CN113670484A - Flexible pressure sensor with complementary spiral structure, preparation method and application thereof - Google Patents
Flexible pressure sensor with complementary spiral structure, preparation method and application thereof Download PDFInfo
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- CN113670484A CN113670484A CN202110946607.9A CN202110946607A CN113670484A CN 113670484 A CN113670484 A CN 113670484A CN 202110946607 A CN202110946607 A CN 202110946607A CN 113670484 A CN113670484 A CN 113670484A
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- G01—MEASURING; TESTING
- G01L—MEASURING FORCE, STRESS, TORQUE, WORK, MECHANICAL POWER, MECHANICAL EFFICIENCY, OR FLUID PRESSURE
- G01L1/00—Measuring force or stress, in general
- G01L1/14—Measuring force or stress, in general by measuring variations in capacitance or inductance of electrical elements, e.g. by measuring variations of frequency of electrical oscillators
- G01L1/142—Measuring force or stress, in general by measuring variations in capacitance or inductance of electrical elements, e.g. by measuring variations of frequency of electrical oscillators using capacitors
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- 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
- G01L9/12—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 capacitance, i.e. electric circuits therefor
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Abstract
The invention discloses a flexible pressure sensor with a complementary spiral structure, a preparation method and application thereof, belonging to the technical field of laser micro-nano processing; processing the surface of the graphene oxide/silk fibroin composite film by using laser, wherein oxygen-containing functional groups in the graphene oxide can be removed by the photothermal effect of the laser, so that the graphene oxide is reduced and a helical structure electrode is formed at the same time; after the porous adhesive tape is clamped between the pair of electrodes with the complementary spiral structures, the high-performance flexible pressure sensor with the complementary spiral structures is obtained, the double-mode detection of finger bending and finger approaching can be realized, the porous structures of the adhesive tape are beneficial to the large change of capacitance of the sensor during bending, and the accurate detection of finger bending can be realized. Meanwhile, the area of the edge area of the electrode is increased by the spiral structure of the electrode, so that more electric fields can be expanded from the electrode plate area to the outer space, and the sensitive detection of finger approach is realized.
Description
Technical Field
The invention belongs to the technical field of laser micro-nano processing, and particularly relates to a flexible pressure sensor with a complementary spiral structure, a preparation method and application thereof.
Background
The flexible capacitive pressure sensor has wide application prospect in the field of electronic skin, man-machine interaction, wearable health detection and other advanced applications. The innovation of capacitive pressure sensors relies mainly on new electrode materials and structures. Graphene is a commonly used electrode material in various flexible electronic devices due to its excellent conductivity, flexibility and mechanical strength. The graphene electrode prepared by the traditional method for manufacturing the graphene electrode, such as a chemical stripping method, a chemical vapor deposition method, a dispersion adhesion method and the like, is usually required to be attached to a special substrate, so that the flexibility of the graphene electrode is reduced to a greater or lesser extent, and the performance of the sensor is reduced.
In addition, any patterning of the graphene electrode is a technical challenge for limiting performance optimization of the capacitive pressure sensor, and high-temperature reduction, chemical reduction, inkjet reduction and the like adopted by people at present can only realize some simple patterning reduction, and meanwhile, the problems of low resolution, low reduction speed and the like exist. Furthermore, the ductility and mechanical strength of the electrodes also greatly limit the application of graphene electrodes in flexible capacitive pressure sensors.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to solve the problems that: and preparing the flexible pressure sensor with the complementary spiral electrode structure by utilizing laser processing. The laser direct writing technology is used for acting on the surface of the graphene oxide/silk fibroin composite film formed by suction filtration, the photothermal effect of the laser can remove oxygen-containing functional groups in the graphene oxide, so that the graphene oxide in the graphene oxide/silk fibroin composite film is reduced and forms a spiral structure electrode, and the reduced graphene oxide/silk fibroin composite electrode after laser reduction has excellent mechanical properties due to the excellent flexibility and ductility of the graphene oxide/silk fibroin composite film; and then a porous adhesive tape is clamped between the pair of complementary spiral structure electrodes, so that the high-performance flexible pressure sensor with the complementary spiral structure is finally obtained, and the ultra-sensitive detection of two modes of finger bending and finger approaching can be realized. The main detection principle of the sensor is as follows: (1) for contact detection, the formula is given by a parallel plate capacitor
(wherein ε0Is a vacuum dielectric constant,. epsilonrDielectric constant of the dielectric layer, a relative area between two parallel plate electrodes, and d relative distance between two parallel plate electrodes), when an object applies pressure to the sensor, the porous adhesive tape is compressed to reduce the relative distance d between the upper and lower plate electrodes, and air with relatively small dielectric constant in the porous adhesive tape is extruded out, so that the dielectric constant epsilon of the dielectric is larger than that of the other electroderThe capacitance value of the sensor is greatly changed under certain pressure under the combined action of the two, so that the sensitivity is high; (2) for non-contact detection, due to the fringe field effect of the parallel plate capacitor, electric field lines can be expanded to the external space in the fringe area, and for the sensor with the ring-plate structure electrode, when a finger approaches, the finger can intercept the fringe field lines above the upper electrode, so that the electric field intensity between the upper electrode and the lower electrode is reduced, and finally the capacitance is reduced. The electrode structure on the interface of the graphene electrode with the spiral complementary structure can be regarded as the superposition of a plurality of electrodes with ring-disc structures, so that the area of the edge area of the electrode is increased, and the expansion of more electric fields from the electrode plate area to the outer space is facilitated. Thus when a finger is in close proximity, the sensor exhibits a large change in capacitance, which is more sensitive to finger proximity.
The invention is realized by the following technical scheme:
a flexible pressure sensor with a complementary spiral structure is composed of an upper composite electrode, a lower composite electrode and a dielectric layer, wherein the composite electrodes are composed of a composite film material 1 and a nano spiral structure 2, the dielectric layer is a porous material 3, and the composite film material 1 is a surface smooth composite film material formed by mixing, filtering and forming a graphene oxide solution and a silk fibroin solution; the surface of the composite film material 1 is provided with a nano spiral structure 2, the outer surfaces of the composite film material 1 and the nano spiral structure 2 are adhered with a porous material 3, and the upper electrode, the lower electrode and the dielectric layer form a multi-stage micro-nano structure of the composite film material 1-the nano spiral structure 2-the porous material 3-the nano spiral structure 2-the composite film material 1.
When the nano spiral structure 2 is used for carrying out patterned reduction on the composite film material 1 by laser processing, a spiral patterning structure and a nano hole structure are formed simultaneously when oxygen-containing functional groups in the composite film are removed;
further, the thickness of the composite film material 1 is 50-200 μm.
Further, the porous material 3 is a porous foam adhesive tape, a porous sponge, a ceramic porous material, or the like.
Furthermore, the pore diameter of the nano-spiral structure 2 is 500nm-2 μm, the total number of turns of the spiral structure is 3-8 turns, the width of each turn of the spiral structure is 200-300 μm, the spiral width of the unprocessed part is 100-200 μm, and the size of the whole spiral part is 0.3mm-0.8 mm.
A method for preparing a flexible pressure sensor with a complementary spiral structure based on laser processing comprises the following specific steps:
(1) preparing a graphene oxide/silk fibroin mixed solution;
dropwise adding a sodium hydroxide solution into a certain amount of graphene oxide solution to keep the graphene oxide solution neutral, and then mixing the graphene oxide solution with a silk fibroin solution to prepare a graphene oxide/silk fibroin mixed solution;
(2) preparing a graphene oxide/silk fibroin composite film;
firstly fixing a microporous filter membrane on a suction filtration device, wetting the filter membrane by deionized water, and finally dripping a graphene oxide/silk fibroin mixed solution for suction filtration, thereby successfully preparing a graphene oxide/silk fibroin composite film;
(3) processing the graphene oxide/silk fibroin composite film by using a laser direct writing method to prepare a complementary helical structure reduced graphene oxide/silk fibroin composite electrode;
cutting the graphene oxide/silk fibroin composite film, fixing the film on a flat substrate, ensuring the surface of the film to be flat, placing the substrate on an optical platform of a laser, and adjusting the relative position of a laser light source and the surface of the substrate to focus laser on the surface of the film; inputting a preprocessing graph and processing parameters at an interface of a laser control program, and then performing laser direct writing to obtain a complementary helical structure reduced graphene oxide/silk fibroin composite electrode;
(4) preparing a pressure sensor with a spiral complementary structure;
and cutting the porous adhesive tape, fixing the silver wire on the electrode by using conductive silver adhesive, and clamping the porous adhesive tape between two complementary spiral reduced graphene oxide/silk fibroin composite electrodes to obtain the pressure sensor with a spiral complementary structure.
Further, the preparation in the step (1) comprises the following specific steps:
putting 15-30mL of graphene oxide solution with the concentration of 5-10mg/mL into a beaker with the measuring range of 100mL, then dropwise adding 2-5mL of sodium hydroxide solution with the concentration of 0.05-0.2mol/L to enable the pH value of the graphene oxide solution to be 7, then adding 2-6mL of silk fibroin solution with the concentration of 30-60mg/mL, then putting the beaker filled with the graphene oxide/silk fibroin mixture on a magnetic stirrer to stir for 10s-1min, and uniformly mixing to obtain the graphene oxide/silk fibroin mixed solution.
Further, the specific synthesis steps of the graphene oxide solution in the step (1) are as follows:
firstly, mixing graphite and sodium nitrate according to the mass ratio of 1: 1-1: 3 under the ice bath condition of 0-5 ℃, and then adding 90-100mL of concentrated sulfuric acid with the mass fraction of 98%; then 5-20g of potassium permanganate is added, and the mixture is stirred for 45-120min at the ice bath condition of 0-5 ℃ and the rotating speed of 500-; then heating to 35 ℃, keeping the temperature for 120min, adding 80ml of deionized water, heating to 95 ℃, keeping the temperature for 15min, and adding 200ml of deionized water, wherein the water injection time is 35min and 5min respectively; then adding 10mL of hydrogen peroxide with volume concentration of 30%, turning off heating and stirring for 5-15min, and then turning off stirring to naturally settle for 20-30 h; pouring out the supernatant after sedimentation, repeatedly diluting the acidic product with deionized water, centrifuging at the rotation speed of 8000-12000r/min for 10-20min, and repeating for 10-18 times until the pH value of the supernatant is 7; and finally, centrifuging the lower-layer product at the rotation speed of 1000-1500r/min for 10-20min, repeating for 3-5 times until no obvious black graphite particles visible to the naked eye exist, then centrifuging at the rotation speed of 8000-10000r/min for 15-20min, pouring out the supernatant, and shaking up to obtain the graphene oxide solution with the concentration of 5-10 mg/mL.
Further, the specific synthesis steps of the fibroin solution in the step (1) are as follows:
firstly, 6-9g of sodium carbonate powder is added into 3000-5000mL of deionized water, and is fully dissolved by using a glass rod or other stirring devices, and then the mixture is placed in a hot table or other heating devices for heating, so that the sodium carbonate solution keeps a boiling state. Then shearing the silkworm cocoon shell into 1-2cm area by using scissors or other cutting tools2Weighing 8-12g silkworm pieces by using a tray balance or other weighing instruments, putting the silkworm pieces into a boiling sodium carbonate solution, boiling for 20-50min, and taking out. And then preparing a part of boiling sodium carbonate solution with the same concentration by adopting the same method, then putting the silk into the newly prepared sodium carbonate solution to boil for 20-50min, taking out the silk, repeatedly soaking the silk into deionized water for 15-25 times, extruding out water, spreading the silk on an aluminum foil or other flat substrates, placing the silk on a fume hood or other dry and ventilated places for 20-30h, and naturally airing to obtain the silk fibroin fibers. And then 2-8g of dried silk fibroin fiber is put into a beaker, 15-25mL of lithium bromide solution with the concentration of 8-10mg/mL is absorbed by using a rubber head dropper or other sampling tools, and then the mixture is placed in a vacuum drying oven or other heating devices at 50-80 ℃ to be heated for 5-8h, so as to obtain dark yellow viscous liquid. Then pouring the viscous liquid into a dialysis bag with the molecular weight of 10000-18000, clamping the dialysis bag by using a clamp or other clamping tools, then placing the dialysis bag into a beaker filled with deionized water, dialyzing for 60-80h at the temperature of 0-10 ℃, replacing the deionized water every 10h to remove salt ions in the solution, and after the dialysis is finished, centrifuging for 15-30min at the rotating speed of 6000-12000r/min to obtain supernatant, namely the silk fibroin solution with the concentration of 30-60 mg/mL.
Further, the preparation in the step (2) comprises the following specific steps:
opening a switch of a suction filtration device, and fixing a purchased water system microporous filter membrane with the aperture of 0.2-0.25 μm and the diameter of 45-55mm below a suction filtration bottle; 3-5ml of deionized water is absorbed by using a rubber head dropper or other sampling tools and is dripped onto a water system microporous filter membrane, when the filter membrane is completely wetted by the deionized water, 10-15ml of graphene oxide/silk fibroin mixed solution is absorbed by using the rubber head dropper or other sampling tools and is subsequently dripped onto the water system microporous filter membrane, and after 12-15 hours, the graphene oxide/silk fibroin composite film with the thickness of 50-200 mu m is obtained.
Further, the specific processing steps in the step (2) are as follows:
fixing the filtered graphene oxide/silk fibroin composite membrane on a glass slide by using a 3M adhesive tape, and stripping the graphene oxide/silk fibroin composite membrane and a water system microporous filter membrane after completely airing; cutting a rectangle with the size of 5mm by 10mm-10mm by 20mm by using a pair of scissors; fixing the graphene oxide/silk fibroin composite film on a substrate with the thickness of 50mm x 1mm by using a fixing tool, wherein the area of a set processing area is 3mm x 6mm-8mm x 16mm, the distance between a laser head and the film is adjusted to be 8-12cm, and the laser focusing position is ensured to be the surface of the film; opening computer control software connected with a laser, adjusting relevant parameters such as line spacing, laser power and processing speed, inputting a preprocessed spiral structure pattern with the area of 3mm 6mm-8mm 16mm, adjusting an initial processing position, and ensuring that a processing area is positioned on the graphene oxide/silk fibroin composite film; processing to obtain a complementary helical structure reduced graphene oxide/silk fibroin composite electrode which is prepared by a laser direct writing method and has the area size of 3mm 6mm-8mm 16 mm; wherein the pore diameter of the nano-spiral structure part is 500nm-2 μm, the total number of turns of the spiral structure is 3-8 turns, the width of each turn of the spiral structure is 200-300 μm, and the spiral width of the unprocessed part is 100-200 μm.
Further, in computer control software connected with a laser, the used laser wavelength is 343nm, the laser power parameter is set to be 15% -20%, the line spacing is 0.005-0.01mm, the scanning speed is 200-500mm/s, and the processing frequency is 20-40kHz, so that the surface of the graphene oxide forms a complementary spiral structure.
Further, the specific steps for preparing the flexible pressure sensor with the spiral complementary structure in the step (3) are as follows:
firstly, a porous adhesive tape with the thickness of 2-3mm is cut into a rectangle with the size of 5mm 10mm-10mm 20mm by using a pair of scissors or other cutting tools, then a silver wire is fixed at the tail end of the complementary helical structure reduced graphene oxide/silk fibroin composite electrode by using conductive silver adhesive, the conductive silver adhesive is dried after 5-10min, and finally the porous adhesive tape is clamped between two complementary helical structure reduced graphene oxide/silk fibroin composite electrodes with the size of 5mm 10mm-10mm 20mm, so that the helical complementary structure pressure sensor can be successfully prepared.
The invention also aims to provide an application of the flexible pressure sensor with the complementary spiral structure prepared by laser processing in finger bending detection, in particular to an application of the flexible pressure sensor with the complementary spiral structure prepared by using 3M adhesive tape or other fixing devices to attach the pressure sensor with the spiral structure to an index finger joint (attached when a finger is straightened), then connecting wires at two ends of the pressure sensor with an LCR-6200 digital bridge tester, calibrating a bending angle at the index finger joint by using a protractor, and when the index finger joint is bent by 0 degrees, 30 degrees, 60 degrees and 90 degrees, the relative change (delta C/C) of the capacitance of the pressure sensor with the spiral structure prepared by laser processing0) In the range of 0-0.5; when the pressure sensor with the spiral complementary structure is bent on a finger, the formula is expressed by a parallel plate capacitor
Can be obtained (wherein epsilon)0Is a vacuum dielectric constant,. epsilonrDielectric layer dielectric constant, a is the relative area between two parallel plate electrodes, and d is the relative distance between two parallel plate electrodes), bending causes the distance between the upper and lower electrodes to become smaller, resulting in a larger capacitance. In addition, air with a smaller dielectric constant in the porous double-sided adhesive tape is extruded when the pressure sensor is bent, so that the dielectric constant of the dielectric layer is increased, the capacitance is increased, and the spiral complementary structure pressure sensor can accurately detect the bending degree of the finger under the combined action of the dielectric layer and the dielectric layer.
The third purpose of the invention is to provide a laser processing method for preparing a flexible pressure sensor with a complementary spiral structure for detecting the proximity of fingersIn the aspect of application, specifically, the spiral complementary structure pressure sensor is attached to a glass slide or other flat substrate by using 3M adhesive tape or other fixing devices, then wires at two ends of the spiral complementary structure pressure sensor are connected to an LCR-6200 digital bridge tester, and when a finger is 0-6cm away from the surface of an electrode on the sensor, the capacitance change value (C/C) of the spiral complementary structure pressure sensor is obtained0) Is 0.86-1.0.
For comparison, the capacitance change value (C/C) of the pressure sensor with the ring-disk structure at a finger distance of 0-6cm from the upper electrode surface of the sensor was measured by the same method0) The value is 0.9-1.01, which shows that the complementary helical structure sensor is more sensitive to the detection of the finger proximity; because the fringe electric field effect of parallel plate capacitor, can expand to the exterior space at fringe region electric field line, for the sensor of ring dish structure electrode, when the finger was close, the fringe electric field line of upper electrode top can be intercepted to the finger to reduce the electric field intensity between the upper and lower electrode, finally lead to the electric capacity to reduce. The electrode structure on the interface of the graphene electrode with the spiral complementary structure can be regarded as the superposition of a plurality of electrodes with ring-disc structures, so that the area of the edge area of the electrode is increased, and the expansion of more electric fields from the electrode plate area to the outer space is facilitated. Thus when a finger is in close proximity, the sensor exhibits a large change in capacitance, which is more sensitive to finger proximity.
Compared with the prior art, the invention has the following advantages:
(1) the composite film material 1-nano spiral structure 2 composite electrode with the complementary spiral structure is prepared by laser processing, so that the self-supporting reduced graphene oxide/silk fibroin composite film can be rapidly and finely reduced in any complex patterning;
(2) the graphene oxide solution, the silkworm cocoon and the porous double faced adhesive tape are used as raw materials, so that the method has the advantages of easiness in obtaining, low cost, good biocompatibility and the like;
(3) the composite film material 1-nano spiral structure 2 composite electrode prepared by laser processing is adopted, and the silk fibroin is modified by the graphene oxide, so that the composite electrode has the characteristics of excellent flexibility, strong ductility and the like, and has good mechanical tensile property;
(4) the multi-stage micro-nano structure sensor of the composite film material 1-nano spiral structure 2-porous material 3-nano spiral structure 2-composite film material 1, which is prepared by assembling the composite film material 1-nano spiral structure 2 composite electrode with the complementary spiral structure and the porous material 3 through laser processing, can realize the ultra-sensitive detection of two modes of object contact (finger bending) and non-contact (finger approaching).
Drawings
In order to more clearly illustrate the detailed description of the invention or the technical solutions in the prior art, the drawings that are needed in the detailed description of the invention or the prior art will be briefly described below. Throughout the drawings, like elements or portions are generally identified by like reference numerals. In the drawings, elements or portions are not necessarily drawn to scale.
FIG. 1 is a schematic structural diagram of a device for manufacturing a flexible pressure sensor with a complementary spiral structure based on laser processing according to the present invention;
FIG. 2 is a schematic diagram of a process for preparing a pressure sensor assembled by multistage micro-nano structures of a composite film material 1, a nano spiral structure 2, a porous material 3, a nano spiral structure 2 and a composite film material 1 based on laser processing;
FIG. 3 is a laser scanning confocal microscope image of a composite thin film material 1-nano helical structure 2 composite electrode local part in a pressure sensor with a complementary helical structure prepared based on laser processing according to the present invention;
FIG. 4 is a scanning electron microscope image of a pressure sensor assembled by multistage micro-nano structures of a composite film material 1, a nano spiral structure 2, a porous material 3, a nano spiral structure 2 and a composite film material 1 based on laser processing; wherein, (a) is a scanning electron microscope image of a sensor section consisting of a composite film material 1, a nano spiral structure 2, a porous material 3, a nano spiral structure 2 and a multi-stage micro-nano structure of the composite film material 1; (b) scanning electron microscope images of the composite film material 1 in the composite electrode of the composite film material 1-nano spiral structure 2 in the complementary spiral structure pressure sensor; (c) the method comprises the following steps of (1) reducing a scanning electron microscope image of a composite electrode of a composite film material 1-a nano spiral structure 2 by laser in a complementary spiral structure pressure sensor;
FIG. 5 is a graph of the relative change value of capacitance of a pressure sensor with a complementary spiral structure assembled by multistage micro-nano structures of a composite film material 1, a nano spiral structure 2, a porous material 3, a nano spiral structure 2 and a composite film material 1 based on laser processing, and the graph shows the change of the finger bending angle;
FIG. 6 is a schematic diagram of the distribution of an electric field around a pressure sensor with a complementary spiral structure, which is prepared by assembling a composite film material 1, a nano spiral structure 2, a porous material 3, a nano spiral structure 2 and a multi-level micro-nano structure of the composite film material 1 based on laser processing, when a finger approaches the pressure sensor;
fig. 7 is an image of a change value of capacitance along with a change in distance between a finger and an electrode on a sensor, which is obtained by assembling a multi-level micro-nano structure of a composite film material 1, a nano-spiral structure 2, a porous material 3, a nano-spiral structure 2, and a composite film material 1, to form a pressure sensor having a complementary spiral structure and a pressure sensor having a ring disk structure according to the present invention based on laser processing.
Detailed Description
The invention will be further described with reference to the accompanying drawings.
Example 1
A flexible pressure sensor with a complementary spiral structure is composed of an upper composite electrode, a lower composite electrode and a dielectric layer, wherein the composite electrodes are composed of a composite film material 1 and a nano spiral structure 2, the dielectric layer is a porous material 3, and the composite film material 1 is a surface smooth composite film material formed by mixing, filtering and forming a graphene oxide solution and a silk fibroin solution; the surface of the composite film material 1 is provided with a nano spiral structure 2, the outer surfaces of the composite film material 1 and the nano spiral structure 2 are adhered with a porous material 3, and the upper electrode, the lower electrode and the dielectric layer form a multi-stage micro-nano structure of the composite film material 1-the nano spiral structure 2-the porous material 3-the nano spiral structure 2-the composite film material 1.
When the nano spiral structure 2 is used for carrying out patterned reduction on the composite film material 1 by laser processing, a spiral patterning structure and a nano hole structure are formed simultaneously when oxygen-containing functional groups in the composite film are removed;
the thickness of the composite film material 1 is 50-200 μm.
The porous material 3 is a porous foam adhesive tape, a porous sponge, a ceramic porous material and the like.
The pore diameter of the nano spiral structure 2 is 500nm-2 μm, the total number of turns of the spiral structure is 3-8 turns, the width of each turn of the spiral structure is 200-300 μm, the spiral width of the unprocessed part is 100-200 μm, and the size of the whole spiral part is 0.3mm-0.8 mm.
Example 2
As shown in fig. 1, a method for manufacturing a flexible pressure sensor with a complementary spiral structure based on laser processing includes the following steps:
(1) preparing a graphene oxide/silk fibroin mixed solution;
20mL of graphene oxide solution with the concentration of 8mg/mL is sucked by a rubber head dropper and is placed into a beaker with the measuring range of 100mL, 3mL of sodium hydroxide solution with the concentration of 0.05mol/L is added dropwise to enable the pH value of the graphene oxide solution to be 7, 2mL of silk fibroin solution with the concentration of 40mg/mL is added, then the beaker filled with the graphene oxide/silk fibroin mixture is placed on a magnetic stirrer to be stirred for 10s-1min, and the graphene oxide/silk fibroin mixed solution is obtained after uniform mixing.
The graphene oxide solution is synthesized by using a Hummer's method, and the specific synthesis steps are as follows: firstly, mixing graphite and sodium nitrate according to a mass ratio of 1: 1, mixing under an ice bath condition at 0 ℃, and adding 90mL of concentrated sulfuric acid with the mass fraction of 98%; adding 7g of potassium permanganate, and stirring for 60min at the rotating speed of 800r/min under the ice bath condition of 0-5 ℃; then heating to 35 ℃, keeping the temperature for 120min, adding 80ml of deionized water, heating to 95 ℃, keeping the temperature for 15min, and adding 200ml of deionized water, wherein the water injection time is 35min and 5min respectively; then adding 10mL of hydrogen peroxide with the volume concentration of 30%, turning off heating and stirring for 10min, and then turning off stirring to naturally settle for 24 h; pouring out the supernatant after sedimentation, repeatedly diluting the acidic product with deionized water, centrifuging at the rotating speed of 12000r/min for 15min, and repeating for 15 times until the pH value of the supernatant is 7; and finally, centrifuging the lower-layer product at the rotating speed of 1000r/min for 10min, repeating the centrifuging for 3 times until no black graphite particles visible to naked eyes exist, then centrifuging at the rotating speed of 8000r/min for 15min, pouring out the supernatant, and shaking up to obtain the graphene oxide solution with the concentration of 8 mg/mL.
The silk fibroin solution used is prepared by the following specific steps: firstly, 8g of sodium carbonate powder is added into 5000mL of deionized water, the mixture is stirred by a glass rod to be fully dissolved, and then the mixture is placed on a hot table to be heated, so that the sodium carbonate solution keeps a boiling state. Then shearing the silkworm cocoon shell into 1cm area by using scissors2The silk shape of (2) is obtained by weighing 10g of silkworm pieces with a tray balance, putting into boiling sodium carbonate solution, boiling for 30min, and taking out. And then preparing a part of boiling sodium carbonate solution with the same concentration by adopting the same method, then putting the silk into the newly prepared sodium carbonate solution to boil for 30min, taking out the silk, repeatedly soaking the silk into deionized water for 20 times, extruding water, spreading the silk on an aluminum foil, placing the aluminum foil in a fume hood for 24h, and naturally airing to obtain the silk fibroin fiber. Then 6g of dried silk fibroin fiber was put into a beaker, 20mL of a 9mg/mL lithium bromide solution was pipetted using a rubber-tipped dropper, and the mixture was placed in a vacuum oven at 70 ℃ and heated for 5 hours to obtain a dark yellow viscous liquid. And then pouring the viscous liquid into a dialysis bag with the molecular weight of 14000, clamping the dialysis bag by using a clamp, then placing the dialysis bag into a beaker filled with deionized water, dialyzing for 72 hours at 4 ℃, replacing the deionized water every 10 hours, removing salt ions in the solution, centrifuging for 20 minutes at the rotating speed of 10000r/min after dialysis is finished, and taking supernatant, namely the silk fibroin solution with the concentration of 40 mg/mL.
(2) Preparing a graphene oxide/silk fibroin composite film;
selecting and clamping a water system (mixed cellulose) microporous filter membrane with a smooth surface, the diameter of 50mm and the aperture of 0.22 mu m by using tweezers, starting an oil-free diaphragm type vacuum pump, fixing the filter membrane on a funnel base, then covering a filter cup, and fixing the filter cup by using an aluminum clamp; 3ml of deionized water is absorbed by using a rubber head dropper with the capacity of 5ml and is completely dripped on the water system microporous filter membrane, when the filter membrane is in a completely wet state, 12ml of graphene oxide/silk fibroin mixed solution is absorbed by using the rubber head dropper with the capacity of 5ml and is dripped on the water system microporous filter membrane. And after 12 hours, obtaining the graphene oxide/silk fibroin composite film formed by the composite film material 1 with the thickness of 100 mu m.
(3) Processing the graphene oxide/silk fibroin composite film formed by the composite film material 1 by using a laser direct writing method to prepare a complementary helical structure reduced graphene oxide/silk fibroin composite electrode;
the laser wavelength of the ultraviolet laser used by the invention is 343nm, and the power, the line spacing, the scanning speed and the processing frequency of the laser have high adjustability; fixing the filtered graphene oxide/silk fibroin composite membrane on a glass slide by using a 3M adhesive tape, and manually stripping the graphene oxide/silk fibroin composite membrane and a microporous filter membrane after completely airing; cutting a rectangle with the size of 8mm by 16mm by using a pair of scissors; fixing the graphene oxide/silk fibroin composite film on a substrate of 50mm by 1mm by using a 3M adhesive tape, wherein the set processing area is 6mm by 12 mm; when the distance between the laser head and the film is adjusted to be 10cm, laser is focused on the surface of the film; opening computer control software connected with a laser, setting the laser power to be 20%, the line spacing to be 0.01, the scanning speed to be 500mm/s, the processing frequency to be 40Hz, inputting a preprocessed spiral structure pattern, adjusting the initial processing position, and ensuring that a processing area is positioned on the graphene oxide/silk fibroin composite film; and processing to obtain the complementary helical structure reduced graphene oxide/silk fibroin composite electrode which is prepared by the composite film material 1 prepared by the laser direct writing method with the area size of 6mm x 12mm and is formed by the nano helical structure 2. Wherein the aperture of the nano-spiral structure part is 1 μm, the total number of turns of the spiral structure is 6 turns, the width of each turn of the spiral structure is 250 μm, and the spiral width of the unprocessed part is 125 μm.
(4) Preparing a flexible pressure sensor with a spiral complementary structure;
cutting a porous adhesive tape with the thickness of 2.65mm (the thickness is obtained by a cross-sectional scanning electron microscope image of a device in fig. 4 (a)) into a rectangle with the size of 6mm × 12mm by using a scissors, fixing silver wires with the diameter of 0.1mm at two ends of a complementary helical structure reduced graphene oxide/silk fibroin composite electrode by using conductive silver adhesive, drying the conductive silver adhesive after 5min, and finally clamping the porous adhesive tape between two helical complementary graphene electrodes with the size of 6mm × 12mm to successfully prepare the pressure sensor with the complementary helical structure assembled by the multistage micro-nano structures of the composite film material 1-the nano helical structure 2-the porous material 3-the nano helical structure 2-the composite film material 1.
Fig. 1 and fig. 2 are schematic diagrams of a device structure and a preparation process of the present invention, respectively, and it can be seen from the diagrams that the operation process is simple and the complicated and tedious processing process is avoided;
fig. 3 and 4 show the surface morphology of the reduced graphene oxide/silk fibroin composite electrode formed by the patterned composite thin film material 1-the nano-helical structure 2 in the helical complementary structure pressure sensor and the microstructure of the overall structure of the device; the thickness of the complementary spiral structure pressure sensor assembled by the multistage micro-nano structures of the composite film material 1, the nano spiral structure 2, the porous material 3, the nano spiral structure 2 and the composite film material 1 is 2.65 mm.
Example 3
The embodiment provides an application of a flexible pressure sensor with a complementary spiral structure in finger bending detection based on laser processing, which comprises the following specific steps:
firstly, a pressure sensor with a spiral complementary structure is attached to an index finger joint (attached when a finger is straightened) by using a 3M adhesive tape, then wires at two ends of the pressure sensor with the spiral complementary structure are connected to an LCR-6200 digital bridge tester, a protractor is used for calibrating the bending angle of the index finger joint, and when the finger joint is bent by 0 degree, 30 degrees, 60 degrees and 90 degrees, the capacitance of the pressure sensor with the spiral complementary structure is relatively changed (delta C/C)0) 0, 0.21, 0.33, 0.48 respectively; when the finger is bent, the finger is electrically connected with the parallel plateContainer with a lid
It can be obtained that the distance d between the upper and lower electrodes is reduced when bending, and air with smaller dielectric constant in the porous double-sided adhesive tape is extruded out, so that the dielectric constant epsilon of the dielectric layerrThe size of the pressure sensor is increased, and the pressure sensor with the complementary spiral structure can realize accurate detection of the bending degree of the fingers under the combined action of the two parts;
FIG. 5 shows that when a pressure sensor with a spiral complementary structure, which is formed by assembling a composite film material 1, a nano spiral structure 2, a porous material 3, a nano spiral structure 2 and a multi-stage micro-nano structure of the composite film material 1, is attached to a finger joint, the relative capacitance change of the sensor is related to the change of the bending angle of a finger, and the larger the bending degree of the finger is, the larger the change value of the capacitance is;
example 4
The embodiment provides an application of a flexible pressure sensor with a complementary spiral structure in finger proximity detection based on laser processing, which comprises the following specific steps: attaching the pressure sensor with the spiral complementary structure on a glass slide by using a 3M adhesive tape, connecting wires at two ends of the pressure sensor with the LCR-6200 digital bridge tester, and respectively measuring the capacitance change value (C/C) of the pressure sensor with the spiral complementary structure when the finger is 6cm, 4cm, 2cm and 0.1cm away from the upper surface of the pressure sensor0) 0.99, 0.98, 0.93 and 0.86 respectively. For comparison, the pressure sensor with the ring-disk structure was measured using the same method, and the capacitance change value (C/C) of the pressure sensor with the ring-disk structure was measured when the finger was located 6cm, 4cm, 2cm, and 0.1cm from the upper surface of the sensor, respectively0) 1.01, 0.99, 0.95 and 0.9 respectively, and the comparison result is shown in fig. 6, so that the complementary helical structure sensor is more sensitive to the detection of the finger proximity; based on the fringe field effect of the parallel plate capacitor, the electric field lines in the fringe region will extend to the external space, as shown in fig. 6, for the sensor with the ring-plate structure electrode, when a finger approaches, the finger will intercept the fringe field lines above the upper electrode, thereby reducing the electric field intensity between the upper and lower electrodes, and the electric charges stored in the capacitorDecrease, ultimately resulting in a decrease in capacitance. The reduced graphene oxide/silk fibroin composite electrode with the spiral complementary structure has the advantages that the electrode structure on the interface can be regarded as the superposition of a plurality of ring-disk structure electrodes, the edge area of the electrode is increased, and the expansion of more electric fields from the electrode plate area to the outer space is facilitated. Thus when a finger is in close proximity, the sensor exhibits a large change in capacitance, which is more sensitive to finger proximity.
FIG. 6 is a schematic diagram of the distribution of the fringe electric fields around the finger and the sensor when the finger is in proximity over the sensor;
FIG. 7 is a schematic diagram of the capacitance variation of two different electrode structures (composite thin film material 1-nano-helix structure 2 electrode structure, ring disc electrode structure) when a finger approaches the upper surface of the sensor, as a function of the vertical distance between the finger and the upper surface of the sensor, wherein the sensor of the composite thin film material 1-nano-helix structure 2 electrode structure is more sensitive to the proximity of the finger and has a larger diffusion of the fringe electric field to the outer space;
the preferred embodiments of the present invention have been described in detail with reference to the accompanying drawings, however, the present invention is not limited to the specific details of the above embodiments, and various simple modifications can be made to the technical solution of the present invention within the technical idea of the present invention, and these simple modifications are within the protective scope of the present invention.
It should be noted that the various technical features described in the above embodiments can be combined in any suitable manner without contradiction, and the invention is not described in any way for the possible combinations in order to avoid unnecessary repetition.
In addition, any combination of the various embodiments of the present invention is also possible, and the same should be considered as the disclosure of the present invention as long as it does not depart from the spirit of the present invention.
Claims (10)
1. The flexible pressure sensor with the complementary spiral structure is characterized by comprising an upper composite electrode, a lower composite electrode and a dielectric layer, wherein the composite electrodes comprise a composite film material (1) and a nano spiral structure (2), the dielectric layer is a porous material (3), and the composite film material (1) is a smooth-surface composite film material formed by mixing and suction-filtering a graphene oxide solution and a silk fibroin solution; the surface of the composite film material (1) is provided with a nano spiral structure (2), the outer surfaces of the composite film material (1) and the nano spiral structure (2) are adhered with a porous material (3), and the upper electrode, the lower electrode and the dielectric layer form a multi-stage micro-nano structure of the composite film material (1) -the nano spiral structure (2) -the porous material (3) -the nano spiral structure (2) -the composite film material (1).
2. The flexible pressure sensor with complementary helical structures as claimed in claim 1, wherein the thickness of the composite film material (1) is 50-200 μm, the pore diameter of the nano-helical structure (2) is 500nm-2 μm, the total number of turns of the helical structure is 3-8 turns, the width of each turn of the helical structure is 200-300 μm, the width of the helical structure at the unprocessed part is 100-200 μm, and the size of the whole portion of the helix is 0.3mm-0.8 mm; the porous material (3) is a porous foam adhesive tape, a porous sponge or a ceramic porous material.
3. The method for preparing a flexible pressure sensor with a complementary spiral structure according to claim 1, comprising the following steps:
(1) preparing a graphene oxide/silk fibroin mixed solution;
dropwise adding a sodium hydroxide solution into a certain amount of graphene oxide solution to keep the graphene oxide solution neutral, and then mixing the graphene oxide solution with a silk fibroin solution to prepare a graphene oxide/silk fibroin mixed solution;
(2) preparing a graphene oxide/silk fibroin composite film;
firstly fixing a microporous filter membrane on a suction filtration device, wetting the filter membrane by deionized water, and finally dripping a graphene oxide/silk fibroin mixed solution for suction filtration, thereby successfully preparing a graphene oxide/silk fibroin composite film;
(3) processing the graphene oxide/silk fibroin composite film by using a laser direct writing method to prepare a complementary helical structure reduced graphene oxide/silk fibroin composite electrode;
cutting the graphene oxide/silk fibroin composite film, fixing the film on a flat substrate, ensuring the surface of the film to be flat, placing the substrate on an optical platform of a laser, and adjusting the relative position of a laser light source and the surface of the substrate to focus laser on the surface of the film; inputting a preprocessing graph and processing parameters at an interface of a laser control program, and then performing laser direct writing to obtain a complementary helical structure reduced graphene oxide/silk fibroin composite electrode;
(4) preparing a pressure sensor with a spiral complementary structure;
and cutting the porous adhesive tape, fixing the silver wire on the electrode by using conductive silver adhesive, and clamping the porous adhesive tape between two complementary spiral reduced graphene oxide/silk fibroin composite electrodes to obtain the pressure sensor with a spiral complementary structure.
4. The method for preparing a flexible pressure sensor with a complementary spiral structure according to claim 3, wherein the specific steps of the preparation in the step (1) are as follows:
putting 15-30mL of graphene oxide solution with the concentration of 5-10mg/mL into a beaker with the measuring range of 100mL, then dropwise adding 2-5mL of sodium hydroxide solution with the concentration of 0.05-0.2mol/L to enable the pH value of the graphene oxide solution to be 7, then adding 2-6mL of silk fibroin solution with the concentration of 30-60mg/mL, then putting the beaker filled with the graphene oxide/silk fibroin mixture on a magnetic stirrer to stir for 10s-1min, and uniformly mixing to obtain the graphene oxide/silk fibroin mixed solution.
5. A method of manufacturing a flexible pressure sensor having a complementary helical structure according to claim 3,
the specific synthesis steps of the graphene oxide solution in the step (1) are as follows:
firstly, mixing graphite and sodium nitrate according to a mass ratio of 1: 1-1: 3, mixing under an ice bath condition at 0-5 ℃, and then adding 90-100mL of concentrated sulfuric acid with the mass fraction of 98%; then 5-20g of potassium permanganate is added, and the mixture is stirred for 45-120min at the ice bath condition of 0-5 ℃ and the rotating speed of 500-; then heating to 35 ℃, keeping the temperature for 120min, adding 80ml of deionized water, heating to 95 ℃, keeping the temperature for 15min, and adding 200ml of deionized water, wherein the water injection time is 35min and 5min respectively; then adding 10mL of hydrogen peroxide with volume concentration of 30%, turning off heating and stirring for 5-15min, and then turning off stirring to naturally settle for 20-30 h; pouring out the supernatant after sedimentation, repeatedly diluting the acidic product with deionized water, centrifuging at the rotation speed of 8000-12000r/min for 10-20min, and repeating for 10-18 times until the pH value of the supernatant is 7; finally, centrifuging the lower-layer product at the rotating speed of 1000-;
the specific synthesis steps of the fibroin solution in the step (1) are as follows:
firstly, 6-9g of sodium carbonate powder is added into 3000-5000mL of deionized water, and is fully dissolved by using a glass rod or other stirring devices, and then the mixture is placed in a hot table or other heating devices for heating, so that the sodium carbonate solution keeps a boiling state. Then shearing the silkworm cocoon shell into 1-2cm area by using scissors or other cutting tools2Weighing 8-12g silkworm pieces by using a tray balance or other weighing instruments, putting the silkworm pieces into a boiling sodium carbonate solution, boiling for 20-50min, and taking out. And then preparing a part of boiling sodium carbonate solution with the same concentration by adopting the same method, then putting the silk into the newly prepared sodium carbonate solution to boil for 20-50min, taking out the silk, repeatedly soaking the silk into deionized water for 15-25 times, extruding out water, spreading the silk on an aluminum foil or other flat substrates, placing the silk on a fume hood or other dry and ventilated places for 20-30h, and naturally airing to obtain the silk fibroin fibers. Then 2-8g of dry silk fibroin fiber is put into a beaker, 15-25mL of lithium bromide solution with the concentration of 8-10mg/mL is absorbed by using a rubber head dropper or other sampling tools, and then the mixture is mixedHeating the mixture in a vacuum drying oven or other heating device at 50-80 deg.C for 5-8 hr to obtain dark yellow viscous liquid. Then pouring the viscous liquid into a dialysis bag with the molecular weight of 10000-18000, clamping the dialysis bag by using a clamp or other clamping tools, then placing the dialysis bag into a beaker filled with deionized water, dialyzing for 60-80h at the temperature of 0-10 ℃, replacing the deionized water every 10h to remove salt ions in the solution, and after the dialysis is finished, centrifuging for 15-30min at the rotating speed of 6000-12000r/min to obtain supernatant, namely the silk fibroin solution with the concentration of 30-60 mg/mL.
6. The method for preparing a flexible pressure sensor with a complementary spiral structure according to claim 3, wherein the specific steps of the preparation in the step (2) are as follows:
opening a switch of a suction filtration device, and fixing a purchased water system microporous filter membrane with the aperture of 0.2-0.25 μm and the diameter of 45-55mm below a suction filtration bottle; 3-5ml of deionized water is absorbed by using a rubber head dropper or other sampling tools and is dripped onto a water system microporous filter membrane, when the filter membrane is completely wetted by the deionized water, 10-15ml of graphene oxide/silk fibroin mixed solution is absorbed by using the rubber head dropper or other sampling tools and is subsequently dripped onto the water system microporous filter membrane, and after 12-15 hours, the graphene oxide/silk fibroin composite film with the thickness of 50-200 mu m is obtained.
7. The method for preparing a flexible pressure sensor with a complementary spiral structure according to claim 3, wherein the specific processing steps in the step (2) are as follows:
fixing the filtered graphene oxide/silk fibroin composite membrane on a glass slide by using a 3M adhesive tape, and stripping the graphene oxide/silk fibroin composite membrane and a water system microporous filter membrane after completely airing; cutting a rectangle with the size of 5mm by 10mm-10mm by 20mm by using a pair of scissors; fixing the graphene oxide/silk fibroin composite film on a substrate with the thickness of 50mm x 1mm by using a fixing tool, wherein the area of a set processing area is 3mm x 6mm-8mm x 16mm, the distance between a laser head and the film is adjusted to be 8-12cm, and the laser focusing position is ensured to be the surface of the film; opening computer control software connected with a laser, adjusting relevant parameters such as line spacing, laser power and processing speed, inputting a preprocessed spiral structure pattern with the area of 3mm 6mm-8mm 16mm, adjusting an initial processing position, and ensuring that a processing area is positioned on the graphene oxide/silk fibroin composite film; processing to obtain a complementary helical structure reduced graphene oxide/silk fibroin composite electrode which is prepared by a laser direct writing method and has the area size of 3mm 6mm-8mm 16 mm; wherein the aperture of the nano-spiral structure part is 500nm-2 μm, the total number of turns of the spiral structure is 3-8 turns, the width of each turn of the spiral structure is 200-300 μm, and the spiral width of the unprocessed part is 100-200 μm; in computer control software connected with a laser, the used laser wavelength is 343nm, the laser power parameter is set to be 15-20%, the line spacing is 0.005-0.01mm, the scanning speed is 200-500mm/s, and the processing frequency is 20-40kHz, so that the surface of the graphene oxide forms a complementary spiral structure.
8. The method for preparing a flexible pressure sensor with a complementary spiral structure according to claim 3, wherein the step (3) for preparing the flexible pressure sensor with a complementary spiral structure comprises the following specific steps:
firstly, a porous adhesive tape with the thickness of 2-3mm is cut into a rectangle with the size of 5mm 10mm-10mm 20mm by using a pair of scissors or other cutting tools, then a silver wire is fixed at the tail end of the complementary helical structure reduced graphene oxide/silk fibroin composite electrode by using conductive silver adhesive, the conductive silver adhesive is dried after 5-10min, and finally the porous adhesive tape is clamped between two complementary helical structure reduced graphene oxide/silk fibroin composite electrodes with the size of 5mm 10mm-10mm 20mm, so that the helical complementary structure pressure sensor can be successfully prepared.
9. The use of a flexible pressure sensor with complementary helical structure for finger bending detection as claimed in claim 1, wherein the helical structure pressure sensor is attached to the knuckle of the index finger using 3M tape or other fastening means, and then the two wires of the helical structure pressure sensor are connected to LCR-6200 digital bridge testerThe bending angle of the index finger joint is calibrated by using the protractor, and when the index finger joint is bent by 0 degrees, 30 degrees, 60 degrees and 90 degrees, the relative change (delta C/C) of the capacitance of the pressure sensor with the spiral complementary structure is realized0) The range is 0-0.5.
10. The use of a flexible pressure sensor with complementary helical structures for finger proximity detection as claimed in claim 1, wherein the pressure sensor is attached to a glass slide or other flat substrate using 3M tape or other fastening means, and then the two ends of the pressure sensor are wired to LCR-6200 digital bridge tester, wherein the capacitance of the pressure sensor changes (c/c) when the finger is 0-6cm away from the top electrode surface of the sensor0) Is 0.86-1.0.
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