CN112309609B - Water-based graphene conductive paste, preparation method thereof and RFID label - Google Patents
Water-based graphene conductive paste, preparation method thereof and RFID label Download PDFInfo
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/20—Conductive material dispersed in non-conductive organic material
- H01B1/24—Conductive material dispersed in non-conductive organic material the conductive material comprising carbon-silicon compounds, carbon or silicon
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- G—PHYSICS
- G06—COMPUTING; CALCULATING OR COUNTING
- G06K—GRAPHICAL DATA READING; PRESENTATION OF DATA; RECORD CARRIERS; HANDLING RECORD CARRIERS
- G06K19/00—Record carriers for use with machines and with at least a part designed to carry digital markings
- G06K19/06—Record carriers for use with machines and with at least a part designed to carry digital markings characterised by the kind of the digital marking, e.g. shape, nature, code
- G06K19/067—Record carriers with conductive marks, printed circuits or semiconductor circuit elements, e.g. credit or identity cards also with resonating or responding marks without active components
- G06K19/07—Record carriers with conductive marks, printed circuits or semiconductor circuit elements, e.g. credit or identity cards also with resonating or responding marks without active components with integrated circuit chips
- G06K19/077—Constructional details, e.g. mounting of circuits in the carrier
- G06K19/0772—Physical layout of the record carrier
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- G—PHYSICS
- G06—COMPUTING; CALCULATING OR COUNTING
- G06K—GRAPHICAL DATA READING; PRESENTATION OF DATA; RECORD CARRIERS; HANDLING RECORD CARRIERS
- G06K19/00—Record carriers for use with machines and with at least a part designed to carry digital markings
- G06K19/06—Record carriers for use with machines and with at least a part designed to carry digital markings characterised by the kind of the digital marking, e.g. shape, nature, code
- G06K19/067—Record carriers with conductive marks, printed circuits or semiconductor circuit elements, e.g. credit or identity cards also with resonating or responding marks without active components
- G06K19/07—Record carriers with conductive marks, printed circuits or semiconductor circuit elements, e.g. credit or identity cards also with resonating or responding marks without active components with integrated circuit chips
- G06K19/077—Constructional details, e.g. mounting of circuits in the carrier
- G06K19/07749—Constructional details, e.g. mounting of circuits in the carrier the record carrier being capable of non-contact communication, e.g. constructional details of the antenna of a non-contact smart card
- G06K19/07773—Antenna details
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
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Abstract
The application provides a water-based graphene conductive paste which comprises the following components in parts by weight: 10-15 parts of graphene, 40-60 parts of deionized water, 1-3 parts of a surfactant, 5-8 parts of a gelling agent, 30-35 parts of a binder, 0.5-2 parts of a light curing agent and 1-5 parts of an auxiliary agent, wherein the surfactant is selected from one or more of tea saponin, cyclic lipopeptide salt, lignosulfonate and dodecyl benzene sulfonate; the gel is selected from one or more of alginate, cellulose, polyvinyl alcohol, xanthan gum and agar powder. The application provides a waterborne graphite alkene conductive paste, through disperse in the deionized water under specific surfactant exists, assist specific binder, light curing agent and auxiliary agent again, finally make waterborne conductive paste with the aquogel form under the effect of gel, with the dispersion form that maintains graphite alkene, and show and promote stability, can effectively resist the compression and prolong deformation in intaglio printing, bonding effect and wear-resisting effect have also obtained effective promotion, better printing adaptability has.
Description
Technical Field
The application relates to the technical field of graphene, in particular to aqueous graphene conductive paste, a preparation method thereof and an RFID tag.
Background
At present, some foreign manufacturers developing radio frequency identification technology RFID have started key technologies and industrialization researches for printing RFID electronic tags with graphene paste, such as BGTM company in england. However, the graphene has different appearance and conductivity from the conventional conductive silver filler, so that the formulation and process of the conductive paste using graphene as a substrate are different. In addition, the conductive paste using graphene as a substrate has the problems of difficult dispersion, easy agglomeration and poor printing adaptability in the actual production.
Firstly, in order to meet the environmental protection standard, the printing paste is more likely to be selected from water-soluble pastes, and the hydrophobic property of graphene makes graphene extremely easy to agglomerate through strong van der waals force, and the conductivity of graphene is remarkably reduced after agglomeration. In the prior art, in order to obtain graphene slurry with better dispersibility and stability, modes such as oxidized graphene, reduced oxidized graphene or chemical grafting modification of graphene are adopted, however, the oxidized graphene has good dispersibility but poor conductivity, a large number of defects exist on the surface of the reduced oxidized graphene, the performance of the reduced oxidized graphene is affected, and the chemical modification mode is unknown.
Therefore, in industrial production, a more suitable dispersion system is more likely to be selected for graphene, for example, organic solvents are used as dispersion liquid, and N-methylpyrrolidone (NMP) and Dimethylformamide (DMF) are known to have better dispersibility, so as to prevent aggregation and improve dispersibility. However, organic solvents are volatile and toxic, which is not good for the health of the manufacturer and the user, and also has pollution and harm to the environment.
Meanwhile, the intaglio printing technology is an image-text copying technology which is high in precision and yield and suitable for ink printing, and can be applied to production of RFID electronic tags. However, in actual production, it is found that when the existing commercial graphene conductive paste is attached to a base material by using a gravure printing method, the mobility is too strong, the adhesion force after curing is poor, and defects such as cracks and curling are easy to occur; meanwhile, the ink layer profile deformation is easy to generate after the roller rolling, and the sensitivity and yield of the RFID are affected.
Disclosure of Invention
In order to solve the above problems, the present application aims to provide an aqueous graphene conductive paste which has better dispersibility and stability and is environmentally friendly, and the aqueous graphene conductive paste has significantly improved adaptability when an RFID electronic tag is prepared by using a gravure printing technology.
In one aspect, the application provides an aqueous graphene conductive paste, which comprises the following components in parts by weight: 10-15 parts of graphene, 40-60 parts of deionized water, 1-3 parts of surfactant, 5-8 parts of gelling agent, 30-35 parts of binding material, 0.5-2 parts of light curing agent and 1-5 parts of auxiliary agent,
the surfactant is selected from one or more of tea saponin, cyclic lipopeptide salt, lignosulfonate and dodecyl benzene sulfonate; the gel is selected from one or more of alginate, cellulose, polyvinyl alcohol, xanthan gum and agar powder.
The aqueous graphene conductive slurry provided by the application is dispersed in deionized water in the presence of a surfactant, and is finally prepared into the aqueous conductive slurry in a hydrogel form under the action of a gelling agent, so that the dispersion form of graphene is maintained, and the stability is remarkably improved; the used components are green and environment-friendly and are harmless to the environment and human health; and a specific binding material, a light curing agent and an auxiliary agent are added, so that the UV-curable gravure ink can be cured under ultraviolet light, can effectively resist tensile deformation in gravure printing, and has better printing adaptability.
Further, the graphene adopts powdery graphene nano sheets, the particle size is 10-50 micrometers, and the thickness of the sheet layer is 1-15 nanometers.
Compared with other forms such as a sheet form or a linear form, the powdered graphene has the advantages of low cost and strong compatibility, but is often easy to generate an agglomeration phenomenon, and the aqueous conductive slurry provided by the application has good dispersibility due to the adoption of the graphene powder.
Further, the surfactant is prepared from the following components in a mass ratio of (1.5-1.8): (0.7-0.8): (0.5-0.7) sodium lignosulfonate, tea saponin and surfactin sodium; the gel is prepared from the following components in percentage by mass (4-5): 1: (2-3) polyvinyl alcohol, alginate and carboxymethyl cellulose.
Further, the binder is prepared from the following components in percentage by mass (18-20): 8: (5-7) hydrophilic epoxy resin, acrylic resin and polyvinylpyrrolidone.
Further, the light curing agent comprises a photoinitiator and a photosensitive resin, wherein the photoinitiator is 1-hydroxy cycloethyl phenyl ketone; the photosensitive resin is selected from one or more of hydroxyethyl acrylate, terephthalic acid and tripropylene glycol diacrylate.
Preferably, the light curing agent consists of 1-hydroxy ethyl phenyl ketone and hydroxyethyl acrylate, and more preferably, the parts by weight of the two are respectively 0.3 part and 1.7 parts.
Further, the auxiliary agent is selected from a leveling agent and/or an antifoaming agent, the leveling agent is an acrylic acid copolymer, preferably MONENG-1153; the defoaming agent is polydimethylsiloxane.
In another aspect, the present application also provides a method for preparing the aqueous graphene conductive paste, including the following steps:
adding a surfactant into deionized water, adding graphene under the conditions of ultrasonic and magnetic stirring to disperse the graphene, adding a binding material, a light curing agent and an auxiliary agent, then adding a gelling agent, heating, cooling under the condition of high-speed shearing, and grinding to obtain the graphene nano-composite material.
Further, the heating temperature is 60-70 ℃.
In a preferred embodiment, the preparation method specifically comprises the following steps:
adding a surfactant into deionized water under the condition of simultaneously starting ultrasonic dispersion and magnetic stirring, uniformly mixing, adding graphene 8-10 times after uniformly mixing, and performing ultrasonic dispersion and magnetic stirring for 4-6 hours to obtain a mixed system, wherein the ultrasonic frequency is 20kHz and the magnetic stirring speed is 1800 r/min;
and step two, adding the bonding material, the light curing agent and the auxiliary agent into the mixed system, continuously stirring for 2 hours, adding the gelling agent, heating to 65 ℃ for 2 hours, cooling under the high-speed shearing condition, and grinding in a three-roll grinder until the fineness is less than 10 microns to obtain the nano-silver colloid material.
On the other hand, the application also provides an RFID tag, which comprises the aqueous graphene conductive paste and/or the aqueous graphene conductive paste prepared by the preparation method.
Preferably, the aqueous graphene conductive paste is used as an antenna or a printing paste of an RFID tag.
Further, the RFID tag is prepared by printing the aqueous graphene conductive paste on a substrate by adopting a gravure printing method, and when the gravure printing method is used, the temperature of the aqueous graphene conductive paste in an ink groove is 30-35 ℃, and ultraviolet light is used for curing.
The following beneficial effects can be brought through the application:
the aqueous graphene conductive paste provided by the application is dispersed in deionized water in the presence of a specific surfactant, and is supplemented with a specific binding material, a light curing agent and an auxiliary agent, and finally prepared into the aqueous conductive paste in a hydrogel form under the action of a gelling agent, so that the dispersion form of graphene is maintained, the stability is remarkably improved, the conductive advantage of graphene is fully exerted, and the used components are green and environment-friendly and harmless to the environment and human health; and can effectively resist the deformation of extending in intaglio printing, bonding effect and wear-resisting effect have also obtained effective promotion, have better printing adaptability.
Detailed Description
In order to more clearly explain the overall concept of the present application, the following detailed description of the overall scheme of the present invention is made by way of example. In the following description, numerous specific details are set forth in order to provide a more thorough understanding of the present invention. It will be apparent, however, to one skilled in the art, that the present invention may be practiced without one or more of these specific details. In other instances, well-known features have not been described in order to avoid obscuring the invention.
Unless otherwise specified, the starting components in the examples below are commercially available, and the laboratory instruments used are laboratory conventional laboratory instruments and the performance testing methods are those known in the art.
Example 1
The embodiment provides a water-based graphene conductive paste, which is composed of the following components in parts by weight:
12 parts of graphene nanosheet powder (average particle size of 30 microns and thickness of a lamella of 1-15 nanometers), 40 parts of deionized water, 3 parts of surfactant, 8 parts of gel, 33 parts of bisphenol A type glycidyl ether epoxy resin, 0.3 part of 1-hydroxycyclohexyl phenyl ketone, 1.7 parts of hydroxyethyl acrylate, 1 part of MONENG-1153 and 1 part of polydimethylsiloxane.
The aqueous graphene conductive paste is prepared from the raw material components by the following method:
adding a surfactant into deionized water under the condition of simultaneously starting ultrasonic dispersion and magnetic stirring, uniformly mixing, adding graphene 8-10 times after uniformly mixing, and performing ultrasonic dispersion and magnetic stirring for 4-6 hours to obtain a mixed system, wherein the ultrasonic frequency is 20kHz and the magnetic stirring speed is 1800 r/min;
and step two, adding bisphenol A glycidyl ether epoxy resin, 1-hydroxy ethyl phenyl ketone, hydroxyethyl acrylate, MONENG-1153 and polydimethylsiloxane into the mixed system, continuing stirring for 2h, adding a gelling agent, heating to 65 ℃ for 2h, cooling under a high-speed shearing condition, and grinding in a three-roll grinder until the fineness is less than 10 microns to obtain the nano-silver acrylate gel.
The aqueous conductive paste prepared by the method is uniform and stable in appearance and is a gel liquid with certain fluidity, the viscosity is 500-800 cp measured at 25 ℃, and the aqueous conductive paste is suitable for being printed by a gravure printing method.
The aqueous conductive pastes of examples 1-7 were prepared as described above and were identified as aqueous conductive paste series, except that the surfactant and gelling agent used were different in the same parts by weight. Printing and rolling the aqueous conductive paste prepared in each example by a gravure printing method by using a polyester PET (polyethylene terephthalate) film as a base material to form a film with the length of 30mm, the width of 20mm and the thickness of 20 microns, and performing ultraviolet irradiation curing, wherein the ultraviolet wavelength is 365nm, and the intensity is 80mW/cm2And the time length is 40 s.
Comparative example 1
The aqueous conductive paste of comparative example 1 was substantially the same as example 1 except that 48 parts by weight of dimethylformamide DMF was used as a dispersion instead of deionized water and a gelling agent, and the rest of the auxiliary materials and parts by weight were the same, and was directly ultrasonically mixed at 30 ℃.
Comparative example 2
Comparative example 2 an aqueous graphene conductive paste available from Ningbo ink science and technology Inc. was used.
And (3) carrying out performance tests on sheet resistance, adhesive force and rolling deformation of the roller on the aqueous conductive slurry after the printing and film forming. The sheet resistance is measured by adopting a four-probe method, the measured sheet resistance of the ink film prepared from the water-based graphene conductive slurry without any treatment is marked as sheet resistance one, the sheet resistance of the ink film prepared from the water-based graphene conductive slurry after the water-based graphene conductive slurry is centrifuged at 6000rpm for 5 minutes is marked as sheet resistance two, the sheet resistance change rate before and after centrifugation is calculated, and the stability and the settleability of the ink film are judged according to the sheet resistance change rate.
TABLE 1
As can be seen from the data in table 1, compared with graphene conductive paste prepared by dispersing organic solvent and surfactant in the prior art and commercial water-soluble graphene conductive paste sold in the market, the sheet resistance value measured by the aqueous graphene conductive paste provided by the application is smaller, and after high-speed centrifugal treatment, a smaller sheet resistance value can be still maintained, so that the dispersibility and stability of the aqueous graphene conductive paste are significantly improved, the graphene agglomeration can be effectively reduced, and the conductive performance advantage of the graphene nanosheet can be more favorably exerted. Meanwhile, the application also finds that the improvement capability of the dispersion stability of the aqueous graphene conductive paste obtained by dispersing the graphene powder is different by adopting different surfactants and gels, wherein when the surfactant is a compound mixture of sodium lignosulfonate, tea saponin and sodium surfactin and the gel is a compound of polyvinyl alcohol, sodium alginate and carboxymethyl cellulose, the obtained aqueous graphene conductive paste has the best improvement effect on the dispersion and stability of the graphene nanosheet powder.
Meanwhile, the above examples also show a good effect of resisting the rolling of the roller, but the adhesion performance on the substrate is not obviously improved, so the following example 7 with the best effect is taken as the base material, the composition of the binder in the example 7 is adjusted to further improve the adhesion, wear resistance and effect of resisting the rolling of the roller of the aqueous graphene conductive paste on the PET film, and the obtained aqueous graphene conductive paste is marked as the second aqueous graphene conductive paste series. The selection of the type of binder and the results of the performance tests in the specific examples are shown in table 2.
TABLE 2
As can be seen from the data in table 2, in the aqueous graphene conductive paste based on example 7, different binder types have different lifting capacities for the adhesion performance, the anti-stretching deformation performance and the wear-resistant hardness of the ink layer on the polyester PET film substrate, and the lifting effects of examples 12 and 13 are the best.
It can be known from the above summary that the aqueous graphene conductive paste provided by the application is environment-friendly, and can also significantly assist in promoting the dispersibility of graphene, reducing the agglomeration of graphene, and has better adaptability to gravure printing. The most preferable components and parts by weight of the aqueous graphene conductive paste are as follows:
12 parts of graphene nanosheet powder (with the average particle size of 30 microns and the thickness of a lamella of 1-15 nanometers), 40 parts of deionized water, 1.5-1.8 parts of sodium lignosulfonate, 0.7-0.8 part of tea saponin, 0.5-0.7 part of sodium surfactin, 4-5 parts of polyvinyl alcohol, 1 part of sodium alginate, 2-3 parts of carboxymethyl cellulose, 18-20 parts of bisphenol A type glycidyl ether epoxy resin, 8 parts of acrylic resin, 5-7 parts of polyvinylpyrrolidone, 0.3 part of 1-hydroxycycloethylphenyl ketone, 1.7 parts of hydroxyethyl acrylate, 1 part of MONENG-1153 and 1 part of polydimethylsiloxane.
The above description is only an example of the present application and is not intended to limit the present application. Various modifications and changes may occur to those skilled in the art. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present application should be included in the scope of the claims of the present application.
Claims (11)
1. The aqueous graphene conductive paste is characterized by comprising the following components in parts by weight: 10-15 parts of graphene, 40-60 parts of deionized water, 1-3 parts of surfactant, 5-8 parts of gelling agent, 30-35 parts of binding material, 0.5-2 parts of light curing agent and 1-5 parts of auxiliary agent,
the surfactant is selected from one or more of tea saponin, cyclic lipopeptide salt, lignosulfonate and dodecyl benzene sulfonate; the gel is selected from one or more of alginate, cellulose, polyvinyl alcohol, xanthan gum and agar powder.
2. The aqueous graphene conductive paste according to claim 1, wherein the graphene is prepared from powdered graphene nanosheets, the particle size of the powdered graphene nanosheets is 10-50 microns, and the thickness of the sheet layer is 1-15 nanometers.
3. The aqueous graphene conductive paste according to claim 1, wherein the surfactant is a mixture of (1.5-1.8) by mass: (0.7-0.8): (0.5-0.7) sodium lignosulfonate, tea saponin and surfactin sodium; the gel is prepared from the following components in percentage by mass (4-5): 1: (2-3) polyvinyl alcohol, alginate and carboxymethyl cellulose.
4. The aqueous graphene conductive paste according to claim 1, wherein the binder is prepared from (18-20) by mass: 8: (5-7) hydrophilic epoxy resin, acrylic resin and polyvinylpyrrolidone.
5. The aqueous graphene conductive paste according to claim 1, wherein the photo-curing agent comprises a photo-initiator and a photosensitive resin, and the photo-initiator is 1-hydroxycycloethylphenyl ketone; the photosensitive resin is selected from one or more of hydroxyethyl acrylate, terephthalic acid and tripropylene glycol diacrylate.
6. The aqueous graphene conductive paste according to claim 1, wherein the auxiliary agent is selected from a leveling agent and/or an antifoaming agent, wherein the leveling agent is an acrylic copolymer, and the antifoaming agent is polydimethylsiloxane.
7. The aqueous graphene conductive paste according to claim 6, wherein the leveling agent is MONENG-1153.
8. A method for preparing the aqueous graphene conductive paste according to any one of claims 1 to 7, wherein the method comprises the following steps:
adding a surfactant into deionized water, adding graphene under the conditions of ultrasonic and magnetic stirring to disperse the graphene, adding a binding material, a light curing agent and an auxiliary agent, then adding a gelling agent, heating, cooling under the condition of high-speed shearing, and grinding to obtain the graphene nano-composite material.
9. The method according to claim 8, wherein the heating temperature is 60 to 70 ℃.
10. An RFID label, comprising the aqueous graphene conductive paste according to any one of claims 1 to 7, or the aqueous graphene conductive paste prepared by the method according to claim 8 or 9.
11. The RFID tag according to claim 10, wherein the RFID tag is prepared by printing the aqueous graphene conductive paste onto a substrate by a gravure printing method, and when the gravure printing method is used, the temperature of the aqueous graphene conductive paste in an ink tank is 30-35 ℃, and the aqueous graphene conductive paste is cured by ultraviolet light.
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| CN114864135B (en) * | 2022-06-13 | 2023-04-28 | 山东华冠智能卡有限公司 | Degradable graphene conductive paste and RFID electronic tag |
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| CN108933216A (en) * | 2017-05-27 | 2018-12-04 | 北京师范大学 | It is a kind of to include graphene/cellulose composite material diaphragm and preparation method thereof |
| JP2019189858A (en) * | 2018-04-20 | 2019-10-31 | ナガセケムテックス株式会社 | Transparent conductive coating |
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| US10081550B2 (en) * | 2016-06-26 | 2018-09-25 | Nanotek Instruments, Inc. | Direct ultrasonication production of graphene sheets from coke or coal |
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| CN106867316A (en) * | 2017-03-17 | 2017-06-20 | 青岛瑞利特新材料科技有限公司 | A kind of watersoluble plumbago alkene electrically conductive ink |
| CN108933216A (en) * | 2017-05-27 | 2018-12-04 | 北京师范大学 | It is a kind of to include graphene/cellulose composite material diaphragm and preparation method thereof |
| JP2019189858A (en) * | 2018-04-20 | 2019-10-31 | ナガセケムテックス株式会社 | Transparent conductive coating |
| CN110436447A (en) * | 2019-07-26 | 2019-11-12 | 江西联锴新材料有限公司 | A kind of glue type graphene aqueous slurry and preparation method thereof |
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