CN112284579B - Self-powered flexible piezoresistive pressure sensor based on biological film and preparation method and application thereof - Google Patents
Self-powered flexible piezoresistive pressure sensor based on biological film and preparation method and application thereof Download PDFInfo
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- CN112284579B CN112284579B CN202011058605.8A CN202011058605A CN112284579B CN 112284579 B CN112284579 B CN 112284579B CN 202011058605 A CN202011058605 A CN 202011058605A CN 112284579 B CN112284579 B CN 112284579B
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01L—MEASURING FORCE, STRESS, TORQUE, WORK, MECHANICAL POWER, MECHANICAL EFFICIENCY, OR FLUID PRESSURE
- G01L1/00—Measuring force or stress, in general
- G01L1/20—Measuring force or stress, in general by measuring variations in ohmic resistance of solid materials or of electrically-conductive fluids; by making use of electrokinetic cells, i.e. liquid-containing cells wherein an electrical potential is produced or varied upon the application of stress
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J7/00—Adhesives in the form of films or foils
- C09J7/20—Adhesives in the form of films or foils characterised by their carriers
- C09J7/22—Plastics; Metallised plastics
- C09J7/25—Plastics; Metallised plastics based on macromolecular compounds obtained otherwise than by reactions involving only carbon-to-carbon unsaturated bonds
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J7/00—Adhesives in the form of films or foils
- C09J7/20—Adhesives in the form of films or foils characterised by their carriers
- C09J7/29—Laminated material
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01L—MEASURING FORCE, STRESS, TORQUE, WORK, MECHANICAL POWER, MECHANICAL EFFICIENCY, OR FLUID PRESSURE
- G01L9/00—Measuring steady of quasi-steady pressure of fluid or fluent solid material by electric or magnetic pressure-sensitive elements; Transmitting or indicating the displacement of mechanical pressure-sensitive elements, used to measure the steady or quasi-steady pressure of a fluid or fluent solid material, by electric or magnetic means
- G01L9/02—Measuring steady of quasi-steady pressure of fluid or fluent solid material by electric or magnetic pressure-sensitive elements; Transmitting or indicating the displacement of mechanical pressure-sensitive elements, used to measure the steady or quasi-steady pressure of a fluid or fluent solid material, by electric or magnetic means by making use of variations in ohmic resistance, e.g. of potentiometers, electric circuits therefor, e.g. bridges, amplifiers or signal conditioning
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- H—ELECTRICITY
- H02—GENERATION; CONVERSION OR DISTRIBUTION OF ELECTRIC POWER
- H02N—ELECTRIC MACHINES NOT OTHERWISE PROVIDED FOR
- H02N1/00—Electrostatic generators or motors using a solid moving electrostatic charge carrier
- H02N1/04—Friction generators
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J2479/00—Presence of polyamine or polyimide
- C09J2479/08—Presence of polyamine or polyimide polyimide
- C09J2479/086—Presence of polyamine or polyimide polyimide in the substrate
Abstract
The invention provides a self-powered flexible piezoresistive pressure sensor based on a biological film and a preparation method and application thereof, wherein the pressure sensor is of a laminated structure, and a polyimide adhesive tape layer, a poly (3, 4-ethylenedioxythiophene) -polystyrene sulfonate conducting polymer film resistance layer, a copper foil, an egg film modified by a carbon nano tube, a polydimethylsiloxane film and an egg film modified by poly (3, 4-ethylenedioxythiophene) -polystyrene sulfonate are sequentially arranged from one side to the other side; wherein, one side of the copper foil is processed with a microstructure which is arranged towards the egg membrane modified by the carbon nano tube; the egg membrane is an outer layer egg shell membrane; one side of the polydimethylsiloxane film is processed with a random microstructure, and the other side of the polydimethylsiloxane film is provided with a silver electrode. The pressure sensor has ultrahigh sensitivity, quick response and recovery time, wide sensing range and can generate energy by itself.
Description
Technical Field
The invention belongs to the technical field of pressure sensor preparation, and particularly relates to a self-powered flexible piezoresistive pressure sensor based on a biological film, and a preparation method and application thereof.
Background
The information in this background section is only for enhancement of understanding of the general background of the invention and is not necessarily to be construed as an admission or any form of suggestion that this information forms the prior art that is already known to a person of ordinary skill in the art.
The flexible pressure sensor can convert external pressure stimulation into an electric signal, realizes pressure monitoring, and has the function similar to human skin touch sensing. The wearable electronic device has the advantages of high sensitivity, quick response time, good flexibility, wearability, stretching, convenient carrying, convenient attachment to a human body and the like, and has wide application prospect in the fields of human health detection, medical diagnosis, wearable electronic devices, intelligent artificial limbs, electronic skins and the like. According to different working mechanisms, the flexible pressure sensor can be divided into a piezoresistive type sensor, a capacitive type sensor, a piezoelectric type sensor, a triboelectric type sensor and the like, and the piezoresistive type sensor has the advantages of simple structure and induction mechanism, convenience in preparation, high sensitivity and the like, and becomes the research focus of the flexible pressure sensor. Currently, most flexible pressure sensors require an external power supply to provide energy, which hinders the development of portable, miniaturized and intelligent pressure sensors, and therefore, flexible pressure sensors capable of self-powering become a hot point of research.
At present, the flexible piezoresistive pressure sensor has the following problems: (1) the sensing layer of the flexible piezoresistive pressure sensor is complex to prepare, the required materials are expensive and pollute the environment, and the flexible piezoresistive pressure sensor is not friendly to human bodies, and the natural material film directly adopting biocompatibility cannot show good performance in the original state, so that the sensitivity of the device is low. (2) In order to improve the sensitivity of the device, a proper microstructure needs to be prepared, the photoetching technology has high cost and complex process and is not easy to prepare, and the natural template has the defects of uncontrollable structure and size and cannot directly prepare a microstructure electrode on hard materials such as copper foil and the like. (3) Moreover, most piezoresistive pressure sensors have the defects of low response sensitivity, small response range, unstable initial resistance, resistance jump after response recovery, unadjustable sensitivity and the like. (4) Meanwhile, a single flexible piezoresistive pressure sensor needs to be supplied with external energy to work, and the energy supply is lacked. The triboelectric nano-generator can generate energy, but is insensitive to force response in a tiny range or even cannot respond when pressure detection is carried out. In addition, the problem how to combine the two is also needed to be solved by utilizing the triboelectric nano-generator to provide energy for the piezoresistive pressure sensor.
Disclosure of Invention
Aiming at the technical problems in the prior art, the invention provides a self-powered flexible piezoresistive pressure sensor based on a biological film and a preparation method and application thereof. The piezoresistive pressure sensor is simple in preparation process, environment-friendly, high in sensitivity and adjustable in sensitivity of devices, stable in initial resistance and low in energy consumption, and can realize self-supply of energy.
To solve the above technical problem, one or more of the following embodiments of the present invention provide the following technical solutions:
in a first aspect, the invention provides a self-powered flexible piezoresistive pressure sensor based on a biological film, which is a laminated structure, and a polyimide adhesive tape layer, a poly (3, 4-ethylenedioxythiophene) -polystyrene sulfonate (PEDOT: PSS) conductive polymer film resistance layer, a copper foil, an egg film modified by a carbon nano tube, a polydimethylsiloxane film and an egg film modified by poly (3, 4-ethylenedioxythiophene) -polystyrene sulfonate are sequentially arranged from one side to the other side;
wherein, one side of the copper foil is processed with a microstructure which is arranged towards the egg membrane modified by the carbon nano tube;
the egg membrane is an outer layer egg shell membrane;
one side of the polydimethylsiloxane film is processed with a random microstructure, and the other side of the polydimethylsiloxane film is provided with a silver electrode.
In a second aspect, the invention provides a preparation method of the self-powered flexible piezoresistive pressure sensor based on the biological film, which comprises the following steps:
intercepting the polyimide adhesive tape, treating the polyimide adhesive tape by using oxygen plasma, and spin-coating a poly (3, 4-ethylenedioxythiophene) -polystyrene sulfonate conductive polymer thin film resistor layer on the surface of the polyimide adhesive tape to prepare a P-PI adhesive tape;
carrying out laser marking on the copper foil, preparing a micro-grid structure on the surface of the copper foil, and uniformly distributing micro-cone structures in the micro-grid structure;
taking the egg membrane out of the egg shell, and tearing off the inner layer egg shell membrane to obtain an outer layer egg shell membrane;
immersing the outer layer egg shell membrane in the carbon nano tube suspension, and performing ultrasonic treatment to obtain a C-egg membrane;
copying a surface microstructure of the abrasive paper on one surface of the polydimethylsiloxane film, and sputtering a metal silver layer on the other surface of the polydimethylsiloxane film to obtain a microstructure-Ag-PDMS;
soaking the outer layer egg shell membrane in poly (3, 4-ethylenedioxythiophene) -polystyrene sulfonate solution to obtain a P-egg membrane;
and assembling the P-PI adhesive tape, the copper foil, the C-egg membrane, the microstructure-Ag-PDMS and the P-egg membrane in sequence to obtain the composite material.
In a third aspect, the invention provides applications of the self-powered flexible piezoresistive pressure sensor based on the biological film in the fields of artificial intelligence, medical diagnosis, wearable electronic devices, intelligent artificial limbs, electronic skin and man-machine interaction.
Compared with the prior art, one or more technical schemes of the invention have the following beneficial effects:
in terms of performance, the piezoresistive pressure sensor prepared by the invention has ultrahigh sensitivity under a wide range of pressure and is always maintainedThe stable initial resistance value is maintained, and the resistance value can be quickly restored to the initial state after the pressure is released, which is beneficial to the induction mechanism and the prepared microstructure copper foil. PSS is made to form one layer of film resistor with fixed resistance and one layer of C-egg film is set on the side with microstructure to form one parallel circuit with total resistance R expressed as R ═ Ra//(Rb+Rc) Where R isaIs PEDOT PSS film resistance, RbIs the resistance of C-egg membrane itself, RcIs the contact resistance of the C-egg membrane and the microstructure copper foil electrode.
The response mechanism of the piezoresistive pressure sensor is as follows: when no pressure is applied, the contact of the C-egg membrane with the electrode is very little due to the micro-structure on the copper foil, resulting in RcIs much greater than RaIn this case, R is mainly represented by RaDetermine, and RaThe resistance value of the sensor is always kept unchanged and is not influenced by external pressure, so that the sensor can keep a stable initial resistance value. When pressure is applied, the contact area between the C-egg membrane and the microstructure electrode is rapidly increased, and the conductive path is increased, so that R is increasedcRapid decrease of resistance value, RaWill be much larger than RcWhen R is predominantly comprised of RcIt was determined that there is also a large drop in the value of R, which ensures an ultra high sensitivity in a small force range. Along with the continuous increase of the pressure, the contact area is also continuously increased, the filamentous fiber structure of the C-egg membrane is also compressed, so that the contact points between the silk and the silk are increased, and the R is reducedbAt this time RbAnd RcSimultaneously decrease, R is mainly formed by RbAnd RcAnd (6) determining. And due to the effect of the unique microstructure, the contact area is continuously increased along with the continuous increase of the pressure, the contact area is also greatly changed in a relatively wide range, and the contact area cannot reach a saturation state quickly, so that the relatively wide induction range and the ultrahigh sensitivity are ensured. When the pressure is released, the contact between the C-egg membrane and the copper electrode can be quickly recovered to the initial state because the copper electrode and the C-egg membrane do not have adhesionInitial state, resistance R at this timecWill also increase instantaneously and far more than RaThe value of R is restored to RaIn the determined initial state, the resistance value is restored to the initial value and is maintained stable. Therefore, the structure and the sensing mechanism of the piezoresistive sensor provided by the invention greatly improve the sensitivity of the piezoresistive sensor in a simple parallel resistor mode, so that the piezoresistive sensor has ultrahigh sensitivity in a relatively wide range. Based on this, R can be variedaThe sensitivity can be obtained by spin coating different thicknesses of PEDOT and PSS, or can be adjusted by using other materials.
In addition, the cost is saved by utilizing the natural filamentous structure of the egg membrane, and the performance of the device is effectively improved by utilizing the modification of CNTs and PEDOT: PSS. The egg membrane treated by the PEDOT and PSS increases the surface charge density, the triboelectric performance and the electrostatic induction capacity, so that the performance of the triboelectric nano generator is greatly improved, the output voltage is increased along with the increase of the pressure, the pressure response capacity is shown, the egg membrane is combined with the piezoresistive pressure sensor, the pressure response range of the device is further expanded, and enough energy can be provided to support the normal operation of the device.
In the aspect of the preparation process, the micro-fences are uniformly distributed with the micro-cone structures by the laser marking technology, and the preparation method has the advantages of simple preparation, low cost, easy realization and batch production. The microstructure prepared by laser marking can be controlled in shape and size, the surface of the copper foil is roughened by laser sintering, and a layer of secondary structure is added to the microstructure. And the microstructure is prepared on the copper foil by directly utilizing laser marking, so that the viscosity and the hysteresis of the sensor can be reduced, and the sensor has quick response and recovery time.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this specification, are included to provide a further understanding of the invention, and are incorporated in and constitute a part of this specification, illustrate exemplary embodiments of the invention and together with the description serve to explain the invention and not to limit the invention.
FIG. 1 is a flow chart of a method for manufacturing a self-powered flexible piezoresistive pressure sensor based on a biological film;
FIG. 2 is a schematic structural diagram of a self-powered flexible piezoresistive pressure sensor based on a biofilm;
FIG. 3 is a Field Emission Scanning Electron Microscope (FESEM) image of a microstructure fabricated on a copper foil based on laser marking techniques;
FIG. 4 is a FESEM image of a natural filamentous fibrous structure of egg membrane;
FIG. 5 is a FESEM image of an egg membrane modified with CNTs;
FIG. 6 is a FESEM image of an egg membrane modified with PEDOT PSS;
FIG. 7 is a graph of the sensitivity of a piezoresistive pressure sensor to pressure response for a self-powered flexible piezoresistive pressure sensor based on a biofilm over different pressure ranges;
FIG. 8 is a graph of response and recovery time for a self-powered flexible piezoresistive pressure sensor based on a biofilm;
FIG. 9 is a graph of output voltage as a function of pressure for a biofilm-based, self-powered, flexible piezoresistive pressure sensor, modified with different PEDOT: PSS concentrations, for an egg membrane.
In the figure: 1. a PDMS film; 2. egg membrane modified by PEDOT: PSS; 3. metal Ag; 4. a polydimethylsiloxane film; 5. the carbon nano tube modified egg membrane; 6. copper foil; 7. PEDOT, PSS film; 8. a polyimide tape layer; 9. a triboelectric nano-generator based on a biological film and working in a single-electrode mode; 10. a bio-film based piezoresistive pressure sensor.
Detailed Description
It is to be understood that the following detailed description is exemplary and is intended to provide further explanation of the invention as claimed. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs.
It is noted that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of exemplary embodiments according to the invention. As used herein, the singular forms "a", "an" and "the" are intended to include the plural forms as well, and it should be understood that when the terms "comprises" and/or "comprising" are used in this specification, they specify the presence of stated features, steps, operations, devices, components, and/or combinations thereof, unless the context clearly indicates otherwise.
In a first aspect, the invention provides a self-powered flexible piezoresistive pressure sensor based on a biological film, which is of a laminated structure, and a polyimide adhesive tape layer, a poly (3, 4-ethylenedioxythiophene) -polystyrene sulfonate conducting polymer film resistance layer, a copper foil, an egg film modified by a carbon nano tube, a polydimethylsiloxane film and an egg film modified by poly (3, 4-ethylenedioxythiophene) -polystyrene sulfonate are sequentially arranged from one side to the other side;
wherein, one side of the copper foil is processed with a microstructure which is arranged towards the egg membrane modified by the carbon nano tube;
the egg membrane is an outer layer egg shell membrane;
one side of the polydimethylsiloxane packaging layer is processed with a random microstructure, the other side of the polydimethylsiloxane packaging layer is provided with a silver electrode, and the silver electrode is positioned on the outer side.
In some embodiments, the microstructure on the copper foil is a micro-grid structure, and micro-cone structures are uniformly distributed in the micro-grid structure.
Furthermore, the number of the copper foils is two, and the two copper foils are arranged in parallel and are respectively arranged on two sides of the poly (3, 4-ethylenedioxythiophene) -polystyrene sulfonate conductive polymer thin film resistor layer.
In some embodiments, the egg membrane modified by PEDOT: PSS is positioned on the outer side of the polydimethylsiloxane membrane and is in contact with the silver electrode.
Further, the egg membrane is an outer layer egg shell membrane.
Furthermore, the egg membrane modified by the PEDOT PSS also comprises a PDMS membrane which is positioned at the outer side of the egg membrane modified by the PEDOT PSS.
The thicknesses of the P-PI adhesive tape, the copper foil, the C-egg film, the microstructure-Ag-PDMS, the egg film modified by PEDOT PSS and the PDMS film are 50-150 μm, 40-80 μm, 30-65 μm, 10-40 μm, 30-65 μm and 30-70 μm in sequence.
In a second aspect, the invention provides a preparation method of the self-powered flexible piezoresistive pressure sensor based on the biological film, which comprises the following steps:
intercepting a polyimide adhesive tape, treating the polyimide adhesive tape by using oxygen plasma, and spin-coating a poly (3, 4-ethylenedioxythiophene) -polystyrene sulfonate (PEDOT: PSS) conductive polymer thin film resistor layer on the surface of the polyimide adhesive tape to prepare a P-PI adhesive tape;
carrying out laser marking on the copper foil, preparing a micro-grid structure on the surface of the copper foil, and uniformly distributing micro-cone structures in the micro-grid structure;
taking the egg membrane out of the egg shell, and tearing off the inner layer egg shell membrane to obtain an outer layer egg shell membrane;
immersing the outer layer egg shell membrane in the carbon nano tube suspension, and performing ultrasonic treatment to obtain a C-egg membrane;
copying a surface microstructure of the abrasive paper on one surface of the polydimethylsiloxane film, and sputtering a metal silver layer on the other surface of the polydimethylsiloxane film to obtain a microstructure-Ag-PDMS;
soaking the outer layer egg shell membrane in poly (3, 4-ethylenedioxythiophene) -polystyrene sulfonate solution to obtain a P-egg membrane;
and assembling the P-PI adhesive tape, the copper foil, the C-egg membrane, the microstructure-Ag-PDMS and the P-egg membrane in sequence to obtain the composite material.
In some embodiments, the oxygen plasma treatment is performed for a period of time ranging from 5s to 60s, at a power ranging from 30W to 100W, and at an oxygen flow rate ranging from 10sccm to 20 sccm.
In some embodiments, the spin coating speed of the PEDOT: PSS solution is 200rmp-2000rmp, and after the spin coating is finished, the PEDOT: PSS solution is dried on a hot plate at the temperature of 30-80 ℃ for 1-2 h.
Different rotating speeds cause different thicknesses of PEDOT: PSS films, so that different resistances are caused, and the prepared different resistances can realize the adjustability of the sensitivity of the device, so that the PI adhesive tape (P-PI adhesive tape) coated with the PEDOT: PSS is obtained. The PI adhesive tape treated by the oxygen plasma improves the hydrophilicity, so that the PEDOT and PSS are adhered more firmly.
In some embodiments, the copper foil is cleaned with ethanol and deionized water and dried for use.
Furthermore, the laser marking power is 10% -30%, the frequency is 5KHz-20KHz, and the speed is 200mm/s-600 mm/s.
The structure which is provided with the micro-grids and is uniformly distributed with the micro cones is directly prepared on the surface of the copper foil, the sensitivity and the induction range of the device are greatly improved by a unique microstructure designed on the copper foil, and meanwhile, the adhesion between an electrode and an induction layer is reduced by directly preparing the microstructure on the copper foil, so that the device can rapidly respond and recover.
In some embodiments, the dispersant in the carbon nanotube suspension is sodium dodecylbenzene sulfonate (SDBS) or Sodium Dodecyl Sulfate (SDS).
Furthermore, the mass ratio of the carbon nano tube to the dispersing agent is 1:5-1: 10.
Furthermore, the concentration of the CNTs in the carbon nano tube suspension is 2.5 wt% -8 wt%.
Further, the egg membrane is soaked in the carbon nano tube suspension in an ultrasonic mode for 3h-5h, and the CNTs modified egg membrane (C-egg membrane) is dried on a hot plate at the temperature of 45-70 ℃ for 4h-6h after being washed by deionized water.
The egg membrane with a filamentous fiber structure with good biocompatibility is filled with a conductive material to serve as a sensing layer, and by utilizing the hydrophilicity of the egg membrane, the CNTs and PEDOT: PSS can be easily wrapped on each filamentous fiber of the egg membrane, so that the performance of a pressure sensor and a nano generator is greatly promoted.
The CNTs endow the egg membrane with the function of a sensing layer of a piezoresistive pressure sensor, and play a very important role in the high-sensitivity pressure sensing of a device.
In some embodiments, the method of replicating the surface microstructure of sandpaper on one side of a polydimethylsiloxane film is: and mixing PDMS and a curing agent in proportion, spin-coating on the surface of the cleaned sand paper, drying, and separating the film from the surface of the sand paper.
Further, the cleaning step of the sand paper is as follows: and cleaning the substrate by using acetone, ethanol and deionized water in sequence, and drying the substrate by using an oven after cleaning.
Furthermore, the drying temperature of the oven is 50-70 ℃, and the drying time is 20-40 min.
Further, the model of the sand paper is 400#, 600#, 1000#, 1200#, 1500# or 2000 #.
400#, 600#, 1000#, 1200#, 1500#, 2000# refer to 400 mesh, 600 mesh, 1000 mesh, 1200 mesh, 1500 mesh, or 2000 mesh, respectively.
In some embodiments, PDMS with sandpaper surface microstructure was treated in oxygen plasma for 60s to 90s at a power of 60W to 100W, followed by sputtering of an Ag layer on the side without microstructure.
Furthermore, the sputtering power is 70W-100W, and the sputtering time is 50min-70 min.
The PDMS (microstructure-Ag-PDMS) with the irregular microstructure and the metal Ag on the other surface can be used as an upper packaging layer of the flexible piezoresistive pressure sensor, the irregular microstructure is beneficial to improving the sensitivity of the sensor, and the PDMS can also be used as an electrode of a triboelectric nano generator.
In some embodiments, the method further comprises the step of preparing the PEDOT PSS modified egg membrane.
Further, the method comprises the following specific steps: and soaking the outer layer eggshell membrane in a PEDOT (PSS) solution for 5 to 10 hours, taking out, and drying on a hot plate at the temperature of between 45 and 70 ℃ for 4 to 6 hours to obtain the eggshell membrane.
Further, the preparation method of the PEDOT/PSS solution comprises the following steps: dissolving PEDOT and PSS in a solvent, carrying out ultrasonic treatment, carrying out centrifugal separation, and taking supernatant.
Still further, the solvent is water or an organic solvent, and the organic solvent is one or a mixture of ethanol, N-dimethylformamide, acetone and N-methylpyrrolidone.
In a third aspect, the invention provides applications of the self-powered flexible piezoresistive pressure sensor based on the biological film in the fields of artificial intelligence, medical diagnosis, wearable electronic devices, intelligent artificial limbs, electronic skin and man-machine interaction.
Example 1
1) The preparation method of the P-PI adhesive tape comprises the following specific steps:
(1-1) intercepting a section of PI adhesive tape, cleaning with ethanol, then cleaning with deionized water, drying, and treating with oxygen plasma, wherein the oxygen flow is 20sccm, the power is 65W, and the time is 30 s;
(1-2) spin-coating a layer of PEDOT: PSS solution on the treated PI adhesive tape at the rotating speed of 400rmp, then drying the solution on a hot plate at the temperature of 60 ℃ for 2 hours until the PEDOT: PSS is dried, and obtaining the P-PI adhesive tape;
2) preparing a copper foil with micro-grids and uniformly distributed micro-cone structures: cleaning a copper foil with ethanol and deionized water, drying for later use, and directly preparing a microstructure on the surface of the copper foil according to a distributed line by a designed wiring mode and a laser with the power of 20%, the frequency of 5KHz and the speed of 200mm/s, wherein a field emission electron scanning microscope (FESEM) picture of the microstructure is shown in figure 3;
3) the preparation method of the C-egg membrane comprises the following specific steps:
(3-1) manually peeling the egg membrane from the egg shell, then tearing off the inner membrane close to one side of the egg white, washing with deionized water for 3 times, and drying at normal temperature to obtain a clean egg membrane with a double-sided filamentous fiber structure, wherein the FESEM image is shown in figure 4;
(3-2) mixing CNTs and Sodium Dodecyl Sulfate (SDS) according to the weight ratio of 1:10, and dissolving in water, wherein the concentration of the CNTs in the obtained solution is 7.6 wt%, and then carrying out ultrasonic treatment for 8h for later use;
(3-3) putting the egg membrane treated in the step (3-1) into the prepared CNTs solution, performing ultrasonic treatment for 4h, then washing the egg membrane wrapped by the CNTs with deionized water, and drying the egg membrane on a hot plate at 55 ℃ for 4h to prepare a C-egg membrane, wherein an FESEM image is shown in FIG. 5;
4) the preparation method of the P-egg membrane comprises the following specific steps:
(4-1) mixing PEDOT to PSS according to a volume ratio of 1: 2 in proportion, dissolving in ethanol, performing ultrasonic treatment for 3 hours, centrifuging for 6min at the rotating speed of 12000rmp, and taking out supernatant;
(4-2) mixing the centrifuged supernatant with water according to a volume ratio of 1: 0.5,1: 2,1: 4, preparing solutions with different PEDOT to PSS concentrations;
(4-3) putting the egg membrane treated in the step (3-1) into prepared solutions with three different PEDOT: PSS concentrations, soaking for 8h, taking out, and drying on a hot plate at 60 ℃ for 4h to obtain a P-egg membrane, wherein an FESEM image is shown in FIG. 6;
5) the preparation method of the microstructure-Ag-PDMS comprises the following specific steps:
(5-1) shearing a piece of 6cm × 6cm abrasive paper with the model number of 1200#, cleaning for 3 times according to the sequence of acetone, ethanol and deionized water, then drying in an oven at 60 ℃ for 30min, and taking out for later use;
(5-2) base and curing agent of PDMS the ratio of 10: 1, stirred for 30min and then placed in a vacuum box to remove bubbles by evacuating for 1 h.
(5-3) spin-coating the mixed PDMS on the surface of the sand paper processed in the step (5-1) for 60s at the rotating speed of 400rmp, then drying the coated sand paper on a hot plate at the temperature of 70 ℃ for 4h, and separating the PDMS from the surface of the sand paper after the PDMS is completely dried;
(5-4) treating the PDMS prepared in the step (5-3) in oxygen plasma for 60s at 85W, then sputtering a layer of metal Ag on one side without the microstructure at 90W for 60min, and preparing a microstructure-Ag-PDMS with a random microstructure on one side and metal Ag on the other side;
6) spin coating PDMS on a plastic culture dish according to the procedure in (5-3) to obtain flat PDMS without microstructure;
7) a self-powered flexible piezoresistive pressure sensor is assembled from bottom to top according to the sequence of a P-PI adhesive tape, a microstructure copper foil, a C-egg membrane, a microstructure-Ag-PDMS, a P-egg membrane and a non-structure flat PDMS, and the structure of the pressure sensor is shown in figure 2.
Fig. 7 shows the response sensitivity of the piezoresistive pressure sensor in different pressure ranges, fig. 8 shows the response and recovery time of the piezoresistive pressure sensor, and fig. 9 shows the output voltage of the triboelectric nano-generator, which is composed of egg membranes modified by PEDOT: PSS concentration in single electrode mode, and varies with the pressure, which confirms that the self-powered flexible piezoresistive pressure sensor based on the biological membrane provided by the invention has ultrahigh sensitivity, fast response and recovery time, wide pressure induction range and can generate enough energy to meet the energy consumption of the device.
Example 2
1) The preparation method of the P-PI adhesive tape comprises the following specific steps:
(1-1) intercepting a section of PI adhesive tape, cleaning with ethanol, then cleaning with deionized water, drying, and treating with oxygen plasma, wherein the oxygen flow is 10sccm, the power is 85W, and the time is 40 s;
(1-2) spin-coating a layer of PEDOT: PSS solution on the treated PI adhesive tape at the rotating speed of 800rmp, then drying the solution on a hot plate at the temperature of 80 ℃ for 1.5h, and obtaining the P-PI adhesive tape after the PEDOT: PSS solution is dried;
2) preparing a copper foil with micro-grids and uniformly distributed micro-cone structures: cleaning and drying the copper foil by using ethanol and deionized water for later use, and directly preparing a microstructure on the surface of the copper foil according to the distributed lines by using a laser with the power of 30%, the frequency of 15KHz and the speed of 500mm/s in a designed wiring mode;
3) the preparation method of the C-egg membrane comprises the following specific steps:
(3-1) manually stripping the egg membrane from the egg shell, then tearing off the inner membrane close to one side of the egg white, washing for 3 times by using deionized water, and drying at normal temperature to obtain a clean egg membrane with a double-sided filamentous fiber structure;
(3-2) mixing CNTs and sodium dodecyl benzene sulfonate according to the weight ratio of 1: 7, and dissolving in water, wherein the concentration of the obtained solution of the CNTs is 3 wt%, and then carrying out ultrasonic treatment for 10h for later use;
(3-3) putting the egg membrane processed in the step (3-1) into a prepared CNTs solution, performing ultrasonic treatment for 3h, then washing the egg membrane wrapped by the CNTs with deionized water, and drying on a hot plate at 65 ℃ for 5h to prepare a C-egg membrane;
4) the preparation method of the P-egg membrane comprises the following specific steps:
(4-1) mixing PEDOT to PSS according to a volume ratio of 1: 2 in proportion, dissolving in ethanol, performing ultrasonic treatment for 3h, centrifuging for 6min at the rotating speed of 10000rmp, and taking out supernatant;
(4-2) mixing the centrifuged supernatant with water according to a volume ratio of 1: 2, preparing a solution of PEDOT and PSS;
(4-3) putting the egg membrane treated in the step (3-1) into a prepared solution with PEDOT (PSS) concentration, soaking for 8h, taking out, and drying on a hot plate at 60 ℃ for 4h to obtain a P-egg membrane;
5) the preparation method of the microstructure-Ag-PDMS comprises the following specific steps:
(5-1) shearing a piece of sand paper with the model number of 1000 being 6cm multiplied by 6cm, cleaning for 3 times according to the sequence of acetone, ethanol and deionized water, then drying in an oven at 60 ℃ for 30min, and taking out for later use;
(5-2) base and curing agent of PDMS the ratio of 10: 1, stirred for 30min and then placed in a vacuum box to remove bubbles by evacuating for 1 h.
(5-3) spin-coating the mixed PDMS on the surface of the sand paper processed in the step (5-1) for 60s at the rotating speed of 400rmp, then drying the coated sand paper on a hot plate at the temperature of 70 ℃ for 4h, and separating the PDMS from the surface of the sand paper after the PDMS is completely dried;
(5-4) treating the PDMS prepared in the step (5-3) in oxygen plasma for 60s at 85W, then sputtering a layer of metal Ag on one side without the microstructure at 90W for 60min, and preparing a microstructure-Ag-PDMS with a random microstructure on one side and metal Ag on the other side;
6) spin coating PDMS on a plastic culture dish according to the procedure in (5-3) to obtain flat PDMS without microstructure;
7) the self-powered flexible piezoresistive pressure sensor is assembled from bottom to top according to the sequence of a P-PI adhesive tape, a microstructure copper foil, a C-egg membrane, a microstructure-Ag-PDMS, a P-egg membrane and a microstructure-free flat PDMS.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. A self-powered flexible piezoresistive pressure sensor based on a biological film is characterized in that: the conductive polymer film resistor layer is of a laminated structure, and the polyimide tape layer, the poly (3, 4-ethylenedioxythiophene) -polystyrene sulfonate conductive polymer film resistor layer, the copper foil, the egg film modified by the carbon nano tube, the polydimethylsiloxane film and the egg film modified by the poly (3, 4-ethylenedioxythiophene) -polystyrene sulfonate are sequentially arranged from one side to the other side;
wherein, one side of the copper foil is processed with a microstructure which is arranged towards the egg membrane modified by the carbon nano tube;
the egg membrane is an outer layer egg shell membrane;
one side of the polydimethylsiloxane film is processed with a random microstructure, the other side of the polydimethylsiloxane film is provided with a silver electrode, and the silver electrode is positioned on the outer side.
2. A bio film based self powered flexible piezoresistive pressure sensor according to claim 1, characterised in that: the microstructure on the copper foil is a micro-grid structure, and micro cone structures are uniformly distributed in the micro-grid structure;
furthermore, the number of the copper foils is two, and the two copper foils are arranged in parallel and are respectively arranged on two sides of the poly (3, 4-ethylenedioxythiophene) -polystyrene sulfonate conductive polymer thin film resistor layer.
3. A bio film based self powered flexible piezoresistive pressure sensor according to claim 1, characterised in that: PEDOT, namely, the egg membrane modified by PSS is positioned on the outer side of the polydimethylsiloxane membrane and is contacted with the silver electrode;
further, the egg membrane is an outer layer egg shell membrane;
furthermore, the egg membrane modified by the PEDOT PSS also comprises a PDMS membrane which is positioned at the outer side of the egg membrane modified by the PEDOT PSS.
4. A method for preparing a self-powered flexible piezoresistive pressure sensor based on biofilm according to any of claims 1 to 3, wherein: the method comprises the following steps:
intercepting the polyimide adhesive tape, treating the polyimide adhesive tape by using oxygen plasma, and spin-coating a poly (3, 4-ethylenedioxythiophene) -polystyrene sulfonate conductive polymer thin film resistor layer on the surface of the polyimide adhesive tape to prepare a P-PI adhesive tape;
carrying out laser marking on the copper foil, preparing a micro-grid structure on the surface of the copper foil, and uniformly distributing micro-cone structures in the micro-grid structure;
taking the egg membrane out of the egg shell, and tearing off the inner layer egg shell membrane to obtain an outer layer egg shell membrane;
immersing the outer layer egg shell membrane in the carbon nano tube suspension, and performing ultrasonic treatment to obtain a C-egg membrane;
copying a surface microstructure of the abrasive paper on one surface of the polydimethylsiloxane film, and sputtering a metal silver layer on the other surface of the polydimethylsiloxane film to obtain a microstructure-Ag-PDMS;
soaking the outer layer egg shell membrane in poly (3, 4-ethylenedioxythiophene) -polystyrene sulfonate solution to obtain a P-egg membrane;
and assembling the P-PI adhesive tape, the copper foil, the C-egg membrane, the microstructure-Ag-PDMS and the P-egg membrane in sequence to obtain the composite material.
5. The method of claim 4, wherein: the oxygen plasma treatment time is 5-60 s, the power is 30-100W, and the oxygen flow is 10-20 sccm;
in some embodiments, the spin coating speed of the PEDOT: PSS solution is 200rmp-2000rmp, and after the spin coating is finished, the PEDOT: PSS solution is dried on a hot plate at the temperature of 30-80 ℃ for 1-2 h.
6. The method of claim 4, wherein: cleaning the copper foil with ethanol and deionized water, and drying for later use;
furthermore, the laser marking power is 10% -30%, the frequency is 5KHz-20KHz, and the speed is 200mm/s-600 mm/s;
in some embodiments, the dispersant in the carbon nanotube suspension is sodium dodecylbenzene sulfonate or sodium dodecyl sulfate;
further, the mass ratio of the carbon nano tube to the dispersing agent is 1:5-1: 10;
furthermore, the concentration of the CNTs in the carbon nano tube suspension is 2.5 wt% -8 wt%;
further, the egg membrane is soaked in the carbon nano tube suspension in an ultrasonic mode for 3h-5h, and the egg membrane modified by the CNTs is washed by deionized water and dried on a hot plate at the temperature of 45-70 ℃ for 4h-6 h.
7. The method of claim 4, wherein: the method for duplicating the surface microstructure of the sandpaper on one side of the polydimethylsiloxane film comprises the following steps: mixing PDMS and a curing agent in proportion, spin-coating on the surface of cleaned sand paper, drying, and separating the film from the surface of the sand paper;
further, the cleaning step of the sand paper is as follows: sequentially cleaning with acetone, ethanol and deionized water, and drying with an oven;
furthermore, the drying temperature of the oven is 50-70 ℃, and the drying time is 20-40 min;
further, the model of the sand paper is 400#, 600#, 1000#, 1200#, 1500# or 2000 #.
8. The method of claim 4, wherein: treating PDMS with the sand paper surface microstructure in oxygen plasma for 60s-90s at the power of 60W-100W, and then sputtering an Ag layer on the side without the microstructure;
furthermore, the sputtering power is 70W-100W, and the sputtering time is 50min-70 min.
9. The method of claim 4, wherein: the preparation method also comprises the step of preparing PEDOT, namely the egg membrane modified by PSS;
further, the method comprises the following specific steps: soaking the outer layer eggshell membrane in PEDOT (PSS) solution for 5-10 h, taking out, and drying on a hot plate at 45-70 ℃ for 4-6 h to obtain the membrane;
further, the preparation method of the PEDOT/PSS solution comprises the following steps: dissolving PEDOT, PSS in a solvent, performing ultrasonic treatment, performing centrifugal separation, and taking supernatant;
still further, the solvent is water or an organic solvent, and the organic solvent is one or a mixture of ethanol, N-dimethylformamide, acetone and N-methylpyrrolidone.
10. Use of a biofilm based self-powered flexible piezoresistive pressure sensor according to any of the claims 1-3 in the fields of artificial intelligence, medical diagnostics, wearable electronics, intelligent prosthetics, electronic skin, human-computer interaction.
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