WO2021232597A1 - Film conducteur flexible de réparation thermique à la lumière du proche infrarouge et procédé de préparation associé - Google Patents

Film conducteur flexible de réparation thermique à la lumière du proche infrarouge et procédé de préparation associé Download PDF

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Publication number
WO2021232597A1
WO2021232597A1 PCT/CN2020/106757 CN2020106757W WO2021232597A1 WO 2021232597 A1 WO2021232597 A1 WO 2021232597A1 CN 2020106757 W CN2020106757 W CN 2020106757W WO 2021232597 A1 WO2021232597 A1 WO 2021232597A1
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Prior art keywords
conductive film
preparation
silver
composite material
thermoplastic polyurethane
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PCT/CN2020/106757
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English (en)
Chinese (zh)
Inventor
王悦辉
周志敏
赵玉珍
王可
林凯文
张小宾
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电子科技大学中山学院
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Publication of WO2021232597A1 publication Critical patent/WO2021232597A1/fr

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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B5/00—Non-insulated conductors or conductive bodies characterised by their form
    • H01B5/14—Non-insulated conductors or conductive bodies characterised by their form comprising conductive layers or films on insulating-supports
    • 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
    • H01B1/22—Conductive material dispersed in non-conductive organic material the conductive material comprising metals or alloys
    • 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
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B13/00—Apparatus or processes specially adapted for manufacturing conductors or cables

Definitions

  • the invention relates to the technical field of self-healing materials, in particular to a near-infrared thermal repairing flexible conductive film and a preparation method thereof.
  • the purpose of the present invention is to provide a near-infrared thermal repair flexible conductive film and a preparation method thereof.
  • the conductive film prepared by the present invention has high electrical conductivity and thermal conductivity, and has high repair efficiency under the action of near-infrared light, and can achieve rapid multiplication. Repairs.
  • the invention provides a method for preparing a near-infrared thermal repair flexible conductive film, which includes the following steps:
  • the silver nanowire-graphene composite material, thermoplastic polyurethane and N,N-dimethylformamide are mixed, and the resulting mixed slurry is formed into a film, and after drying, a near-infrared thermal repair flexible conductive film is obtained.
  • the temperature of the solvothermal reaction is 150-180°C, and the time is 3-5 hours.
  • the mass content of silver nitrate is 0.5-1.0%
  • the mass ratio of graphene oxide and silver nitrate is (0.03-0.1):1
  • the mass content of polyvinylpyrrolidone is 1.0-1.3%
  • the mass content of ferric chloride is 0.0015 to 0.003%.
  • the mass of the silver nanowire-graphene composite material accounts for 20-40% of the total mass of the silver nanowire-graphene composite material and the thermoplastic polyurethane.
  • the mass of the thermoplastic polyurethane accounts for 20-30% of the total mass of the thermoplastic polyurethane and N,N-dimethylformamide.
  • the film formation method is casting film formation.
  • the drying temperature is 60-75°C, and the time is 12-36 hours.
  • the process of mixing graphene oxide, silver nitrate and ethylene glycol includes: adding graphene oxide to ethylene glycol for ultrasound, and then adding silver nitrate and stirring until it is completely dissolved.
  • the present invention provides a near-infrared thermal repair flexible conductive film prepared by the preparation method described in the above solution, which includes a silver nanowire-graphene composite material and a thermoplastic polyurethane.
  • the mass content of the silver nanowire-graphene composite material is 20-40%, and the balance is thermoplastic polyurethane.
  • the invention provides a method for preparing a near-infrared thermal repair flexible conductive film, which comprises the following steps: mixing graphene oxide, silver nitrate and ethylene glycol to obtain a first mixed liquid; Mixing with ethylene glycol to obtain a second mixed material liquid; mixing the first mixed material liquid and the second mixed material liquid, and subjecting the obtained reaction material liquid to a solvothermal reaction to obtain a silver nanowire-graphene composite material; The silver nanowire-graphene composite material, thermoplastic polyurethane and N,N-dimethylformamide are mixed, the resulting mixed slurry is formed into a film, and after drying, a near-infrared thermal repair flexible conductive film is obtained.
  • graphene oxide, silver nitrate and ethylene glycol are mixed, and silver nitrate ions can be adsorbed on the surface and between layers of graphene oxide sheets to form a graphene oxide/silver ion composite system.
  • the graphene oxide is also reduced to graphene, which is conducive to the adhesion of the silver nanowires to the graphene surface and the insertion into the graphene layer during formation.
  • a silver nanowire-graphene hybrid structure is formed.
  • the silver nanowire-graphene hybrid structure on the one hand avoids the stacking of graphene sheets and improves the dispersibility, thereby helping to improve the conductivity of the film. On the other hand, it compensates for the influence of silver nanowires on the mechanical properties of the conductive film.
  • polyvinylpyrrolidone, ferric chloride and ethylene glycol are mixed to obtain a second mixed material liquid.
  • polyvinylpyrrolidone is used as a surface modifier and has the functions of controlling the growth of silver nanowires and morphology control.
  • ferric chloride acts as an inhibitor.
  • the graphene oxide/silver ion composite system in the reaction material liquid can form a small amount with ferric chloride and polyvinylpyrrolidone
  • the chloride ion present in the reaction feed solution can provide electrostatic stability for the first silver seed crystal, and the chloride ion can combine with the silver ion to form AgCl colloid, which reduces the initial
  • the concentration of free silver ions in the solution reduces the speed at which silver ions are reduced and silver seed crystals grow; this slow reaction process is conducive to the formation of thermodynamically stable multiple twin seed crystals; polyvinylpyrrolidone is preferentially adsorbed on The ⁇ 100 ⁇ crystal plane family of multiple twin seed crystals enables it to grow along the ⁇ 111 ⁇ crystal plane and grow into silver nanowires through anisotropy; as the reaction progresses, the concentration of free silver ions in the solution gradually decreases In order to
  • the formation and growth of seed crystals provide better conditions, which is conducive to obtaining silver nanowires with larger diameters.
  • the graphene oxide is reduced to graphene by ethylene glycol during the solvothermal reaction, and the formed silver nanowires are attached to the surface of the graphene and inserted between the graphene layers to obtain a silver nanowire-graphene with a hybrid structure.
  • Composite materials are used.
  • Fe 3+ can be reduced to Fe 2+ by ethylene glycol, and oxygen can reduce Fe 2+ is re-oxidized to Fe 3+ and circulates in sequence. This process can consume the residual oxygen in the reaction liquid and eliminate its etching effect on the silver seed crystal.
  • the present invention uses thermoplastic polyurethane as a matrix and a silver nanowire-graphene composite material with a hybrid structure as a conductive filler (in which silver nanowires are the main conductive phase and graphene is the auxiliary phase), and the thermoplastic polyurethane system is based on The high-efficiency energy conversion unit and conductive path of silver nanowire-graphene, the flexible conductive film obtained has high conductivity; at the same time, the use of silver nanowire and graphene's absorption characteristics of near-infrared light can not only achieve local heating in small areas The damaged thermoplastic polyurethane material can be repaired, and the repair efficiency of the thermoplastic polyurethane conductive film can be improved, and rapid multiple repairs can be realized.
  • the silver nanowire-graphene composite material absorbs the near-infrared light to heat the thermoplastic polyurethane, and the thermoplastic polyurethane itself absorbs part of the heat.
  • the two work together to promote the melting of the thermoplastic polyurethane.
  • the flow realizes the self-repair of the damaged membrane, which greatly improves the repair efficiency; and during the self-repair process, the silver nanowire-graphene composite material is pulled to reorganize to form a new conductive network, and the final repair will still have high conductivity.
  • graphene helps to improve the mechanical properties of the thermoplastic polyurethane material, so as to ensure that the repaired conductive film still has good mechanical properties.
  • the near-infrared thermal repair flexible conductive film prepared by the present invention has high conductivity, and when microcracks appear on the surface of the conductive film, the microcracks disappear after 5-10 minutes of irradiation under an infrared lamp with a wavelength of 0.76-5 ⁇ m. Achieve a complete repair.
  • the invention provides a method for preparing a near-infrared thermal repair flexible conductive film, which includes the following steps:
  • the silver nanowire-graphene composite material, thermoplastic polyurethane and N,N-dimethylformamide are mixed, the resulting mixed slurry is formed into a film, and after drying, a near-infrared thermal repair flexible conductive film is obtained.
  • the raw materials used are all commercially available products well known in the art.
  • graphene oxide, silver nitrate and ethylene glycol are mixed to obtain the first mixed material liquid.
  • the mixing process is preferably: adding graphene oxide to ethylene glycol for ultrasound, and then adding silver nitrate and stirring until it is completely dissolved.
  • the power of the ultrasound is preferably 300W
  • the time of the ultrasound is preferably 1 hour.
  • the invention uniformly disperses graphene oxide into ethylene glycol through ultrasound.
  • the present invention has no special requirements on the stirring conditions, as long as the silver nitrate can be completely dissolved. Regarding the amount of each raw material, the present invention will be described later.
  • silver nitrate ions can be adsorbed on the surface and between layers of graphene oxide sheets to form a graphene oxide/silver ion composite system.
  • graphene oxide/silver ion when graphene oxide/silver ion When the silver ions in the composite system are reduced to form silver nanowires, graphene oxide is also reduced to graphene, which is conducive to the adhesion of silver nanowires to the surface of graphene and intercalation between graphene layers to form silver nanowires.
  • -Graphene hybrid structure when graphene oxide/silver ion When the silver ions in the composite system are reduced to form silver nanowires, graphene oxide is also reduced to graphene, which is conducive to the adhesion of silver nanowires to the surface of graphene and intercalation between graphene layers to form silver nanowires.
  • polyvinylpyrrolidone, ferric chloride and ethylene glycol are mixed to obtain a second mixed material liquid.
  • the present invention has no special requirements on the stirring conditions, and it is enough to ensure that the substances are completely dissolved.
  • polyvinylpyrrolidone is used as a surface modifier to control the growth and morphology of silver nanowires
  • ethylene glycol is used as a reducing agent and solvent
  • ferric chloride is used as an inhibitor. The dosage will be discussed in detail later.
  • the present invention mixes the first mixed material liquid and the second mixed material liquid to obtain a reaction material liquid.
  • the mass content of silver nitrate is preferably 0.5-1.0%, more preferably 0.6-0.9%; the mass ratio of graphene oxide and silver nitrate is preferably (0.03-0.1):1, more preferably (0.05 ⁇ 0.1):1; the mass content of polyvinylpyrrolidone is preferably 1.0 to 1.3%, more preferably 1.1 to 1.2%; the mass content of ferric chloride is preferably 0.0015 to 0.003%, more preferably 0.002 to 0.0025 %.
  • the masses of ethylene glycol in the first mixed material liquid and the second mixed material liquid are preferably equal.
  • the present invention does not have special requirements for the graphene oxide, and it is sufficient to use industrially general graphene oxide (multilayer graphene oxide).
  • the content of polyvinylpyrrolidone in the reaction feed liquid is controlled within the above range, which is beneficial to better control the growth of silver nanowires.
  • the content of polyvinylpyrrolidone is too high or too low, nano-silver particles or particles are easily formed Hybrid with wire and rod.
  • the graphene oxide/silver ion composite system can form a small amount of silver seed crystals with ferric chloride and polyvinylpyrrolidone.
  • the present invention subjects the reaction material liquid to a solvothermal reaction to obtain a silver nanowire-graphene composite material.
  • the reaction material liquid is placed in a reaction kettle, and then the reaction kettle is placed in a vacuum drying box for solvothermal reaction.
  • the temperature of the solvothermal reaction is preferably 150 to 180°C, more preferably 160 to 170°C; the time of the solvothermal reaction is preferably 3 to 5 hours, more preferably 3.5 to 4.5 hours.
  • the chloride ions present in the reaction feed solution can provide electrostatic stability for the first silver seed crystals.
  • the chloride ions can combine with the silver ions to form AgCl colloids, which reduces the concentration of free silver ions in the initial solution and reduces the silver
  • the speed at which ions are reduced and the silver seed crystal grows; this slow reaction process is conducive to the formation of thermodynamically stable multiple twin seed crystals; polyvinylpyrrolidone preferentially adsorbs on the ⁇ 100 ⁇ crystal plane of the multiple twin seed crystals It can grow along the ⁇ 111 ⁇ crystal plane and grow into silver nanowires through anisotropy; as the reaction progresses, the concentration of free silver ions in the solution gradually decreases, in order to maintain the balance of silver ions and AgCl colloid The silver ions are gradually released from the AgCl colloid and grow into silver nanowires; as the concentration of silver nanowires increases, the free silver ions in the solution are further reduced, providing more opportunities for the formation and growth of multiple twin
  • the graphene oxide is reduced to graphene by ethylene glycol during the solvothermal reaction, and the formed silver nanowires are attached to the surface of the graphene and inserted between the graphene layers to obtain a silver nanowire-graphene with a hybrid structure.
  • Composite materials due to the presence of residual oxygen in the reaction feed liquid, it will have an etching effect on the multiple twin seed crystals and hinder their growth into silver nanowires.
  • Fe 3+ can be reduced to Fe 2+ by ethylene glycol, and oxygen can reduce Fe 2+ is re-oxidized to Fe 3+ and circulates in sequence. This process can consume the residual oxygen in the reaction liquid and eliminate its etching effect on the silver seed crystal.
  • the present invention preferably further includes natural cooling and washing of the reaction system.
  • the washing process is preferably: adding acetone to the product system after natural cooling for two centrifugal washing, and then using ethanol for centrifugal washing twice to obtain a slurry.
  • the present invention uses acetone to wash away the ethylene glycol in the product system.
  • the silver nanowire-graphene composite material of the present invention is present in the slurry.
  • the present invention preferably does not perform drying.
  • the slurry obtained by centrifuging the ethanol is directly subjected to the subsequent steps to prevent agglomeration of the silver nanowire-graphene composite material after drying. .
  • the present invention has no special requirements on the solid content of the slurry, and the ethanol in the slurry will volatilize after the film is formed.
  • the present invention mixes the silver nanowire-graphene composite material, thermoplastic polyurethane and N,N-dimethylformamide to obtain a mixed slurry.
  • the mass of the thermoplastic polyurethane preferably accounts for 20-30% of the total mass of the thermoplastic polyurethane and N,N-dimethylformamide; the mass of the silver nanowire-graphene composite material preferably accounts for the mass of the silver nanowire -20-40% of the total mass of graphene composite material and thermoplastic polyurethane.
  • the thermoplastic polyurethane is preferably added to N,N-dimethylformamide, then the silver nanowire-graphene composite material is added, and the nano-dispersing machine is used for stirring treatment to obtain a mixed slurry.
  • the rotation speed of the nano-dispersing machine is preferably 2000-4000 rpm, more preferably 3000 rpm; the time of the stirring treatment is preferably 0.5-2 hours, more preferably 1 hour.
  • the temperature of the stirring treatment preferably does not exceed 30°C.
  • the nano-dispersing machine is used for mixing in the present invention, and the film-forming state is better.
  • the present invention processes the mixed slurry to form a film, and after drying, a near-infrared thermal repair flexible conductive film is obtained.
  • the method of film formation is preferably cast film formation.
  • it is preferable to cast a film on a polytetrafluoroethylene plate.
  • the present invention does not have special requirements on the thickness of the cast film, and only needs to be controlled according to actual requirements.
  • the drying temperature is preferably 60 to 75°C, and the time is preferably 12 to 36 hours.
  • N,N-dimethylformamide is evaporated to obtain a near-infrared thermal repair flexible conductive film.
  • the present invention provides a near-infrared thermal repair flexible conductive film prepared by the preparation method described in the above solution, which includes a silver nanowire-graphene composite material and a thermoplastic polyurethane.
  • the mass content of the silver nanowire-graphene composite material in the near-infrared thermal repair flexible conductive film is preferably 20-40%, and the balance is thermoplastic polyurethane.
  • the thickness of the near-infrared thermal repair flexible conductive film is preferably 30-800 ⁇ m.
  • the present invention uses thermoplastic polyurethane as a matrix and a silver nanowire-graphene composite material with a hybrid structure as a conductive filler (in which silver nanowires are the main conductive phase and graphene is the auxiliary phase), and the thermoplastic polyurethane system is based on The high-efficiency energy conversion unit and conductive path of silver nanowire-graphene, the flexible conductive film obtained has high conductivity; at the same time, the use of silver nanowire and graphene's absorption characteristics of near-infrared light can not only achieve local heating in small areas The damaged thermoplastic polyurethane material can be repaired, and the repair efficiency of the thermoplastic polyurethane conductive film can be improved, and rapid multiple repairs can be realized.
  • the silver nanowire-graphene composite material absorbs the near-infrared light to heat the thermoplastic polyurethane, and the thermoplastic polyurethane itself absorbs part of the heat.
  • the two work together to promote the melting of the thermoplastic polyurethane.
  • the flow realizes the self-repair of the damaged membrane, which greatly improves the efficiency of repair; and during the self-repair process, the silver nanowire-graphene composite material is pulled to reorganize to form a new conductive network, and the final repair will still have high conductivity.
  • thermoplastic polyurethane Prepare 500 ml of N,N-dimethylformamide solution of thermoplastic polyurethane with a mass concentration of 30%, and then mix the above-mentioned silver nanowire-graphene composite material slurry (containing 45 grams of silver nanowire-graphene composite material , Silver nanowire-graphene composite material in the conductive film with a mass percentage of 30%) is added to the thermoplastic polyurethane solution; the mixed solution is stirred for 1 hour with a nano-disperser, the rotating speed is 3000rpm, and the temperature is controlled not to exceed 30°C; Then, the mixed solution is cast on a polytetrafluoroethylene plate to form a film, and then heat-treated on a heating plate at 70° C. for 12 hours until the mass remains unchanged, to obtain a conductive film.
  • the thickness of the conductive film is about 200 ⁇ m, and the resistivity of the conductive film is 1.2 ⁇ mm.
  • thermoplastic polyurethane Prepare 500 ml of N,N-dimethylformamide solution of thermoplastic polyurethane with a mass concentration of 30%, and then mix the above-mentioned silver nanowire-graphene composite slurry (containing 30 grams of silver nanowire-graphene composite material) , Silver nanowire-graphene composite material in the conductive film with a mass percentage of 20%) is added to the thermoplastic polyurethane solution; the mixed solution is stirred for 1 hour with a nano-disperser, the rotation speed is 3000 rpm, and the temperature is controlled not to exceed 30°C; The mixed solution was cast on a polytetrafluoroethylene plate to form a film, and then heat-treated on a heating plate at 70° C. for 12 hours until the mass remained unchanged, to obtain a conductive film.
  • the thickness of the conductive film is about 200 ⁇ m, and the resistivity of the conductive film is 312.7 ⁇ mm.
  • thermoplastic polyurethane Prepare 500 ml of N,N-dimethylformamide solution of thermoplastic polyurethane with a mass concentration of 30%. Then add the above-mentioned silver nanowire-graphene composite material slurry (containing 60 grams of silver nanowire-graphene composite material, the content of the silver nanowire-graphene composite material in the conductive film is 40% by weight) is added to the thermoplastic Polyurethane solution; stir the mixed solution with a nano-disperser for 1 hour at 3000 rpm and control the temperature not to exceed 30°C; then cast the mixed solution on a polytetrafluoroethylene plate to form a film, and then place it on a heating plate at 70°C Heat treatment for 12 hours until the mass does not change to obtain a conductive film.
  • the thickness of the conductive film is about 200 ⁇ m, and the resistivity of the conductive film is 0.07 ⁇ mm.
  • thermoplastic polyurethane Prepare 500 ml of N,N-dimethylformamide solution of thermoplastic polyurethane with a mass concentration of 30%, and then mix the slurry containing silver nanowire-graphene composite material (containing 60 grams of silver nanowire-graphene composite material , The silver nanowire-graphene composite material in the conductive film is 40% by weight) is added to the thermoplastic polyurethane solution; the mixed solution is stirred for 1 hour with a nano-disperser, the rotating speed is 3000 rpm, and the temperature is controlled not to exceed 30 °C; The mixed solution was cast on a polytetrafluoroethylene plate to form a film, and then heat-treated on a heating plate at 70° C. for 12 hours until the mass remained unchanged, to obtain a conductive film.
  • the thickness of the conductive film is about 200 ⁇ m, and the resistivity of the conductive film is 0.15 ⁇ mm.
  • thermoplastic polyurethane Prepare 500 ml of N,N-dimethylformamide solution of thermoplastic polyurethane with a mass concentration of 30%, and then mix the above-mentioned silver nanowire-graphene composite material slurry (containing 45 grams of silver nanowire-graphene composite material , The silver nanowire-graphene composite material in the conductive film is 30% by weight) is added to the thermoplastic polyurethane solution; the mixed solution is stirred for 1 hour with a nano-disperser, the rotating speed is 3000 rpm, and the temperature is controlled not to exceed 30°C; The mixed solution was cast on a polytetrafluoroethylene plate to form a film, and then heat-treated on a heating plate at 70° C. for 12 hours until the mass remained unchanged, to obtain a conductive film.
  • the thickness of the conductive film is about 200 ⁇ m, and the resistivity of the conductive film is 11.8 ⁇ mm.
  • the present invention provides a near-infrared thermal repair flexible conductive film and a preparation method thereof.
  • the conductive film prepared by the present invention has high electrical conductivity and thermal conductivity, and has high repair efficiency under the action of near-infrared light. It can be repaired multiple times quickly.

Abstract

L'invention concerne un film conducteur flexible de réparation thermique à la lumière du proche infrarouge et un procédé de préparation associé, se rapportant au domaine technique des matériaux d'autoréparation. Le procédé de préparation selon la présente invention comprend les étapes suivantes consistant à : mélanger de l'oxyde de graphène, du nitrate d'argent et de l'éthylène glycol pour obtenir un premier liquide de substances mélangées ; mélanger de la polyvinylpyrrolidone, du trichlorure ferrique et de l'éthylène glycol pour obtenir un second liquide de substances mélangées ; mélanger le premier liquide de substances mélangées et le second liquide de substances mélangées, et soumettre le liquide de substances de réaction ainsi obtenu à une réaction solvothermique de façon à obtenir un matériau composite nanofils d'argent-graphène ; et mélanger le matériau composite nanofils d'argent-graphène, un polyuréthane thermoplastique et du N,N-diméthylformamide, former un film à partir de la suspension de mélange obtenue, et le sécher pour obtenir le film conducteur flexible de réparation thermique à la lumière du proche infrarouge. Le film conducteur préparé au moyen de la présente invention a une haute conductivité électrique et une haute conductivité thermique, a une haute efficacité de réparation sous l'action de la lumière du proche infrarouge, et permet d'effectuer de multiples réparations rapidement.
PCT/CN2020/106757 2020-05-21 2020-08-04 Film conducteur flexible de réparation thermique à la lumière du proche infrarouge et procédé de préparation associé WO2021232597A1 (fr)

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CN202010434712.XA CN111564237B (zh) 2020-05-21 2020-05-21 一种近红外热修复柔性导电膜的制备方法
CN202010434712.X 2020-05-21

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