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CN103555067A - Conductive ink for regulating power as well as preparation method and application of conductive ink - Google Patents

Conductive ink for regulating power as well as preparation method and application of conductive ink Download PDF

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Publication number
CN103555067A
CN103555067A CN201310504189.3A CN201310504189A CN103555067A CN 103555067 A CN103555067 A CN 103555067A CN 201310504189 A CN201310504189 A CN 201310504189A CN 103555067 A CN103555067 A CN 103555067A
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Prior art keywords
conductive ink
electrically conductive
regulating power
solvent
ink
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CN201310504189.3A
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CN103555067B (en
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张贤波
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TIANTAI HONGTAI ELECTRONICS Co.,Ltd.
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Abstract

The invention relates to a conductive ink for regulating power as well as a preparation method and application of the conductive ink. The conductive ink comprises the following components in percentage by mass: 4-50% of conductive material, 8-30% of polyolefin jointing material, 40-86% of organic solvent and 2-15 parts of auxiliary material. The conductive ink for regulating power has the advantages of PTC (Positive Temperature Coefficient) function, automatic constant temperature, cost reduction because of temperature control element reduction, energy saving and the like.

Description

Electrically conductive ink of a kind of regulating power and its preparation method and application
[technical field]
The invention belongs to ink class material technology field, 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, by electrically conductive particles (silver, copper, carbon etc.), is dispersed in a kind of conductive composite material forming in binder, is printed onto after fixing film forming on stock, plays due effect.Electrically conductive ink is that a kind of important electronic material , China has huge market.
Wherein, the electrical heating element that the electrically conductive ink of capable 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 (being PTC functional materials), possess the material of PTC performance, can greatly improve the temperature homogeneity of heating element, can quick at low temperatures high-power heating, when reaching design temperature, can reduce to greatest extent power.Therefore the ink that possesses PTC function has automatic constant-temperature function because of it, reduce temperature control component and saved equipment cost, and possess the advantages such as energy-conservation, for the research of the electrically conductive ink of regulating power, also become the emphasis research topic of many heating element manufacturers and many scientific research institutions, but the electrically conductive ink of the regulating power obtaining at present still cannot produce good effect.
In view of this, need to invent a kind of electrically conductive ink 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 good, 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, ground hotting mask, and need to be printed on the application in the product that plays heat effect on other objects or use and so on as temperature sensor.
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 of specifically taking is as follows:
A kind of electrically conductive ink of regulating power comprises the component of following massfraction:
Figure BSA0000096587190000021
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, ethylene methacrylic acid methyl terpolymer, ethylene acrylic acid co polymer, ethylene-ethyl acrylate copolymer a kind of or one or more.
As a further improvement on the present invention, described organic solvent aromatic hydrocarbon solvent, optionally adds 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) electro-conductive material and polyolefins connecting material are mixed to high temperature granulation;
(2) by the resulting particle of step (1), through cross-linking radiation; Particle after crosslinked is pulverized, obtained micro mist;
(3) the resulting micro mist of step (2) is put in organic solvent, 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 resulting electroconductive paste of step (3), mix, form electrically conductive ink.
As a further improvement on the present invention, also comprise the runner milling ink of milling for step (5).
As a further improvement on the present invention, the particle diameter of described step (2) micro mist is 0.2-200 μ m.
As a further improvement on the present invention, the pulverizing in described step (2) is for being first crushed to below median size 1mm with pulverizer, then pulverizes 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, ground hotting mask, and need to be printed on the purposes in the product that plays heat effect on other objects or use and so on as temperature sensor.
In the present invention, organic solvent can be the solvent of a kind of solvent or multi-solvents composition, as the toluene of aromatic hydrocarbons, dimethylbenzene, petroleum naphtha, gasoline, kautschin, naphthalane, naphthane etc., also can add ketones solvent, as: if acetone, butanone, pimelinketone, ratio alkane ketone etc. can add a small amount of lipid solvent as methyl acetate, ethyl acetate, 2-Butoxyethyl acetate etc. simultaneously.
Electro-conductive material can as metal powder, carbon dust, metal oxide etc., wherein most preferably have the carbon black of high electrical conductivity energy for the conventional electro-conductive material in electrically conductive ink field, as Cabot VXC72, or Graphite Powder 99.
Polyolefins connecting material can be selected 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 variation in electroconductibility.
In the present invention, the particle after being cross-linked is preferably crushed to 0.2-200 μ m, can accelerate dissolution form conduction electricity paste.
In the present invention, add subsidiary material, the organic solvent that increases rubber is stuck with paste, and can increase like this viscosity and the thixotropy of ink, makes ink can adapt to silk screen printing.In subsidiary material, can also add rubber ingredients, guarantee 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, reduced temperature control component and cost-saving, the advantage such as energy-conservation.
The present invention is preferred, can adopt macromolecular material, 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, the product made from the present invention, particularly rear vision mirror heating unit, has-50 ℃ of-90 ℃ of temperature alternatings 20,000 times, the good characteristic that the 5000 hours products of switching on continuously still can work, can be applied under harsh environment, and energy guaranteed performance is stable.
The method of 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:
Figure BSA0000096587190000051
The preparation method of the electrically conductive ink of regulating power is as follows:
1, the carbon black of high conductivity is sneaked in the high density polyethylene(HDPE) of high crystalline to granulation after 200 ℃ of high temperature fully mix.
2, the particle of making is crosslinked through nuclear radiation, carbon black and high density polyethylene(HDPE) can be firmly cross-linked, prevent carbon black migration.If carbon black migration will make product at high low temperature circulation time, there is expendable variation in electroconductibility.
3, the particle after crosslinked is pulverized with pulverizer, reached median size below 1 millimeter.
4, by reaching 1 millimeter of following particle of median size, with micronizer mill, be crushed to 0.2-200 micron.
5, the mixed solvent of the micro mist after pulverizing being put into dimethylbenzene, acetone and 2-Butoxyethyl acetate is heated to 120 ℃, with stirrer, slowly stirs, and micro mist is dissolved, and is then positioned under normal temperature cooling 48 hours, has so just formed conductive paste.
6, terpolymer EP rubber is dissolved into pasty state through dimethylbenzene agent, adds rubber ingredients sulphur, then add aforesaid conductive paste, be mixed to get ink.
7, with the runner milling ink of milling, make ink not exist large particle to filter through filter.
Embodiment 2
An electrically conductive ink for regulating power, comprises following component:
Figure BSA0000096587190000061
The preparation method of the electrically conductive ink of regulating power is as follows:
1, the carbon black of high conductivity is sneaked in the high density polyethylene(HDPE) of high crystalline to granulation after 200 ℃ of high temperature fully mix.
2, the particle of making is crosslinked through nuclear radiation, carbon black and high density polyethylene(HDPE) can be firmly cross-linked, prevent carbon black migration.If carbon black migration will make product at high low temperature circulation time, there is expendable variation in electroconductibility.
3, the particle after crosslinked is pulverized with pulverizer, reached median size below 1 millimeter.
4, by reaching 1 millimeter of following particle of median size, with micronizer mill, be crushed to 0.2-200 micron.
5, the mixed solvent of the micro mist after pulverizing being put into dimethylbenzene and acetone is heated to 120 ℃, with stirrer, slowly stirs, and micro mist is dissolved, and is then positioned under normal temperature cooling 48 hours, has so just formed conductive paste.
6, terpolymer EP rubber is dissolved into pasty state through dimethylbenzene agent, adds rubber ingredients sulphur, then add aforesaid conductive paste, be mixed to get ink.
7, with the runner milling ink of milling, make ink not exist large particle to filter through filter.
Embodiment 3 test cases
Take PET as base material complex metal layer, then remove unnecessary part formation electrode with etch, between positive and negative electrode, distance is 4 millimeters, is and arranges inserting pectination, and printing embodiment 1 and 2 resulting ink thickness are 25 microns, drying test.
Test result is as follows:
The ink of embodiment 1 gained: in the time of-40 ℃, resistance is 9.6 Ω; In the time of 0 ℃, resistance is 10 Ω; In the time of 90 ℃, resistance is 125 Ω.Present significant ptc characteristics.Through-40 ℃-90 ℃ circulations 1000 times, resistance change 5%.Energising 12V5000 hour, resistance change 5%.
The ink of embodiment 2 gained: in the time of-40 ℃, resistance is 10.5 Ω; In the time of 0 ℃, resistance is 11 Ω; In the time of 90 ℃, resistance is 150 Ω.Present significant ptc characteristics.Through-40 ℃-90 ℃ 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
Figure BSA0000096587190000081
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 is not the exhaustive of the feasible enforcement of the present invention.For persons skilled in the art, any apparent change of under the prerequisite that does not deviate from the principle of the invention and spirit, it having been done, within all should being contemplated as falling with claim protection domain of the present invention.

Claims (10)

1. an electrically conductive ink for regulating power, is characterized in that: the component that comprises following massfraction:
Figure 1
2. the electrically conductive ink of a kind of regulating power as claimed in claim 1, is characterized in that: described electro-conductive material is selected from carbon black Graphite Powder 99, metal powder, metal oxide.
3. the electrically conductive ink of a kind of regulating power as claimed in claim 1, it is characterized in that: described connecting material is selected from polyethylene, polyvinylidene difluoride (PVDF), ethylene-vinyl acetate copolymer, ethylene-methyl acrylate multipolymer, ethylene methacrylic acid methyl terpolymer, ethylene acrylic acid co polymer, ethylene-ethyl acrylate copolymer a kind of or one or more.
4. the electrically conductive ink of a kind of regulating power as claimed in claim 1, it is characterized in that: described organic solvent is selected from aromatic hydrocarbon solvent, optional ketones solvent or lipid solvent, the toluene that described aromatic hydrocarbon solvent can be selected from, dimethylbenzene, petroleum naphtha, gasoline, kautschin, naphthalane, the naphthane of adding; 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.
5. the electrically conductive ink of a kind of regulating power as claimed in claim 1, is characterized in that: described subsidiary material can be selected from Hypalon, styrene-butadiene rubber(SBR), one or more of terpolymer EP rubber and paracril.
6. the electrically conductive ink of a kind of regulating power as claimed in claim 1, is characterized in that: described subsidiary material also comprise rubber ingredients.
7. a preparation method for the electrically conductive ink of regulating power as claimed in claim 1, is characterized in that: it specifically comprises the following steps:
(1) electro-conductive material and polyolefins connecting material are mixed to high temperature granulation;
(2) by the resulting particle of step (1), through cross-linking radiation; Particle after crosslinked is pulverized, obtained micro mist;
(3) the resulting micro mist of step (2) is put in organic solvent, be heated to 100-350 ℃, stirring and dissolving, cooling 24-72 hour, obtains electroconductive paste;
(4) with organic solvent, subsidiary material are dissolved, add the resulting electroconductive paste of step (3), mix, form electrically conductive ink.
8. the preparation method of the electrically conductive ink of a kind of regulating power as claimed in claim 7, is characterized in that: it also comprises the runner milling ink of milling for step (5).
9. the preparation method of the electrically conductive ink of a kind of regulating power as claimed in claim 7, is characterized in that: the particle diameter of described step (2) micro mist is 0.2-200 μ m.
10. the electrically conductive ink of a regulating power as claimed in claim 1 is for heating device for reference mirror of car, automobile seat heating device, Electric radiant Heating Film, ground hotting mask, and need to be printed on the purposes in the product that plays heat effect on other objects or use and so on as temperature sensor.
CN201310504189.3A 2013-10-24 2013-10-24 Electrically conductive ink of a kind of regulating power and its preparation method and application Active CN103555067B (en)

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Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103805066A (en) * 2014-03-12 2014-05-21 黑龙江中惠地热股份有限公司 Synthetic slurry with positive temperature characteristics
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
CN104212244A (en) * 2014-09-29 2014-12-17 广东东莞市天润电子材料有限公司 Electrostatic dust collection ink and preparation method thereof
CN104449046A (en) * 2014-12-09 2015-03-25 上海宥拓化学有限公司 Conductive ink and application thereof
CN104497714A (en) * 2014-12-09 2015-04-08 上海印钞有限公司 Carving gravure ink with conductivity and anti-counterfeiting file printed by same
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
CN110283497A (en) * 2019-06-28 2019-09-27 深圳烯材科技有限公司 A method of printing the silk-screened conductive ink of accurate self limiting temperature flexible electrothermal membrane

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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
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
CN103305051A (en) * 2013-05-20 2013-09-18 Kmt纳米科技(香港)有限公司 Low-temperature radiation electrothermal film and preparation method thereof

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Publication number Priority date Publication date Assignee Title
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
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
CN103305051A (en) * 2013-05-20 2013-09-18 Kmt纳米科技(香港)有限公司 Low-temperature radiation electrothermal film and preparation method thereof

Cited By (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103805066A (en) * 2014-03-12 2014-05-21 黑龙江中惠地热股份有限公司 Synthetic slurry with positive temperature characteristics
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
CN104212244A (en) * 2014-09-29 2014-12-17 广东东莞市天润电子材料有限公司 Electrostatic dust collection ink and preparation method thereof
CN104449046A (en) * 2014-12-09 2015-03-25 上海宥拓化学有限公司 Conductive ink and application thereof
CN104497714A (en) * 2014-12-09 2015-04-08 上海印钞有限公司 Carving gravure ink with conductivity and anti-counterfeiting file printed by same
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
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
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
CN110283497A (en) * 2019-06-28 2019-09-27 深圳烯材科技有限公司 A method of printing the silk-screened conductive ink of accurate self limiting temperature flexible electrothermal membrane
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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Effective date of registration: 20231214

Address after: No. 21 Youyi Village, Fuxi Street, Tiantai County, Taizhou City, Zhejiang Province, 318000

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