CN103555067B - Electrically conductive ink of a kind of regulating power and its preparation method and application - Google Patents
Electrically conductive ink of a kind of regulating power and its preparation method and application Download PDFInfo
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- CN103555067B CN103555067B CN201310504189.3A CN201310504189A CN103555067B CN 103555067 B CN103555067 B CN 103555067B CN 201310504189 A CN201310504189 A CN 201310504189A CN 103555067 B CN103555067 B CN 103555067B
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- carbon black
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- 230000001105 regulatory effect Effects 0.000 title claims abstract description 26
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 239000000463 material Substances 0.000 claims abstract description 19
- 239000002245 particle Substances 0.000 claims description 26
- 239000006229 carbon black Substances 0.000 claims description 19
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims description 16
- 229920001903 high density polyethylene Polymers 0.000 claims description 16
- 239000004700 high-density polyethylene Substances 0.000 claims description 16
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 12
- 229920001971 elastomer Polymers 0.000 claims description 12
- 239000005060 rubber Substances 0.000 claims description 12
- 239000003595 mist Substances 0.000 claims description 11
- 238000003801 milling Methods 0.000 claims description 9
- 230000004087 circulation Effects 0.000 claims description 7
- 239000004615 ingredient Substances 0.000 claims description 6
- 238000013508 migration Methods 0.000 claims description 6
- 230000005012 migration Effects 0.000 claims description 6
- 230000005855 radiation Effects 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 5
- 238000010298 pulverizing process Methods 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- 229920001897 terpolymer Polymers 0.000 claims description 5
- NQBXSWAWVZHKBZ-UHFFFAOYSA-N 2-butoxyethyl acetate Chemical compound CCCCOCCOC(C)=O NQBXSWAWVZHKBZ-UHFFFAOYSA-N 0.000 claims description 4
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 4
- 239000005864 Sulphur Substances 0.000 claims description 4
- 239000012046 mixed solvent Substances 0.000 claims description 4
- 235000011837 pasties Nutrition 0.000 claims description 4
- 239000008096 xylene Substances 0.000 claims description 4
- 239000004020 conductor Substances 0.000 abstract description 7
- 239000003960 organic solvent Substances 0.000 abstract description 6
- 230000007423 decrease Effects 0.000 abstract description 3
- 238000004134 energy conservation Methods 0.000 abstract description 3
- 229920000098 polyolefin Polymers 0.000 abstract description 3
- 239000000976 ink Substances 0.000 description 41
- 239000002904 solvent Substances 0.000 description 13
- 238000010438 heat treatment Methods 0.000 description 10
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 6
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 6
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 4
- 150000004945 aromatic hydrocarbons Chemical class 0.000 description 4
- NNBZCPXTIHJBJL-UHFFFAOYSA-N decalin Chemical compound C1CCCC2CCCCC21 NNBZCPXTIHJBJL-UHFFFAOYSA-N 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- XMGQYMWWDOXHJM-UHFFFAOYSA-N limonene Chemical compound CC(=C)C1CCC(C)=CC1 XMGQYMWWDOXHJM-UHFFFAOYSA-N 0.000 description 4
- -1 polyethylene Polymers 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 3
- 150000002576 ketones Chemical class 0.000 description 3
- 150000002632 lipids Chemical class 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- XBDQKXXYIPTUBI-UHFFFAOYSA-M Propionate Chemical compound CCC([O-])=O XBDQKXXYIPTUBI-UHFFFAOYSA-M 0.000 description 2
- KXKVLQRXCPHEJC-UHFFFAOYSA-N acetic acid trimethyl ester Natural products COC(C)=O KXKVLQRXCPHEJC-UHFFFAOYSA-N 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 238000004132 cross linking Methods 0.000 description 2
- JHIVVAPYMSGYDF-UHFFFAOYSA-N cyclohexanone Chemical compound O=C1CCCCC1 JHIVVAPYMSGYDF-UHFFFAOYSA-N 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000008204 material by function Substances 0.000 description 2
- 229910044991 metal oxide Inorganic materials 0.000 description 2
- 150000004706 metal oxides Chemical class 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000003208 petroleum Substances 0.000 description 2
- 229920002981 polyvinylidene fluoride Polymers 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 238000007639 printing Methods 0.000 description 2
- 238000007650 screen-printing Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 229920013649 Paracril Polymers 0.000 description 1
- 239000004698 Polyethylene Substances 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 229920001577 copolymer Polymers 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 239000012776 electronic material Substances 0.000 description 1
- 125000002573 ethenylidene group Chemical group [*]=C=C([H])[H] 0.000 description 1
- 229920006242 ethylene acrylic acid copolymer Polymers 0.000 description 1
- 239000005038 ethylene vinyl acetate Substances 0.000 description 1
- 229920006244 ethylene-ethyl acrylate Polymers 0.000 description 1
- 229920006225 ethylene-methyl acrylate Polymers 0.000 description 1
- 239000005043 ethylene-methyl acrylate Substances 0.000 description 1
- 229920002681 hypalon Polymers 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 229920001200 poly(ethylene-vinyl acetate) Polymers 0.000 description 1
- 229920000573 polyethylene Polymers 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 229920003048 styrene butadiene rubber Polymers 0.000 description 1
Abstract
The present invention relates to electrically conductive ink of a kind of regulating power and its preparation method and application, this electrically conductive ink comprises the component of following massfraction: 4-50% electro-conductive material, 8-30% polyolefins connecting material, 40-86% organic solvent, 2-15% subsidiary material.The electrically conductive ink of this regulating power, has PTC function, can automatic constant-temperature, decreases temperature control component and cost-saving, the advantage such as energy-conservation.
Description
[technical field]
The invention belongs to ink class field of material technology, be specifically related to electrically conductive ink of a kind of regulating power and its preparation method and application.
[background technology]
Electrically conductive ink is a kind of specialty inks with conductivity, is dispersed in a kind of conductive composite material formed in binder, is printed onto after fixing film forming on stock, plays due effect by electrically conductive particles (silver, copper, carbon etc.).Electrically conductive ink is a kind of important electronic material, has huge market in China.
Wherein, the electrical heating element that the electrically conductive ink of regulating power is made has with temperature rising and automatically improves resistance, reduce electric current, reduce the function of power, belong to positive temperature coefficient functional materials (i.e. PTC functional materials), possess the material of PTC performance, greatly can improve the temperature homogeneity of heating element, can quick at low temperatures high-power heating, power can be reduced to greatest extent when reaching design temperature.Therefore the ink possessing PTC function has automatic constant-temperature function because of it, decrease temperature control component and save equipment cost, and possess the advantages such as energy-conservation, research for the electrically conductive ink of regulating power also becomes the emphasis research topic of many heating element manufacturers and many scientific research institutions, but the electrically conductive ink of the regulating power obtained at present still cannot produce good effect.
In view of this, need the electrically conductive ink inventing a kind of regulating power, possess the advantages such as manufacture craft is simple.
[summary of the invention]
Technical problem to be solved by this invention is to provide that a kind of printing performance is excellent, the electrically conductive ink of the regulating power of good stability, the preparation method of the electrically conductive ink of this regulating power is also provided accordingly, and the electrically conductive ink of this regulating power is at heating device for reference mirror of car, automobile seat heating device, Electric radiant Heating Film, geothermal film, and need to be printed on other objects play heat effect or to use and so on as temperature sensor product in application.
For solving the problems of the technologies described above, one aspect of the present invention provides a kind of electrically conductive ink of regulating power, and the technical scheme specifically taked is as follows:
A kind of electrically conductive ink of regulating power comprises the component of following massfraction:
As a further improvement on the present invention, described electro-conductive material is selected from carbon black, Graphite Powder 99, metal powder, metal oxide.
As a further improvement on the present invention, described connecting material is selected from polyethylene, polyvinylidene difluoride (PVDF), ethylene-vinyl acetate copolymer, ethylene-methyl acrylate multipolymer, ethylenemethylmethacrylate multipolymer, ethylene acrylic acid co polymer, the one of ethylene-ethyl acrylate copolymer or one or more.
As a further improvement on the present invention, described organic solvent aromatic hydrocarbon solvent, optional interpolation ketones solvent or lipid solvent, the toluene that described aromatic hydrocarbon solvent can be selected from, dimethylbenzene, petroleum naphtha, gasoline, kautschin, naphthalane, naphthane; If described interpolation ketones solvent can be selected from acetone, butanone, pimelinketone, ratio alkane ketone; Described lipid solvent can be selected from methyl acetate, ethyl acetate, 2-Butoxyethyl acetate.
As a further improvement on the present invention, described subsidiary material can be selected from Hypalon, styrene-butadiene rubber(SBR), one or more of terpolymer EP rubber and paracril.
As a further improvement on the present invention, described subsidiary material also comprise rubber ingredients.
The present invention provides a kind of preparation method of electrically conductive ink of above-mentioned regulating power on the other hand, and it specifically comprises the following steps:
(1) by electro-conductive material and the mixing of polyolefins connecting material, high temperature makes particle;
(2) by the particle that step (1) obtains, through cross-linking radiation; Particle after crosslinked is pulverized, obtains micro mist;
(3) put in organic solvent by the micro mist that step (2) obtains, be heated to 100-350 (can according to material different choice suitable temp), stirring and dissolving, cooling 24-72 hour, obtains electroconductive paste;
(4) with organic solvent, subsidiary material are dissolved, add the electroconductive paste that step (3) obtains, mix, form electrically conductive ink.
As a further improvement on the present invention, also comprise step (5) runner milling to mill ink.
As a further improvement on the present invention, the particle diameter of described step (2) micro mist is 0.2-200 μm.
As a further improvement on the present invention, the pulverizing in described step (2) for be first crushed to below median size 1mm with pulverizer, then is pulverized with micronizer mill.
Last aspect of the present invention provides a kind of electrically conductive ink of above-mentioned regulating power for heating device for reference mirror of car, automobile seat heating device, Electric radiant Heating Film, geothermal film, and need to be printed on other objects play heat effect or to use and so on as temperature sensor product in purposes.
In the present invention, organic solvent can be the solvent of a kind of solvent or multi-solvents composition, as the toluene, dimethylbenzene, petroleum naphtha, gasoline, kautschin, naphthalane, naphthane etc. of aromatic hydrocarbons, also ketones solvent can be added, as: if acetone, butanone, pimelinketone, ratio alkane ketone etc., a small amount of lipid solvent can be added as methyl acetate, ethyl acetate, 2-Butoxyethyl acetate etc. simultaneously.
The electro-conductive material that electro-conductive material can be commonly used for electrically conductive ink field, as metal powder, carbon dust, metal oxide etc., wherein most preferably has the carbon black of high electrical conductivity energy, as Cabot VXC72, or Graphite Powder 99.
Polyolefins connecting material can select polyethylene, ethylene acrylic acid co polymer or vinylidene etc.Cross-linking radiation can prevent the migration of electro-conductive material.If electro-conductive material migration will make product at high/low temperature circulation time, there is expendable change in electroconductibility.
In the present invention, the particle after crosslinked is preferably crushed to 0.2-200 μm, accelerate dissolution can form conduction electricity paste.
In the present invention, add subsidiary material, the organic solvent namely increasing rubber is stuck with paste, and can increase viscosity and the thixotropy of ink like this, enable ink adapt to silk screen printing.Can also rubber ingredients be added in subsidiary material, ensure the stability of the character of electrically conductive ink of the present invention.
Compared with prior art, the beneficial effect that the present invention obtains is:
The electrically conductive ink of regulating power provided by the present invention, has PTC function, can automatic constant-temperature, decreases temperature control component and cost-saving, the advantage such as energy-conservation.
The present invention is preferred, macromolecular material can be adopted, using graphitized carbon black as conductive carrier, using aromatic hydrocarbon solvent as solvent, the PTC electrically conductive ink of preparation is applicable to silk screen printing, with the product that the present invention makes, particularly mirror heater device, has-50 DEG C of-90 DEG C of temperature alternatings 20,000 times, continuously energising 5000 hours products good characteristic that still can normally work, under can being applied to harsh environment, and energy guaranteed performance is stable.
The method preparing electrically conductive ink provided by the invention is simple, is applicable to suitability for industrialized production.
[embodiment]
Below in conjunction with specific embodiment, the present invention is described in more detail.
Embodiment 1
An electrically conductive ink for regulating power, comprises following component:
The preparation method of the electrically conductive ink of regulating power is as follows:
1, the carbon black of high conductivity is mixed in the high density polyethylene(HDPE) of high crystalline, after high temperature 200 DEG C fully mixing, makes particle.
2, the particle made is cross-linked through nuclear radiation, carbon black and high density polyethylene(HDPE) is firmly cross-linked, prevents carbon black from moving.If carbon black migration will make product at high/low temperature circulation time, there is expendable change in electroconductibility.
3, the particle pulverizer after crosslinked is pulverized, reach median size less than 1 millimeter.
4, the particle micronizer mill reaching median size less than 1 millimeter is crushed to 0.2-200 micron.
5, the mixed solvent micro mist after pulverizing being put into dimethylbenzene, acetone and 2-Butoxyethyl acetate is heated to 120 DEG C, slowly stirs, micro mist is dissolved with stirrer, cools 48 hours, material is thus formed conductive paste under being then positioned over normal temperature.
6, terpolymer EP rubber is become pasty state through xylene soluble, add rubber ingredients sulphur, then add aforesaid conductive paste, be mixed to get ink.
7, make ink there is not large particle to filter through filter with runner milling ink of milling.
Embodiment 2
An electrically conductive ink for regulating power, comprises following component:
The preparation method of the electrically conductive ink of regulating power is as follows:
1, the carbon black of high conductivity is mixed in the high density polyethylene(HDPE) of high crystalline, after high temperature 200 DEG C fully mixing, makes particle.
2, the particle made is cross-linked through nuclear radiation, carbon black and high density polyethylene(HDPE) is firmly cross-linked, prevents carbon black from moving.If carbon black migration will make product at high/low temperature circulation time, there is expendable change in electroconductibility.
3, the particle pulverizer after crosslinked is pulverized, reach median size less than 1 millimeter.
4, the particle micronizer mill reaching median size less than 1 millimeter is crushed to 0.2-200 micron.
5, the mixed solvent micro mist after pulverizing being put into dimethylbenzene and acetone is heated to 120 DEG C, slowly stirs, micro mist is dissolved with stirrer, cools 48 hours, material is thus formed conductive paste under being then positioned over normal temperature.
6, terpolymer EP rubber is become pasty state through xylene soluble, add rubber ingredients sulphur, then add aforesaid conductive paste, be mixed to get ink.
7, make ink there is not large particle to filter through filter with runner milling ink of milling.
Embodiment 3 test case
Take PET as base material complex metal layer, then remove unnecessary part formation electrode with etch, the spacing of positive and negative electrode is 4 millimeters, and in arranging slotting pectination, the ink thickness that printing embodiment 1 and 2 obtains is 25 microns, and drying is tested.
Test result is as follows:
The ink of embodiment 1 gained: when-40 DEG C, resistance is 9.6 Ω; When 0 DEG C, resistance is 10 Ω; When 90 DEG C, resistance is 125 Ω.Present significant ptc characteristics.Through-40 DEG C-90 DEG C circulations 1000 times, resistance change 5%.Energising 12V5000 hour, resistance change 5%.
The ink of embodiment 2 gained: when-40 DEG C, resistance is 10.5 Ω; When 0 DEG C, resistance is 11 Ω; When 90 DEG C, resistance is 150 Ω.Present significant ptc characteristics.Through-40 DEG C-90 DEG C circulations 1000 times, resistance change 5%.Energising 12V5000 hour, resistance change 5%.
Embodiment 4-6
Each embodiment prescription is as follows: preparation method is with embodiment 1
Conclusion, the electrically conductive ink of regulating power prepared by embodiment 4-6 all possess PTC performance.
The above embodiment is only the preferred embodiments of the present invention, and and the feasible enforcement of non-invention exhaustive.For persons skilled in the art, to any apparent change done by it under the prerequisite not deviating from the principle of the invention and spirit, all should be contemplated as falling with within claims of the present invention.
Claims (2)
1. a preparation method for the electrically conductive ink of regulating power, is characterized in that: the electrically conductive ink of described regulating power, comprises following component:
It specifically comprises the following steps:
(1), the carbon black of high conductivity is mixed in the high density polyethylene(HDPE) of high crystalline, after high temperature 200 DEG C fully mixing, makes particle;
(2), by the particle made be cross-linked through nuclear radiation, carbon black and high density polyethylene(HDPE) be firmly cross-linked, prevent carbon black from moving, if carbon black migration will make product at high/low temperature circulation time, there is expendable change in electroconductibility;
(3), by the particle pulverizer after crosslinked pulverize, reach median size less than 1 millimeter;
(4), the particle micronizer mill reaching median size less than 1 millimeter is crushed to 0.2-200 micron;
(5) mixed solvent, the micro mist after pulverizing being put into dimethylbenzene, acetone and 2-Butoxyethyl acetate is heated to 120 DEG C, slowly stir with stirrer, micro mist is dissolved, cools 48 hours under being then positioned over normal temperature, material is thus formed conductive paste;
(6), by terpolymer EP rubber become pasty state through xylene soluble, add rubber ingredients sulphur, then add aforesaid conductive paste, be mixed to get ink;
(7), make ink there is not large particle to filter through filter with runner milling ink of milling.
2. a preparation method for the electrically conductive ink of regulating power, is characterized in that: the electrically conductive ink of described regulating power, comprises following component:
It specifically comprises the following steps:
(1), the carbon black of high conductivity is mixed in the high density polyethylene(HDPE) of high crystalline, after high temperature 200 DEG C fully mixing, makes particle;
(2), by the particle made be cross-linked through nuclear radiation, carbon black and high density polyethylene(HDPE) be firmly cross-linked, prevent carbon black from moving, if carbon black migration will make product at high/low temperature circulation time, there is expendable change in electroconductibility;
(3), by the particle pulverizer after crosslinked pulverize, reach median size less than 1 millimeter;
(4), the particle micronizer mill reaching median size less than 1 millimeter is crushed to 0.2-200 micron;
(5) mixed solvent, by the micro mist after pulverizing putting into dimethylbenzene and acetone is heated to 120 DEG C, slowly stirs, micro mist is dissolved with stirrer, cools 48 hours, material is thus formed conductive paste under being then positioned over normal temperature;
(6), by terpolymer EP rubber become pasty state through xylene soluble, add rubber ingredients sulphur, then add aforesaid conductive paste, be mixed to get ink;
(7), make ink there is not large particle to filter through filter with runner milling ink of milling.
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CN103805066B (en) * | 2014-03-12 | 2016-10-19 | 黑龙江中惠地热股份有限公司 | Positive temperature characterisitic synthetic slurry |
CN103965696A (en) * | 2014-05-22 | 2014-08-06 | 宁波市加一新材料有限公司 | Double temperature-control PTC (Positive Temperature Coefficient) conductive printing ink and preparation method thereof |
CN104212244B (en) * | 2014-09-29 | 2015-12-09 | 广东东莞市天润电子材料有限公司 | A kind of electrostatic precipitation ink and preparation method thereof |
CN104449046B (en) * | 2014-12-09 | 2017-08-18 | 上海宥拓化学有限公司 | A kind of electrically conductive ink and its application |
CN104497714B (en) * | 2014-12-09 | 2017-06-13 | 上海印钞有限公司 | A kind of engraving intaglio printing ink of conductive energy and the security document printed by the ink |
CN107722730A (en) * | 2017-09-28 | 2018-02-23 | 深圳市兴鸿昌电器有限公司 | A kind of PTC electrically conductive inks, its preparation method and use its heating pad for pets |
CN110003719A (en) * | 2019-04-03 | 2019-07-12 | 新奥石墨烯技术有限公司 | Self limiting temperature electric heating ink and preparation method thereof, electric calorifie installation |
CN110283497B (en) * | 2019-06-28 | 2022-07-12 | 深圳烯材科技有限公司 | Method for printing screen printing conductive ink of precise self-temperature-limiting flexible electrothermal film |
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CN103146259A (en) * | 2013-03-20 | 2013-06-12 | 中国人民解放军国防科学技术大学 | Screen printing conductive printing ink composition and preparation method thereof |
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KR20120124257A (en) * | 2011-05-03 | 2012-11-13 | 동아대학교 산학협력단 | Conductive Ink Composite for stamp printing And Manufacturing Method of electrode pattern using the same |
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CN103113786A (en) * | 2013-03-07 | 2013-05-22 | 苏州牛剑新材料有限公司 | Graphene conductive ink and preparation method thereof |
CN103146259A (en) * | 2013-03-20 | 2013-06-12 | 中国人民解放军国防科学技术大学 | Screen printing conductive printing ink composition and preparation method thereof |
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Effective date of registration: 20231214 Address after: No. 21 Youyi Village, Fuxi Street, Tiantai County, Taizhou City, Zhejiang Province, 318000 Patentee after: TIANTAI HONGTAI ELECTRONICS Co.,Ltd. Address before: Room 108, Building 10, Fengze Community, Chicheng Street, Tiantai County, Zhejiang Province, 317200 Patentee before: Zhang Xianbo |