CN117735536A - Graphene RFID tag and preparation method and application thereof - Google Patents
Graphene RFID tag and preparation method and application thereof Download PDFInfo
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Abstract
The invention belongs to the technical field of radio frequency identification (Radio Frequency Identification, RFID), and particularly relates to a graphene RFID tag and a preparation method and application thereof. The graphene prepared by the method has high dispersion performance and stability, is easy to disperse uniformly in a solvent and is stable to store, meanwhile, the prepared graphene sheet is distinct in layer and excellent in conductivity, and the conductivity of the graphene after dispersion is basically not influenced. The graphene conductive paste and the multilayer ink direct-writing printing technology based on the graphene conductive paste are environment-friendly, and can also be used for remarkably assisting in improving the conductivity of the graphene RFID tag antenna. Meanwhile, the adhesive has high adhesion, is not easy to fall off, has good toughness and is not easy to break, the service life is prolonged, the production efficiency can be effectively improved in mass production, the cost is reduced, and the time is saved.
Description
Technical Field
The invention belongs to the technical field of radio frequency identification (Radio Frequency Identification, RFID), and particularly relates to a graphene RFID tag and a preparation method and application thereof.
Background
The internet of things (Internet of Things, ioT) connects any object with the internet through information sensing devices such as Radio Frequency Identification (RFID), a positioning system and the like according to a contracted protocol, and performs information exchange and communication so as to realize intelligent identification, positioning, tracking, monitoring and management. Has been widely used in retail, transportation, military and other independent fields.
Radio frequency identification (radio frequency identification, RFID) technology is a technology that uses Radio Frequency (RF) waves for two-way information transfer through spatial coupling to achieve intelligent identification of targets. The RFID has strong anti-interference capability and long communication distance, can adapt to various complex application environments, improves working efficiency, reduces management cost, and is applied to various aspects including medical care, logistics, intelligent shopping, public security and the like. The RFID technology can be used for reading and writing information of the RFID tag, so that the purpose of identifying articles and exchanging data can be achieved.
The RFID antenna is generally made of metal materials such as copper and aluminum, and the mechanical, chemical and thermal stability of the metal tag is poor, so that the tag is extremely easy to damage in the practical application of the Internet of things, and meanwhile, electronic waste is generated. Therefore, replacement of metals with environmentally friendly, highly conductive materials is extremely urgent.
Disclosure of Invention
The invention aims to prepare a graphene material with high dispersion performance and stability by adopting an environment-friendly method, and the slurry prepared by the graphene material can be printed into an RFID antenna by a multilayer ink direct-writing technology to obtain the graphene RFID tag antenna with high conductivity.
The technical scheme adopted by the invention is as follows:
the invention provides a preparation method of graphene dispersion liquid, which comprises the following steps: and (3) after heating the expanded graphite by microwaves, cleaning the expanded graphite by deionized water until the pH value is 6.5-7.5, and dispersing the expanded graphite in an organic solvent for ultrasonic treatment after vacuum drying to obtain the graphene dispersion liquid.
Further, the microwave heating power is 780-820W, and the time is 20-30s; preferably, the microwave heating power is 800W and the time is 30s. According to the invention, the expanded graphite is subjected to secondary expansion under mild microwave conditions, so that the expanded graphite with fewer layers is obtained in advance, and then the graphene solid with distinct layers and more excellent conductivity is obtained through intercalation stripping in an organic solvent.
Further, the organic solvent is at least one of N, N-dimethylformamide, N-methylpyrrolidone, isopropanol or dihydro-l-glucosone; preferably, the organic solvent is dihydro-L-glucosone, and has the characteristics of no toxicity, biodegradability and the like.
Further, the vacuum drying condition is that the temperature is 80-120 ℃ and the drying time is 4-6 hours; preferably, the condition of vacuum drying is 100 ℃ drying for 5 hours. The vacuum degree of the vacuum drying is preferably 50-200Pa, more preferably less than or equal to 100Pa, and graphite reformation of peeled graphene stacks in the drying process can be avoided by adopting the vacuum drying.
Further, the ultrasonic treatment time is 6-10 hours; preferably, the time of the ultrasound is 8 hours.
The invention also provides the graphene dispersion prepared by the method.
The invention also provides graphene conductive paste prepared from the graphene dispersion liquid, and the preparation method of the conductive paste comprises the following steps: and filtering the graphene dispersion liquid, performing vacuum drying to obtain graphene solid, and mixing and ultrasonically stirring the graphene solid, the polymer stabilizer and the ethanol water solution.
Further, the polymer stabilizer is one of polyvinylpyrrolidone or cellulose; cellulose acetate butyrate is preferred.
Further, the polymer stabilizer is added in an amount of 0.5 to 5wt.%, preferably, 0.5 to 1.5wt.%.
Further, the volume ratio of ethanol to water in the ethanol aqueous solution is 1:0.25-4; preferably, the volume ratio is 1:1-3; more preferably, the volume ratio is 1:1.5.
further, the concentration of graphene in the graphene conductive paste is 10-60mg/mL; preferably, the concentration is 20-40mg/mL, more preferably, the concentration is 30mg/mL.
The invention also provides application of the graphene conductive paste in preparation of a graphene RFID antenna.
The invention also provides a graphene RFID antenna prepared from the graphene conductive paste, and the preparation method of the graphene RFID antenna comprises the following steps: and printing the graphene conductive paste on an antenna substrate through a multilayer ink direct writing technology.
Further, the antenna substrate comprises at least one of PET, PVC, PP, PC, paperboard, offset paper, coated paper, glass paperboard, laser paper, kraft paper, fluorescent paper, aluminum foil paper or anti-counterfeiting paper.
Specifically, the specific preparation method of the RFID antenna comprises the following steps: the graphene conductive slurry is placed into a charging barrel of an injector, is connected with a spray head, is installed on a triaxial CNC (computer numerical control) platform, an air pressure control system is opened, then an antenna substrate is fixed on a heating plate, the moving speed and the moving route of the spray head are set by a computer, the slurry extrusion speed is set, the heating plate is opened, and after the operation is started, the graphene conductive slurry is extruded from the spray head through a spiral extrusion or pneumatic pressure control system and is formed on the substrate. The technology can print continuous, uniform-thickness and good-adhesion antenna circuits on the substrate in multiple layers, accurately control the printing of complex circuit shapes, has short working time and high efficiency, and greatly improves the circuit conductivity.
Further, in the heating plate, the heating temperature is 60-80 ℃, and the moving speed of the workbench is 5-8; the extrusion speed of the slurry is 10-100 mu L/min; the ink jet needle is any one of 19 # number, 20 # number and 21 # number; the number of layers of the RFID antenna is 5-20 when in multilayer printing.
Further, the number of ink direct-write printing layers is preferably 8 to 11.
Further, the condition of compression treatment is that the pressure is maintained for 1-10min under 5-30 MPa.
The invention also provides application of the graphene RFID antenna in preparation of RFID electronic tags.
The invention has the beneficial effects that:
the invention provides a graphene material and a preparation method thereof, which can be used for preparing conductive paste and RFID antennas. The preparation method and the use process of the graphene provided by the invention are green and environment-friendly, strong acid, strong alkali and toxic solvents are not added in the preparation process of the graphene, heavy metal ions are not generated, and the graphene is harmless to the environment and human health; and the prepared graphene has high dispersion performance and stability, and is easy to disperse uniformly in a solvent and is stable to store. Meanwhile, the prepared graphene sheet is distinct in layer, excellent in conductivity, and the conductivity can reach 180S/mm. And the conductivity of the graphene is not affected basically after dispersion.
The invention further provides the graphene conductive paste, and the graphene conductive paste and the multilayer ink direct-writing printing technology based on the graphene conductive paste are environment-friendly, and meanwhile, the graphene conductive paste and the multilayer ink direct-writing printing technology based on the graphene conductive paste can be used for remarkably assisting in improving the conductivity of the graphene RFID tag antenna. Meanwhile, the adhesive has high adhesion, is not easy to fall off, has good toughness and is not easy to break, and the service life is prolonged. In addition, the production efficiency can be effectively improved, the cost can be reduced, and the time can be saved in mass production.
Common manufacturing processes for RFID antennas include chemical etching and printed circuit boards, which are cumbersome and not environmentally friendly. The direct writing technology is used as a forming technology which is developed faster in recent years, can accurately control the complex printing of the antenna circuit, and has the advantages of short working time, high efficiency and remarkable advantages. However, the direct-writing parameters (pressure and speed) and the direct-writing environment (temperature and direct-writing medium) of the ink direct-writing process can greatly influence the direct-writing process, and the ink needs to be matched with proper direct-writing parameters and the direct-writing environment to construct a stable structure.
The invention also provides an RFID antenna and an RFID electronic tag comprising the RFID antenna. The cost of the RFID electronic tag can be reduced by researching and developing the graphene RFID, the manufacturing technology of the RFID electronic tag is improved, the cost performance of the Gao Danmo graphene RFID electronic tag is generally improved, meanwhile, the green and clean performance in the manufacturing and using processes is ensured, the cost is reduced economically, and the manufacturing process is finished.
Therefore, the RFID antenna conductive paste is prepared by dispersing graphene in the environment-friendly and performance aspects. The application provides a multilayer ink direct-writing printing technology based on graphene conductive paste while providing a paste preparation scheme, and the technology can accurately control the complex printing of an antenna circuit, and is short in working time and high in efficiency. The multilayer printing technology fully exerts the conductive advantage of graphene, improves the conductivity, has high adhesion degree, is not easy to fall off, has good toughness and is not easy to break, the service life is prolonged, the stability is good, and the influence of environmental factors such as bending wrinkles on the resistance value is reduced.
Drawings
Fig. 1 is a diagram of a complex antenna circuit printed matter.
Fig. 2 SEM image of an embodiment of the antenna wire surface.
Fig. 3 prints graphene antenna line embodiment thickness measurement step gauge results at a time.
Detailed Description
The present invention will be described in detail with reference to the following specific embodiments, which are only preferred embodiments of the present invention and are not limiting.
1. Preparation of graphene conductive paste
Example 1
The expandable graphite was placed in a ceramic crucible and then heated in an 800W commercial microwave oven for 30s to obtain an expanded graphite having fewer layers. The expanded graphite flakes were stirred and washed in deionized water until the pH was near 7 and dried under vacuum at 100 ℃ for 5 hours. The dried expanded graphite was deposited on dihydrol-glucosone (10 mg mL) -1 ) After that, the mixture was sonicated in an ultrasonic bath. And (5) carrying out ultrasonic treatment for 8 hours to obtain a graphene dispersion liquid with uniform dispersion. And filtering the graphene dispersion liquid, centrifuging at a low speed, and obtaining graphene sheets through vacuum rotary evaporation. Adding the graphene sheets into an ethanol/water mixed solution, and addingAnd (3) 1wt.% of CAB, and carrying out ultrasonic treatment, stirring and obtaining the uniformly dispersed graphene conductive paste. Wherein ethanol and water are mixed according to the volume ratio of 1:3, 1:2, 1:1.5 and 1:1, and are dispersed with graphene sheets to prepare uniform graphene conductive slurry with the concentration of 40mg/ml, 30mg/ml, 20mg/ml and 10 mg/ml.
Comparative example 1
The expandable graphite was placed in a ceramic crucible and then heated in an 8kW commercial microwave oven for 30 seconds to obtain expanded graphite with fewer layers. The expanded graphite flakes were stirred and washed in deionized water until the pH was near 7 and dried under vacuum at 100 ℃ for 5 hours. The dried expanded graphite was deposited on dihydrol-glucosone (10 mg mL) -1 ) After that, the mixture was sonicated in an ultrasonic bath. And (5) carrying out ultrasonic treatment for 8 hours to obtain a graphene dispersion liquid with uniform dispersion. And filtering the graphene dispersion liquid, centrifuging at a low speed, and obtaining graphene solid through vacuum rotary evaporation. And adding the graphene solid into the ethanol/water mixed solution, adding 1wt.% of CAB, and carrying out ultrasonic treatment and stirring to obtain the graphene conductive paste with uniform dispersion. Wherein ethanol and water are mixed according to a volume ratio of 1:1, and are dispersed and prepared with graphene sheets to obtain the graphene conductive paste comparative example 1 with the uniform concentration of 30mg/mL.
Comparative example 2
Heating graphite oxide to 400 ℃ at a rate of 10 ℃ per minute under nitrogen, calcining, adding a mixed solution of ethylene glycol and water, uniformly dispersing under ultrasonic combined magnetic stirring, adding a mixed solution of NaOH and ethylene glycol, regulating the pH value to 10-12, sealing, heating to 700 ℃ by microwaves for about 2min, and repeating heating for 3 times. And magnetically stirring and cooling to room temperature, washing, filtering and drying to obtain the graphene material, adding the graphene material into a solvent (dimethylformamide (DMF)), adding 1wt.% CAB, carrying out ultrasonic treatment, stirring, and uniformly dispersing to obtain 30mg/ml of the graphene conductive paste as comparative example 2.
Comparative example 3
Heating graphite oxide to 400 ℃ at a rate of 10 ℃ per minute under nitrogen, calcining, adding a mixed solution of ethylene glycol and water, uniformly dispersing under ultrasonic combined magnetic stirring, adding a mixed solution of NaOH and ethylene glycol, regulating the pH value to 10-12, sealing, heating to 700 ℃ by microwaves for about 2min, and repeating heating for 3 times. And magnetically stirring and cooling to room temperature, washing, filtering and drying to obtain the graphene material. And filtering the graphene material, centrifuging at a low speed, and obtaining graphene solid through vacuum rotary evaporation. Graphene solid is added into an ethanol/water mixed solution, and 1wt.% of CAB is added, and then ultrasonic treatment and stirring are carried out, so that 30mg/ml of graphene conductive slurry which is uniformly dispersed is obtained, and comparative example 3.
Comparative example 4
Graphite columns were etched on HOPG first, one side of the graphite columns was pressed against a glass sheet coated with a wet photoresist 1 μm thick, and baking was performed to leave the graphite columns on the photoresist. Repeatedly peeling off the photoresist with transparent adhesive tape, dissolving the photoresist with propanol, and collecting SiO 2 After the Si substrate is soaked in the propanol solution, a large amount of water and propanol are used for flushing the substrate, and the graphene sheet is obtained after drying. Graphene sheets were added to an ethanol/water mixed solution, and 1wt.% CAB was added, wherein water and ethanol were mixed in a volume ratio of 1:1, and then sonicated and stirred to obtain a uniform graphene conductive paste comparative example 4 having a concentration of 30mg/mL.
2. Preparation of graphene RFID antenna
Example 2
Graphene sheets of example 1 were added to a mixed solution of ethanol and water in a volume ratio of 1:1, and 1wt.% CAB was added to prepare a graphene conductive paste having a concentration of 10 mg/ml. Taking 4mL of the 10mg/mL graphene conductive slurry, placing the graphene conductive slurry into a charging barrel of an injector, connecting the charging barrel with a spray nozzle, installing the charging barrel on a triaxial CNC platform, opening an air pressure control system, fixing a PET (polyethylene terephthalate) substrate on a heating plate, setting the moving speed of the spray nozzle to 7 by using a computer, setting the moving route of the spray nozzle, setting the extruding speed of the slurry to 15 microliters per minute, opening the heating plate, setting the temperature of the heating plate to 70 ℃, starting to operate after the temperature of the heating plate rises and is stabilized at 70 ℃, extruding the graphene conductive slurry from the spray nozzle through a screw extrusion or pneumatic pressure control system, and forming the graphene conductive slurry on the substrate.
The formed antenna circuit covering substrate is placed into a manual press machine, the set pressure is 25MPa, the substrate is placed into an ion sputtering instrument after pressure maintaining for 3 minutes, the sputtering time is set for 5 minutes, and the test conductivity is shown in Table 1.
Example 3
Graphene sheets of example 1 were added to a mixed solution of ethanol and water in a volume ratio of 1:1, and 1wt.% CAB was added to prepare a graphene conductive paste having a concentration of 20 mg/ml. Taking 4mL of the 20mg/mL graphene conductive slurry, placing the graphene conductive slurry into a charging barrel of an injector, connecting the charging barrel with a spray nozzle, installing the charging barrel on a triaxial CNC platform, opening an air pressure control system, fixing a PP matrix on a heating plate, setting the moving speed of the spray nozzle to 7 by using a computer, setting the moving route of the spray nozzle, setting the extruding speed of the slurry to 15 microliters per minute, opening the heating plate, setting the temperature of the heating plate to 70 ℃, starting to operate after the temperature of the heating plate rises and is stabilized at 70 ℃, extruding the graphene conductive slurry from the spray nozzle through a screw extrusion or pneumatic pressure control system, and forming the graphene conductive slurry on the matrix.
The formed antenna circuit covering substrate is placed into a manual press machine, the set pressure is 25MPa, the substrate is placed into an ion sputtering instrument after pressure maintaining for 3 minutes, the sputtering time is set for 5 minutes, and the test conductivity is shown in Table 1.
Example 4
Graphene sheets of example 1 were added to a mixed solution of ethanol and water in a volume ratio of 1:1, and 1wt.% CAB was added to prepare a graphene conductive paste having a concentration of 30mg/ml. Taking 4mL of the 30mg/mL graphene conductive slurry, placing the graphene conductive slurry into a charging barrel of an injector, connecting the charging barrel with a spray head, installing the charging barrel on a triaxial CNC (computer numerical control) platform, opening an air pressure control system, fixing coated paper on a heating plate, setting the moving speed of the spray head to 7 by using a computer, setting the moving route of the spray head, setting the extruding speed of the slurry to 15 microliters per minute, opening the heating plate, setting the temperature of the heating plate to 70 ℃, starting to operate after the temperature of the heating plate rises and is stabilized at 70 ℃, extruding the graphene conductive slurry from the spray head through a screw extrusion or pneumatic pressure control system, and forming the graphene conductive slurry on a substrate.
The formed antenna circuit covering substrate is placed into a manual press machine, the set pressure is 25MPa, the substrate is placed into an ion sputtering instrument after pressure maintaining for 3 minutes, the sputtering time is set for 5 minutes, and the test conductivity is shown in Table 1.
Example 5
Graphene sheets of example 1 were added to a mixed solution of ethanol and water at a volume ratio of 1:1.5, and 1wt.% CAB was added to prepare a graphene conductive paste at a concentration of 30mg/ml. Taking 4ml of the 30mg/ml graphene conductive slurry, placing the graphene conductive slurry into a charging barrel of an injector, connecting the injector with a spray head, installing the injector on a triaxial CNC (computer numerical control) platform, opening an air pressure control system, fixing a PP (polypropylene) substrate on a heating plate, setting the moving speed of the spray head to 7 by using a computer, setting the moving route of the spray head, setting the extruding speed of the slurry to 15 microlitres per minute, opening the heating plate, setting the temperature of the heating plate to 70 ℃, starting to operate after the temperature of the heating plate rises and is stabilized at 70 ℃, extruding the graphene conductive slurry from the spray head through a screw extrusion or pneumatic pressure control system, and forming the graphene conductive slurry on the substrate.
The formed antenna circuit covering substrate is placed into a manual press machine, the set pressure is 25MPa, the substrate is placed into an ion sputtering instrument after pressure maintaining for 3 minutes, the sputtering time is set for 5 minutes, and the test conductivity is shown in Table 1.
Example 6
Graphene sheets of example 1 were added to a mixed solution of ethanol and water at a volume ratio of 1:2, and 1wt.% CAB was added to prepare a graphene conductive paste at a concentration of 30mg/ml. Taking 4ml of the 30mg/ml graphene conductive slurry, placing the graphene conductive slurry into a charging barrel of an injector, connecting the injector with a spray head, installing the injector on a triaxial CNC (computer numerical control) platform, opening an air pressure control system, fixing a PP (polypropylene) substrate on a heating plate, setting the moving speed of the spray head to 7 by using a computer, setting the moving route of the spray head, setting the extruding speed of the slurry to 15 microlitres per minute, opening the heating plate, setting the temperature of the heating plate to 70 ℃, starting to operate after the temperature of the heating plate rises and is stabilized at 70 ℃, extruding the graphene conductive slurry from the spray head through a screw extrusion or pneumatic pressure control system, and forming the graphene conductive slurry on the substrate.
The formed antenna circuit covering substrate is placed into a manual press machine, the set pressure is 25MPa, the substrate is placed into an ion sputtering instrument after pressure maintaining for 3 minutes, the sputtering time is set for 5 minutes, and the test conductivity is shown in Table 1.
Example 7
Graphene sheets of example 1 were added to a mixed solution of ethanol and water in a volume ratio of 1:3, and 1wt.% CAB was added to prepare a graphene conductive paste with a concentration of 30mg/ml. Taking 4ml of the 30mg/ml graphene conductive slurry, placing the graphene conductive slurry into a charging barrel of an injector, connecting the injector with a spray head, installing the injector on a triaxial CNC (computer numerical control) platform, opening an air pressure control system, fixing a PP (polypropylene) substrate on a heating plate, setting the moving speed of the spray head to 7 by using a computer, setting the moving route of the spray head, setting the extruding speed of the slurry to 15 microlitres per minute, opening the heating plate, setting the temperature of the heating plate to 70 ℃, starting to operate after the temperature of the heating plate rises and is stabilized at 70 ℃, extruding the graphene conductive slurry from the spray head through a screw extrusion or pneumatic pressure control system, and forming the graphene conductive slurry on the substrate.
The formed antenna circuit covering substrate is placed into a manual press machine, the set pressure is 25MPa, the substrate is placed into an ion sputtering instrument after pressure maintaining for 3 minutes, the sputtering time is set for 5 minutes, and the test conductivity is shown in Table 1.
Comparative example 5
Taking 4mL of comparative example 1, placing the same into a syringe charging barrel, connecting the same with a spray nozzle, installing the same on a triaxial CNC platform, opening an air pressure control system, then fixing a PET matrix on a heating plate, setting the moving speed of the spray nozzle to 7 by using a computer, setting the moving route of the spray nozzle, setting the extrusion speed of slurry to 15 microliters per minute, opening the heating plate, setting the temperature of the heating plate to 70 ℃, starting to operate after the temperature of the heating plate rises and is stabilized at 70 ℃, extruding graphene conductive slurry from the spray nozzle through a spiral extrusion or pneumatic pressure control system, and forming the graphene conductive slurry on the matrix.
The formed antenna circuit covering substrate is placed into a manual press machine, the set pressure is 25MPa, the substrate is placed into an ion sputtering instrument after pressure maintaining for 3 minutes, the sputtering time is set for 5 minutes, and the test conductivity is shown in Table 1.
Comparative example 6
Weighing 4ml of the comparative example 2, placing the comparative example into a charging barrel of an injector, connecting the charging barrel with a spray nozzle, installing the charging barrel on a triaxial CNC platform, opening an air pressure control system, then fixing a PET matrix on a heating plate, setting the moving speed of the spray nozzle to 7 by using a computer, setting the moving route of the spray nozzle, setting the extrusion speed of slurry to 15 microlitres per minute at the same time, opening the heating plate, setting the temperature of the heating plate to 70 ℃, starting to operate after the temperature of the heating plate rises and is stabilized at 70 ℃, and extruding graphene conductive slurry from the spray nozzle through a screw extrusion or pneumatic pressure control system and forming the graphene conductive slurry on the matrix.
The formed antenna circuit covering substrate is placed into a manual press machine, the set pressure is 25MPa, the substrate is placed into an ion sputtering instrument after pressure maintaining for 3 minutes, the sputtering time is set for 5 minutes, and the test conductivity is shown in Table 1.
Comparative example 7
Weighing 4ml of the comparative example 3, placing the comparative example into a charging barrel of an injector, connecting the charging barrel with a spray nozzle, installing the charging barrel on a triaxial CNC platform, opening an air pressure control system, then fixing a PET matrix on a heating plate, setting the moving speed of the spray nozzle to 7 by using a computer, setting the moving route of the spray nozzle, setting the extrusion speed of slurry to 15 microlitres per minute at the same time, opening the heating plate, setting the temperature of the heating plate to 70 ℃, starting to operate after the temperature of the heating plate rises and is stabilized at 70 ℃, and extruding graphene conductive slurry from the spray nozzle through a screw extrusion or pneumatic pressure control system and forming the graphene conductive slurry on the matrix.
The formed antenna circuit covering substrate is placed into a manual press machine, the set pressure is 25MPa, the substrate is placed into an ion sputtering instrument after pressure maintaining for 3 minutes, the sputtering time is set for 5 minutes, and the test conductivity is shown in Table 1.
Comparative example 8
Weighing 4mL of the graphene conductive slurry of the comparative example 4, placing the graphene conductive slurry into a charging barrel of an injector, connecting the charging barrel with a spray nozzle, installing the charging barrel on a triaxial CNC platform, opening a pneumatic control system, fixing a PET substrate on a heating plate, setting the moving speed of the spray nozzle to 7 by using a computer, setting the moving route of the spray nozzle, setting the extruding speed of the slurry to 15 microliters per minute, opening the heating plate, setting the temperature of the heating plate to 70 ℃, starting operation after the temperature of the heating plate rises and is stabilized at 70 ℃, extruding the graphene conductive slurry from the spray nozzle through a screw extrusion or pneumatic pressure control system, and forming the graphene conductive slurry on the substrate.
The formed antenna circuit covering substrate is placed into a manual press machine, the set pressure is 25MPa, the substrate is placed into an ion sputtering instrument after pressure maintaining for 3 minutes, the sputtering time is set for 5 minutes, and the test conductivity is shown in Table 1.
Comparative example 9
The graphene sheet of example 1 was added to pure water, and 1wt.% CAB was added to prepare a graphene conductive paste having a concentration of 30mg/ml. Weighing 4ml of the 30mg/ml graphene conductive slurry, placing the graphene conductive slurry into a charging barrel of an injector, connecting the injector with a spray head, installing the injector on a triaxial CNC (computer numerical control) platform, opening an air pressure control system, fixing a PP (polypropylene) substrate on a heating plate, setting the moving speed of the spray head to 7 by using a computer, setting the moving route of the spray head, setting the extruding speed of the slurry to 15 microlitres per minute, opening the heating plate, setting the temperature of the heating plate to 70 ℃, starting to operate after the temperature of the heating plate rises and is stabilized at 70 ℃, extruding the graphene conductive slurry from the spray head through a screw extrusion or pneumatic pressure control system, and forming the graphene conductive slurry on the substrate.
The formed antenna circuit covering substrate is placed into a manual press machine, the set pressure is 25MPa, the substrate is placed into an ion sputtering instrument after pressure maintaining for 3 minutes, the sputtering time is set for 5 minutes, and the test conductivity is shown in Table 1.
Comparative example 10
Graphene sheets of example 1 were added to a mixed solution of ethanol and water in a volume ratio of 1:1, and 1wt.% CAB was added to prepare a graphene conductive paste having a concentration of 40 mg/ml. Taking 4mL of the 40mg/mL graphene conductive slurry, placing the graphene conductive slurry into a charging barrel of an injector, connecting the charging barrel with a spray nozzle, installing the charging barrel on a triaxial CNC platform, opening an air pressure control system, fixing a PET (polyethylene terephthalate) substrate on a heating plate, setting the moving speed of the spray nozzle to 7 by using a computer, setting the moving route of the spray nozzle, setting the extruding speed of the slurry to 15 microliters per minute, opening the heating plate, setting the temperature of the heating plate to 70 ℃, starting to operate after the temperature of the heating plate rises and is stabilized at 70 ℃, extruding the graphene conductive slurry from the spray nozzle through a screw extrusion or pneumatic pressure control system, and forming the graphene conductive slurry on the substrate.
The graphene conductive paste prepared by the method is serious in agglomeration, difficult to stir and disperse uniformly, a needle is blocked in the direct writing process, the extrusion difficulty is high, the direct writing circuit is uneven due to the fact that the extrusion pressure is too large, the thickness of the circuit is different, and the conductivity difference of each part of the circuit is large.
Comparative example 11
Graphene sheets of example 1 were added to a mixed solution of ethanol and water in a volume ratio of 1:1, and 1wt.% CAB was added to prepare a graphene conductive paste having a concentration of 30mg/ml. Taking 4mL of the 30mg/mL graphene conductive slurry, placing the graphene conductive slurry into a charging barrel of an injector, connecting the charging barrel with a spray nozzle, installing the charging barrel on a triaxial CNC platform, opening an air pressure control system, fixing a PP matrix on a heating plate, setting the moving speed of the spray nozzle to 7 by using a computer, setting the moving route of the spray nozzle, setting the extruding speed of the slurry to 15 microliters per minute, opening the heating plate, setting the temperature of the heating plate to 70 ℃, starting to operate after the temperature of the heating plate rises and is stabilized at 70 ℃, extruding the graphene conductive slurry from the spray nozzle through a screw extrusion or pneumatic pressure control system, and forming the graphene conductive slurry on the matrix.
The molded antenna circuit was placed in an ion sputtering apparatus, the sputtering time was set to 5 minutes, and the test conductivity was shown in table 2.
TABLE 1 antenna conductivity test results for examples 2-7, comparative examples 5-9
| Project | Graphene concentration | Ethanol/water | conductivity/(S/mm) |
| Example 2 | 10mg/ml | 1:1 | 0.24 |
| Example 3 | 20mg/ml | 1:1 | 0.82 |
| Example 4 | 30mg/ml | 1:1 | 1.67 |
| Example 5 | 30mg/ml | 1:1.5 | 7.82 |
| Example 6 | 30mg/ml | 1:2 | 0.96 |
| Example 7 | 30mg/ml | 1:3 | 0.23 |
| Comparative example 5 | 30mg/ml | 1:1 | 0.78 |
| Comparative example 6 | 30mg/ml | 1:1 | 0.12 |
| Comparative example 7 | 30mg/ml | 1:1 | 0.25 |
| Comparative example 8 | 30mg/ml | 1:1 | 0.39 |
| Comparative example 9 | 30mg/ml | 0:1 | 0.43 |
Table 2 results of antenna conductivity test of example 4 and comparative example 11
| Project | Example 4 | Comparative example 11 |
| conductivity/(S/mm) | 1.67 | 0.25 |
| Thickness/(μm) | 0.4 | 3 |
| Sheet resistance/(Ω/sq.) | 1497 | 1333 |
The result shows that the graphene preparation method is used for remarkably assisting in improving the conductivity of the graphene RFID tag antenna, the conductivity reaches the highest when the graphene concentration is 30mg/mL, the conductive paste added with the ethanol is used for remarkably assisting in improving the conductivity of the graphene RFID tag antenna, and the volume ratio of the ethanol to the water is 1:1.5, so that the conductivity of the graphene conductive antenna is remarkably improved.
The graphene conductive paste prepared in example 5 was extruded from a spray head through a screw extrusion or pneumatic pressure control system and molded on a substrate, and was repeatedly printed 5 to 11 times to obtain an antenna line. The formed antenna circuit covering substrate is placed into a manual press machine, the set pressure is 25MPa, the substrate is placed into an ion sputtering instrument after pressure maintaining for 3 minutes, the sputtering time is set for 5 minutes, and the test conductivity is shown in Table 3.
TABLE 3 influence of the number of repeated printing of graphene conductive pastes on conductivity in example 5
As can be seen from the results in Table 3, the 11-layer direct write conductivity has little improvement effect and similar sheet resistance compared with the 10-layer direct write. The direct writing effect of more layers is close, the time cost is too high, and the efficiency is reduced, so that the optimal number of layers of the multilayer printing is 10-11.
The graphene conductive paste prepared in example 5 is extruded from a spray head through a screw extrusion or pneumatic pressure control system and is molded on a substrate, the antenna circuit is obtained by repeated printing for 10 times, the prepared antenna circuit is continuously bent and folded in half, the conductivity and the adhesive force of the antenna circuit are tested, and the test results are shown in tables 4 and 5 below.
Table 4 results of test on conductivity and adhesion after the antenna was bent and folded 100 times at different angles
Table 5 results of test for conductivity and adhesion after 90 ° different bends of antenna
The results in tables 4 and 5 show that the prepared antenna circuit has high adhesiveness, good toughness and difficult breakage, is not easy to fall off, prolongs the service life, has good stability, and reduces the influence of environmental factors such as bending wrinkles and the like on the resistance value of the antenna circuit.
It will be understood that the above embodiments are further illustrative of the present invention and are not intended to limit the scope of the invention, and that all other modifications and variations which may be obtained without the inventive effort by those skilled in the art are within the scope of the invention.
Claims (10)
1. The preparation method of the graphene dispersion liquid is characterized by comprising the following steps of: and (3) after heating the expanded graphite by microwaves, cleaning the expanded graphite by deionized water until the pH value is 6.5-7.5, and dispersing the expanded graphite in an organic solvent for ultrasonic treatment after vacuum drying to obtain the graphene dispersion liquid.
2. The method according to claim 1, wherein the microwave heating power is 780-820W for 20-30s.
3. The method according to claim 1, wherein the organic solvent is at least one of N, N-dimethylformamide, N-methylpyrrolidone, isopropanol, and dihydrol-glucosone.
4. A graphene dispersion prepared by the method of any one of claims 1-3.
5. The preparation method of the graphene conductive paste is characterized by comprising the following steps of: the graphene dispersion liquid of claim 4 is filtered and dried in vacuum to obtain graphene solid, and the graphene solid is mixed with a polymer stabilizer and an ethanol water solution and stirred in an ultrasonic manner.
6. The method of claim 5, wherein the polymer stabilizer is one of polyvinylpyrrolidone or cellulose.
7. A graphene conductive paste prepared by the method of any one of claims 5-6.
8. Use of the graphene dispersion of claim 4 or the graphene conductive paste of claim 7 in the preparation of a graphene RFID antenna.
9. The preparation method of the graphene RFID antenna is characterized by comprising the following steps of: the graphene conductive paste of claim 7 is printed on an antenna substrate by a multilayer ink direct writing technique.
10. Use of the graphene RFID antenna according to claim 9 for the preparation of RFID electronic tags.
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