CN110926663A - Preparation method of washable wearable high-sensitivity pressure sensor - Google Patents
Preparation method of washable wearable high-sensitivity pressure sensor Download PDFInfo
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- CN110926663A CN110926663A CN201911222483.9A CN201911222483A CN110926663A CN 110926663 A CN110926663 A CN 110926663A CN 201911222483 A CN201911222483 A CN 201911222483A CN 110926663 A CN110926663 A CN 110926663A
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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
- G01L1/14—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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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y15/00—Nanotechnology for interacting, sensing or actuating, e.g. quantum dots as markers in protein assays or molecular motors
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/31—Coating with metals
- C23C18/42—Coating with noble metals
- C23C18/44—Coating with noble metals using reducing agents
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/0007—Electro-spinning
- D01D5/0015—Electro-spinning characterised by the initial state of the material
- D01D5/003—Electro-spinning characterised by the initial state of the material the material being a polymer solution or dispersion
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/0007—Electro-spinning
- D01D5/0061—Electro-spinning characterised by the electro-spinning apparatus
- D01D5/0069—Electro-spinning characterised by the electro-spinning apparatus characterised by the spinning section, e.g. capillary tube, protrusion or pin
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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
- G01L9/12—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
Abstract
The invention relates to a preparation method of a washable wearable high-sensitivity pressure sensor. The method comprises the following steps: carrying out electrostatic spinning on spinning solution containing a palladium source and PAN, and then carrying out chemical silvering; and taking the obtained conductive nanofiber membrane electrode as an upper layer and a lower layer, connecting a lead, taking the middle layer as a dielectric layer, and packaging. The sensor is wearable and still has high sensitivity after being washed by water. The method is simple in process, the obtained sensor is wearable, still has high sensitivity after being washed, is light, thin, flexible, high in accuracy and high in fatigue resistance, and plays an important role in the field of artificial intelligence.
Description
Technical Field
The invention belongs to the field of pressure sensor preparation, and particularly relates to a preparation method of a washable wearable high-sensitivity pressure sensor.
Background
Along with the improvement of science and technology level, the sensor plays important role in artificial intelligence development in the future, and people have realized through nanotechnology and flexible electronic technology that pressure sensor develops to flexible, wearable and washing direction, and the sensor flexibility gradually becomes the trend and the direction of development, has more application in aspects such as medical health, human skill detection, real-time feedback.
Pressure sensors are generally divided into three types: the pressure sensor comprises a resistance type pressure sensor, a piezoelectric type pressure sensor and a capacitance type pressure sensor, wherein the capacitance type pressure sensor responds to capacitance change caused by external pressure change and converts the capacitance change into an electric signal for output, and the pressure sensor has the advantages of good dynamic response, stable signal output, low power consumption, severe condition resistance and the like, and is widely welcomed.
The flexible sensor designed at present needs to be adjusted for the problems of sensitivity improvement, monitoring range increase, process simplification, cost reduction and the like under the condition of ensuring relatively light, thin and flexible and simple production process. Therefore, the problem of how to improve the sensitivity of the sensor has been increasingly emphasized. Liu nationality china's china (CN 106959176A) designed a and used gold nanorod to imbed PDMS as the electrode, and the polyurethane is the capacitive pressure sensor of dielectric layer, can improve the sensitivity of low pressure intensity state to a certain extent, but the gold nanorod of coating most distributes on the electrode top layer, and the content is less, and the cost is relatively great. A conductive polymer embedded wire made of poly (3, 4-ethylenedioxythiophene) and polystyrene sulfonate of Li Yang (CN109781311A) is used as an electrode, polymer polyvinylidene fluoride-hexafluoropropylene and graphene quantum dots are used as a composite material to be used as a dielectric layer, a novel composite material microstructure array is prepared to form a sawtooth structure, and the sawtooth structure has the advantages of good sensitivity, small hysteresis and good repeatability.
Disclosure of Invention
The invention aims to solve the technical problem of providing a preparation method of a water-washable wearable high-sensitivity flexible capacitive pressure sensor, so as to overcome the defects of low sensitivity, complicated preparation steps and the like of the capacitive pressure sensor in the prior art.
The invention provides a preparation method of a capacitive pressure sensor, which comprises the following steps:
(1) carrying out electrostatic spinning on spinning solution containing a palladium source and PAN to obtain a nanofiber membrane, and then carrying out chemical silver plating to obtain a conductive nanofiber membrane electrode;
(2) and (2) taking the conductive nanofiber membrane electrode in the step (1) as an upper layer and a lower layer, connecting a lead, taking the middle layer as a dielectric layer, and packaging to obtain the capacitive pressure sensor.
In the step (1), the content of the palladium source in the spinning solution is 1.0-2.0 ppm, the PAN concentration is 8-10% wt, and the solvent is DMF.
The electrostatic spinning process parameters in the step (1) are as follows: the diameter of the spray head is 0.6-0.7 mm, the receiving distance is 10-20 cm, the propelling speed is 6.0-7.0 ml/h, the applied voltage is 15-20 kv, and the electrostatic spinning time is 8-12 h.
In the step (1), the palladium source is PdCl2。
The chemical silver plating in the step (1) comprises the following steps: and (3) immersing the nanofiber membrane into a reducing solution, adding a silver plating solution, and reacting for 30-50 min under an ultrasonic condition. Electroless silver plating is a common electroless plating recipe.
The dielectric layer in the step (2) is plastic, polyvinylidene fluoride (PVDF), Polydimethylsiloxane (PDMS) or nylon net, preferably nylon net.
The access wire in the step (2) is as follows: one end of the lead is attached to the surface of the conductive nanofiber membrane electrode, and then the lead is coated with silver paste and cured. The lead is firmly fixed on the electrode.
And (3) in the step (2), the package adopts polydimethylsiloxane PDMS, polyvinyl chloride PVC, EPOXY resin EPOXY, thermoplastic polyurethane elastomer TPU, polyvinylidene fluoride PVDF or polyimide PI, preferably polyimide PI.
The effective overlapping area of the upper layer and the lower layer of the electrodes in the step (2) is 2.2 multiplied by 2.3 mm.
In the step (2), the mass of the capacitive pressure sensor is 345mg, and the thickness of the capacitive pressure sensor is 0.57 mm.
The capacitive pressure sensor in the step (2) adopts a classic sandwich structure.
The invention also provides the capacitive pressure sensor prepared by the method.
The invention also provides application of the capacitive pressure sensor prepared by the method.
The invention designs a flexible porous nanofiber membrane electrode with good conductivity through electrostatic spinning and chemical plating, and a simple capacitive pressure sensor is formed by taking an easily-obtained nylon net as a dielectric layer, and the sensitivity of the capacitive pressure sensor is greatly improved through testing.
Advantageous effects
The invention has simple preparation process, easily obtained raw materials, regular and uniform dielectric layer, easy preparation of the electrode and the dielectric layer, high repetition rate of the assembled pressure sensor, short production period, sensitive reaction on pressure change through capacitance change, and basically no reduction of sensitivity after washing; and the nano fiber membrane has the characteristics of lightness, thinness and flexibility, can be worn for washing, and has more applications in the aspects of human health monitoring, motion detection, joint movement and the like. Meanwhile, the invention provides a selection of the electrode and the dielectric layer of the capacitor and a convenient assembly mode.
Drawings
Fig. 1 is a schematic structural diagram and a flow chart of the capacitive pressure sensor according to the present invention.
Fig. 2 is a sensitivity curve of the capacitive pressure sensor in example 1.
Fig. 3 is a scanning electron microscope image of the electrode layer of the capacitive pressure sensor in embodiment 1 of the present invention.
Fig. 4 is a scanning electron microscope image of the dielectric layer of the capacitive pressure sensor in embodiment 1 of the present invention.
Detailed Description
The invention will be further illustrated with reference to the following specific examples. It should be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present invention. Further, it should be understood that various changes or modifications of the present invention may be made by those skilled in the art after reading the teaching of the present invention, and such equivalents may fall within the scope of the present invention as defined in the appended claims.
In the examples of the present invention, N-dimethylformamide (DMF 99.5%) was purchased from shanghai Linfeng Chemicals Co., Ltd, absolute ethanol was purchased from shanghai and Chemicals Co., Ltd, polyacrylonitrile (PAN, Mw 150,000) was purchased from Wasabau group in china, Anhui, and palladium chloride, silver nitrate, polyethylene glycol 1540, glucose, and ethylenediamine were purchased from Wasabai Chemicals Co., Ltd. All chemicals were analytical grade reagents and were used without further purification.
Example 1
(1) Taking 0.17mgPdCl2And 100ml of DMF are prepared into a 1.7ppm solution, 0.8g of PAN powder is dissolved in 10ml of palladium solution to prepare a spinning solution, the spinning solution is added into an injector, certain spinning parameters are set for spinning, the diameter of a nozzle is set to be 0.67mm, the receiving distance is 15cm, the advancing speed is 6.5ml/h, the applied voltage is 18kv, and the electrostatic spinning time is 10h, so that the nanofiber membrane is obtained.
(2) 1.5g of glucose and 60mg of polyethylene glycol were dissolved in 3ml of ethanol and 47ml of deionized water to prepare 50ml of a reducing solution. With 0.8g silver nitrate (AgNO)3) Preparing 8g/L AgNO with deionized water3Aqueous ammonia (about 0.6ml) was added dropwise to the solution until the solution became clear from turbidity to give a silver ammonia solution, and 1ml of ethylenediamine was added. Firstly, useAnd immersing the nanofiber membrane into a reducing solution, then quickly pouring into a silver plating solution, reacting for 40min under an ultrasonic condition, and drying to obtain the conductive nanofiber membrane.
(3) Assembling a sensor: the capacitive pressure sensor is composed of a three-layer structure, the conductive nanofiber membrane in the step (2) is used as an upper electrode and a lower electrode, one end of a conductive copper wire is attached to the surface of the electrodes, a layer of silver paste is uniformly coated on the copper wire through an injector, then the conductive silver paste is solidified for 1h in an oven at 90 degrees, a nylon net layer is selected as a dielectric layer in the middle layer, the effective overlapping area is 2.2cm multiplied by 2.3cm, the three layers are combined, and packaging is carried out through PI adhesive tapes so as to serve as the capacitive pressure sensor. Testing the capacitance value of the sensor under different pressures to obtain corresponding C, and obtaining the capacitance value of the sensor when the capacitance value is C-C0That is, the capacitance change Δ C, the sensitivity is calculated by the sensitivity calculation formula S ═ d Δ C/d P, as shown in fig. 2 and table 1.
Example 2
According to example 1, the time of electroless plating under ultrasound in step (2) of example 1 was changed to 30min, and the rest was the same as in example 1, to obtain a capacitive pressure sensor. The capacitance value of the sensor was measured, and the sensitivity was calculated from the sensitivity S ═ d Δ C/d P, and the sensitivity was as shown in table 1.
Example 3
And (3) disassembling the electrode and the dielectric layer of the capacitive pressure sensor in the embodiment 1, washing with water, performing ultrasonic water washing for 2min, drying, circulating for 10 times, and assembling according to the embodiment 1 to obtain the capacitive pressure sensor. The capacitance value of the sensor was measured, the sensitivity was calculated from the sensitivity S ═ d Δ C/d P, and the change in performance after washing with water was detected as shown in table 1.
Comparative example 1
According to Chinese patent CN109781311A, a conducting layer is made of poly (3, 4-ethylenedioxythiophene) and polystyrene sulfonate, synthetic polymers of polyvinylidene fluoride-hexafluoropropylene and graphene quantum dots are used as composite dielectric layers, and a substrate adopts PI to manufacture the flexible capacitive pressure sensor.
Table 1:
as can be seen from table 1, the capacitive pressure sensor assembled in example 1 is in a small pressure range (<1kPa) sensitivity of 1.43kPa-1Sensitivity of 0.12kPa in the large pressure range (1-10kPa)-1. Whereas the capacitive pressure sensor in example 2 is in a small pressure range (<1kPa) sensitivity of 1.14kPa-1Sensitivity of 0.11kPa in the large pressure range (1-10kPa)-1. It can be seen that the silver plating time is long in the embodiment 1, the square resistance value is 1.5 omega/□, the electrode conductivity is good, and the sensitivity is higher in the low-pressure range, while the silver plating time is short in the embodiment 2, the square resistance value is 62.4 omega/□, the electrode conductivity is poor, the sensitivity is slightly lower in the low-pressure range, but the responses of the two sensors are sensitive. And the conductivity influence of the electrode in a high-pressure range is reduced, and the sensitivity is closer.
Example 3 in a small pressure range when ultrasonically cleaned 10 times with distilled water (1:)<1kPa) sensitivity of 1.32kPa-1Sensitivity of 0.12kPa in the large pressure range (1-10kPa)-1. The assembled pressure sensor has certain washing capacity, the assembled pressure sensor can be disassembled, the dielectric layer serving as a nylon net can be washed by water as a fabric, the performance is not affected, and chemically plated nano fibers serving as a conductive layer can cause a certain amount of silver on the surface to fall off after washing by water, so that the low-pressure sensitivity is reduced, but the reduction degree is not large, the pressure sensor still shows good induction, and the sensitivity in a high-pressure range is basically unchanged.
In table 1, the inventive example is compared with comparative example CN109781311a, which uses a conductive polymer as an electrode and a composite material as a dielectric layer, and no specific sensitivity is given in the comparative example, but the rate of change of capacitance at different pressures is listed, and it can be calculated that the sensitivity at lower pressure of the comparative example is about 0.33kPa-1(<1kPa) less than the sensitivity of example 1 of the present invention in 1kPa due to the fact that the comparative example uses a conductive polymer as an electrode, does not structure the microstructure of the surface, the dielectric layer designs a saw-tooth microstructure by changing the dielectric layer's sensitivity when under pressureThe sensitivity is improved by changing, the manufacturing process is complex, the steps are multiple, and the cost is higher. The conductive nanofiber membrane electrode designed by the invention has a large number of microporous structures, and the silver completely wraps the nanofibers, so that the whole electrode has an obvious microstructure, the contact area of the electrode and a dielectric layer is greatly increased under pressure, the capacitance change is obvious, the sensitivity is high, and the nylon net material of the dielectric layer has a regular microstructure, and the nylon net material has the advantages of industrialization, easy obtainment, low cost and simple and convenient manufacturing process. The combined action of the electrodes and the dielectric layer brings about an increase in sensitivity.
Example 1 of the test of the present invention, FIG. 2 is a graph of the capacitance change of the sensor with pressure change in example 1, and the sensitivity of the capacitive sensor at low pressure is 1.43kPa-1Sensitivity in the high pressure range of 0.12kPa-1After testing, the pressure is still well identified and the fatigue resistance is high after 500 times of testing under 0.2 kPa. The invention has good low-voltage sensitivity because of the calculation formula according to the capacitance: c ═ epsilon a/d, the change in capacitance depends mainly on the dielectric constant epsilon, the relative area a of the plates and the change in the distance d between the plates. Therefore, as shown in the electrode layer scanning electron microscope of fig. 3, on the one hand, the capacitance change sensitivity of the invention is caused by the irregular staggered arrangement of the conductive layer nanofibers, the nanosilver is densely and uniformly distributed on the nanofibers and is in a coral-shaped structure, the number of the nanofibers directly contacting with the dielectric layer in unit area is small in no-load, when pressure is applied, the distance between the nanofibers is reduced, some nanofibers which are not in contact with the dielectric layer before are extruded and deformed to start to contact with the dielectric layer, the relative area a of the electrode is greatly increased, so that the capacitance change is fast, the pressure is continuously increased, the fiber shape is flattened, the area change increased on a single fiber is small, and therefore, the capacitance change is not obvious under large pressure, and the sensitivity is reduced.
On the other hand, as shown in fig. 4 of a dielectric layer scanning electron microscope, because the selected nylon meshes of the dielectric layer are regularly arranged, microscopic holes uniformly distributed exist in the middle, when a force is applied, the film extrudes the middle layer, so that the distance d between the middle layer is reduced, gaps are reduced, original holes are occupied by fibers, a certain proportion of smaller air dielectric constant is replaced by larger dielectric constant of the nylon meshes of the dielectric layer, and epsilon is increased, thereby causing faster capacitance change and increased sensitivity.
Claims (9)
1. A method of making a capacitive pressure sensor, comprising:
(1) carrying out electrostatic spinning on spinning solution containing a palladium source and PAN to obtain a nanofiber membrane, and then carrying out chemical silver plating to obtain a conductive nanofiber membrane electrode;
(2) and (2) taking the conductive nanofiber membrane electrode in the step (1) as an upper layer and a lower layer, connecting a lead, taking the middle layer as a dielectric layer, and packaging to obtain the capacitive pressure sensor.
2. The method according to claim 1, wherein the content of the palladium source in the dope in the step (1) is 1.0 to 2.0ppm, the PAN concentration is 8 to 10 wt%, and the solvent is N, N-dimethylethylenediamine DMF.
3. The method according to claim 1, wherein the electrostatic spinning in step (1) comprises the following process parameters: the diameter of a spray head is 0.6-0.7 mm, the receiving distance is 10-20 cm, the propelling speed is 6.0-7.0 ml/h, the applied voltage is 15-20 kv, and the electrostatic spinning time is 8-12 h; the palladium source is PdCl2。
4. The method according to claim 1, wherein the electroless silver plating in the step (1) is: and (3) immersing the nanofiber membrane into a reducing solution, adding a silver plating solution, and reacting for 30-50 min under an ultrasonic condition.
5. The method of claim 1, wherein the dielectric layer in step (2) is a plastic, polyvinylidene fluoride (PVDF), Polydimethylsiloxane (PDMS), or nylon mesh.
6. The method of claim 1, wherein the access conductors in step (2) are: one end of the lead is attached to the surface of the conductive nanofiber membrane electrode, and then the lead is coated with silver paste and cured.
7. The method of claim 1, wherein the encapsulation in step (2) is selected from polydimethylsiloxane PDMS, polyvinyl chloride PVC, EPOXY resin EPOXY, thermoplastic polyurethane elastomer rubber TPU, polyvinylidene fluoride PVDF or polyimide PI.
8. A capacitive pressure sensor made according to the method of claim 1.
9. Use of a capacitive pressure sensor prepared according to the method of claim 1.
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Cited By (5)
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| CN111307342A (en) * | 2020-04-08 | 2020-06-19 | 深圳大学 | High-temperature-resistant flexible pressure sensor and preparation method and application thereof |
| CN112161738A (en) * | 2020-09-17 | 2021-01-01 | 五邑大学 | Air pressure sensor and manufacturing method thereof |
| CN112903146A (en) * | 2021-01-22 | 2021-06-04 | 中国科学院重庆绿色智能技术研究院 | Preparation method and application of dermal-based flexible pressure sensor |
| CN113188711A (en) * | 2021-04-29 | 2021-07-30 | 苏州凝智新材料发展有限公司 | Pressure sensor and preparation method and application thereof |
| CN113776698A (en) * | 2021-08-09 | 2021-12-10 | 同济大学 | Flexible bionic electronic skin sensing mechanism |
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| CN113776698A (en) * | 2021-08-09 | 2021-12-10 | 同济大学 | Flexible bionic electronic skin sensing mechanism |
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