WO2021197462A1 - Pellicule composite de conducteur élastique et son procédé de préparation - Google Patents

Pellicule composite de conducteur élastique et son procédé de préparation Download PDF

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Publication number
WO2021197462A1
WO2021197462A1 PCT/CN2021/085210 CN2021085210W WO2021197462A1 WO 2021197462 A1 WO2021197462 A1 WO 2021197462A1 CN 2021085210 W CN2021085210 W CN 2021085210W WO 2021197462 A1 WO2021197462 A1 WO 2021197462A1
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composite film
base film
elastic conductor
film layer
layer
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PCT/CN2021/085210
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Chinese (zh)
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马志军
郑子剑
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香港理工大学
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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
    • H01B13/00—Apparatus or processes specially adapted for manufacturing conductors or cables
    • 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
    • H01B13/0026—Apparatus for manufacturing conducting or semi-conducting layers, e.g. deposition of metal

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  • the invention belongs to the field of conductor materials, and specifically relates to an elastic conductor composite film and a preparation method thereof.
  • Elastic conductors are an indispensable part of wearable electronic products, especially flexible electronic devices such as flexible robots, bio-information-driven devices, and medical implants for health monitoring.
  • the performance of elastic conductors is also an extremely important consideration.
  • Many practical applications such as stretchable electronic circuits, flexible batteries, stretchable light source devices, etc. require conductive materials to have high electrical stability.
  • conductive materials to have high electrical stability.
  • porous film elastic conductors to elastic conductors in wearable electronic products is also urgently needed, and such conductive materials are also required to have good air and vapor permeability properties.
  • the present invention aims to provide an elastic conductor composite film and a preparation method thereof to overcome the above-mentioned defects in the prior art, so that it can satisfy high stretchability, high conductivity and high electrical stability at the same time, and also has both Good vapor permeability and air permeability.
  • An elastic conductor composite film of the present invention comprises: a base film layer and a coating material coated on the surface of the base film layer, wherein the base film layer is an electrospun thermoplastic elastomer, and the coating material is a liquid metal with a melting point lower than room temperature .
  • a nano-silver conductive layer is also formed between the base film layer and the coating material.
  • the elastic conductor composite film has a multilayer structure, which is formed by alternately stacking a base film layer and a coating material in a vertical manner.
  • the elastic conductor composite film has a multilayer structure, which is formed by alternately stacking a base film layer, a nano silver conductive layer, and a coating material in turn.
  • the coating material passes through a patterned mold to form the pattern on the surface of the base film layer.
  • a layer of ion conductive hydrogel is also covered on the surface of the composite film in contact with the biological body, and the pattern formed by the ion conductive hydrogel is coated on the covered surface.
  • the pattern formed by the material is consistent.
  • the electrospunable thermoplastic elastomer is a styrene-butadiene-styrene block copolymer, and the mass percentage concentration of the electrospunable thermoplastic elastomer in the formed electrospun polymer solution is 5 wt% -20wt%.
  • the liquid metal is a room temperature liquid gallium-based alloy.
  • the room temperature liquid gallium-based alloy is a eutectic gallium-indium alloy, wherein the mass ratio of the two elements of gallium-indium is 75:25.
  • the present invention also provides a method for preparing the above-mentioned elastic conductor composite film, which includes:
  • Step S1 Dissolve the electrospun thermoplastic elastomer in the intermediate agent to form an electrospun polymer solution
  • Step S2. Use the electrospinning polymer solution for electrospinning, and collect electrospinning on the steel plate to form the base film layer of the elastic conductor composite film;
  • Step S3. Coating a coating material on the surface of the base film layer, wherein the coating material is a liquid metal with a melting point lower than room temperature.
  • the method further includes:
  • a nano-silver conductive layer is formed on the surface of the base film layer. Specifically, the base film layer is sequentially immersed in a nano-silver solution, a reducing agent, and anhydrous ethanol.
  • step S3 the method further includes:
  • the polymer solution to electrospin a new base film layer on the surface where the base film layer has been coated with the coating material, coat the surface of the new base film layer with the coating material, and so on, alternate electrospinning and coating.
  • the coating material is applied until the elastic conductor composite film with the required number of layers to form a multilayer structure is obtained.
  • step S3 the method further includes:
  • the polymer solution is used to electrospin a new base film layer on the surface where the base film layer has been coated with the coating material, and the nano silver conductive layer and the coating material are sequentially formed on the surface of the new base film layer.
  • electrospinning, nano-silver conductive layer formation and coating material coating are alternately performed until the required number of layers is obtained to form a multilayer structured elastic conductor composite film.
  • forming a nano-silver conductive layer on the surface of the base film layer includes:
  • the nano-silver solution is prepared by dissolving silver trifluoroacetate in ethanol to obtain a solution with a concentration of 0.1-1 g/mL.
  • the reducing agent is an ethanol solution of hydrazine hydrate.
  • coating the coating material on the surface of the base film layer includes:
  • a mold with a pattern is placed on the surface of the base film layer so that the coating material forms the pattern when the surface of the base film layer is coated.
  • the preparation of the elastic conductor composite film further includes:
  • a layer of ion conductive hydrogel is covered on the side of the composite membrane to be in contact with the biological body, and the pattern formed by the ion conductive hydrogel is consistent with the pattern formed by the coating material on the covered surface.
  • the intermediate agent is dichloroethane.
  • dissolving the electrospunable thermoplastic elastomer in the intermediate agent to form the electrospinning polymer solution includes:
  • the mass percentage concentration of the thermoplastic elastomer in the formed electrospinning polymer solution is 5wt%-20wt% .
  • the liquid metal is a room temperature liquid gallium-based alloy.
  • the room temperature liquid gallium-based alloy is a eutectic gallium-indium alloy, wherein the mass ratio of gallium and indium is 75:25.
  • the thickness of the base film layer is positively related to the collection time for collecting electrospinning on the steel plate.
  • the elastic conductor composite film of the present invention has good stretchability, strong conductivity, and has excellent electrical stability while resisting stretching; the base film layer electrospun fiber obtained by electrospinning technology has a net-like pore structure, thus making the The composite film also has good vapor permeability and air permeability; the thermoplastic elastomer and liquid metal used to prepare the composite film are both low-cost materials, which reduces the production cost of the composite film and has good economic applicability; electrospinning and coating Common preparation methods such as cloth are beneficial to the multi-field application of the composite film, suitable for large-scale industrial production, and the composite film can be physically expanded according to actual application requirements. Compared with the existing conductive material, the elastic conductor composite of the present invention The film is more suitable for stretchable electronic circuits, flexible batteries, stretchable light source devices, wearable devices and other fields.
  • Figure 1 is a flow chart of the preparation of an elastic conductor composite film provided by the first embodiment of the present invention
  • Fig. 2 is a scanning electron microscope (SEM) image of SBS electrospun fiber of the base film layer according to an embodiment of the present invention
  • FIG. 3 is a statistical schematic diagram of the diameter distribution of electrospun fibers in the base film layer according to an embodiment of the present invention.
  • FIG. 4 is a schematic diagram of a tensile stress-strain curve of a base film layer according to an embodiment of the present invention
  • 5a and 5b are scanning electron microscope (SEM) images of 0.8EGaIn-SBS in a natural state in Example 1 of the present invention
  • 6a and 6b are scanning electron microscope (SEM) images of 0.8EGaIn-SBS in a stretched state in Example 1 of the present invention
  • Fig. 7 is a schematic diagram of the resistance-tensile strain curve of 0.8EGaIn-SBS in the first embodiment of the present invention.
  • FIG. 8 is a schematic diagram of the resistance growth rate-stretching times curve of 0.8EGaIn-SBS under different tensile strains in the first embodiment of the present invention
  • FIG. 9 is a schematic diagram of the resistance growth rate-tensile strain curve of the composite film with different EGaIn unit area loadings according to the first embodiment of the present invention.
  • FIG. 10 is a schematic diagram showing the variation of conductivity and quality factor with EGaIn per unit area load in the first embodiment of the present invention.
  • 11a to 11e are scanning electron microscope (SEM) images of composite films with different EGaIn loadings per unit area in Example 1 of the present invention.
  • Figure 13 is a scanning electron microscope (SEM) image of EGaIn-AgNPs-SBS according to the second embodiment of the present invention.
  • FIG. 14 is a schematic diagram of a curve diagram of resistance growth rate and quality factor as a function of tensile strain in the second embodiment of the present invention.
  • 15 is a schematic diagram of the resistance growth rate-stretching times curve when the tensile strain is 0% and 60% in the second embodiment of the present invention.
  • 16 is a flow chart of the preparation of the three-layer structure elastic conductor composite film provided by the third embodiment of the present invention.
  • FIG. 17 is a schematic diagram of the structure of a three-layer structure elastic conductor composite membrane provided by Embodiment 3 of the present invention.
  • 19 is a schematic diagram of the highest temperature change of the top layer composite film of the third embodiment of the present invention when a step voltage is applied;
  • 20 is a schematic diagram of the temperature-tensile strain curve of the top composite film of the third embodiment of the present invention when the applied voltage is 0.15V;
  • 21 is a schematic diagram of the temperature change of the heating and cooling electrical stability of the top composite film of the third embodiment of the present invention when the applied voltage is 0.2V;
  • 22 is a schematic diagram of the capacitance-PBS volume curve of the intermediate layer composite film under different tensile strains in the third embodiment of the present invention.
  • FIG. 23 is a schematic diagram of capacitance-NaCl concentration curves of the intermediate layer composite film of the third embodiment of the present invention under different tensile strains;
  • FIG. 24 is a schematic diagram of the ECG signal acquisition waveforms of three wavebands in the natural state of the bottom layer composite membrane of the third embodiment of the present invention.
  • FIG. 25 is a schematic diagram of ECG signal acquisition waveforms in three wavebands when the bottom layer composite film of the third embodiment of the present invention is deformed.
  • this embodiment provides an elastic conductor composite film and a preparation method thereof.
  • the composite film includes a base film layer and a coating material coated on the surface of the base film layer, wherein the base film layer is an electrospun thermoplastic Elastomer, the coating material is liquid metal with a melting point lower than room temperature.
  • the electrospunable thermoplastic elastomer used includes styrene-butadiene-styrene block copolymer (SBS), hydrogenated styrene-butadiene block copolymer (SEBS), benzene Ethylene-isoprene-styrene block copolymer (SIS), hydrogenated styrene/isoprene block copolymer (SEPS), polyester block copolymer (TPEE), polyurethane block copolymer (TPU), polyolefin copolymer (TPO), thermoplastic vulcanized elastomer (TPV), diene block copolymer (TPB) and a series of thermoplastic elastomers that can be used for electrospinning, the present invention does not carry out this Specific restrictions.
  • SBS styrene-butadiene-styrene block copolymer
  • SEBS hydrogenated styrene-butadiene block cop
  • the liquid metal used can be room temperature liquid gallium-based alloys including gallium indium alloy, gallium indium bismuth alloy, gallium indium tin alloy, etc., or a series of other liquid metals with melting points lower than room temperature can be selected, which is not specifically limited in the present invention.
  • SBS is selected as the material of the base film layer, in which the mass ratio of styrene to butadiene is 40:60; the liquid metal coated on the surface of the base film layer is selected from the eutectic Gallium-Indium alloy in this embodiment. Indium alloy, EGaIn), where the mass ratio of gallium and indium is 75:25.
  • Indium alloy, EGaIn Indium alloy, EGaIn
  • the preparation method of the composite membrane is introduced below, and the steps include:
  • Preparation of base film layer preparation materials dissolve SBS in an intermediate agent to prepare a polymer solution for electrospinning, where the intermediate agent is dichloroethane, and the mass percentage concentration of SBS in the polymer solution obtained is 5wt%- 20wt%;
  • the electrospinning process is collected on a steel plate, and the thickness of the base film is controlled by controlling the collection time. The longer the collection time, the thicker the base film. When the preset thickness is reached, the current electrospinning process is stopped and the base film is removed from the steel plate. The layer is used to coat EGaIn afterwards;
  • the coating method can be one or more combinations of knife coating, brushing, Meyer bar coating, silk screen printing, and inkjet printing, but it should be understood that the coating method is not limited to the multiple described above
  • This coating method any coating method that can be coated with a coating material on the surface of the base film layer to form an alloy layer with no essential difference is regarded as the technical solution protected by the present invention.
  • a knife coating method is used, and a scraper is used to form an alloy layer of EGaIn on the surface of the base film layer, and the formed elastic conductor composite film is represented by EGaIn-SBS.
  • the electrical properties of the composite film such as conductivity and electrical stability, can be adjusted. Therefore, in order to express the composite film with different loading per unit area of the alloy layer, xEGaIn-SBS is used.
  • the numerical unit of x is mg/cm 2 , for example 0.8EGaIn-SBS, 1.4EGaIn-SBS, 2.0EGaIn-SBS, 2.6EGaIn-SBS, 5.0EGaIn-SBS respectively represent the unit area load of the alloy layer EGaIn on the base film layer It is 0.8mg/cm 2 , 1.4mg/cm 2 , 2.0mg/cm 2 , 2.6mg/cm 2 , 5.0mg/cm 2 .
  • a mold can also be used to assist in the completion of squeegee coating, specifically by placing a specific pattern on the surface of the base film layer.
  • the alloy material is knife-coated on the mold so that the alloy layer formed on the base film layer presents the specific pattern.
  • the following analyzes the performance of the elastic conductor composite film provided in this embodiment from the microstructure of the composite film.
  • the SBS electrospun fibers of the base film layer are randomly stacked, and the diameter of the fibers is concentrated in the range of 500nm ⁇ 5 ⁇ m. Observe the tensile stress-strain curve of the base film layer as shown in Figure 4, the tensile strain can reach 1200%, with good tensile strength.
  • this embodiment provides another elastic conductor composite film and a preparation method thereof.
  • a nano-silver conductive film is formed between the base film layer and the alloy layer. Layer, so as to achieve the purpose of significantly improving the conductive performance of the composite film.
  • the method for preparing the base film layer and the alloy layer in this embodiment is the same as that of the first embodiment. The difference is that before coating the alloy layer, a silver nanoparticle (AgNPs) conductive layer (silver nanoparticles) needs to be formed on the base film layer.
  • a silver nanoparticle (AgNPs) conductive layer silver nanoparticles
  • Nano silver solution preparation dissolve silver trifluoroacetate (AgTFA) in ethanol (EtOH) to obtain a solution with a concentration of 0.1-1g/mL;
  • the base film layer is immersed in nano-silver solution, reducing agent and absolute ethanol in turn: the electro-spinning base film layer is soaked in nano-silver solution for 5 minutes, and the base film layer is taken out and placed in the air at room temperature to dry naturally.
  • the film layer is immersed in the reducing agent for no less than 5 minutes, so that the nano silver is reduced on the surface of the base film layer; the base film layer is taken out and soaked in absolute ethanol for no less than 10 minutes to remove the residual reducing agent;
  • the base film layer is placed in the air at room temperature to dry naturally.
  • a nano-silver conductive layer is formed on the surface of the base film layer.
  • the semi-finished composite film is represented by Ag-SBS.
  • the reducing agent used in this example is hydrazine hydrate in ethanol.
  • Example 1 The method of Example 1 is used to coat EGaIn on the surface of the nano-silver conductive layer to form an alloy layer, and the obtained elastic conductor composite film is represented by EGaIn-AgNPs-SBS.
  • the microstructure of the elastic conductor composite film with nano-silver conductive layer is shown in Figure 13.
  • the coating of the alloy layer on the SBS base film layer with the nano-silver conductive layer did not affect the network pore structure of the electrospun fiber ; Please refer to Figure 14 and Figure 15.
  • the curve where " ⁇ " in Figure 14 represents the resistance growth rate
  • R s and R on the ordinate both represent the resistance of the composite film after stretching
  • R Both s0 and R 0 represent the resistance of the composite film in its natural state.
  • the initial conductivity of EGaIn-AgNPs-SBS can reach 1658800S/m, and its resistance has only increased by 40.8 times when the tensile strain is 1950%.
  • the quality factor indicating electrical stability drops to 0.48.
  • the quality factor is still 11.9.
  • the composite film can withstand more than 200,000 stretches and the resistance increases by only 38%. The composite membrane can still maintain good electrical stability when it is slowly deformed.
  • this embodiment provides a three-layer structure elastic conductor composite film and a preparation method thereof, and particularly relates to an elastic conductor composite film applied to a wearable thermotherapy device.
  • the preparation method of the base film layer and the alloy layer is the same as in the first embodiment. The difference is that the base film layer and the alloy layer are alternately formed.
  • the base film layer is formed first, and the alloy layer is formed later.
  • the required specific pattern is formed on the base film layer, so it is easy to understand that each layer of elastic conductor composite film contains a base film layer and an alloy layer.
  • the three-layer structure elastic conductor composite film is in accordance with the electrospinning sequence of the base film layer. It is represented as the top layer, the middle layer, and the bottom layer in turn.
  • the top layer is used as a heater, the middle layer is used as a capacitive sweat sensor, and the bottom layer is used as a contact electrode for collecting biological signals of the human body.
  • the three-layer structure elastic conductor composite film prepared in this embodiment The total thickness is 320 ⁇ m.
  • the bottom composite film used as the contact electrode is also covered with a layer of ion conductive hydrogel, the pattern of the hydrogel is consistent with the pattern of the bottom alloy layer , As shown in Figure 16, both are square-shaped and the same size and shape.
  • the composite film obtained by the alternate preparation method of electrospinning and coating of this embodiment is an integrated composite film, which does not cause delamination during repeated use, which greatly improves the composite film
  • the thickness of each layer can be flexibly adjusted for a composite film with a multilayer structure; simple and efficient preparation procedures are conducive to integration
  • the preparation of the elastic conductor composite film of the multilayer structure can also be carried out alternately according to the preparation sequence of the base film layer, the nano-silver conductive layer, and the alloy layer.
  • the multi-layer structure elastic conductor composite film of silver conductive layer The preparation of this composite film will not be repeated here.
  • Those skilled in the art can undoubtedly prepare nano-silver according to the multiple embodiments provided by the present invention.
  • top layer composite film used as a heater fix it to the two ends of the stretching equipment. One end of the splint is movable and the other end is fixed.
  • a DC step voltage of 0 ⁇ 0.45V is applied to the top layer of the composite film, using infrared thermal imaging.
  • the instrument monitors the temperature change of the composite film, and each voltage is applied for at least 60s to ensure that the heating temperature of the composite film can reach a stable state.
  • the infrared thermal imaging monitoring is stopped, and the composite film’s performance under different voltage applications is recorded.
  • the temperature change curve is shown in Figure 18.
  • the temperature of the composite film can be stabilized within 30s during the 6 times of voltage application; and for the heating performance of the composite film, a voltage is applied to the top composite film every 60s.
  • the sub-voltage is increased by 0.07-0.08V, which is different from the previous application of the next voltage after the room temperature is restored.
  • the voltage is applied as soon as the temperature of the composite film reaches a stable value, and the next voltage is applied immediately.
  • the infrared thermal imaging monitoring is stopped until the composite film returns to room temperature.
  • the maximum value that the composite film can reach under different applied voltages is recorded as shown in Figure 19. It can be seen that the temperature increases with the voltage.
  • the composite film can reach 95°C when the last applied voltage is 0.45V, indicating that the provided elastic conductor composite film can accurately control the temperature output; for the tensile performance of the composite film, apply a DC voltage to the composite film 0.15V, stretch the composite film at a constant speed of 3mm/s, record the curve of the temperature of the composite film at this time with the tensile strain as shown in Figure 20, the temperature of the composite film increases from 34.4°C under 0% strain to 100 At 40.1°C under% strain, it only increased by 5.7°C, which means that when the composite film deforms with the human skin, it can still maintain good electrical stability; in addition, the electrical stability of the composite film during repeated heating and cooling is tested.
  • the sweat conduction and ion permeability were tested when it was in a stretched state.
  • fix the intermediate layer composite film on the two splints of the stretching equipment one end of the splint is movable, one end is fixed, and phosphate-buffered saline (PBS) is used to simulate human sweat, and different volumes of PBS are dropped.
  • PBS phosphate-buffered saline
  • the composite film can collect the required ECG signal waveform from 3 bands with a low noise ratio in both the natural state and the deformed state.
  • the ECG signal waveform collected in the deformed state is compared with the natural state. Glitch and noise Not high, the composite film provided by the present invention has the advantages of high signal collection reliability, simple operation, and comfortable touch.

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Abstract

L'invention concerne une pellicule composite de conducteur élastique et son procédé de préparation. Un élastomère thermoplastique pouvant être obtenu par filage électrostatique et un métal liquide servent de matières premières pour la pellicule composite de conducteur élastique, une couche de pellicule de base de la pellicule composite est obtenue au moyen d'une technique de filage électrostatique, une surface de la couche de pellicule de base est recouverte du métal liquide, et la pellicule composite résultante a une bonne extensibilité et une haute conductivité et a une excellente stabilité électrique et une résistance à l'extension excellente ; et des fibres de filage électrostatique de la couche de pellicule de base ont une structure de pores en forme de filet, de sorte la pellicule composite a également une bonne perméabilité à la vapeur et une bonne perméabilité à l'air. L'élastomère thermoplastique et le métal liquide destinés à préparer la pellicule composite sont tous deux des matériaux à bas coût, de sorte que le coût de production de la pellicule composite est réduit, et que l'applicabilité économique est bonne ; et des moyens généraux de préparation tels que le filage électrostatique et le revêtement conduisent à une production industrielle à grande échelle, la pellicule composite peut être étendue physiquement en fonction d'exigences d'application réelle, et par rapport aux matériaux conducteurs existants, la pellicule composite de conducteur élastique selon la présente invention convient mieux à plusieurs champs techniques, tels que les circuits électroniques extensibles, les batteries flexibles, les dispositifs de source de lumière extensibles et les appareils portables.
PCT/CN2021/085210 2020-04-03 2021-04-02 Pellicule composite de conducteur élastique et son procédé de préparation WO2021197462A1 (fr)

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