CN111430062A - Elastic conductor composite film and preparation method thereof - Google Patents
Elastic conductor composite film and preparation method thereof Download PDFInfo
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- CN111430062A CN111430062A CN202010257987.0A CN202010257987A CN111430062A CN 111430062 A CN111430062 A CN 111430062A CN 202010257987 A CN202010257987 A CN 202010257987A CN 111430062 A CN111430062 A CN 111430062A
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- H—ELECTRICITY
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
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- 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
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Abstract
The application provides an elastic conductor composite membrane and a preparation method thereof, the elastic conductor composite membrane adopts an electrospinning thermoplastic elastomer and liquid metal as raw materials, a base membrane layer of the composite membrane is obtained by an electrospinning technology, and the liquid metal is coated on the surface of the base membrane layer, so that the obtained composite membrane has good stretchability, strong conductivity and excellent electric stability; the electrospun fibers of the base film layer are of a mesh pore structure, so that the composite film also has good vapor permeability and air permeability; the thermoplastic elastomer and the liquid metal used for preparing the composite film belong to materials with lower cost, so that the production cost of the composite film is reduced, and the economic applicability is good; the elastic conductor composite film is more suitable for a plurality of fields such as stretchable electronic circuits, flexible batteries, stretchable light source devices, wearable equipment and the like compared with the existing conductive material.
Description
Technical Field
The invention belongs to the field of conductor materials, and particularly relates to an elastic conductor composite film and a preparation method thereof.
Background
The elastic conductor is an indispensable component for wearable electronics, and in particular, flexible electronics such as flexible robots, biological information driven devices, medical implants for health monitoring, and the like. The performance of the elastic conductor is also an extremely important consideration in addition to its conductivity and elasticity, and many practical applications such as stretchable electronic circuits, flexible batteries, stretchable light source devices, etc. require a conductive material with high electrical stability to ensure that the device can still maintain good working performance during deformation, while it is quite challenging for a high-stretch elastic conductor to have high electrical stability. In addition to high electrical stability, the application of porous elastic conductors to wearable electronic products is also highly desirable, and such conductive materials are also required to have good air permeability and vapor permeability. With the development of wearable products, stretchable conductive materials are required to meet the requirements of supporting multiple functions, small packaging volume, high integration level and the like for wearable electronic products in the future so as to support better product performance.
At present, the method for preparing the elastic conductor with the advantages of good stretchability, high conductivity, high stability and the like is not provided.
Disclosure of Invention
Based on the above, the invention aims to provide an elastic conductor composite film and a preparation method thereof, so as to overcome the defects in the prior art, and simultaneously meet the requirements of high stretchability, high conductivity and high electrical stability, and have good vapor permeability and air permeability.
The invention relates to an elastic conductor composite film, which comprises: the coating material is liquid metal with the melting point lower than room temperature.
Preferably, in order to further increase the conductivity of the composite film, a nano silver conductive layer is further formed between the base film layer and the coating material.
Preferably, the elastic conductor composite film is a multilayer structure and is formed by sequentially and alternately vertically stacking a base film layer and a coating material.
Preferably, the elastic conductor composite film is of a multilayer structure and is formed by sequentially and alternately vertically stacking a base film layer, a nano silver conductive layer and a coating material.
Preferably, the coating material is passed through a patterned die to form the pattern on the surface of the base film layer.
Preferably, in order to improve the electrical contact performance of the elastic conductor composite membrane, the contact surface of the composite membrane and the living body is further covered with a layer of ion-conductive hydrogel, and the pattern formed by the ion-conductive hydrogel is consistent with the pattern formed by the coating material on the covered surface.
Preferably, the electrospinnable thermoplastic elastomer is a styrene-butadiene-styrene block copolymer and the concentration of the electrospinnable thermoplastic elastomer in the formed electrospun polymer solution is 5 wt% to 20 wt%.
Preferably, the liquid metal is a room temperature liquid gallium-based alloy.
Preferably, the room-temperature liquid gallium-based alloy is a eutectic gallium-indium alloy, wherein the mass ratio of two elements of gallium and indium is 75: 25.
In another aspect, the present invention further provides a method for preparing the elastic conductor composite film, including:
s1, dissolving an electro-spinnable thermoplastic elastomer in an intermediate agent to form an electro-spun polymer solution;
s2, carrying out electrospinning by using the electrospinning polymer solution, and collecting the electrospinning on a steel plate to form a base film layer of the elastic conductor composite film;
and S3, coating a coating material on the surface of the base film layer, wherein the coating material is liquid metal with the melting point lower than room temperature.
Preferably, before step S3, the method further includes:
forming a nano-silver conductive layer on the surface of the base film layer, and particularly soaking the base film layer in a nano-silver solution, a reducing agent and absolute ethyl alcohol in sequence.
Preferably, step S3 is followed by:
and (3) electrospinning a new base film layer on the surface of the base film layer coated with the coating material by using the polymer solution, coating the coating material on the surface of the new base film layer, and the like, wherein the electrospinning and the coating of the coating material are alternately carried out until the required number of layers is obtained to form the elastic conductor composite film with the multilayer structure.
Preferably, step S3 is followed by:
and (3) electrospinning a new base film layer on the surface of the base film layer coated with the coating material by using the polymer solution, sequentially forming a nano silver conductive layer and the coating material on the surface of the new base film layer, and repeating the steps of electrospinning, forming the nano silver conductive layer and coating the coating material until the required number of layers is obtained to form the multilayer structure elastic conductor composite film.
Preferably, the forming of a nano silver conductive layer on the surface of the base film layer comprises:
soaking the base film layer in the nano-silver solution for 5min, taking out the base film layer, placing the base film layer in the air, and naturally drying at normal temperature, soaking the dried base film layer in a reducing agent for not less than 5min, soaking the base film layer soaked by the reducing agent in absolute ethyl alcohol for not less than 10min, and placing the base film layer soaked by the absolute ethyl alcohol in the air, and naturally drying at normal temperature to form the nano-silver conductive layer on the surface of the base film layer.
Preferably, the nano silver solution is prepared by dissolving silver trifluoroacetate in ethanol to obtain a solution with a concentration of 0.1-1g/m L.
Preferably, the reducing agent is an ethanol solution of hydrazine hydrate.
Preferably, the coating of the coating material on the surface of the base film layer comprises:
a mold with a pattern is placed on the surface of the base film layer such that the coating material forms the pattern when coated on the surface of the base film layer.
Preferably, the preparation of the elastic conductor composite film further comprises:
covering one side of the composite membrane to be contacted with a living body with a layer of ion conductive hydrogel, wherein the pattern formed by the ion conductive hydrogel is consistent with the pattern formed by the coating material on the covered side.
Preferably, the intermediate agent is dichloroethane.
Preferably, dissolving the electrospinnable thermoplastic elastomer in the intermediate agent to form an electrospun polymer solution comprises:
dissolving a styrene-butadiene-styrene block copolymer in dichloroethane to obtain an electrospun polymer solution, wherein the mass percentage concentration of the thermoplastic elastomer in the formed electrospun polymer solution is 5-20 wt%.
Preferably, the liquid metal is a room temperature liquid gallium-based alloy.
Preferably, the room-temperature liquid gallium-based alloy is a eutectic gallium-indium alloy, wherein the mass ratio of gallium to indium is 75: 25.
Preferably, the thickness of the base film layer is positively correlated to the collection time of the collected electrospun filaments on the steel plate.
According to the technical scheme, the invention has the following beneficial effects:
the elastic conductor composite film has good stretchability, strong conductive capability and excellent electrical stability while being resistant to stretching; the electro-spun fiber of the base film layer obtained by the electro-spinning technology is of a mesh pore structure, so that the composite film also has good vapor permeability and air permeability; the thermoplastic elastomer and the liquid metal used for preparing the composite film belong to materials with lower cost, so that the production cost of the composite film is reduced, and the economic applicability is good; the general preparation means such as electrospinning and coating are beneficial to the multi-field application of the composite film, are suitable for large-batch industrial production, can physically expand the composite film according to the actual application requirements, and are more suitable for the fields of stretchable electronic circuits, flexible batteries, stretchable light source devices, wearable equipment and the like compared with the existing conductive material.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the provided drawings without creative efforts.
Fig. 1 is a flow chart of a process for preparing an elastic conductor composite film according to an embodiment of the present invention;
FIG. 2 is a Scanning Electron Microscope (SEM) image of an SBS electrospun fiber of a base film layer according to an embodiment of the invention;
FIG. 3 is a schematic diagram of a statistical distribution of electrospun fiber diameters of a base film layer according to an embodiment of the 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;
FIGS. 5a and 5b are Scanning Electron Microscope (SEM) images of a 0.8EGaIn-SBS in a natural state according to an embodiment of the present invention;
FIGS. 6a and 6b are Scanning Electron Microscope (SEM) images of a 0.8EGaIn-SBS in a stretched state according to an embodiment of the present invention;
FIG. 7 is a graph showing the resistance-tensile strain curve of 0.8EGaIn-SBS according to one embodiment of the present invention;
FIG. 8 is a graph of the rate of resistance increase versus the number of tensile cycles of 0.8EGaIn-SBS at different tensile strains in accordance with one embodiment of the present invention;
FIG. 9 is a graph showing the resistance growth rate-tensile strain curves of composite films with different EGaIn unit area loadings in accordance with one embodiment of the present invention;
FIG. 10 is a graphical representation of conductivity and quality factor as a function of EGaIn loading per unit area in accordance with one embodiment of the present invention;
FIGS. 11 a-11 e are Scanning Electron Microscope (SEM) images of composite films with different EGaIn unit area loadings in accordance with embodiments of the present invention;
FIG. 12 is a flow chart of a process for preparing an elastic conductor composite film according to a second embodiment of the present invention;
FIG. 13 is a Scanning Electron Microscope (SEM) image of a second EGaIn-AgNPs-SBS according to an embodiment of the present invention;
FIG. 14 is a graph illustrating the rate of increase of resistance and the quality factor as a function of tensile strain according to a second embodiment of the present invention;
FIG. 15 is a graph showing the rate of increase in resistance versus the number of times of stretching at 0% and 60% tensile strains according to example two of the present invention;
fig. 16 is a flow chart of a process for preparing a three-layer elastic conductor composite film according to a third embodiment of the present invention;
fig. 17 is a schematic structural view of an elastic conductor composite film with a three-layer structure according to a third embodiment of the present invention;
FIG. 18 is a schematic diagram of a temperature variation curve of the top composite film of the third embodiment of the present invention under different voltages;
FIG. 19 is a schematic diagram of the maximum temperature change of the top composite film of the third embodiment of the present invention when a step voltage is applied;
FIG. 20 is a schematic diagram of the temperature-tensile strain curve of the top composite film of example three of the present invention at an applied voltage of 0.15V;
FIG. 21 is a schematic diagram showing the temperature change of the electrical stability of the top composite film of the third embodiment of the present invention during heating and cooling when a voltage of 0.2V is applied;
FIG. 22 is a schematic diagram of a capacitance-PBS volume curve of the interlayer composite film of the third embodiment of the present invention under different tensile strains;
FIG. 23 is a schematic diagram of a capacitance-NaCl concentration curve of the interlayer composite film according to the third embodiment of the present invention under different tensile strains;
FIG. 24 is a schematic diagram of waveforms collected by electrocardiographic signals of 3 wavebands in a natural state of a bottom-layer composite membrane according to a third embodiment of the present invention;
fig. 25 is a schematic diagram of waveforms acquired by electrocardiographic signals of 3 wavebands in a deformed state of the underlying composite membrane according to the third embodiment of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example one
Referring to fig. 1, the present embodiment provides an elastic conductor composite film and a method for preparing the same, the composite film includes a base film layer and a coating material coated on a surface of the base film layer, wherein the base film layer is an electrospun thermoplastic elastomer, and the coating material is a liquid metal having a melting point lower than room temperature.
It is to be understood that the thermoplastic elastomer that can be electrospun used includes a series of thermoplastic elastomers that can be used for electrospinning, such as styrene-butadiene-styrene block copolymer (SBS), hydrogenated styrene-butadiene block copolymer (SEBS), styrene-isoprene-styrene block copolymer (SIS), hydrogenated styrene/isoprene block copolymer (SEPS), polyester-based block copolymer (TPEE), polyurethane-based block copolymer (TPU), polyolefin-based copolymer (TPO), thermoplastic vulcanizate (TPV), diene-based block copolymer (TPB), and the like, and the present invention is not particularly limited thereto.
The liquid metal may be a room temperature liquid gallium-based alloy including gallium indium alloy, gallium indium bismuth alloy, gallium indium tin alloy, etc., or may be a series of other liquid metals having a melting point lower than room temperature, which is not specifically limited in the present invention.
In the embodiment, SBS is selected as the material of the base film layer, wherein the mass ratio of styrene to butadiene is 40: 60; in this embodiment, eutectic Gallium-indium alloy (EGaIn) is selected as the liquid metal coated on the surface of the base film layer, wherein the mass ratio of the two elements of Gallium and indium is 75: 25.
The following describes a method for preparing the composite membrane, which comprises the steps of:
preparing a base film layer preparation material, namely dissolving SBS in an intermediate agent to prepare a polymer solution for electrospinning, wherein the intermediate agent is dichloroethane, and the mass percent concentration of SBS in the obtained polymer solution is 5-20 wt%;
collecting the electrospinning on a steel plate, controlling the thickness of the base film layer by controlling the collecting time, wherein the longer the collecting time is, the thicker the base film layer is, stopping the current electrospinning process after the preset thickness is reached, and taking the base film layer off the steel plate for later EGaIn coating;
the coating method may be one or more combinations of knife coating, brushing, meyer bar coating, silk screen printing and ink jet printing, but it should be understood that the coating method is not limited to the above-described coating methods, and any coating method that can coat the coating material on the surface of the base film layer to form the alloy layer without any essential difference is considered as the technical solution protected by the present invention.
In this example, a doctor blade coating method was used to form an alloy layer on the surface of a base film layer from EGaIn using a doctor blade, and the elastic conductor composite film formed was denoted by EGaIn-SBS.
The electrical characteristics of the composite film such as conductivity and electrical stability can be adjusted by changing the unit area loading of the alloy layer on the surface of the base film layer, so that in order to represent the composite films with different unit area loading of the alloy layer, xEGaIn-SBS is adopted, and the numerical unit of x is mg/cm2For example, 0.8EGaIn-SBS, 1.4EGaIn-SBS, 2.0EGaIn-SBS, 2.6EGaIn-SBS and 5.0EGaIn-SBS respectively represent the amount of the alloy layer EGaIn on the base film layer per unit area of 0.8mg/cm2、1.4mg/cm2、2.0mg/cm2、2.6mg/cm2、5.0mg/cm2。
As shown in the lower half of fig. 1, on the basis of the first embodiment, in order to form the alloy layer with a specific pattern on the surface of the base film layer, a die can be used to assist in performing the drawing, specifically, a die with a specific pattern is placed on the surface of the base film layer, and the alloy material is drawn on the die so that the alloy layer formed on the base film layer presents the specific pattern.
The properties of the elastic conductor composite film provided in this example were analyzed from the microstructure of the composite film as follows.
Referring to fig. 2 to 4, the SBS electrospun fibers of the base film layer are randomly stacked, the diameters of the fibers are concentrated to 500nm to 5 μm, and the tensile stress-strain curve of the base film layer is observed as shown in fig. 4, which shows that the tensile strain can reach 1200%, and the SBS electrospun fibers have good tensile resistance.
Taking 0.8EGaIn-SBS as an example, the Young modulus is 0.11MPa, the microstructure in the natural state is shown in fig. 5a and 5b, the microstructure in the stretching state is shown in fig. 6a and 6b, the SBS electrospun fiber is a net-shaped pore structure, fig. 7 shows a curve of the resistance of 0.8EGaIn-SBS varying with the stretching strain, the resistance of 0.8EGaIn-SBS is only increased by 2.2% when the stretching strain is 1050%, and in combination with fig. 5a to 6b, the good electrical stability exhibited by the elastic conductor composite film provided by the embodiment in the stretching process is attributed to the deformation of net-shaped pores in the electrospun fiber and the extension of secondary gaps; fig. 8 shows the resistance of 0.8EGaIn-SBS against different tensile strains as a function of the number of elongations, when the tensile strain is 50%, the composite film can withstand up to 20000 elongations without a significant change in resistance, even when the tensile strain is increased to 500% and still withstand more than 1600 elongations with an increase in resistance of only 8.9 times.
Analyzing the influence of the unit area loading of EGaIn on the conductivity and the electrical stability of the composite film, as shown in FIGS. 9 and 10, the curve of ■ in FIG. 10 represents the conductivity, and the curve of ● represents the quality factor, and as the unit area loading of EGaIn increases, the conductivity of the composite film increases, but the electrical stability decreases, and when the unit area increment increases to 5mg/cm2At that time, the conductivity increased to 2.0 × 106S/m, and the quality factor representing electrical stability is reduced to 0.83, and the changes of the two parameters in opposite directions can be attributed to the degradation of the network pore structure of the SBS electrospun fiber along with the increase of the unit area loading of EGaIn as shown in fig. 11a to 11e, however, compared with the stretch-resistant conductor composite film in the prior art, the elastic conductor composite film provided by the embodiment has obvious advantages in both electrical conductivity and electrical stability.
Example two
Referring to fig. 12, in order to further improve the conductivity of the composite film, the present embodiment provides another elastic conductor composite film and a method for manufacturing the same, in which a nano-silver conductive layer is formed between a base film layer and an alloy layer on the basis of the first embodiment, so as to achieve the purpose of significantly improving the conductivity of the composite film.
The method for preparing the base film layer and the alloy layer in this embodiment is the same as that in the first embodiment, except that a nano silver conductive layer (AgNPs) needs to be formed on the base film layer before the alloy layer is coated, and the specific steps are as follows:
preparing a nano silver solution, dissolving silver trifluoroacetate (AgTFA) in ethanol (EtOH) to obtain a solution with the concentration of 0.1-1g/m L;
the base film layer is sequentially soaked in a nano silver solution, a reducing agent and absolute ethyl alcohol: soaking the electrospun base film layer in a nano-silver solution for 5min, taking out the base film layer, placing in air, and naturally drying at normal temperature, wherein the dried base film layer is soaked in a reducing agent for not less than 5min, so that nano-silver is reduced on the surface of the base film layer; taking out the base membrane layer, and soaking in anhydrous ethanol for at least 10min to remove residual reducing agent; and (3) placing the base film layer soaked in the absolute ethyl alcohol in the air, and naturally drying at normal temperature, wherein a nano-silver conductive layer is formed on the surface of the base film layer, and the semi-finished product of the composite film is represented by Ag-SBS.
The reducing agent used in this example was an ethanol solution of hydrazine hydrate.
And (3) coating EGaIn on the surface of the nano silver conductive layer by adopting the method of the first embodiment to form an alloy layer, and expressing the obtained elastic conductor composite film by using EGaIn-AgNPs-SBS.
Referring to fig. 14 and 15, a curve of ■ in fig. 14 shows a resistance increase rate, a curve of ● shows a quality factor, and an R in a vertical axis shows a R in a vertical axissAnd R both represent the electrical resistance of the composite film after stretching, Rs0And R0All show the resistance of the composite film in a natural state, the initial conductivity of the EGaIn-AgNPs-SBS can reach 1658800S/m, the resistance is only increased by 40.8 times when the tensile strain is 1950%, correspondingly, the quality factor of the electrical stability is reduced to 0.48, the quality factor is still 11.9 when the tensile strain is 100%, and the composite film can bear more than 200000 times of stretching when the tensile strain is 60% and the resistance is only increased by 38%, so that the good electrical stability can be still maintained when the composite film is slowly deformed.
EXAMPLE III
Referring to fig. 16, the present embodiment provides an elastic conductor composite membrane with a three-layer structure and a method for preparing the same, and in particular, relates to an elastic conductor composite membrane applied to a wearable thermal therapy device. The preparation method of the base film layer and the alloy layer is the same as that of the first embodiment, and the difference is that the formation of the base film layer and the formation of the alloy layer are alternately carried out, the base film layer is formed firstly, the alloy layer is formed secondly, and each time the alloy layer is coated, a required specific pattern is formed on the base film layer, so that it is easy to understand that each layer of the elastic conductor composite film comprises the base film layer and the alloy layer, the three-layer structure elastic conductor composite film is sequentially represented as a top layer, a middle layer and a bottom layer according to the electrospinning sequence of the base film layer, wherein 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 human biological signals.
In order to enhance the electrical contact performance of the elastic conductor composite membrane when in contact with human skin, the bottom composite membrane used as a contact electrode is covered with a layer of ion conductive hydrogel, the pattern of the hydrogel is consistent with that of the bottom alloy layer, as shown in fig. 16, and both are in a grid shape and consistent in size and shape.
The intermediate layer of the composite membrane is plasma-treated to make it hydrophilic in consideration of the hydrophobicity of SBS, so that the intermediate layer as a sweat sensor can transmit sweat from the skin surface to the sensor through the surface tension of the porous fiber structure of the membrane layer in a compressed state. The elastic conductor composite film with the prepared three-layer structure is shown in figure 17,
different from the preparation of the composite membrane by a lamination method, the composite membrane obtained by adopting the preparation method of the embodiment in which the electrospinning and coating are alternately carried out is an integrated composite membrane, and cannot be layered when being repeatedly used, so that the applicability of the composite membrane is greatly improved; similarly, the thickness of the base film layer is controlled by controlling the collection time of the electrospinning, so that the thickness of each layer can be flexibly adjusted for the composite film with a multilayer structure; the simple and efficient preparation process is beneficial to the design and industrial production of wearable equipment with high integration level and rich functions.
With reference to the first three embodiments, it is easily understood that in a further embodiment, for the preparation of the elastic conductor composite film with a multilayer structure, the elastic conductor composite film with a multilayer structure including the nano-silver conductive layer may be formed alternately according to the preparation sequence of the base film layer, the nano-silver conductive layer, and the alloy layer, and details on the preparation of such a composite film are not repeated herein, and those skilled in the art can clearly prepare the elastic conductor composite film with a multilayer structure including the nano-silver conductive layer according to the embodiments provided by the present invention.
Performance testing
The performance of each layer of the elastic conductor composite film with the three-layer structure in the third embodiment was tested,
for a top-layer composite film used as a heater, the top-layer composite film is respectively fixed on clamping plates at two ends of stretching equipment, one clamping plate is movable, the other clamping plate is fixed, direct-current step voltage of 0-0.45V is applied to the top-layer composite film, the temperature change of the composite film is monitored by using an infrared thermal imager, the voltage application time is at least 60s each time to ensure that the heating temperature of the composite film can reach a stable state, the infrared thermal image monitoring is stopped when the temperature of the composite film is recovered to room temperature, the temperature change curve of the composite film under different voltage application conditions is recorded as shown in figure 18, and the temperature of the composite film can be stable within 30s in 6 voltage application; aiming at the heating performance of the composite film, applying voltage to the top composite film every 60s, gradually increasing the voltage by 0.07-0.08V every time, and applying the next voltage after the temperature of the composite film is recovered to the room temperature, wherein the voltage application is that the next voltage is immediately applied when the temperature of the composite film reaches a stable value, similarly monitoring the temperature change of the composite film by using an infrared thermal imager, stopping infrared thermal image monitoring when all voltage values are applied and the room temperature of the composite film is recovered, recording the maximum value which can be reached by the composite film under different applied voltages as shown in figure 19, and observing the temperature step change along with the voltage, wherein the maximum value of the composite film can reach 95 ℃ when the voltage is applied for 0.45V for the last time, which indicates that the provided elastic conductor composite film can accurately control the temperature output; for the tensile resistance of the composite film, a direct current voltage of 0.15V is applied to the composite film, the composite film is uniformly stretched at a speed of 3mm/s, a curve of the temperature of the composite film changing along with the stretching strain is recorded, and is shown in figure 20, the temperature of the composite film is increased from 34.4 ℃ under 0% strain to 40.1 ℃ under 100% strain, and is only increased by 5.7 ℃, which means that the composite film can still keep good electrical stability when deforming along with human skin; in addition, the electrical stability of the composite film in the repeated heating and cooling process is tested, a direct current voltage of 0.2V is applied to the composite film, the composite film is returned to the room temperature when the temperature of the composite film reaches a stable value, so that the cycle is performed, the temperature change of the composite film in 10 cycle processes is recorded as shown in figure 21, and the composite film can still maintain the stable heating performance in the cycle process.
The interlayer composite membranes used as capacitive sweat sensors were tested for sweat conduction and ion permeability when in a stretched state. Similarly, the middle-layer composite membrane is fixed on the clamping plates at the two ends of the stretching device, one clamping plate is movable, the other clamping plate is fixed, phosphate-buffered saline (PBS) is used for simulating human sweat, PBS with different volumes is dropped on the surface of the composite membrane to simulate the change of different sweating rates to the capacitance value of the composite membrane, and the curve of the capacitance value of the composite membrane along with the change of the PBS volume under different stretching degrees is recorded as shown in fig. 22; sodium ions and chloride ions are important monitoring indexes of human physiological states, so that NaCl aqueous solutions with different ion concentrations are adopted to simulate human physiological states at different stages, the composite membrane is completely soaked in the NaCl aqueous solution, a curve of a composite membrane capacitance stability value changing along with the NaCl concentration under different stretching degrees is monitored as shown in a figure 23, the stretching strain is respectively tested on sweat conduction and ion permeability to be three stretching degrees of 0%, 50% and 100%, and the sweat conduction sensitivity and the ion permeability of the composite membrane are improved along with the increase of the stretching degrees.
Referring to fig. 24 and 25, the bottom composite membrane used as a contact electrode for collecting biological signals is tested for accuracy and stability of signal collection in natural state and deformed state, an electrocardiograph monitor with a quadrupole electrocardiograph monitoring lead is used, wherein 3 lines are respectively connected to the inner sides of the left leg and the right leg of a tester and the left wrist by using a common electrocardiograph ECG patch, the other line is connected to the right wrist by using the bottom composite membrane of the present invention, the bottom composite membrane is squeezed by hands when the signal starts to be collected to simulate the deformed state, the waveforms of the electrocardiograph signals collected in 3 wave bands i, ii and iii in the natural state and the deformed state are respectively recorded as shown in fig. 24 and 25, it can be seen that the composite membrane can collect the required electrocardiograph signal waveforms from 3 wave bands with low noise ratio in the natural state and the deformed state, and the waveforms of the electrocardiograph signals collected in the deformed state are not high in burr and noise compared with the natural state, the composite membrane provided by the invention has the advantages of high signal acquisition reliability, simplicity and convenience in operation and comfortable touch feeling.
The above examples are only intended to illustrate the technical solution of the present invention, but not to limit it; although the invention has been described in detail with reference to the foregoing embodiments, it will be understood by those skilled in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.
Claims (20)
1. An elastic conductor composite film, comprising: the coating material is a liquid metal with the melting point lower than room temperature.
2. An elastic conductor composite film according to claim 1, wherein a nano silver conductive layer is further formed between the base film layer and the coating material.
3. An elastic conductor composite film according to claim 1, wherein the elastic conductor composite film is a multilayer structure formed by sequentially and alternately vertically stacking the base film layer and the coating material.
4. An elastic conductor composite film according to claim 1 or 2, wherein the elastic conductor composite film is a multilayer structure formed by sequentially and alternately vertically stacking the base film layer, the nano silver conductive layer and the coating material.
5. An elastic conductor composite film according to claim 1, wherein the coating material is patterned on the surface of the base film layer through a patterned mold.
6. An elastic conductor composite film according to claim 1, wherein the surface of the elastic conductor composite film which is in contact with a living body is covered with a layer of ion-conducting hydrogel, and the ion-conducting hydrogel is formed in a pattern which is consistent with a pattern formed by a coating material on the covered surface.
7. An elastic conductor composite film according to claim 1, wherein the electrospinnable thermoplastic elastomer is a styrene-butadiene-styrene block copolymer and the concentration of the electrospinnable thermoplastic elastomer in the formed electrospun polymer solution is 5 wt% to 20 wt%.
8. An elastic conductor composite film according to claim 1, wherein the liquid metal is a room temperature liquid gallium-based alloy.
9. A method for preparing an elastic conductor composite film is characterized by comprising the following steps:
s1, dissolving an electro-spinnable thermoplastic elastomer in an intermediate agent to form an electro-spun polymer solution;
s2, carrying out electrospinning by using the electrospinning polymer solution, and collecting the electrospinning on a substrate to form a base film layer of the elastic conductor composite film;
and S3, coating a coating material on the surface of the base film layer, wherein the coating material is liquid metal with the melting point lower than room temperature.
10. The method for preparing an elastic conductor composite film according to claim 9, wherein the step S3 is preceded by:
and sequentially soaking the base film layer in a nano silver solution, a reducing agent and absolute ethyl alcohol to form a nano silver conductive layer on the surface of the base film layer.
11. The method for preparing an elastic conductor composite film according to claim 9, wherein the step S3 is further followed by:
and (3) electrospinning a new base film layer on the surface of the base film layer coated with the coating material by using the electrospinning polymer solution, coating the coating material on the surface of the new base film layer, and repeating the steps of electrospinning and coating the coating material alternately until the required number of layers is obtained to form the elastic conductor composite film with the multilayer structure.
12. The method for preparing an elastic conductor composite film according to claim 10, wherein the step S3 is further followed by:
and (3) electrospinning a new base film layer on the surface of the base film layer coated with the coating material by using the polymer solution, sequentially forming a nano silver conductive layer and the coating material on the surface of the new base film layer, and repeating the steps of electrospinning, forming the nano silver conductive layer and coating the coating material until the required number of layers is obtained to form the multilayer structure elastic conductor composite film.
13. The method of claim 10, wherein the forming the nano silver conductive layer on the surface of the base film layer comprises:
and soaking the base film layer in a nano-silver solution for 5min, taking out the base film layer, placing the base film layer in air, and naturally drying at normal temperature, soaking the air-dried base film layer in a reducing agent for not less than 5min, soaking the base film layer soaked by the reducing agent in absolute ethyl alcohol for not less than 10min, and placing the base film layer soaked by the absolute ethyl alcohol in air, and naturally drying at normal temperature to form the nano-silver conductive layer on the surface of the base film layer.
14. The method of claim 10, wherein the nano silver solution is prepared by dissolving silver trifluoroacetate in ethanol to obtain a solution with a concentration of 0.1-1g/m L.
15. The method of claim 10, wherein the reducing agent is a hydrazine hydrate ethanol solution.
16. The method of claim 9, wherein coating the coating material on the surface of the base film layer comprises:
placing a mold with a pattern on the surface of the base film layer so that the coating material forms the pattern when coated on the surface of the base film layer.
17. The method of making an elastic conductor composite film according to claim 9, further comprising:
and covering one surface of the elastic conductor composite membrane to be contacted with the organism with a layer of ion-conductive hydrogel, wherein the pattern formed by the ion-conductive hydrogel is consistent with the pattern formed by the coating material on the covered surface.
18. The method for preparing an elastic conductor composite film according to claim 9, wherein the step S1 includes:
the intermediate agent is dichloroethane, the styrene-butadiene-styrene block copolymer is dissolved in the dichloroethane to obtain an electrospinning polymer solution, and the mass percentage concentration in the formed electrospinning polymer solution is 5 wt% -20 wt%.
19. The method of manufacturing an elastic conductor composite film according to claim 9, wherein the liquid metal is a room temperature liquid gallium-based alloy.
20. The method of claim 9, wherein the thickness of the base film layer is positively correlated to the collection time of the collected electrospun fibers on the substrate.
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