CN113108954B - Paper-based flexible pressure sensor and preparation method and application thereof - Google Patents
Paper-based flexible pressure sensor and preparation method and application thereof Download PDFInfo
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- CN113108954B CN113108954B CN202110323614.3A CN202110323614A CN113108954B CN 113108954 B CN113108954 B CN 113108954B CN 202110323614 A CN202110323614 A CN 202110323614A CN 113108954 B CN113108954 B CN 113108954B
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Images
Classifications
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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
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E10/00—Energy generation through renewable energy sources
- Y02E10/50—Photovoltaic [PV] energy
- Y02E10/549—Organic PV cells
Abstract
The invention discloses a paper-based flexible pressure sensor and a preparation method and application thereof. The preparation method of the flexible pressure sensor comprises the following steps: (1) dispersing silver nanowires into ethanol to obtain AgNWs dispersion liquid; dispersing the nano microcrystalline cellulose into water to obtain a CNC dispersion liquid; then uniformly mixing the AgNWs dispersion liquid and the CNC dispersion liquid to obtain a mixed liquid of AgNWs and CNC; (2) and (2) taking the paper base as a substrate, depositing a chitosan solution and a mixed solution of AgNWs and CNC on the paper base in sequence by adopting a vacuum filtration mode, and drying to obtain the flexible pressure sensor based on the paper base. The flexible pressure sensor prepared by the invention has the advantages of strong silver nanowire adhesiveness, high sensitivity, good stability, high conductivity and the like, and can be applied to sensing materials, bionic robots and medical real-time monitoring equipment.
Description
Technical Field
The invention belongs to the technical field of sensors, and particularly relates to a paper-based flexible pressure sensor and a preparation method and application thereof.
Background
Along with the development of the flexible pressure sensor, the wearable electronic equipment which can smoothly complete human-computer interaction, can detect human activities in real time and has no rejection response is produced to meet the needs of daily life of people. Wearable electronic equipment can realize with human skin direct contact to reach the real-time supervision to human pulse, rhythm of the heart, limbs motion and the environmental condition that is located, and handle the physical stimulus signal and convert the signal into the signal of telecommunication, make corresponding electronic component react after further enlargiing this signal of telecommunication through amplifier circuit, finally realize signal output, reach the purpose that sensing detected.
Flexible sensors are generally composed of a flexible substrate (or base material) and a conductive layer, wherein the flexible substrate can make the contact between the electronic device and the skin tighter, and enhance the stability of the sensor. In general, materials used as the flexible substrate mainly include Polydimethylsiloxane (PDMS), Polyurethane (PU), polyethylene terephthalate (PET), Polyimide (PI), polyvinyl chloride (PVC), paper, and the like; and the conductive layer material is mainly metal nanowires, such as silver nanowires (AgNWs), gold nanowires and copper nanowires, as well as Carbon Nanotubes (CNTs), Graphene (GO), conductive polymers, and the like. Among various types of conductive materials, silver nanowires are considered as the most promising conductive material for flexible electronic devices due to their outstanding mechanical flexibility and excellent optoelectronic properties. The paper base is widely applied to the flexible sensor base material in recent years due to the advantages of flexibility, light weight, biodegradability, biocompatibility, low cost, wide sources, recyclability, easiness in recycling and the like. For example, patent CN110146556A discloses a flexible humidity sensor based on paper base and a manufacturing method thereof.
However, pure AgNWs is easily separated from the deposited substrate due to its weak adhesion, and thus seriously affects the stability of the sensor. Based on the method, the flexible pressure sensor with strong AgNWs adhesion capability, high conductivity, good stability and certain oxidation resistance is developed, and the method has very important practical significance for further promoting the high-quality development of the paper-based wearable electronic equipment.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provides a preparation method of a paper-based flexible pressure sensor.
The invention also aims to provide the paper-based flexible pressure sensor prepared by the method.
It is a further object of the present invention to provide an application of said paper based flexible pressure sensor.
The purpose of the invention is realized by the following technical scheme:
a preparation method of a paper-based flexible pressure sensor comprises the following steps:
(1) dispersing silver nanowires (AgNWs) into ethanol to obtain AgNWs dispersion liquid; dispersing nano microcrystalline cellulose (CNC) into water to obtain CNC dispersion liquid; then uniformly mixing the AgNWs dispersion liquid and the CNC dispersion liquid to obtain a mixed liquid of AgNWs and CNC;
(2) and (2) taking the paper base as a substrate, depositing a chitosan solution and a mixed solution of AgNWs and CNC on the paper base in sequence by adopting a vacuum filtration mode, and drying to obtain the flexible pressure sensor based on the paper base.
The silver nanowires (AgNWs) in the step (1) are preferably prepared by the following method: adding polyvinyl pyrrolidone copper (PVP) into Ethylene Glycol (EG), heating and stirring uniformly, and then cooling to room temperature to obtain a PVP solution; then silver nitrate (AgNO) 3 ) Adding into PVP solution, stirring rapidly to form transparent and uniform liquid, adding FeCl 3 And (3) the ethylene glycol solution is stirred and mixed uniformly, then the reaction is carried out at the temperature of 125-140 ℃, after the reaction is finished, the reaction product is cooled to room temperature, and the silver nanowire (AgNWs) is obtained after centrifugation and washing.
The polyvinyl pyrrolidone copper (PVP) and the silver nitrate (AgNO) 3 ) And FeCl 3 In a molar ratio of 19:5600 to 8380: 10; preferably 19:7000: 10.
The weight-average molecular weight (Mw) of the polyvinylpyrrolidone (PVP) is 44000-54000.
The concentration of the PVP solution is preferably 0.008 g/ml.
The heating temperature is preferably 60 + -5 deg.C.
The FeCl-containing material 3 The ethylene glycol solution of (a) is preferably prepared by the following method: iron chloride hexahydrate crystals (FeCl) 3 ·6H 2 O) is added into Ethylene Glycol (EG) and stirred evenly to obtain FeCl-containing 3 The ethylene glycol solution of (1).
The FeCl-containing material 3 The concentration of the ethylene glycol solution is 550-650 mu mol/L; preferably 600. mu. mol/L.
The time for rapid stirring is preferably 1-2 min.
The temperature of the reaction is preferably 130 ℃.
The reaction time is 3-6 h; preferably 5 h.
The centrifugation conditions are as follows: centrifuging at 9000rpm for 10-15 min; preferably: centrifuge at 9000rpm for 10 min.
The washing is sequentially washing with acetone and ethanol; preferably, the washing is carried out for 5 to 8 times by sequentially using acetone and ethanol.
The diameter of the silver nanowire (AgNWs) is about 80nm, and the length of the silver nanowire (AgNWs) is more than 50 μm.
The nano microcrystalline cellulose (CNC) in the step (1) is prepared by an acidolysis method; preferably prepared by the following method: crushing wood pulp, adding concentrated sulfuric acid solution, mixing uniformly, stirring and reacting for 80-100 min under the condition of water bath at 45-55 ℃, adding water to stop reaction, cooling to room temperature, centrifuging, and dialyzing to obtain the nano microcrystalline cellulose (CNC).
The wood pulp is preferably hardwood pulp.
The concentration of the concentrated sulfuric acid solution is 55-64% by mass percent; preferably 64% by mass.
The dosage of the concentrated sulfuric acid solution is calculated according to the proportion of 9g concentrated sulfuric acid solution per gram (g) of wood pulp.
The rotation speed of the stirring is 300 rpm.
The reaction conditions are preferably: the reaction was carried out at 50 ℃ for 90 min.
The water addition termination reaction is a water addition termination reaction with the volume 8-10 times that of the system.
The centrifugation is realized by the following steps: the reaction solution (brown liquid) cooled to room temperature was centrifuged at 11000rpm for 10min, and the supernatant was discarded; and adding deionized water for redissolving, centrifuging again, collecting supernatant, and repeating for 5-8 times.
The dialysis is carried out by adopting a dialysis bag with the molecular weight cutoff of 8000-14000; preferably, the dialysis is carried out for 2 to 3 days by adopting a dialysis bag with the molecular weight cutoff of 8000 to 14000.
The dialysate used for dialysis is distilled water.
The concentration of the AgNWs dispersion liquid in the step (1) is 1.0-2.0% by mass; preferably 1.0% by mass.
The mass percentage of the concentration of the CNC dispersion liquid in the step (1) is 0.5-1.0%; preferably 0.5% by mass.
The volume ratio of the AgNWs dispersion liquid to the CNC dispersion liquid in the step (1) is 1-3: 1; preferably 2: 1.
The mass ratio of AgNWs to CNC in the AgNWs and CNC mixed liquid in the step (1) is 0.5-4.5: 1.
Mixing in the step (1) by adopting a vortex oscillator; preferably, the mixture is sufficiently mixed by shaking for 1 hour or more with a vortex shaker.
The paper base in the step (2) is preferably filter paper; more preferably a chemical analysis filter paper.
The chitosan solution in the step (2) is formic acid solution of chitosan; preferably, the chitosan formic acid solution with the concentration of 1.0-3.0 percent by mass and the pH of 2.0 is selected; more preferably a chitosan formic acid solution with a mass percentage of 2.0% and a pH of 2.0.
The deposition amount of the chitosan in the step (2) is 35-120 g/m 2 (ii) a Preferably 39.81 to 119.43g/m 2 (ii) a More preferably 79.62g/m 2 。
The deposition amount of AgNWs in the step (2) is 30-50 g/m 2 (ii) a Preferably 31.85-47.78 g/m 2 (ii) a More preferably 31.85g/m 2 。
The deposition amount of the CNC in the step (2) is 5-20 g/m 2 (ii) a Preferably 7.96-15.92 g/m 2 (ii) a More preferably 7.96g/m 2 。
The drying in the step (2) is drying in a vacuum drying oven: the drying temperature is 45-75 ℃ (preferably 60 ℃) and the time is 30 min.
A flexible paper-based pressure sensor prepared by any one of the above methods.
The flexible pressure sensor based on the paper base is applied to sensing materials, bionic robots and/or medical real-time monitoring equipment.
The sensing material comprises sensing material for sensors and/or for use in wearable electronic devices.
The medical real-time monitoring equipment comprises monitoring equipment for monitoring limb movement, pulse, heart rate and the like of a human body.
Compared with the prior art, the invention has the following advantages and effects:
(1) the preparation method of the flexible pressure sensor comprises the steps of chemically analyzing filter paper, a chitosan solution, a silver nanowire dispersion liquid, a nano microcrystalline cellulose colloid and the like, depositing the chitosan solution, the silver nanowire and the nano microcrystalline cellulose mixed liquid on a paper base in sequence by using a vacuum filtration method, drying and peeling to obtain the flexible pressure sensor based on the paper base.
(2) The preparation method has the advantages of simple and rapid operation, low cost, no pollution and the like, the deposited layers are uniformly distributed, and due to the addition of the chitosan buffer layer, intermolecular hydrogen bonds can be formed between the chitosan buffer layer and the nano microcrystalline cellulose, so that the adhesive force between the silver nanowires and the substrate is indirectly enhanced, and the prepared pressure sensor has the advantages of strong silver nanowire adhesive property, high sensitivity, good stability and the like.
(3) Compared with a template method, an electrochemical method and other methods, the method has the advantages of simple operation, mild reaction conditions, high product yield, low cost and the like; utilize the vacuum filtration method to deposit chitosan solution, silver nano wire and nanometer microcrystalline cellulose mixed solution on the substrate in proper order, compare the coating method, the utilization ratio of vacuum filtration method to the raw materials is higher, has avoided the waste of raw materials, and each sedimentary deposit distributes evenly, more helps the preparation of surfacing, the excellent sensor of performance.
(4) The initial square resistance of the sensor prepared by the invention is between 10 and 20 omega/sq, the conductivity can reach 688.7S/m, and the square resistance is only increased by about 10 percent after 20 times of adhesive tape adhesion-stripping tests; after 500 bending cycles under 20% strain, the resistance has no significant change, and therefore, the silver nanowire of the flexible pressure sensor has strong adhesiveness, good stability and high conductivity.
(5) The chemical analysis filter paper provided by the invention is used as an excellent base material, and has the advantages of flexibility, light weight, biodegradability, biocompatibility, low cost, wide source, recyclability, easiness in recycling treatment and the like, so that the chemical analysis filter paper has a wide application prospect in flexible sensors, especially wearable electronic equipment.
Drawings
FIG. 1 is a flow chart illustrating the preparation of a flexible pressure sensor according to the present invention.
Detailed Description
The present invention will be described in further detail with reference to examples, but the embodiments of the present invention are not limited thereto. The reagents, methods and apparatus employed in the present invention are conventional in the art, except as otherwise indicated. The following examples are given without reference to specific experimental conditions, and are generally in accordance with conventional experimental conditions. Unless otherwise specified, reagents and starting materials for use in the present invention are commercially available.
The wood pulp referred to in the examples of the present invention was hardwood pulp, available from national trade company, juanono, Qingdao.
FeCl referred to in the examples of the invention 3 The preparation method of the salt solution comprises the following steps: 0.0162g of ferric chloride hexahydrate crystal (FeCl) is accurately weighed by a balance 3 ·6H 2 O) was placed in a beaker and Ethylene Glycol (EG) was slowly added until the total mass of the solution was 100g, at which time FeCl 3 The concentration of the solution was 600. mu.M.
Example 1
(1) Preparation of the raw materials
Preparation of silver nanowires (AgNWs): adding 0.2g of polyvinylpyrrolidone (PVP) (Mw 44000-54000) into a beaker containing 25ml of Ethylene Glycol (EG) pure solution, carrying out magnetic stirring in a water bath kettle at 60 ℃, fully dissolving, and cooling to room temperature to obtain a PVP solution; then 0.2g silver nitrate (AgNO) 3 ) Adding the crystal into PVP solution, and quickly stirring until a transparent and uniform solution is formed; finally 3.5g FeCl was added 3 Salt solution (EG as solvent with concentration of 600 μ M) is stirred for 1-2 min (PVP: AgNO) 3 ：FeCl 3 19:5600:10 (mass ratio)), it was immediately transferred to a reaction kettle preheated to 125 ℃ and reacted for 4 h. And cooling the mixed system to room temperature, centrifuging at 9000rpm for 10min, washing the precipitate with acetone and ethanol solution for 5-8 times, dispersing the precipitate in an essence bottle with ethanol, and refrigerating for later use.
Preparing nano microcrystalline cellulose (CNC): after wood pulp is crushed by a crusher, 5g of oven-dried pulp is weighed and placed in a three-neck flask, 45g of concentrated sulfuric acid solution (55 wt%) is added by a dropper, and the raw materials and the acid are fully mixed; then the three-neck flask is placed in a water bath kettle at 45 ℃, the rotating speed of a stirrer is adjusted to 300rpm, after the three-neck flask is heated in a water bath for 80min, 400ml of distilled water is immediately added to terminate the experiment, the three-neck flask is taken down, and the three-neck flask is kept stand and cooled to the room temperature. Subpackaging the prepared brown liquid into a centrifuge tube, putting the centrifuge tube into a high-speed centrifuge, regulating the rotation speed to 11000rpm, centrifuging for 10min, and discarding the supernatant after the first centrifugation; and (3) repeating the balancing and centrifugation of the centrifuge tube (except for the first centrifugation, discarding the supernatant, then collecting the supernatant after each centrifugation, adding deionized water again for balancing and centrifugation, and the same below) for about 5-8 times (the balanced centrifuge tube is placed in an ultrasonic machine (40kHz) for ultrasonic treatment for 7min in an ice bath), collecting the white liquid on the upper layer after each centrifugation, and filling the white liquid into a dialysis bag (the dialysate is distilled water, the molecular weight cutoff MW is 8000-14000) for dialysis for 2-3 days to finally obtain the neutral nano microcrystalline cellulose colloid.
Preparing a AgNWs and CNC mixed system: mixing the prepared AgNWs dispersion liquid (with the concentration of 1.0 wt%) and the CNC dispersion liquid (with the concentration of 0.5 wt%) according to the volume ratio of 1:1, placing the mixture on a vortex oscillator, oscillating for 1 hour, and fully mixing the two to form uniform and stable liquid for later use.
(2) Sensor fabrication and detection
Using a chemical analysis filter paper (purchased from general electric and biological technology (Hangzhou) Co., Ltd.) as a substrate, 5mL of a 1.0 wt% chitosan solution (formic acid as a solvent, pH of about 2.0) was first deposited on the filter paper (the filter paper was previously cut into a circular shape having a radius of 2 cm) by vacuum filtration (the amount of chitosan deposited was 39.81 g/m) 2 ) Drying in a vacuum drying oven at 45 deg.C for 30 min; then mixing the AgNWs prepared in the step (c) with the CNC (computer numerical control) (the AgNWs is 4mL, the deposition amount is 31.85g/m 2 (ii) a CNC 4mL, deposition 15.92g/m 2 ) Depositing on the obtained paper base, and drying in a vacuum drying oven at 45 deg.C for 30 min. Finally, peeling the filter paper from the funnel to obtain the paper-based high-stability flexible pressure sensor (the preparation flow chart is shown in figure 1).
Example 2
(1) Preparation of the raw materials
Preparation of silver nanowires (AgNWs): adding 0.2g of polyvinylpyrrolidone (PVP) into a beaker containing 25ml of Ethylene Glycol (EG) pure solution, carrying out magnetic stirring in a water bath kettle at 60 ℃, and cooling to room temperature after full dissolution to obtain a PVP solution; then 0.25g silver nitrate (AgNO) 3 ) Adding the crystal into PVP solution, and quickly stirring until a transparent and uniform solution is formed; finally 3.5g FeCl was added 3 Salt solution (EG as solvent with concentration of 600 μ M) is stirred for 1-2 min (PVP: AgNO) 3 ：FeCl 3 19:7000:10 (mass ratio)), it was immediately transferred to a reaction kettle preheated to 130 ℃ and reacted for 5 h. And cooling the mixed system to room temperature, centrifuging at 9000rpm for 10min, washing the precipitate with acetone and ethanol solution for 5-8 times, dispersing the precipitate in an essence bottle with ethanol, and refrigerating for later use.
Preparing nano microcrystalline cellulose (CNC): crushing wood pulp by a crusher, weighing 5g of oven-dried pulp, placing the weighed pulp into a three-neck flask, adding 45g of concentrated sulfuric acid solution (64 wt%) by a dropper, and fully mixing the raw materials with acid; then the three-neck flask is placed in a 50 ℃ water bath kettle, the rotating speed of a stirrer is adjusted to 300rpm, after the three-neck flask is heated in a water bath for 90min, 400ml of distilled water is immediately added to terminate the experiment, the three-neck flask is taken off, and the three-neck flask is kept stand and cooled to room temperature. Subpackaging the prepared brown liquid into a centrifuge tube, putting the centrifuge tube into a high-speed centrifuge, regulating the rotation speed to 11000rpm, centrifuging for 10min, and discarding the supernatant after the first centrifugation; repeating the steps of balancing and centrifugal separation of the centrifugal tube for about 5-8 times (placing the centrifugal tube after balancing into an ultrasonic machine (40kHz) for ice bath ultrasonic for 7min), collecting the upper-layer white liquid after each centrifugation, putting the upper-layer white liquid into a dialysis bag (the dialysate is distilled water, and the cut-off molecular weight MW is 8000-14000), and dialyzing for 2-3 days to finally obtain the neutral nano microcrystalline cellulose colloid.
Preparing a AgNWs and CNC mixed system: mixing the prepared AgNWs dispersion liquid (with the concentration of 1.0 wt%) and the CNC dispersion liquid (with the concentration of 0.5 wt%) according to the volume ratio of 2:1, placing the mixture on a vortex oscillator, oscillating for 1 hour, and fully mixing the two to form uniform and stable liquid for later use.
(2) Sensor fabrication and detection
Using a chemical analysis filter paper (purchased from general electric and biological technology (Hangzhou) Co., Ltd.) as a substrate, 5mL of a 2.0 wt% chitosan solution (formic acid as a solvent, pH of about 2.0) was deposited on the filter paper (the filter paper was previously cut into a circle having a radius of 2 cm) by vacuum filtration (the amount of chitosan deposited was 79.62 g/m) 2 ) Drying in a vacuum drying oven at 60 deg.C for 30 min; then mixing the AgNWs prepared in the step (c) with the CNC (computer numerical control) (the AgNWs is 4mL, the deposition amount is 31.85g/m 2 (ii) a CNC 2mL, deposition 7.96g/m 2 ) Depositing on the obtained paper base, and drying in a vacuum drying oven at 60 ℃ for 30 min. And finally, peeling the filter paper from the funnel to obtain the paper-based high-stability flexible pressure sensor.
Example 3
(1) Preparation of the raw materials
Preparation of silver nanowires (AgNWs): adding 0.2g of polyvinylpyrrolidone (PVP) into a beaker containing 25ml of Ethylene Glycol (EG) pure solution, carrying out magnetic stirring in a water bath kettle at 60 ℃, and cooling to room temperature after full dissolution to obtain a PVP solution; then 0.3g of silver nitrate (AgNO) 3 ) Adding the crystal into PVP solution, and quickly stirring until a transparent and uniform solution is formed; finally 3.5g FeCl was added 3 Salt solution (EG as solvent with concentration of 600 μ M) is stirred for 1-2 min (PVP: AgNO) 3 ：FeCl 3 19:8380:10 (mass ratio)), it was immediately transferred to a reaction kettle preheated to 140 ℃ and reacted for 6 h. And cooling the mixed system to room temperature, centrifuging at 9000rpm for 10min, washing the precipitate with acetone and ethanol solution for 5-8 times, dispersing the precipitate in an essence bottle with ethanol, and refrigerating for later use.
Preparing nano microcrystalline cellulose (CNC): crushing wood pulp by a crusher, weighing 5g of oven-dried pulp, placing the oven-dried pulp in a three-neck flask, adding 45g of concentrated sulfuric acid solution (60 wt%) by a dropper, and fully mixing the raw materials with acid; then the three-neck flask is placed in a water bath kettle at 55 ℃, the rotating speed of a stirrer is adjusted to 300rpm, after the three-neck flask is heated in a water bath for 100min, 400ml of distilled water is immediately added to terminate the experiment, the three-neck flask is taken down, and the three-neck flask is kept stand and cooled to the room temperature. Subpackaging the prepared brown liquid into a centrifuge tube, putting the centrifuge tube into a high-speed centrifuge, regulating the rotation speed to 11000rpm, centrifuging for 10min, and discarding the supernatant after the first centrifugation; repeating the steps of balancing and centrifuging the centrifuge tube for about 5-8 times (the balanced centrifuge tube is placed on an ultrasonic machine (40kHz) and subjected to ice bath ultrasonic treatment for 7min), collecting the upper white liquid after each centrifugation, filling the upper white liquid into a dialysis bag (the dialysate is distilled water, and the cut-off molecular weight MW is 8000-14000), and dialyzing for 2-3 days to finally obtain the neutral nano microcrystalline cellulose colloid.
Preparing a AgNWs and CNC mixed system: mixing the prepared AgNWs dispersion liquid (with the concentration of 1.0 wt%) and the CNC dispersion liquid (with the concentration of 0.5 wt%) according to the volume ratio of 3:1, placing the mixture on a vortex oscillator, oscillating for 1 hour, and fully mixing the two to form uniform and stable liquid for later use.
(2) Sensor fabrication and detection
Using a chemical analysis filter paper (purchased from general electric and biological technology (Hangzhou) Co., Ltd.) as a substrate, 5mL of a 3.0 wt% chitosan solution (formic acid as a solvent, pH of about 2.0) was deposited on the filter paper (the filter paper was previously cut into a circle having a radius of 2 cm) by vacuum filtration (the amount of chitosan deposited was 119.43 g/m) 2 ) And drying in a vacuum drying oven at 75 ℃ for 30 min; then mixing the AgNWs prepared in the third step with CNC (6 mL of AgNWs and 47.78g/m of sediment amount) 2 (ii) a CNC 2mL, deposition 7.96g/m 2 ) Depositing on the obtained paper base, and drying in a vacuum drying oven at 75 deg.C for 30 min. And finally, peeling the filter paper from the funnel to obtain the paper-based high-stability flexible pressure sensor.
Comparative example 1
(1) Preparation of the raw materials
Preparation of silver nanowires (AgNWs): adding 0.2g of polyvinylpyrrolidone (PVP) into a beaker containing 25ml of Ethylene Glycol (EG) pure solution, carrying out magnetic stirring in a water bath kettle at 60 ℃, and cooling to room temperature after full dissolution to obtain a PVP solution; then 0.25g silver nitrate (AgNO) 3 ) Adding the crystal into PVP solution, and quickly stirring until a transparent and uniform solution is formed; finally 3.5g FeCl was added 3 Salt solution (EG as solvent with concentration of 600 μ M) is stirred for 1-2 min (PVP: AgNO) 3 ：FeCl 3 19:7000:10 (mass ratio)), it was immediately transferred to a reaction kettle preheated to 130 ℃ and reacted for 5 h. And cooling the mixed system to room temperature, centrifuging at 9000rpm for 10min, washing the precipitate with acetone and ethanol solution for 5-8 times, dispersing the precipitate in an essence bottle with ethanol, and refrigerating for later use.
(2) Sensor fabrication and detection
A chemical analysis filter paper (purchased from general electric and biological technology (Hangzhou) Co., Ltd.) was used as a substrate (the filter paper was previously cut into a circular shape with a radius of 2 cm), and a 1.0 wt% AgNWs dispersion (used in an amount of 4mL, deposited in an amount of 31.85 g/m) was first added 2 ) It was deposited on filter paper by vacuum filtration and dried in a vacuum oven at 60 ℃ for 30 min. And then peeling the filter paper from the funnel to obtain the paper-based flexible pressure sensor.
Comparative example 2
(1) Preparation of the raw materials
Preparation of silver nanowires (AgNWs): adding 0.2g of polyvinylpyrrolidone (PVP) into a beaker containing 25ml of Ethylene Glycol (EG) pure solution, carrying out magnetic stirring in a water bath kettle at 60 ℃, and cooling to room temperature after full dissolution to obtain a PVP solution; then 0.25g silver nitrate (AgNO) 3 ) The crystals were added to the PVP solution and stirred rapidly until a clear, homogeneous solution was formed. Finally 3.5g FeCl was added 3 Salt solution (EG as solvent with concentration of 600 μ M) is stirred for 1-2 min (PVP: AgNO) 3 ：FeCl 3 19:7000:10 (mass ratio)), it was immediately transferred to a reaction kettle preheated to 130 ℃ and reacted for 5 h. And cooling the mixed system to room temperature, centrifuging at 9000rpm for 10min, washing the precipitate with acetone and ethanol solution for 5-8 times, dispersing the precipitate in an essence bottle with ethanol, and refrigerating for later use.
Preparing nano microcrystalline cellulose (CNC): crushing wood pulp by a crusher, weighing 5g of oven-dried pulp, placing the weighed pulp into a three-neck flask, adding 45g of concentrated sulfuric acid solution (64 wt%) by a dropper, and fully mixing the raw materials with acid; then the three-neck flask is placed in a 50 ℃ water bath kettle, the rotating speed of a stirrer is adjusted to 300rpm, after the three-neck flask is heated in a water bath for 90min, 400ml of distilled water is immediately added to terminate the experiment, the three-neck flask is taken down, and the three-neck flask is kept stand and cooled to the room temperature. Subpackaging the prepared brown liquid into a centrifuge tube, putting the centrifuge tube into a high-speed centrifuge, regulating the rotation speed to 11000rpm, centrifuging for 10min, and discarding the supernatant after the first centrifugation; repeating the steps of balancing and centrifuging the centrifuge tube for about 5-8 times (the balanced centrifuge tube is placed on an ultrasonic machine (40kHz) and subjected to ice bath ultrasonic treatment for 7min), collecting the upper white liquid after each centrifugation, filling the upper white liquid into a dialysis bag (the dialysate is distilled water, and the cut-off molecular weight MW is 8000-14000), and dialyzing for 2-3 days to finally obtain the neutral nano microcrystalline cellulose colloid.
Preparing a AgNWs and CNC mixed system: mixing the prepared AgNWs dispersion liquid (with the concentration of 1.0 wt%) and the CNC dispersion liquid (with the concentration of 0.5 wt%) according to the volume ratio of 2:1, placing the mixture on a vortex oscillator, oscillating for 1h, and fully mixing the two to form uniform and stable liquid for later use.
(2) Sensor fabrication and detection
Using chemical analysis filter paper (purchased from general electric and biological technology (Hangzhou) Co., Ltd.) as substrate (the filter paper is cut into a circle with a radius of 2 cm), firstly preparing the AgNWs and CNC mixed solution (AgNWs is 4mL, deposition amount is 31.85 g/m) 2 (ii) a CNC 2mL, deposition 7.96g/m 2 ) Depositing on the substrate, and drying in a vacuum drying oven at 60 deg.C for 30 min. And finally, peeling the filter paper from the funnel to obtain the paper-based flexible pressure sensor.
Comparative example 3
(1) Preparation of the raw materials
Preparation of silver nanowires (AgNWs): adding 0.2g of polyvinylpyrrolidone (PVP) into a beaker containing 25ml of Ethylene Glycol (EG) pure solution, carrying out magnetic stirring in a water bath kettle at 60 ℃, and cooling to room temperature after full dissolution to obtain a PVP solution; then 0.25g silver nitrate (AgNO) 3 ) Adding the crystal into PVP solution, and quickly stirring until a transparent and uniform solution is formed; finally 3.5g FeCl was added 3 Salt solution (EG as solvent with concentration of 600 μ M) is stirred for 1-2 min (PVP: AgNO) 3 ：FeCl 3 19:7000:10 (mass ratio)), it was immediately transferred to a reaction kettle preheated to 130 ℃ and reacted for 5 hours. Will be provided withAnd cooling the mixed system to room temperature, centrifuging for 10min at the rotating speed of 11000rpm, washing the precipitate for 5-8 times by using acetone and ethanol solutions respectively, dispersing the precipitate in an essence bottle by using ethanol, and refrigerating for later use.
(2) Sensor fabrication and detection
First, 5mL of a 2.0 wt% chitosan solution (formic acid as a solvent, pH 2.0) was applied dropwise to a clean petri dish and dried in a vacuum oven at 60 ℃ for 30 min. 4mL of a dispersion of 1.0 wt% AgNWs was then drop-deposited onto the resulting chitosan film (deposited amount of AgNWs was 31.85 g/m) 2 (ii) a The deposition amount of chitosan was 79.62g/m 2 ) And then put into a vacuum drying oven at 60 ℃ for drying for 30min again. And finally, peeling the composite film from the funnel to obtain the flexible pressure sensor.
Effects of the embodiment
The conductivity and stability (i.e., bending resistance, adhesion) of the pressure sensors prepared in examples 1 to 3 and comparative examples 1 to 3 were compared; wherein the content of the first and second substances,
measuring the square resistance of the paper sample by using a four-probe conductivity meter, and calculating the conductivity of the paper sample (a calculation formula rho is 1/(Rs) d, wherein rho is the conductivity, Rs is the sheet resistance of the sample, and d is the thickness of the sample);
the stability test (number of bending cycles) of the pressure sensor was carried out with specific reference to literature (Wei, Yong, Lin, et al. silver nanowires coated on coating for flexible pressure sensors [ J ]. Journal of Materials Chemistry C Materials for Optical & Electronic Devices, 2016.);
the adhesion test (number of tape tests) was carried out with reference to the literature (Bras, Julie, Denneulin, et al.Positive impact of cellulose fibers on silver wires for transfer control films [ J ]. Journal of Materials Chemistry C Materials for Optical & Electronic Devices, 2016).
The results are shown in table 1 below:
table 1 analysis of performance of pressure sensors of examples and comparative examples
As can be seen from the performance test results in Table 1, the flexible pressure sensor provided by the invention has the advantages of good conductivity, strong stability (i.e., good bending resistance and strong adhesion), and the like. In addition, the method has the advantages of simple and quick operation, low cost and no pollution. Compared with a coating method, the vacuum filtration method has higher utilization rate of raw materials, and avoids the waste of the raw materials. Finally, the paper base has the advantages of flexibility, light weight, biodegradability, biocompatibility, low cost, wide source, recyclability, easiness in recycling and the like, so that the flexible pressure sensor provided by the invention has a potential application prospect in wearable electronic equipment.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.
Claims (9)
1. A preparation method of a paper-based flexible pressure sensor is characterized by comprising the following steps:
(1) dispersing silver nanowires into ethanol to obtain AgNWs dispersion liquid; dispersing the nano microcrystalline cellulose into water to obtain a CNC dispersion liquid; then uniformly mixing the AgNWs dispersion liquid and the CNC dispersion liquid to obtain a mixed liquid of AgNWs and CNC;
(2) depositing a chitosan solution and a mixed solution of AgNWs and CNC on the paper base in sequence by taking the paper base as a substrate in a vacuum filtration mode, and drying to obtain the flexible pressure sensor based on the paper base;
the deposition amount of the chitosan in the step (2) is 35-120 g/m 2 ；
The deposition amount of AgNWs in the step (2) is 30-50 g/m 2 ；
The deposition amount of the CNC in the step (2) is 5-20 g/m 2 ；
The nano microcrystalline cellulose in the step (1) is prepared by the following method: crushing wood pulp, adding a concentrated sulfuric acid solution, uniformly mixing, stirring and reacting for 80-100 min under the condition of water bath at 45-55 ℃, adding water to stop the reaction, cooling to room temperature, centrifuging, and dialyzing to obtain nano microcrystalline cellulose;
the wood pulp is hardwood pulp;
the concentration of the concentrated sulfuric acid solution is 55-64% by mass percent;
the dialysis is carried out by adopting a dialysis bag with the molecular weight cutoff of 8000-14000; wherein the dialyzate used for dialysis is distilled water.
2. The method of making a paper-based flexible pressure sensor as defined in claim 1, wherein:
the deposition amount of the chitosan in the step (2) is 39.81-119.43 g/m 2
The deposition amount of AgNWs in the step (2) is 31.85-47.78 g/m 2 ；
The deposition amount of the CNC in the step (2) is 7.96-15.92 g/m 2 。
3. The method of making a paper-based flexible pressure sensor as defined in claim 1, wherein:
the silver nanowire in the step (1) is prepared by the following method: adding copper polyvinylpyrrolidone into ethylene glycol, heating and stirring uniformly, and then cooling to room temperature to obtain a PVP solution; then adding silver nitrate into PVP solution, quickly stirring to form transparent and uniform liquid, then adding FeCl 3 The ethylene glycol solution is stirred and mixed uniformly, then the reaction is carried out at the temperature of 125-140 ℃, after the reaction is finished, the solution is cooled to room temperature, and the solution is centrifuged and washed to obtain silver nanowires;
the polyvinyl pyrrolidine copper, the silver nitrate and the FeCl 3 In a molar ratio of 19:5600 to 8380: 10;
the weight average molecular weight of the polyvinyl pyrrolidone copper is 44000-54000;
the heating temperature is 60 +/-5 ℃;
the FeCl-containing material 3 The concentration of the ethylene glycol solution is 550-650 mu mol/L;
the rapid stirring time is 1-2 min;
the reaction time is 3-6 h;
the centrifugation conditions are as follows: centrifuging at 9000rpm for 10-15 min;
the washing is sequentially carried out by using acetone and ethanol.
4. The method of making a paper-based flexible pressure sensor as defined in claim 1, wherein:
the reaction conditions are as follows: reacting at 50 ℃ for 90 min;
the water addition termination reaction is a water addition termination reaction with the volume 8-10 times that of the system.
5. The method of making a paper-based flexible pressure sensor as defined in claim 1, wherein:
the concentration of the AgNWs dispersion liquid in the step (1) is 1.0-2.0% by mass;
the mass percentage of the concentration of the CNC dispersion liquid in the step (1) is 0.5-1.0%;
the volume ratio of the AgNWs dispersion liquid to the CNC dispersion liquid in the step (1) is 1-3: 1;
the chitosan solution in the step (2) is a chitosan formic acid solution with the mass percentage of 1.0-3.0% and the pH value of 2.0.
6. The method of making a paper-based flexible pressure sensor as defined in claim 1, wherein:
mixing in the step (1) by adopting a vortex oscillator;
the paper base in the step (2) is filter paper;
the drying in the step (2) is drying in a vacuum drying oven: the drying temperature is 45-75 ℃, and the drying time is 30 min.
7. A flexible pressure sensor based on paper base, characterized in that: prepared by the method of any one of claims 1 to 6.
8. Use of the paper-based flexible pressure sensor of claim 7 in sensing materials, biomimetic robots and/or medical real-time monitoring devices.
9. Use according to claim 8, characterized in that:
the sensing material is used for a sensor and/or a wearable electronic device;
the medical real-time monitoring equipment comprises monitoring equipment for monitoring limb movement, pulse and heart rate of a human body.
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| CN103440907A (en) * | 2013-09-05 | 2013-12-11 | 中国科学院青岛生物能源与过程研究所 | Cellulose nanofibers and silver nanowires composite conductive film and preparation method of composite conductive film |
| CN106854842A (en) * | 2017-01-18 | 2017-06-16 | 华南理工大学 | A kind of technique of synchronously producing cellulosic element nano whisker and ethanol |
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| CN109445224A (en) * | 2018-12-24 | 2019-03-08 | 中山大学 | Promote the Electronic Paper device preparation method of wearing comfort |
| CN109992169A (en) * | 2019-03-27 | 2019-07-09 | 华南理工大学 | A kind of nano-cellulose paper base touch sensing and the preparation method and application thereof |
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| CN103440907A (en) * | 2013-09-05 | 2013-12-11 | 中国科学院青岛生物能源与过程研究所 | Cellulose nanofibers and silver nanowires composite conductive film and preparation method of composite conductive film |
| CN106854842A (en) * | 2017-01-18 | 2017-06-16 | 华南理工大学 | A kind of technique of synchronously producing cellulosic element nano whisker and ethanol |
| CN109081388A (en) * | 2018-08-30 | 2018-12-25 | 盐城市新能源化学储能与动力电源研究中心 | A kind of method of quickly cleaning water |
| CN109445224A (en) * | 2018-12-24 | 2019-03-08 | 中山大学 | Promote the Electronic Paper device preparation method of wearing comfort |
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