CN113969080A - Water-based conductive ink for medium-high temperature electric heating and preparation method thereof - Google Patents
Water-based conductive ink for medium-high temperature electric heating and preparation method thereof Download PDFInfo
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- CN113969080A CN113969080A CN202111413618.7A CN202111413618A CN113969080A CN 113969080 A CN113969080 A CN 113969080A CN 202111413618 A CN202111413618 A CN 202111413618A CN 113969080 A CN113969080 A CN 113969080A
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D11/00—Inks
- C09D11/52—Electrically conductive inks
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D11/00—Inks
- C09D11/02—Printing inks
- C09D11/03—Printing inks characterised by features other than the chemical nature of the binder
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D11/00—Inks
- C09D11/02—Printing inks
- C09D11/10—Printing inks based on artificial resins
- C09D11/102—Printing inks based on artificial resins containing macromolecular compounds obtained by reactions other than those only involving unsaturated carbon-to-carbon bonds
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- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
- H05B3/00—Ohmic-resistance heating
- H05B3/10—Heater elements characterised by the composition or nature of the materials or by the arrangement of the conductor
- H05B3/12—Heater elements characterised by the composition or nature of the materials or by the arrangement of the conductor characterised by the composition or nature of the conductive material
- H05B3/14—Heater elements characterised by the composition or nature of the materials or by the arrangement of the conductor characterised by the composition or nature of the conductive material the material being non-metallic
- H05B3/145—Carbon only, e.g. carbon black, graphite
Abstract
The invention relates to the technical field of printing ink, and discloses safe, environment-friendly and nontoxic middle-high temperature electric heating water-based conductive printing ink which is prepared from the following raw materials in percentage by weight: 0.1-1.0% of wetting dispersant, 0.05-0.5% of defoaming agent, 10-20% of conductive component, 4-8% of polythiophene with a side chain containing hydrophilic groups, 2-4% of aromatic hyperbranched polyester, 0.6-1.2% of N-sodium lauroyl sarcosinate, 0.8-1.5% of guar gum hydroxypropyl trimethyl ammonium chloride, 0-20% of aluminum oxide, 0-20% of kaolin, 30-60% of silicone resin emulsion, 0.1-1% of bactericide, 0.1-1% of thickening agent and the balance of deionized water. Printing ink on a high-temperature resistant base material such as a PI film/plate, a mica plate and a ceramic plate by adopting a screen printing mode, a gravure printing mode and the like to prepare a surface heating electric heater material which is electrified and works at a high temperature of 200-350 ℃, wherein a conductive film formed by the printing ink is flexible and bendable.
Description
Technical Field
The invention relates to the technical field of printing ink, in particular to middle-high temperature electric heating water-based conductive printing ink and a preparation method thereof.
Background
In recent years, a molding technique of coating a conductive ink on a surface of a flexible polymer film has been widely used in the fields of electric heaters, radio frequency identification, printed circuit boards, electronic screen displays, sensors, solar cells, membrane switches, and the like. The electrothermal film printed by the conductive ink is a planar heating electrothermal device with large heating area and uniform heating, has good flexibility and safety, becomes a preferred product for replacing other heating modes or devices in certain application fields, and has very wide application prospect. The film forming substance-high molecular polymer resin in the conductive ink can be quickly thermally degraded at medium and high temperature of more than 200 ℃, and is limited by the heat-resistant defect, the existing film type electric heating film mainly uses a low-temperature electric heating film, and the heating temperature is only about 100 ℃. A medium-high temperature surface heating electric heating apparatus with heating temperature above 200 ℃ is mainly prepared by printing conductive slurry prepared by matching glass powder inorganic binder with conductive powder on a ceramic or mica plate and sintering at high temperature; the medium-high temperature surface heating electric heating device has the advantages of brittle and hard property and poor impact resistance, and needs to be carefully used, otherwise, the device is easy to break and has high rejection rate.
Chinese patent application No.: CN201910865012.3 discloses an organic high-temperature electrothermal composite film and a preparation method thereof, wherein the high-temperature electrothermal composite ink is obtained by respectively weighing 5-20 parts of glass fiber, 5-15 parts of grinding dispersion filler and 30-60 parts of high-conductivity filler according to mass proportion, mixing, grinding, uniformly dispersing, adding into high-temperature electrothermal polymer glue, and mechanically stirring uniformly, and the electrothermal film assembled by the high-temperature electrothermal composite ink has good heat resistance and is used at 300 ℃ for a long time. However, solvents used for preparing the high-temperature electrothermal composite ink, such as dimethylformamide, dimethylacetamide and dimethyl sulfoxide, belong to strong-polarity toxic and carcinogenic substances. Chinese patent application No.: CN202021301369.3 discloses a graphene far infrared high temperature electric heating mica plate, which comprises a lower layer high temperature resistant insulating mica plate, a conductive thick film resistor formed by curing organic/inorganic composite high temperature resistant conductive ink, a conductive electrode formed by curing high temperature resistant silver paste, a high temperature resistant adhesive and an upper layer high temperature resistant insulating mica plate which are arranged from bottom to top in sequence. The utility model discloses only mention and use organic/inorganic compound high temperature resistant electrically conductive printing ink as the core heat-generating body, do not introduce the formula component and the preparation method of this printing ink, do not have the characteristics and the constitution of graphite alkene material yet.
Disclosure of Invention
Therefore, the invention provides the water-based conductive ink for medium-high temperature electric heating, which has good adhesive force and excellent heat resistance and solves the problems existing in the prior art. The electric heating device can be printed on high-temperature resistant base materials such as PI films/plates, mica plates and ceramic plates by adopting the modes of silk screen printing, gravure printing and the like, and can be manufactured into the electric heating device which works at the high temperature of 200-350 ℃ by electrifying.
The invention also aims to provide a preparation method of the water-based conductive ink for medium-high temperature electric heating.
In order to achieve the purpose, the invention is realized by the following technical scheme:
the water-based conductive ink for medium-high temperature electric heating comprises the following raw materials in percentage by weight: 0.1-1.0% of wetting dispersant, 0.05-0.5% of defoaming agent, 10-20% of conductive component, 4-8% of polythiophene with a hydrophilic group on a side chain, 2-4% of aromatic hyperbranched polyester, 0.6-1.2% of N-sodium lauroyl sarcosine, 0.8-1.5% of guar gum hydroxypropyl trimethyl ammonium chloride, 0-20% of aluminum oxide, 0-20% of kaolin, 30-60% of silicone resin emulsion, 0.1-1% of bactericide, 0.1-1% of thickening agent and the balance of deionized water, wherein the conductive component comprises a carbon nanotube material, a few-layer graphene material and a multi-layer graphene material.
The further improvement is that: the conductive component comprises the following substances in percentage by weight: 20-30% of carbon nanotube material, 30-45% of few-layer graphene material and 30-45% of multi-layer graphene material.
The further improvement is that: the wetting dispersant is an acrylic block copolymer containing pigment affinity groups.
The further improvement is that: the defoaming agent is any one or a mixture of more than two of organic silicon defoaming agent, non-silicone organic ester hydrocarbon and mineral oil mixture containing hydrophobic particles in any ratio.
The further improvement is that: the number of layers of the few-layer graphene material is less than or equal to 10, the diameter of D50 sheets is 4-7 mu m, and the diameter of D90 sheets is 9-13 mu m.
The further improvement is that: the fineness of the alumina is 800-1500 meshes.
The further improvement is that: the fineness of the kaolin is 800-1500 meshes.
The further improvement is that: the solid content of the silicone resin emulsion is 60 +/-2%, the pH value is 9.0-10.0, and the particle size of Dv50 is less than 1.0 mu m.
The further improvement is that: the active ingredient of the bactericide is isothiazolinone.
The further improvement is that: the thickener is one or a mixture of two of polyurethane thickener and modified polyurea thickener mixed in any ratio.
The invention also provides a preparation method of the water-based conductive ink for medium-high temperature electric heating, which comprises the following steps:
(1) preparing the raw materials according to the weight percentage;
(2) adding deionized water, a wetting dispersant, a defoaming agent, a conductive component, polythiophene with a side chain containing a hydrophilic group, aromatic hyperbranched polyester, N-sodium lauroyl sarcosine, guar gum hydroxypropyl trimethyl ammonium chloride, aluminum oxide and kaolin into a stirring device, uniformly dispersing at a high speed, grinding until the fineness is less than 5 mu m, then starting low-speed stirring, adding a silicone resin emulsion, a bactericide and a thickening agent, uniformly stirring, detecting, filtering and packaging after the detection is qualified.
The prepared medium-high temperature electric heating water-based conductive ink is printed on a high temperature resistant base material such as a PI film/plate, a mica plate and a ceramic plate by adopting a screen printing mode, a gravure printing mode and the like, and is dried by adopting an infrared oven heating and drying mode, so that an electric heating device which works at the high temperature of 200-350 ℃ can be prepared.
By adopting the technical scheme, the invention has the beneficial effects that:
the invention prepares safe, environment-friendly and nontoxic middle-high temperature electric heating water-based conductive ink, which takes silicone resin emulsion with excellent middle-high temperature resistance of more than 200 ℃ as film-forming resin, takes graphene as a conductive material and takes alumina and kaolin as fillers. The conductive film formed by drying the ink at 200 ℃ for 1 hour is flexible and bendable and has good impact resistance. Printing ink on a high-temperature resistant base material such as a PI film/plate, a mica plate and a ceramic plate by adopting a screen printing mode, a gravure printing mode and the like to prepare the surface heating electric equipment which is electrified and works in a high-temperature environment of 200-350 ℃.
The conductive components in the formula are a carbon nano tube material-few-layer graphene material-multi-layer graphene material compound system which are connected in series in different dimensions, so that the number of conductive channels of the system is increased, a compact conductive channel is formed, and the conductive performance of the ink is improved. The graphene has strong van der Waals force and pi-pi interaction force between the graphene sheets, aggregation is easy to occur, and the graphene is difficult to uniformly disperse in a polymer matrix, so that the graphene exerts the characteristics of the graphene seriously. The polythiophene with the hydrophilic group on the side chain is added, so that the interfacial interaction force among the conductive components can be enhanced, the one-dimensional material (carbon nano tube) and the two-dimensional material (few-layer graphene and multi-layer graphene) are mutually crosslinked, the stacking of graphene is reduced, a three-dimensional space conductive network structure is formed, and the conductive performance of the ink is enhanced. Meanwhile, the flexibility of the conductive film is improved after crosslinking. In the research, the compounding of the few-layer graphene and the multi-layer graphene is unexpectedly found to form a porous network structure, so that the conductivity of the ink is obviously improved. The aromatic hyperbranched polyester has a large pi conjugated structure, and can form strong pi-pi bond interaction with graphene, so that the graphene can be well dispersed in a system. In addition, the aromatic hyperbranched polyester is added, so that the conductive film formed after printing and drying of the ink has flexibility and can be repeatedly bent and stretched. Through the action, the agglomeration phenomenon of the graphene is obviously improved, and the printing ink with excellent conductivity and flexibility is obtained.
According to the invention, N-sodium lauroyl sarcosine and guar gum hydroxypropyl trimethyl ammonium chloride are added in the formula, and the compound use of the N-sodium lauroyl sarcosine and the guar gum hydroxypropyl trimethyl ammonium chloride can improve the dispersion effect of graphene in water and reduce the occurrence of agglomeration, and the specific action mechanism is as follows: (1) the hydrophilic group of the N-sodium lauroyl sarcosine and the hydrophilic group of the guar gum hydroxypropyl trimethyl ammonium chloride generate steric hindrance effect, and the mutual aggregation of inorganic conductive particles can be effectively prevented; (2) sodium ions and chloride ions inserted between graphene sheets generate electrostatic repulsion with the head of guar gum hydroxypropyl trimethyl ammonium chloride with positive charge and the head of N-lauroyl sarcosine sodium with negative charge respectively, so that aggregation between the graphene sheets is prevented.
Kaolin with a platy structure is used as a filler, so that the problem of film cracking (namely circuit interruption) can be effectively solved, and the electric heating equipment cannot work normally.
Detailed Description
The following detailed description will be provided for the embodiments of the present invention with reference to specific embodiments, so that how to apply the technical means to solve the technical problems and achieve the technical effects can be fully understood and implemented.
Unless otherwise indicated, the techniques employed in the examples are conventional and well known to those skilled in the art, and the reagents and products employed are also commercially available. The source, trade name and if necessary the constituents of the reagents used are indicated at the first appearance.
Example 1
The water-based conductive ink for medium-high temperature electric heating comprises the following raw materials in percentage by weight:
wherein the polythiophene having a hydrophilic group in the side chain is according to patent application No.: 201610225149.9 is prepared. The aromatic hyperbranched polyester is prepared by reference to the prior literature (Lixiameng, Sun Yisi)Synthesis and characterization of aromatic hyperbranched polyester (J)]Novel chemical materials 2007,35(10): 36-39.). The number of layers of the few-layer graphene material is less than or equal to 10, the diameter of D50 sheets is 4-7 mu m, and the diameter of D90 sheets is 9-13 mu m; the number of the layers of the multilayer graphene material is more than 10, and the thickness of the multilayer graphene material is less than or equal to 10 nm. The fineness of the alumina powder is 1500 meshes; the fineness of the kaolin powder is 1500 meshes; the solid content of the silicone resin emulsion is 60 +/-2%, the pH value is 9.0-10.0, and the particle size (Markov method) Dv50 is less than 1.0 mu m; the thickener is formed by mixing a polyurethane thickener and a modified polyurea thickener according to the mass ratio of 1:1.5, wherein the polyurethane thickener is produced by Wanhua chemistry and has the type
9240NP, model BYK-420 from Bike, Germany.
The preparation method of the water-based conductive ink for medium-high temperature electric heating comprises the following steps:
(1) preparing the raw materials according to the weight percentage;
(2) adding deionized water, a wetting dispersant, a defoaming agent, a carbon nanotube material, a few-layer graphene material, a multi-layer graphene material, polythiophene with a side chain containing a hydrophilic group, aromatic hyperbranched polyester, N-sodium lauroyl sarcosinate, guar gum hydroxypropyl trimethyl ammonium chloride, aluminum oxide and kaolin into a stirring device, uniformly dispersing at a high speed, grinding until the fineness is less than 5 mu m, then starting low-speed stirring, adding a silicone resin emulsion, a bactericide and a thickening agent, uniformly stirring, detecting, filtering after the detection is qualified, and packaging.
The prepared medium-high temperature electric heating water-based conductive ink is printed on a high temperature resistant base material such as a PI film/plate, a mica plate and a ceramic plate by adopting a screen printing mode, a gravure printing mode and the like, and is dried by adopting an infrared oven heating and drying mode, wherein the drying temperature is 200 ℃ and the drying time is 1h, and then the electric heating equipment which works at the high temperature of 200-350 ℃ can be prepared.
The aqueous conductive ink prepared in the embodiment is coated on a substrate, the thickness of a dry film is 25 micrometers, and then the sample is placed in an oven at 300 ℃ for baking for 1d, 7d and 14d, so that the surface appearance of the ink coating is stable and has no crack or shedding phenomenon, and the surface resistance is not obviously changed, which indicates that the conductive ink coating has good temperature resistance.
The measured properties of the electric heating film/plate prepared according to this example were: the surface resistance was 450. omega./□ (film thickness 25 μm. + -. 10%). Folding resistance test: the aqueous conductive ink prepared in the embodiment is coated on a PI film, an electrode is made of copper wires or silver paste, then plastic packaging is carried out on the PI film through a plastic packaging film coated with hot melt adhesive, a sample is placed on a smooth wood block, the PI film is folded for 1500 times at 90 degrees at a speed of 30 times per minute, and the surface resistance change value is less than 5%. The aqueous conductive ink prepared in the example was coated on a PI film, and subjected to a hardness test using a Chinese pencil according to GB/T6739-. The adhesion test is carried out according to GB/T1720-89 paint film adhesion determination method, and the test result is 0 grade.
Example 2:
the water-based conductive ink for medium-high temperature electric heating comprises the following raw materials in percentage by weight:
the fineness of the alumina powder is 800 meshes; the fineness of the kaolin powder is 800 meshes; the solid content of the silicone resin emulsion is 60 +/-2%, the pH value is 9.0-10.0, and the particle size (Markov method) Dv50 is less than 1.0 mu m.
A preparation method of water-based conductive ink for medium-high temperature electric heating comprises the following steps:
(1) preparing the raw materials according to the weight percentage;
(2) adding deionized water, a wetting dispersant, a defoaming agent, a carbon nanotube material, a few-layer graphene material, a multi-layer graphene material, polythiophene with a side chain containing a hydrophilic group, aromatic hyperbranched polyester, N-sodium lauroyl sarcosinate, guar gum hydroxypropyl trimethyl ammonium chloride, aluminum oxide and kaolin into a stirring device, uniformly dispersing at a high speed, grinding until the fineness is less than 5 mu m, then starting low-speed stirring, adding a silicone resin emulsion, a bactericide and a thickening agent, uniformly stirring, detecting, filtering after the detection is qualified, and packaging.
The aqueous conductive ink prepared in the embodiment is coated on a substrate, the thickness of a dry film is 25 micrometers, and then the sample is placed in an oven at 300 ℃ for baking for 1d, 7d and 14d, so that the surface appearance of the ink coating is stable and has no crack or shedding phenomenon, and the surface resistance is not obviously changed, which indicates that the conductive ink coating has good temperature resistance.
The measured properties of the electric heating film/plate prepared according to this example were: the surface resistance was 300. omega./□ (film thickness 25 μm. + -. 10%). The folding resistance test shows that the surface resistance change value is less than 5 percent after 1500 times of 90-degree folding. The aqueous conductive ink prepared in the example was coated on a PI film, and subjected to a hardness test using a Chinese pencil according to GB/T6739-. The adhesion test is carried out according to GB/T1720-89 paint film adhesion determination method, and the test result is 0 grade.
Example 3:
the water-based conductive ink for medium-high temperature electric heating comprises the following raw materials in percentage by weight:
the fineness of the alumina powder is 1200 meshes; the fineness of the kaolin powder is 1200 meshes; the solid content of the silicone resin emulsion is 60 +/-2%, the pH value is 9.0-10.0, and the particle size (Markov method) Dv50 is less than 1.0 mu m.
A preparation method of water-based conductive ink for medium-high temperature electric heating is characterized by comprising the following steps: comprises the following steps:
(1) preparing the raw materials according to the weight percentage;
(2) adding deionized water, a wetting dispersant, a defoaming agent, a carbon nanotube material, a few-layer graphene material, a multi-layer graphene material, polythiophene with a side chain containing a hydrophilic group, aromatic hyperbranched polyester, N-sodium lauroyl sarcosinate, guar gum hydroxypropyl trimethyl ammonium chloride, aluminum oxide and kaolin into a stirring device, uniformly dispersing at a high speed, grinding until the fineness is less than 5 mu m, then starting low-speed stirring, adding a silicone resin emulsion, a bactericide and a thickening agent, uniformly stirring, detecting, filtering after the detection is qualified, and packaging.
The aqueous conductive ink prepared in the embodiment is coated on a substrate, the thickness of a dry film is 25 micrometers, and then the sample is placed in an oven at 300 ℃ for baking for 1d, 7d and 14d, so that the surface appearance of the ink coating is stable and has no crack or shedding phenomenon, and the surface resistance is not obviously changed, which indicates that the conductive ink coating has good temperature resistance.
The measured properties of the electric heating film/plate prepared according to this example were: the surface resistance was 720. omega./□ (film thickness 25 μm. + -. 10%). The folding resistance test shows that the surface resistance change value is less than 5 percent after 1500 times of 90-degree folding. The aqueous conductive ink prepared in the example was coated on a PI film, and subjected to a hardness test using a Chinese pencil according to GB/T6739-. The adhesion test is carried out according to GB/T1720-89 paint film adhesion determination method, and the test result is 0 grade.
Comparative example 1
The kinds and contents of the respective components were the same as those of example 1 except that polythiophene having a hydrophilic group in a side chain was not contained.
The conductive ink film prepared in this comparative example was examined for surface resistance of 630. omega./□ (film thickness 25 μm. + -. 10%). The folding resistance test shows that the surface resistance change value is 10 percent when the film is folded at 90 degrees for 1500 times. The hardness of the pencil was measured by using a Chinese pencil, and the hardness was 2H. The adhesion test result is 0 grade.
Comparative example 2
The kinds and contents of the components were the same as those of example 1 except that the aromatic hyperbranched polyester was not contained.
The conductive ink film prepared in this comparative example was examined for surface resistance of 520. omega./□ (film thickness 25 μm. + -. 10%). The folding resistance test shows that the surface resistance change value is 12 percent when the glass is folded at 90 degrees for 1500 times. The hardness of the pencil was measured by using a Chinese pencil, and the hardness was H. The adhesion test result is grade 1.
Comparative example 3
The kinds and contents of the components were the same as those of example 1 except that N-lauroyl sarcosine sodium and guar hydroxypropyltrimonium chloride were not contained.
The conductive ink film prepared in this comparative example was examined for surface resistance of 540. omega./□ (film thickness 25 μm. + -. 10%). The folding resistance test shows that the surface resistance change value is less than 5 percent after the product is folded for 1500 times at 90 degrees. The hardness of the pencil was measured by using a Chinese pencil, and the hardness was 2H. The adhesion test result is grade 1.
Comparative example 4
The kinds and contents of the components were the same as those in example 1 except that N-lauroyl sarcosine sodium was not contained.
The conductive ink film prepared in this comparative example was examined for surface resistance of 480. omega./□ (film thickness 25 μm. + -. 10%). The folding resistance test shows that the surface resistance change value is less than 5 percent after the product is folded for 1500 times at 90 degrees. The hardness of the pencil was measured by using a Chinese pencil, and the hardness was 2H. The adhesion test result is grade 1.
Comparative example 5
The kinds and contents of the components were the same as those of example 1 except that guar hydroxypropyltrimonium chloride was not contained.
The conductive ink film prepared in this comparative example was examined for surface resistance of 500. omega./□ (film thickness 25 μm. + -. 10%). The folding resistance test shows that the surface resistance change value is less than 5 percent after the product is folded for 1500 times at 90 degrees. The hardness of the pencil was measured by using a Chinese pencil, and the hardness was 2H. The adhesion test result is grade 1.
Comparative example 6
The kind and content of each component were the same as those in example 1 except that the carbon nanotube material was replaced with the few-layer graphene material.
The conductive ink film prepared in this comparative example was examined for surface resistance of 550. omega./□ (film thickness 25 μm. + -. 10%). The folding resistance test shows that the surface resistance change value is less than 5 percent after the product is folded for 1500 times at 90 degrees. The hardness of the pencil was measured by using a Chinese pencil, and the hardness was 2H. The adhesion test result is 0 grade.
Comparative example 7
The kind and content of each component were the same as those in example 1 except that the multi-layer graphene material was replaced with the less-layer graphene material.
The conductive ink film prepared in this comparative example was examined for surface resistance of 570. omega./□ (film thickness 25 μm. + -. 10%). The folding resistance test shows that the surface resistance change value is less than 5 percent after the product is folded for 1500 times at 90 degrees. The hardness of the pencil was measured by using a Chinese pencil, and the hardness was H. The adhesion test result is 0 grade.
Comparative example 8
The types and contents of the components were the same as those in example 1, except that the conductive component was entirely a few-layer graphene material.
The conductive ink film prepared in this comparative example was examined for surface resistance of 600. omega./□ (film thickness 25 μm. + -. 10%). The folding resistance test shows that the surface resistance change value is less than 5 percent after the product is folded for 1500 times at 90 degrees. The hardness of the pencil was measured by using a Chinese pencil, and the hardness was H. The adhesion test result is 0 grade.
The above description is only an embodiment utilizing the technical content of the present disclosure, and any modification and variation made by those skilled in the art can be covered by the claims of the present disclosure, and not limited to the embodiments disclosed.
Claims (10)
1. The water-based conductive ink for medium-high temperature electric heating is characterized in that: the water-based conductive ink is prepared from the following raw materials in percentage by weight: 0.1-1.0% of wetting dispersant, 0.05-0.5% of defoaming agent, 10-20% of conductive component, 4-8% of polythiophene with a hydrophilic group on a side chain, 2-4% of aromatic hyperbranched polyester, 0.6-1.2% of N-sodium lauroyl sarcosine, 0.8-1.5% of guar gum hydroxypropyl trimethyl ammonium chloride, 0-20% of aluminum oxide, 0-20% of kaolin, 30-60% of silicone resin emulsion, 0.1-1% of bactericide, 0.1-1% of thickening agent and the balance of deionized water, wherein the conductive component comprises a carbon nanotube material, a few-layer graphene material and a multi-layer graphene material.
2. The water-based conductive ink for medium-high temperature electric heating according to claim 1, characterized in that: the conductive component comprises the following substances in percentage by weight: 20-30% of carbon nanotube material, 30-45% of few-layer graphene material and 30-45% of multi-layer graphene material.
3. The water-based conductive ink for medium-high temperature electric heating according to claim 1, characterized in that: the wetting dispersant is an acrylic block copolymer containing pigment affinity groups.
4. The water-based conductive ink for medium-high temperature electric heating according to claim 1, characterized in that: the defoaming agent is any one or a mixture of more than two of organic silicon defoaming agent, non-silicone organic ester hydrocarbon and mineral oil mixture containing hydrophobic particles in any ratio.
5. The water-based conductive ink for medium-high temperature electric heating according to claim 1, characterized in that: the number of layers of the few-layer graphene material is less than or equal to 10, the diameter of D50 sheets is 4-7 mu m, and the diameter of D90 sheets is 9-13 mu m.
6. The water-based conductive ink for medium-high temperature electric heating according to claim 1, characterized in that: the fineness of the alumina is 800-1500 meshes.
7. The water-based conductive ink for medium-high temperature electric heating according to claim 1, characterized in that: the fineness of the kaolin is 800-1500 meshes.
8. The water-based conductive ink for medium-high temperature electric heating according to claim 1, characterized in that: the solid content of the silicone resin emulsion is 60 +/-2%, the pH value is 9.0-10.0, and the particle size of Dv50 is less than 1.0 mu m.
9. The water-based conductive ink for medium-high temperature electric heating according to claim 1, characterized in that: the active ingredient of the bactericide is isothiazolinone.
10. The water-based conductive ink for medium-high temperature electric heating according to claim 1, characterized in that: the thickener is one or a mixture of two of polyurethane thickener and modified polyurea thickener mixed in any ratio.
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