.
Detailed description of the invention
Embodiment 1
A kind of photoactive electrode slurry, is prepared from weight portion by following component: 4 parts of glass dust, silicon powder 1 part, ball shaped nano Silver 10 parts, acrylic resin 1 part, propylene glycol alginate 2 parts, NC Nitroncellulose 2 parts, polyvinyl acetate 1 part, trihydroxy methyl third Alkane triacrylate 2 parts, lauroylamidopropyl betaine 3 parts, isopropyl thioxanthone 2 parts, 1-hydroxycyclohexyl phenyl ketone 2 Part, epoxy soybean oil 1 part, terpinol 50 parts, isopropanol 10 parts.
The preparation method of above-mentioned photoactive electrode slurry is: (1) by acrylic resin, propylene glycol alginate, NC Nitroncellulose, Polyvinyl acetate, terpinol and isopropanol mixing, with magnetic stirrer temperature 90 DEG C, stir 30 points under rotating speed 100r/min Clock;(2) add trimethylolpropane trimethacrylate, isopropyl thioxanthone and 1-hydroxycyclohexyl phenyl ketone, be placed in row In celestial body grinding machine under rotating speed 150r/min ball milling 1 hour;(3) glass dust, silicon powder and spherical nano-silver, celestial body of being expert at are added With rotating speed 250r/min ball milling 10 hours in grinding machine;(4) filter, remove bulky grain;(5) add lauroylamidopropyl betaine and Epoxy soybean oil, continues ball milling 1 hour;(6) put into and carry out on three-roll grinder rolling 3 times and get final product.
Embodiment 2
A kind of photoactive electrode slurry, is prepared from weight portion by following component: 5 parts of glass dust, silicon powder 1.5 parts, spherical receive Rice silver 12 parts, acrylic resin 1.5 parts, propylene glycol alginate 2.5 parts, NC Nitroncellulose 3 parts, polyvinyl acetate 1.5 parts, three Hydroxymethyl-propane triacrylate 3 parts, lauroylamidopropyl betaine 4 parts, isopropyl thioxanthone 3 parts, 1-hydroxy-cyclohexyl Phenyl ketone 2.5 parts, epoxy soybean oil 1.5 parts, terpinol 60 parts, isopropanol 15 parts.
The preparation method of above-mentioned photoactive electrode slurry is: (1) by acrylic resin, propylene glycol alginate, NC Nitroncellulose, Polyvinyl acetate, terpinol and isopropanol mixing, with magnetic stirrer temperature 91 DEG C, stir 35 points under rotating speed 110r/min Clock;(2) add trimethylolpropane trimethacrylate, isopropyl thioxanthone and 1-hydroxycyclohexyl phenyl ketone, be placed in row In celestial body grinding machine under rotating speed 160r/min ball milling 1.5 hours;(3) glass dust, silicon powder and spherical nano-silver are added, at planet With rotating speed 260r/min ball milling 11 hours in ball mill;(4) filter, remove bulky grain;(5) lauroylamidopropyl betaine is added And epoxy soybean oil, continue ball milling 1.5 hours;(6) put into and carry out on three-roll grinder rolling 3 times and get final product.
Embodiment 3
A kind of photoactive electrode slurry, is prepared from weight portion by following component: 6 parts of glass dust, silicon powder 2 parts, ball shaped nano Silver 15 parts, acrylic resin 2 parts, propylene glycol alginate 2-4 part, NC Nitroncellulose 3.5 parts, polyvinyl acetate 2 parts, three hydroxyl first Base propane triacrylate 3.5 parts, lauroylamidopropyl betaine 3-6 part, isopropyl thioxanthone 3.5 parts, 1-hydroxy cyclohexylphenyl Base phenyl ketone 3 parts, epoxy soybean oil 2 parts, terpinol 65 parts, isopropanol 20 parts.
The preparation method of above-mentioned photoactive electrode slurry is: (1) by acrylic resin, propylene glycol alginate, NC Nitroncellulose, Polyvinyl acetate, terpinol and isopropanol mixing, with magnetic stirrer temperature 92 DEG C, stir 40 points under rotating speed 115r/min Clock;(2) add trimethylolpropane trimethacrylate, isopropyl thioxanthone and 1-hydroxycyclohexyl phenyl ketone, be placed in row In celestial body grinding machine under rotating speed 175r/min ball milling 2 hours;(3) glass dust, silicon powder and spherical nano-silver, celestial body of being expert at are added With rotating speed 265r/min ball milling 11.5 hours in grinding machine;(4) filter, remove bulky grain;(5) lauroylamidopropyl betaine is added And epoxy soybean oil, continue ball milling 1.5 hours;(6) put into and carry out on three-roll grinder rolling 4 times and get final product.
Embodiment 4
A kind of photoactive electrode slurry, is prepared from weight portion by following component: 7 parts of glass dust, silicon powder 2.5 parts, spherical receive Rice silver 18 parts, acrylic resin 2.5 parts, propylene glycol alginate 3.5 parts, NC Nitroncellulose 4 parts, polyvinyl acetate 2.5 parts, three Hydroxymethyl-propane triacrylate 4 parts, lauroylamidopropyl betaine 5 parts, isopropyl thioxanthone 4 parts, 1-hydroxy-cyclohexyl Phenyl ketone 3.5 parts, epoxy soybean oil 2.5 parts, terpinol 70 parts, isopropanol 25 parts.
The preparation method of above-mentioned photoactive electrode slurry is: (1) by acrylic resin, propylene glycol alginate, NC Nitroncellulose, Polyvinyl acetate, terpinol and isopropanol mixing, with magnetic stirrer temperature 94 DEG C, stir 45 points under rotating speed 120r/min Clock;(2) add trimethylolpropane trimethacrylate, isopropyl thioxanthone and 1-hydroxycyclohexyl phenyl ketone, be placed in row In celestial body grinding machine under rotating speed 190r/min ball milling 2.5 hours;(3) glass dust, silicon powder and spherical nano-silver are added, at planet With rotating speed 270r/min ball milling 12 hours in ball mill;(4) filter, remove bulky grain;(5) lauroylamidopropyl betaine is added And epoxy soybean oil, continue ball milling 1.5 hours;(6) put into and carry out on three-roll grinder rolling 4 times and get final product.
Embodiment 5
A kind of photoactive electrode slurry, is prepared from weight portion by following component: 8 parts of glass dust, silicon powder 3 parts, ball shaped nano Silver 20 parts, acrylic resin 3 parts, propylene glycol alginate 4 parts, NC Nitroncellulose 5 parts, polyvinyl acetate 3 parts, trihydroxy methyl third Alkane triacrylate 5 parts, lauroylamidopropyl betaine 6 parts, isopropyl thioxanthone 5 parts, 1-hydroxycyclohexyl phenyl ketone 4 Part, epoxy soybean oil 3 parts, terpinol 80 parts, isopropanol 30 parts.
The preparation method of above-mentioned photoactive electrode slurry is: (1) by acrylic resin, propylene glycol alginate, NC Nitroncellulose, Polyvinyl acetate, terpinol and isopropanol mixing, with magnetic stirrer temperature 95 DEG C, stir 50 points under rotating speed 130r/min Clock;(2) add trimethylolpropane trimethacrylate, isopropyl thioxanthone and 1-hydroxycyclohexyl phenyl ketone, be placed in row In celestial body grinding machine under rotating speed 200r/min ball milling 3 hours;(3) glass dust, silicon powder and spherical nano-silver, celestial body of being expert at are added With rotating speed 280r/min ball milling 13 hours in grinding machine;(4) filter, remove bulky grain;(5) add lauroylamidopropyl betaine and Epoxy soybean oil, continues ball milling 2 hours;(6) put into and carry out on three-roll grinder rolling 4 times and get final product.
Comparative example 1
The present embodiment is not contain NC Nitroncellulose and polyvinyl acetate with the difference of embodiment 5.Specifically:
A kind of photoactive electrode slurry, is prepared from weight portion by following component: 8 parts of glass dust, silicon powder 3 parts, ball shaped nano Silver 20 parts, acrylic resin 3 parts, propylene glycol alginate 4 parts, trimethylolpropane trimethacrylate 5 parts, dodecanamide propyl are sweet 6 parts of dish alkali, isopropyl thioxanthone 5 parts, 1-hydroxycyclohexyl phenyl ketone 4 parts, epoxy soybean oil 3 parts, terpinol 80 parts, different Propanol 30 parts.
The preparation method of above-mentioned photoactive electrode slurry is: (1) is by acrylic resin, propylene glycol alginate, terpinol and different Propanol mixes, and with magnetic stirrer temperature 95 DEG C, stirs 50 minutes under rotating speed 130r/min;(2) trimethylolpropane is added Triacrylate, isopropyl thioxanthone and 1-hydroxycyclohexyl phenyl ketone, be placed in planetary ball mill at rotating speed 200r/ Ball milling 3 hours under min;(3) glass dust, silicon powder and spherical nano-silver are added, with rotating speed 280r/min in planetary ball mill Ball milling 13 hours;(4) filter, remove bulky grain;(5) add lauroylamidopropyl betaine and epoxy soybean oil, continue ball milling 2 Hour;(6) put into and carry out on three-roll grinder rolling 4 times and get final product.
Comparative example 2
The present embodiment is not contain acrylic resin and propylene glycol alginate with the difference of embodiment 5.Specifically:
A kind of photoactive electrode slurry, is prepared from weight portion by following component: 8 parts of glass dust, silicon powder 3 parts, ball shaped nano Silver 20 parts, NC Nitroncellulose 5 parts, polyvinyl acetate 3 parts, trimethylolpropane trimethacrylate 5 parts, dodecanamide propyl are sweet 6 parts of dish alkali, isopropyl thioxanthone 5 parts, 1-hydroxycyclohexyl phenyl ketone 4 parts, epoxy soybean oil 3 parts, terpinol 80 parts, different Propanol 30 parts.
The preparation method of above-mentioned photoactive electrode slurry is: (1) is by NC Nitroncellulose, polyvinyl acetate, terpinol and different Propanol mixes, and with magnetic stirrer temperature 95 DEG C, stirs 50 minutes under rotating speed 130r/min;(2) trimethylolpropane is added Triacrylate, isopropyl thioxanthone and 1-hydroxycyclohexyl phenyl ketone, be placed in planetary ball mill at rotating speed 200r/ Ball milling 3 hours under min;(3) glass dust, silicon powder and spherical nano-silver are added, with rotating speed 280r/min in planetary ball mill Ball milling 13 hours;(4) filter, remove bulky grain;(5) add lauroylamidopropyl betaine and epoxy soybean oil, continue ball milling 2 Hour;(6) put into and carry out on three-roll grinder rolling 4 times and get final product.
The partial properties index of material of the present invention see table, during it may be seen that this film layer pencil hardness reaches 6H The exposure intensity needed is only 316mJ/cm2, exposure intensity is the lowest, then its Light-Curing Efficiency is high, and hardening time is the shortest, its resistance Rate is the lowest, and minimum only 6.97 × 10-3Ω cm, electric conductivity is good, and its adhesive force is up to 0.89kgf/mm simultaneously2, have very Strong adhesive force is good with interface attachment.
The partial properties index of table 1 photoactive electrode slurry
Name of product Exposure intensity (mJ/cm2) Resistivity (Ω cm) Adhesive force (kgf/mm2)
Embodiment 1 325 7.05×10-3 0.87
Embodiment 2 321 7.03×10-3 0.88
Embodiment 3 319 6.99×10-3 0.88
Embodiment 4 316 6.97×10-3 0.89
Embodiment 5 318 7.02×10-3 0.88
Comparative example 1 327 7.06×10-3 0.77
Comparative example 2 336 7.04×10-3 0.81
Note: exposure intensity is the exposure intensity that film layer pencil hardness reaches to need during 6H.

Claims (7)

1. a photoactive electrode slurry, it is characterised in that: it is prepared from weight portion by following component: glass dust 4-8 part, silicon are micro- Powder 1-3 part, spherical nano-silver 10-20 part, acrylic resin 1-3 part, propylene glycol alginate 2-4 part, NC Nitroncellulose 2-5 part, Polyvinyl acetate 1-3 part, trimethylolpropane trimethacrylate 2-5 part, lauroylamidopropyl betaine 3-6 part, isopropyl Thioxanthone 2-5 part, 1-hydroxycyclohexyl phenyl ketone 2-4 part, epoxy soybean oil 1-3 part, terpinol 50-80 part, isopropanol 10-30 part.
A kind of photoactive electrode slurry the most according to claim 1, it is characterised in that: by following component with weight portion preparation Become: glass dust 5-7 part, silicon powder 1.5-2.5 part, spherical nano-silver 12-18 part, acrylic resin 1.5-2.5 part, alginic acid the third two Alcohol ester 2.5-3.5 part, NC Nitroncellulose 3-4 part, polyvinyl acetate 1.5-2.5 part, trimethylolpropane trimethacrylate 3-4 Part, lauroylamidopropyl betaine 4-5 part, isopropyl thioxanthone 3-4 part, 1-hydroxycyclohexyl phenyl ketone 2.5-3.5 part, Epoxy soybean oil 1.5-2.5 part, terpinol 60-70 part, isopropanol 15-25 part.
3. the preparation method of a kind of photoactive electrode slurry described in any one of claim 1 to 2, it is characterised in that: include following Step:
(1) acrylic resin, propylene glycol alginate, NC Nitroncellulose, polyvinyl acetate, terpinol and isopropanol are mixed, Stir 30-50 minute at temperature 90-95 DEG C, rotating speed 100-130r/min with magnetic stirrer;
(2) add trimethylolpropane trimethacrylate, isopropyl thioxanthone and 1-hydroxycyclohexyl phenyl ketone, be placed in In planetary ball mill under rotating speed 150-200r/min ball milling 1-3 hour;
(3) glass dust, silicon powder and spherical nano-silver are added, with rotating speed 250-280r/min ball milling 10-in planetary ball mill 13 hours;
(4) filter, remove bulky grain;
(5) add lauroylamidopropyl betaine and epoxy soybean oil, continue ball milling 1-2 hour;
(6) put into and carry out rolling 3-4 time on three-roll grinder and get final product.
The preparation method of a kind of photoactive electrode slurry the most according to claim 3, it is characterised in that: in described step (1) Temperature is 91-94 DEG C, and rotating speed is 110-120r/min, and mixing time is 35-45 minute.
The preparation method of a kind of photoactive electrode slurry the most according to claim 3, it is characterised in that: in described step (2) Rotating speed is 160-190r/min, and Ball-milling Time is 1.5-2.5 hour.
The preparation method of a kind of photoactive electrode slurry the most according to claim 3, it is characterised in that: in described step (3) Rotating speed is 260-270r/min, and Ball-milling Time is 11-12 hour.
The preparation method of a kind of photoactive electrode slurry the most according to claim 3, it is characterised in that: in described step (5) Ball-milling Time is 1.5 hours.
CN201610633070.XA 2016-08-05 2016-08-05 A kind of photoactive electrode slurry and preparation method thereof Active CN106057278B (en)

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Publication number Priority date Publication date Assignee Title
CN109461516A (en) * 2018-11-07 2019-03-12 刘紫嫣 A kind of conductive silver glue and preparation method thereof
CN109686498A (en) * 2018-12-25 2019-04-26 深圳市欧科力科技有限公司 A kind of preparation method of photoactive electrode slurry

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CN102969039A (en) * 2012-10-31 2013-03-13 彩虹集团公司 Photosensitive conductive silver electrode slurry and preparation method thereof
CN104966544A (en) * 2015-05-26 2015-10-07 富泰华工业(深圳)有限公司 Photosensitive silver paste and touch screen and electronic apparatus employing photosensitive silver paste

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CN101718953A (en) * 2008-10-09 2010-06-02 北京印刷学院 Ultraviolet light curing conductive silver slurry for manufacturing radio frequency identification (RFID) tag antenna
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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109461516A (en) * 2018-11-07 2019-03-12 刘紫嫣 A kind of conductive silver glue and preparation method thereof
CN109686498A (en) * 2018-12-25 2019-04-26 深圳市欧科力科技有限公司 A kind of preparation method of photoactive electrode slurry

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Denomination of invention: Photosensitive electrode slurry and preparation method thereof

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Denomination of invention: A photosensitive electrode slurry and its preparation method

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