CN108997841B - Water-based environment-friendly graphene conductive ink - Google Patents
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- CN108997841B CN108997841B CN201810932057.3A CN201810932057A CN108997841B CN 108997841 B CN108997841 B CN 108997841B CN 201810932057 A CN201810932057 A CN 201810932057A CN 108997841 B CN108997841 B CN 108997841B
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Abstract
The invention belongs to the technical field of conductive ink, and provides water-based environment-friendly graphene conductive ink for solving the problems of poor environment-friendly performance and low conductivity of the conventional conductive ink. The conductive ink is prepared from 10-30 parts of aqueous high polymer resin, 10-20 parts of conductive filler, 50-120 parts of solvent, 0.5-3 parts of dispersant, 0.5-3 parts of defoamer and 1-5 parts of thickener, wherein the aqueous high polymer resin is used as a connecting material, and is compounded, stirred and ground with the conductive filler, the solvent, a cosolvent and related auxiliaries. Has the characteristics of adjustable resistivity, stable conductivity, good bending resistance, strong adhesive force and no harm to the environment and human bodies in use. Overcomes the defects that the oily solvent used by the traditional conductive ink is toxic and harmful, pollutes the environment, harms the health of operators, and has high solvent cost, etc. The ink is suitable for printing processes such as silk-screen printing, flexography, gravure printing, coating and the like.
Description
Technical Field
The invention belongs to the technical field of conductive ink, and particularly relates to water-based environment-friendly graphene conductive ink.
Background
The conductive ink is paste ink prepared by dispersing conductive materials in a binder, has a certain conductive property, and can be used for printing conductive points or conductive circuits. With the development of the electronic industry, the combination of the electronic technology and the printing technology is more and more compact, the demand for the conductive ink is more and more increased, the conductive ink applied at present is mostly solvent-based, and the solvent-based ink has the problem of organic volatile compounds (VOC) emission. With the gradual enhancement of the environmental protection consciousness of people, environmental-friendly and green conductive ink is urgently needed in the market.
The carbon powder filler commonly used in the current conductive ink has low cost, but has poor conductivity, so the application of the carbon powder filler is limited. Graphene is a new material of single-layer sheet-like bonds composed of carbon atoms. The graphene can be used as a good conductive filler to be applied to conductive ink after being effectively functionalized.
At present, the research and development of conductive ink are mainly focused on solvent-based ink, and the main measure for improving the conductivity of the ink is to increase the content of a conductive agent, which generally reaches 30-95%, so that the conductivity of the ink can be greatly improved, but in the actual use process, because the content of the conductive agent is too high, the properties of a coating film, such as construction performance, appearance quality, use stability and the like, are poor, the flexibility and adhesion of the coating film are poor, and phenomena of microcracks, falling-off and the like are easily generated, and the solvent-based ink contains a large amount of toxic and harmful volatile organic matters, which seriously affects the health of human bodies and environmental pollution.
Therefore, how to prepare the water-based conductive ink with low conductive filler content, high conductivity and good mechanical properties is yet to be further researched and developed.
Disclosure of Invention
The invention provides water-based environment-friendly graphene conductive ink, which aims to solve the problems of poor environment-friendly performance and low conductivity of the existing conductive ink.
The invention is realized by the following technical scheme: the water-based environment-friendly graphene conductive ink is prepared from the following raw materials in parts by weight: 10-30 parts of water-based high polymer resin, 10-20 parts of conductive filler, 50-120 parts of solvent, 0.5-3 parts of dispersing agent, 0.5-3 parts of defoaming agent and 1-5 parts of thickening agent.
The water-based high polymer resin is one or more of water-based acrylic emulsion, silicone-acrylic emulsion, water-based acrylic resin liquid, SBR (styrene butadiene rubber) latex and water-based polyurethane resin liquid.
The conductive filler is 1-5 parts of graphene, 0-10 parts of acetylene black and 0-15 parts of conductive graphite.
The solvent is deionized water, and the cosolvent such as alcohols, esters or ethers required by the commercial product is completely not needed, so that the printing ink is completely environment-friendly, and the problem of organic volatile compounds (VOC) emission is solved.
The dispersing agent is one or more of sodium oleate, sodium carboxylate, sodium sulfate, sodium sulfonate, sodium polyacrylate, sodium polycarboxylate, polyethylene glycol, octyl phenyl polyoxyethylene ether and the like.
The defoaming agent is one or more of BYK-028 aqueous defoaming agent, BYK-024 aqueous defoaming agent, Dow Corning DC-65 aqueous defoaming agent, Dow Corning DC-69 organic silicon defoaming agent and Pasteur 2190 defoaming agent.
The thickener is any one of carboxymethyl cellulose CMC, thickener TT-935, sodium carboxymethyl cellulose and polyacrylic acid.
The method for preparing the water-based environment-friendly graphene conductive ink comprises the following steps: mixing deionized water, a dispersing agent, a defoaming agent and a thickening agent in proportion, and ultrasonically stirring for 10-30 minutes at the ultrasonic power of 300W, the frequency of 40-60 kHz and the stirring speed of 300 r/min; adding graphene according to a proportion, and ultrasonically stirring for 1-3 hours at an ultrasonic power of 300W and a frequency of 40-60 kHz and at a stirring speed of 500 r/min; adding acetylene black, and carrying out ultrasonic stirring for 2-4 hours at an ultrasonic power of 300W and a frequency of 40 kHz-60 kHz and at a stirring speed of 1000 r/min; adding water-based polymer resin, stirring for 2-3 hours at 2500r/min, and stirring for 20 minutes at 500 r/min; and grinding the mixed solution on a three-roll grinder for 3-5 times, and stirring for 20 minutes at a speed of 500r/min after grinding is finished to obtain the water-based environment-friendly graphene conductive ink.
Graphene is the best two-dimensional material for electrical conductivity found at present. Due to the lamellar microstructure, lamellar lapping conductive networks are easily formed in the conductive ink, can be used as high-quality conductive functional units, is applied to preparation of novel conductive ink, and has wide prospects. However, most of graphene on the market is prepared by an oxidation-reduction process at present, the number of layers is high, and due to the preparation process of the oxidation-reduction graphene (Rgo for short), holes appear on Rgo sheet layers, oxygen-containing functional groups remain on part of carbon atoms, the conductive capability of Rgo is reduced, and agglomeration is easy to occur and is not easy to disperse in a solvent.
The graphene used in the invention is the graphene produced by Daqinxi science and technology Limited liability company by using a physical catalysis method, and has the characteristics of zero oxygen content, no functional group, low layer number, easy dispersion and difficult agglomeration, the thickness of the graphene is less than 2 nanometers, the sheet diameter is less than 3 micrometers, and the specific surface area is 800m2And about/g. The acetylene black is of a nano spherical structure, and the specific surface area is 60m2And about/g. The conductive graphite powder is of a micron lamellar structure, and the specific surface area is 10m2And about/g. The three conductive fillers are mutually filled in the vacant areas in the constructed conductive network by the unique particle structures in the solvent, finally the conductive networks of the three specific surface area systems are formed in parallel to form a complete conductive network, and the impact resistance and the complete resistance of the ink after printing and film forming are improved.
The Graphene used in the invention has the advantages that the carbon content is 99.65%, the nitrogen content is 0.24%, the oxygen is free, the hydrogen content is 0.006%, and the sulfur content is 0.101% by detection of elements in the Graphene, and the detection result is provided by Jiangsu Special Equipment Safety Supervision and Inspection research Institute (Jiangsu Special Equipment Safety Supervision and Inspection Institute) and Jiangsu Graphene Inspection Technology Key Laboratory.
The product obtained by the invention has no pungent odor, the content of Volatile Organic Compounds (VOC) is low, the solvent is completely nontoxic and pollution-free, and the operator does not need chemical protection. The product can be directly diluted by water in the using process, and the printing equipment can be directly cleaned by water after printing. The product is cured at low temperature, the ink layer is cured quickly, the adhesive force is strong, the product can be cured slowly at normal temperature, and the product can be cured completely within 5 minutes at 100 ℃. The sheet resistance of the printed product is 5-8000 omega/cm2The range is adjustable, and the device is suitable for various application scenes; through a water soaking experiment and a bending experiment, the sheet resistance change is less than 10%, and the conductivity is stable; through 3000-hour fatigue experiments, the sheet resistance change rate is less than 5%, and the service life is long. No harm to the environment and human body in use. Overcomes the defects of the traditional conductive inkThe used oily solvent has the disadvantages of toxicity, harm, environmental pollution, harm to the health of operators, high solvent cost and the like. The ink is suitable for printing processes such as silk-screen printing, flexography, gravure printing, coating and the like.
Drawings
FIG. 1 is an atomic force micrograph of Daomonxi graphene used in the present invention; fig. 2 is a raman spectrum graph of macyoxi graphene.
Detailed Description
Example 1: the water-based environment-friendly graphene conductive ink is prepared from the following raw materials in parts by mass: 15 parts of aqueous polyurethane resin liquid, 72.5 parts of deionized water, 1.5 parts of graphite of Daqinxi science and technology Limited liability company, 8.5 parts of acetylene black, 1 part of sodium polycarboxylate, 1.2 parts of BYK-024 aqueous defoaming agent and 1.3 parts of carboxymethyl cellulose CMC.
The method for preparing the water-based environment-friendly graphene conductive ink comprises the following steps: mixing deionized water, a dispersing agent, a defoaming agent and a thickening agent in proportion, and ultrasonically stirring for 30 minutes at the ultrasonic power of 300W and the frequency of 40-60 kHz at the stirring speed of 300 r/min; adding graphene according to a proportion, and ultrasonically stirring for 1-3 hours at an ultrasonic power of 300W and a frequency of 40-60 kHz and at a stirring speed of 500 r/min; adding acetylene black, and carrying out ultrasonic stirring for 2-4 hours at an ultrasonic power of 300W and a frequency of 40-60 kHz and at a stirring speed of 1000 r/min; adding 2500r/min of aqueous polymer resin, stirring for 2-3 hours, and stirring for 20 minutes at 500 r/min; and grinding the mixed solution on a three-roll grinder for 3-5 times, and stirring for 20 minutes at a speed of 500r/min after grinding is finished to obtain the water-based environment-friendly graphene conductive ink.
The thickness of the graphene is less than or equal to 2nm, the sheet diameter is less than or equal to 3 mu m, and the specific surface area is 750-850m2/g。
The water-based environment-friendly graphene conductive ink prepared according to the proportion has the main technical indexes that: the viscosity is 12000mPa.s, the solid content is 16.3%, the water-based environment-friendly graphene conductive ink is silk-screen printed on a PET substrate, the water-based environment-friendly graphene conductive ink is dried for 5 minutes at 100 ℃ and then completely dried, the thickness of the film is 15 mu m through testing, and the sheet resistance is 8 omega/cm2. The adhesive force with the PET film is tested by a 3M adhesive tape, and the result is more than 4 grades, thereby meeting the use requirement. The change of the resistivity after 20 times of bending is less than 10 percent.
Example 2: the water-based environment-friendly graphene conductive ink is prepared from the following raw materials in parts by mass: 18 parts of water-based acrylic emulsion, 65.3 parts of deionized water, 2.5 parts of graphite of Daqinxi science and technology Limited liability company, 10 parts of conductive graphite, 1.5 parts of sodium polycarboxylate, 1.2 parts of Dow Corning DC-69 water-based defoaming agent and 1.5 parts of carboxymethyl cellulose CMC. The preparation method is the same as that described in example 1.
The water-based environment-friendly graphene conductive ink prepared according to the proportion has the main technical indexes that: the viscosity is 13500mPa.s, the solid content is 19.4%, the water-based environment-friendly graphene conductive ink is silk-screen printed on a PET substrate, and is dried for 5 minutes at 100 ℃ to be completely dried, the thickness of the film is 15 mu m, and the sheet resistance is 12 omega/cm through testing2. The adhesive force with the PET film is tested by a 3M adhesive tape, and the result is more than 4 grades, thereby meeting the use requirement. The change of the resistivity after 20 times of bending is less than 10 percent.
Example 3: the water-based environment-friendly graphene conductive ink is prepared from the following raw materials in parts by mass: 20 parts of silicone-acrylic emulsion, 60.5 parts of deionized water, 1 part of graphite of Daqinxi science and technology Limited liability company, 6 parts of acetylene black, 10 parts of conductive graphite, 1 part of sodium oleate, 1.2 parts of Dow Corning DC-65 aqueous defoaming agent and 1 part of carboxymethyl cellulose CMC. The preparation method is the same as that described in example 1.
The water-based environment-friendly graphene conductive ink prepared according to the proportion has the main technical indexes that: the viscosity is 9200mPa.s, the solid content is 23.3%, the water-based environment-friendly graphene conductive ink is silk-screen printed on a PET substrate, and is dried for 5 minutes at 100 ℃, and then is completely dried, the thickness of the film is 15 mu m, and the sheet resistance is 15 omega/cm through testing2. The adhesive force with the PET film is tested by a 3M adhesive tape, and the result is more than 4 grades, thereby meeting the use requirement. The change of the resistivity after 20 times of bending is less than 10 percent.
Example 4: the water-based environment-friendly graphene conductive ink is prepared from the following raw materials in parts by mass: 10 parts of aqueous acrylic resin liquid, 120 parts of deionized water, 5 parts of graphite of Daqinxi science and technology Limited liability company, 10 parts of acetylene black, 5 parts of conductive graphite, 0.5 part of sodium carboxylate, 0.5 part of BYK-028 aqueous defoaming agent and TT-9355 parts of thickening agent. The preparation method is the same as that described in example 1.
Example 5: the water-based environment-friendly graphene conductive ink is prepared from the following raw materials in parts by mass: 30 parts of SBR latex, 120 parts of deionized water, 1 part of graphite of Daqimo Xishi science and technology Limited liability company, 15 parts of conductive graphite, 3 parts of sodium sulfate, 3 parts of a Pasteur 2190 defoaming agent and 2 parts of sodium carboxymethylcellulose. The preparation method is the same as that described in example 1.
The high-conductivity aqueous graphene conductive ink prepared by the embodiment of the invention can be used in the fields of electromagnetic shielding, conductive circuits, radio frequency identification, film switches, printed resistors, far infrared heating and the like. Because the whole water-based ink formula does not use organic solvent at all, and all the components are nontoxic and harmless to human bodies, the environmental protection problem and the safety protection problem of constructors in the ink construction process are thoroughly solved. The solvent with the largest usage amount in the whole components is deionized water, so that the cost of the ink is greatly reduced, and the competitiveness of the product is improved.
Claims (5)
1. The water-based environment-friendly graphene conductive ink is characterized in that: the composite material is prepared from the following raw materials in parts by mass: 10-30 parts of water-based high polymer resin, 10-20 parts of conductive filler, 50-120 parts of solvent, 0.5-3 parts of dispersing agent, 0.5-3 parts of defoaming agent and 1-5 parts of thickening agent;
the water-based high polymer resin is one or more of water-based acrylic emulsion, silicone-acrylic emulsion, water-based acrylic resin liquid, SBR latex and water-based polyurethane resin liquid;
the conductive filler is 1-5 parts of graphene, 6-10 parts of acetylene black and 5-10 parts of conductive graphite; the thickness of the graphene is less than or equal to 2nm, the sheet diameter is less than or equal to 3 mu m, and the specific surface area is 750-850m2(ii)/g; the acetylene black is of a nano spherical structure, and the specific surface area is 60m2(ii)/g; the conductive graphite powder is of a micron lamellar structure, and the specific surface area is 10m2(ii)/g; the solvent is deionized water.
2. The aqueous environment-friendly graphene conductive ink according to claim 1, characterized in that: the dispersing agent is one or more of sodium oleate, sodium carboxylate, sodium sulfate, sodium sulfonate, sodium polyacrylate, sodium polycarboxylate, polyethylene glycol and octyl phenyl polyoxyethylene ether.
3. The aqueous environment-friendly graphene conductive ink according to claim 1, characterized in that: the defoaming agent is one or more of BYK-028 aqueous defoaming agent, BYK-024 aqueous defoaming agent, Dow Corning DC-65 aqueous defoaming agent, Dow Corning DC-69 organic silicon defoaming agent and Pasteur 2190 defoaming agent.
4. The aqueous environment-friendly graphene conductive ink according to claim 1, characterized in that: the thickener is any one of carboxymethyl cellulose CMC, thickener TT-935, sodium carboxymethyl cellulose and polyacrylic acid.
5. The method for preparing the aqueous environment-friendly graphene conductive ink as claimed in any one of claims 1 to 4, is characterized in that: the method comprises the following steps: mixing deionized water, a dispersing agent, a defoaming agent and a thickening agent in proportion, and ultrasonically stirring for 30 minutes at the ultrasonic power of 300W and the frequency of 40-60 kHz at the stirring speed of 300 r/min; adding graphene according to a proportion, and ultrasonically stirring for 1-3 hours at an ultrasonic power of 300W and a frequency of 40-60 kHz and at a stirring speed of 500 r/min; adding acetylene black, and carrying out ultrasonic stirring for 2-4 hours at an ultrasonic power of 300W and a frequency of 40-60 kHz and at a stirring speed of 1000 r/min; adding 2500r/min of aqueous polymer resin, stirring for 2-3 hours, and stirring for 20 minutes at 500 r/min; and grinding the mixed solution on a three-roll grinder for 3-5 times, and stirring for 20 minutes at a speed of 500r/min after grinding is finished to obtain the water-based environment-friendly graphene conductive ink.
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| CN112680030B (en) * | 2020-12-14 | 2021-12-07 | 厦门捌斗新材料科技有限公司 | Conductive microcapsule, graphene conductive ink, preparation method and application of conductive microcapsule, graphene conductive film and self-repairing method of graphene conductive film |
| CN112430411A (en) * | 2020-12-15 | 2021-03-02 | 大同墨西科技有限责任公司 | Environment-friendly shielding coating and preparation device thereof |
| CN113652119A (en) * | 2021-09-22 | 2021-11-16 | 桂林清研皓隆新材料有限公司 | Graphene conductive heating ink and application thereof, and graphene antibacterial heating fiber chip and preparation method thereof |
| CN114907725A (en) * | 2022-05-09 | 2022-08-16 | 魏宇琦 | Water-based graphene conductive ink and preparation method and application thereof |
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