CN114754906A - Ultra-sensitive flexible pressure sensor inspired by biology and preparation method thereof - Google Patents
Ultra-sensitive flexible pressure sensor inspired by biology and preparation method thereof Download PDFInfo
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- CN114754906A CN114754906A CN202210267149.0A CN202210267149A CN114754906A CN 114754906 A CN114754906 A CN 114754906A CN 202210267149 A CN202210267149 A CN 202210267149A CN 114754906 A CN114754906 A CN 114754906A
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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
- G01L1/22—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 using resistance strain gauges
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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
Abstract
The invention relates to an ultrasensitive flexible pressure sensor inspired by biology and a preparation method thereof. For this film, a nano-scale polyaniline spiny array was uniformly distributed over a micro-scale polydimethylsiloxane columnar array. The structure can generate two times of interlocking effect when being subjected to external force, thereby ensuring the use range of the sensor and greatly improving the sensitivity. The preparation method comprises the following steps: (1) preparing a micron-sized polydimethylsiloxane columnar array; (2) preparing a nano-scale polyaniline thorn-shaped array; (3) an ultra-sensitive pressure sensor based on a hierarchical polyaniline/polydimethylsiloxane array was assembled. The product prepared by the invention has the advantages of ultrahigh sensitivity, ultralow detection limit, rapid response time, excellent cycle stability and excellent environmental adaptability, and the preparation method is simple, the process is mature, the environment is not polluted, and the product has considerable application prospects in the fields of human health monitoring, human-computer interaction and the like.
Description
Technical Field
The invention relates to an ultrasensitive pressure flexible sensor and a preparation method thereof, belonging to the technical field of preparation of flexible electronic materials.
Background
A pressure sensor is a device or apparatus that senses a pressure signal and converts the pressure signal into a usable output electrical signal according to a certain rule. The pressure sensor is the most common sensor in industrial practice, is widely applied to various industrial automatic control environments, and relates to a plurality of industries such as water conservancy and hydropower, railway traffic, intelligent buildings, production automatic control, aerospace, military industry, petrochemical industry, oil wells, electric power, ships, machine tools, pipelines and the like.
The traditional pressure sensor usually uses a micro-electro-mechanical system sensor, the stability is good, the testing precision is relatively high, but the application of the traditional pressure sensor in the fields of human physiological signal monitoring, human-computer interaction and the like is greatly limited due to the high rigidity. In recent years, flexible pressure sensors based on organic polymers have received much attention due to their great application prospects in the field of artificial skin.
The flexible pressure sensor can be roughly divided into four types, namely a compression resistance type, a capacitance type, a piezoelectric type and a friction type according to different sensing mechanisms of the flexible pressure sensor, wherein the compression resistance type is concerned by a plurality of scientific researchers due to simple preparation process and principle. However, the conventional composite compression resistance type flexible pressure sensor often has performance defects of long response time, poor temperature stability and the like due to the problems of filler dispersibility, inherent viscoelasticity of resin and the like, so that it is necessary to design a compression resistance type flexible pressure sensor with high sensitivity, short response time and good environmental stability. Accordingly, the present invention is generally directed to the design and fabrication of a flexible pressure sensor having a biomimetic hierarchical structure.
Disclosure of Invention
The invention aims to provide a biologically inspired ultrahigh-sensitivity flexible pressure sensor and a preparation method thereof. The invention has ultrahigh sensitivity, can realize ultralow detection limit, quick response time and excellent circulation stability, and has continuous and stable monitoring capability on large-amplitude muscle movement of a human body and tiny vital signs such as pulse, respiration and the like. In addition, the sensor can show good environmental stability in different humidity and temperature environments, and application scenes of the sensor in various fields are greatly widened. Meanwhile, the preparation process has the technical advantages of simplicity and environmental protection, and has good theoretical research and practical application values by combining the mature film preparation processes such as casting, spin coating and the like at present.
The invention provides a biologically inspired ultrasensitive flexible pressure sensor, which is formed by assembling two hierarchical composite structure films of polydimethylsiloxane microcolumns/polyaniline nano spines with the same structure in a face-to-face mode, and the thickness of the ultrasensitive flexible pressure sensor is 160-1000 mu m.
The invention provides a method for preparing an ultrasensitive flexible pressure sensor inspired by biology, which comprises the following specific steps:
(1) curing polydimethylsiloxane on a glass substrate for 1-6 hours at the temperature of 60-90 ℃ through a curing agent to obtain polydimethylsiloxane resin;
(2) preparing a microsphere template by taking microspheres as a sacrificial layer, and heating the microsphere template in an oven at 220 ℃ to obtain a densely arranged microsphere template sacrificial layer;
(3) adding 1-3 g of mixed solution consisting of an organic diluent and the polydimethylsiloxane resin obtained in the step (1) to the microsphere template sacrificial layer obtained in the step (2), adopting a film forming process, exhausting air in a vacuum drier for 30-60 minutes to enable the polydimethylsiloxane resin to completely enter a microsphere array gap, curing for 1-6 hours on a hot table at the temperature of 60-90 ℃, taking down, and stripping the polydimethylsiloxane resin layer to obtain a polydimethylsiloxane film with a micron column;
(4) placing the polydimethylsiloxane film with the micron column obtained in the step (3) into a glass container, sequentially adding an aniline monomer and a perchloric acid solution of ammonium persulfate, and controlling the molar ratio of the aniline monomer to the ammonium persulfate to be 1.5: 1, carrying out stirring reaction on perchloric acid solution with the concentration of 1M by magnetons, reacting for 20-26 hours at the temperature of-5 ℃, taking out a polydimethylsiloxane film with a micron column, and washing the polydimethylsiloxane film with deionized water to obtain a composite structure film with polyaniline nano-spines uniformly distributed on a polydimethylsiloxane micron column array;
(5) and (5) taking two composite structure films with polyaniline nano-spines prepared in the step (4) uniformly distributed on the polydimethylsiloxane micro-column array, respectively solidifying the edges of the composite structure films together by silver paste and copper conductive adhesive tapes, and assembling the films face to obtain the hierarchical polyaniline/polydimethylsiloxane array-based ultrasensitive pressure sensor.
In the invention, the mass ratio of the polydimethylsiloxane monomer to the curing agent on the glass substrate in the step (1) is 1: 1-10: 1.
in the invention, the microsphere template in the step (2) is at least one of a micron polystyrene microsphere, a micron silicon dioxide microsphere or a micron polymethyl methacrylate microsphere.
In the invention, the heating time of the microsphere template in the step (2) in the oven is 24-96 hours.
In the invention, the particle size of the microspheres of the microsphere template in the step (2) is 3-15 μm.
In the invention, the preparation method of the microsphere array template in the step (3) is a one-way friction method.
In the invention, the organic diluent in the step (3) is at least one of toluene, ethyl acetate, cyclohexane or n-hexane.
In the present invention, the film forming process in step (3) is any one of a spin coating method, a tape casting method, a spray coating method, a blade coating method, a drop coating method, or an inverse mold method.
The pressure sensor prepared in the invention has the advantages that:
(1) the sensor has ultrahigh sensitivity and extremely low detection limit, has excellent performance in all aspects due to the bionic structural design, and can stably monitor human physiological signals (including large-amplitude muscle movement, extremely fine vital signs such as respiration and pulse) in real time.
(2) The flexible pressure sensor is mainly formed by assembling films with hierarchical polyaniline/polydimethylsiloxane arrays, and polyaniline and polydimethylsiloxane which are main bodies of the films with the composite structures are both organic polymers, so that the flexible pressure sensor has excellent flexibility, can be bent and twisted in any form, and is good in fitting performance with human skin.
(3) The nano-scale polyaniline thorn-shaped arrays can be interlocked under the fine pressure, so that the conductive path is greatly increased, the contact resistance is sharply reduced, the ultra-low detection limit is realized, and the ultra-high sensitivity is realized under the ultra-low pressure.
(4) The micron-sized polydimethylsiloxane columnar array can be subjected to secondary interlocking under larger pressure, so that a conductive path is further enlarged, the contact resistance is reduced, the sensor has good response in a larger pressure range, and the use range of the sensor is widened.
(5) The array structure of the hierarchical polyaniline nanoneedle/polydimethylsiloxane microcolumn enables the surface of the composite film to have excellent hydrophobicity, so that the pressure sensor has excellent signal stability in a wide humidity range.
(6) The synthesis process is simple, the preparation process is environment-friendly and pollution-free, and the composite film forming process is mature, so that convenience is provided for batch preparation and subsequent further development and research.
Drawings
FIG. 1 is a scanning electron microscope and atomic force microscope image of a hierarchical polyaniline/polydimethylsiloxane array film. Wherein: (a) scanning electron micrographs, and (b) atomic force microscope photographs.
Fig. 2 is a physical diagram of the pressure sensor.
Fig. 3 is a resistance-pressure curve and a sensitivity-pressure curve of the sensor film.
Fig. 4 is a response time curve of the sensor.
Fig. 5 is a fatigue response test curve of the sensor.
FIG. 6 is a graph of the change in resistance of the sensor to the same pressure over a range of 1.8% to 93.1% humidity.
FIG. 7 is a resistance change curve of the sensor at a temperature range of 30 ℃ to 90 ℃ for the same pressure.
Fig. 8 is a graph showing the resistance change of the sensor for the contraction and relaxation movements of the biceps brachii muscle of the human body.
Fig. 9 is a current variation curve of the sensor for the pulse signal of the wrist of the human body.
Detailed Description
The present invention will be further described with reference to the following specific examples and drawings, but the present invention is not limited to the following examples. The method is a conventional method unless otherwise specified. The starting materials are commercially available from the open literature unless otherwise specified.
Firstly, a polydimethylsiloxane prepolymer (Dow Corning 184) and a curing agent are mixed in a proportion of 2: mix at a ratio of 1 and remove air bubbles in a vacuum desiccator. The mixture was then spin coated on a glass substrate and cured in an oven at 80 ℃ for 3 hours. An appropriate amount of 5 μm dry powder of silica particles was placed on the above-mentioned polydimethylsiloxane substrate, and another piece of polydimethylsiloxane cured by the same procedure (prepolymer: curing agent = 10: 1) was unidirectionally rubbed to obtain a single-layer silica array template. The templates were then heated at 220 ℃ for 72 hours.
And then diluting polydimethylsiloxane to 70 wt% by using toluene, dropwise coating the mixed solution on the heated silicon dioxide substrate, placing the silicon dioxide substrate in a vacuum drier for 1 hour of air suction to ensure that the space between the microspheres is completely filled with the polydimethylsiloxane, curing the silicon dioxide substrate on a hot table at 80 ℃ for 3 hours, and then demolding to obtain the PDMS film with the micro-columnar ordered array.
The polydimethylsiloxane film was placed in a glass container, and a solution of aniline monomer and ammonium persulfate in perchloric acid was mixed in a ratio of 1.5: 1, the perchloric acid solution with the concentration of 1M is added into a container, and the reaction is carried out for 22 hours under the condition of low temperature and magnetic stirring, wherein the temperature is controlled to be-2 ℃. Fig. 1 is a microscopic photograph of a scanning electron microscope and an atomic force microscope thereof.
Taking out the film, and washing the film with deionized water to obtain the composite structure film with polyaniline nano-thorns uniformly distributed on the polydimethylsiloxane micro-column array, as shown in figure 2.
And (3) taking two films with the composite structures, respectively solidifying the edges of the two films together by using silver paste and a copper conductive adhesive tape, and then assembling the films in a face-to-face manner to obtain the hierarchical polyaniline/polydimethylsiloxane array-based ultrasensitive pressure sensor.
Fig. 3 shows the resistance change of the sensor under different pressure conditions, and calculates the specific sensitivity index of the sensor.
Fig. 4 shows the response speed of the sensor to pressure, and the response time of the sensor to pressure is within 30 ms.
Fig. 5 shows the pressure response signal of the sensor during 10000 loads-unloads.
FIG. 6 shows the resistance signal of the sensor for the same pressure over a wide humidity range of 1.8% to 93.1%.
FIG. 7 shows the resistance signal of the sensor for the same pressure over a temperature range of 30 deg.C to 90 deg.C.
Fig. 8 shows the resistance change signals of the sensor for the contraction and relaxation movements of the biceps brachii muscle of the human body, demonstrating the continuous monitoring ability of the sensor for the large muscular movements of the human body.
Fig. 9 shows the current variation signal of the sensor for the human wrist pulse, which proves the continuous monitoring capability of the sensor for the human body fine vital signs.
Claims (9)
1. The pressure sensor is characterized by being formed by assembling two polydimethylsiloxane micro-column/polyaniline nano-thorn hierarchical composite structure films with the same structure in a face-to-face mode, and the thickness of the ultra-sensitive flexible pressure sensor is 160-1000 micrometers.
2. The method for preparing the biologically inspired ultrasensitive flexible pressure sensor of claim 1, comprising the steps of:
(1) curing polydimethylsiloxane on a glass substrate for 1-6 hours at the temperature of 60-90 ℃ through a curing agent to obtain polydimethylsiloxane resin;
(2) preparing a microsphere template by taking microspheres as a sacrificial layer, and heating the microsphere template in an oven at 220 ℃ to obtain a densely arranged microsphere template sacrificial layer;
(3) adding 1-3 g of mixed solution consisting of an organic diluent and the polydimethylsiloxane resin obtained in the step (1) to the microsphere template sacrificial layer obtained in the step (2), adopting a film forming process, exhausting air in a vacuum drier for 30-60 minutes to enable the polydimethylsiloxane resin to completely enter a microsphere array gap, curing for 1-6 hours on a hot table at the temperature of 60-90 ℃, taking down, and stripping the polydimethylsiloxane resin layer to obtain a polydimethylsiloxane film with a micron column;
(4) placing the polydimethylsiloxane film with the micron column obtained in the step (3) into a glass container, sequentially adding an aniline monomer and a perchloric acid solution of ammonium persulfate, and controlling the molar ratio of the aniline monomer to the ammonium persulfate to be 1.5: 1, carrying out stirring reaction on perchloric acid solution with the concentration of 1M by magnetons, reacting for 20-26 hours at the temperature of-5 ℃, taking out a polydimethylsiloxane film with a micron column, and washing the polydimethylsiloxane film with deionized water to obtain a composite structure film with polyaniline nano-spines uniformly distributed on a polydimethylsiloxane micron column array;
(5) and (4) taking two composite structure films with the polyaniline nano-spines prepared in the step (4) uniformly distributed on the polydimethylsiloxane micro-column array, respectively curing the edges of the composite structure films together by using silver paste and a copper conductive adhesive tape, and assembling the composite structure films face to obtain the hierarchical polyaniline/polydimethylsiloxane array-based ultrasensitive pressure sensor.
3. The method for preparing the biologically inspired ultrasensitive flexible pressure sensor according to claim 2, wherein the mass ratio of the polydimethylsiloxane monomer to the curing agent on the glass substrate in the step (1) is 1: 1-10: 1.
4. the method for preparing a biologically inspired ultrasensitive flexible pressure sensor, according to claim 2, wherein in step (2), the microsphere template is at least one of a micro polystyrene microsphere, a micro silica microsphere, or a micro polymethyl methacrylate microsphere.
5. The method for preparing the biologically inspired ultrasensitive flexible pressure sensor, according to claim 2, wherein the microsphere template is heated in the oven for 24-96 hours in the step (2).
6. The method for preparing a biologically inspired ultrasensitive flexible pressure sensor according to claim 2, wherein the microsphere particle size of the microsphere template in step (2) is 3 μm to 15 μm.
7. The method for preparing the biologically inspired ultrasensitive flexible pressure sensor according to claim 2, wherein the method for preparing the microsphere array template in the step (3) is a one-way friction method.
8. The method for preparing a biologically inspired ultrasensitive flexible pressure sensor, according to claim 2, wherein the organic diluent in step (3) is at least one of toluene, ethyl acetate, cyclohexane or n-hexane.
9. The method for preparing the biologically inspired ultrasensitive flexible pressure sensor, according to claim 2, wherein the film forming process in the step (3) is any one of spin coating, tape casting, spray coating, blade coating, drop coating or reverse molding.
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