CN114136506A - Preparation and recovery method of stress sensor - Google Patents
Preparation and recovery method of stress sensor Download PDFInfo
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- CN114136506A CN114136506A CN202111388511.1A CN202111388511A CN114136506A CN 114136506 A CN114136506 A CN 114136506A CN 202111388511 A CN202111388511 A CN 202111388511A CN 114136506 A CN114136506 A CN 114136506A
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- 229920002451 polyvinyl alcohol Polymers 0.000 claims abstract description 63
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Images
Classifications
-
- 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
- G01L1/16—Measuring force or stress, in general using properties of piezoelectric devices
Abstract
The invention discloses a preparation process and a recovery process of a semi-coating structure stress sensor taking polyvinyl alcohol and metal nanowires as main materials. The preparation process comprises the following steps: firstly, evaporating a polyvinyl alcohol aqueous solution to a viscous state, then uniformly coating the aqueous dispersion of the metal nanowires on polyvinyl alcohol, and continuously evaporating at room temperature to form a film to prepare the stress sensor with the semi-coating structure. The stress sensor has good responsiveness to deformation such as stretching and pressure, has the characteristics of high response speed, high sensitivity, good stability, excellent repeatability and the like, and can be applied to the fields of monitoring various actions of a human body, human-computer interaction in the future and the like. In addition, the sensor after being used can adopt simple processes of solvent dissolution, drying and ultrasonic dispersion to realize the high-efficiency recovery and reutilization of the metal nanowires, and is suitable for popularization and application.
Description
Technical Field
The invention belongs to the technical field of functional materials and preparation thereof, and particularly relates to a method for preparing and recovering a stress sensor.
Background
With the rapid popularization and wide application of consumer electronics products such as mobile phones, tablet computers, wearable electronics and the like, the demand is increasing day by day. In order to gain a larger market and obtain a richer profit, the competition among consumer electronics manufacturers is unprecedented and intense, so that the update iteration period of the consumer electronics is greatly shortened, and the problem of eliminating electronic products or electronic garbage is more and more obvious. On one hand, the consumption of noble metals for manufacturing electronic components is rapidly increased, a large amount of noble metals are required to be exploited, the cost of electronic products is difficult to be effectively reduced, and huge pressure is brought to earth resources; on the other hand, the electronic waste, particularly harmful metals such as lead, mercury and the like contained in the electronic waste have potential threat to the earth ecological environment and are not beneficial to sustainable development. Therefore, the development of green, environment-friendly and recyclable electronic products is one of the key development directions in the future. In addition, the stress sensor with flexibility and stretchability has wide application in the fields of motion health monitoring, robots, human-computer interaction and the like.
At present, the conductive film is mainly prepared by means of ink-jet printing, spin coating and the like, the introduced conductive materials are usually completely attached to the surface of the substrate and are in direct contact with air, the risk of performance reduction caused by oxidation exists, and the corresponding problem needs to be solved by further adopting complex methods such as packaging and the like; meanwhile, the conductive material attached to the surface of the substrate is easy to fall off, displace and the like in the using process, and great influence is generated on the stability of the conductive film.
Disclosure of Invention
The invention mainly aims to solve the problems and the defects in the prior art, and provides a stress sensor which is based on a half-coating structure formed by polyvinyl alcohol and metal nanowires, has higher tensile strength and better flexibility, and has the characteristics of quick response, high sensitivity, good stability and excellent repeatability on various external force strain monitoring; and the related preparation and recovery process has the advantages of simple operation, low cost, environmental protection and good repeatability, and is suitable for popularization and application.
In order to achieve the purpose, the invention adopts the technical scheme that:
a method for preparing a stress sensor comprises the following steps:
1) heating and dissolving polyvinyl alcohol in water to obtain a polyvinyl alcohol solution; adding the mixture into a mold (room temperature), and evaporating at room temperature to obtain viscous polyvinyl alcohol;
2) the method comprises the following steps of (1) dripping and casting a metal nanowire dispersion liquid on the surface of viscous polyvinyl alcohol, and carrying out natural evaporation to form a film, wherein in the dripping and natural evaporation processes, the metal nanowires are gradually and uniformly distributed on the upper part of a polyvinyl alcohol matrix, wherein most of the metal nanowires are coated on the upper part of the polyvinyl alcohol matrix, and a small amount of the metal nanowires are exposed on the surface of the polyvinyl alcohol matrix; forming a stress sensor which is laminated and combined and has a semi-coating structure.
In the scheme, the heating and dissolving temperature in the step 1) is 40-150 ℃.
In the scheme, the dosage ratio of the polyvinyl alcohol to the water is 1g: 20-200 mL.
In the scheme, the room-temperature evaporation temperature is 10-30 ℃, and the time is 1-30 min.
In the scheme, the diameter of the metal nanowire is 30-120 nm, and the length of the metal nanowire is 30-200 mu m.
In the above scheme, the metal nanowire includes, but is not limited to, one or more of a silver nanowire, a copper nanowire, a gold nanowire, and the like.
In the scheme, the concentration of the metal nanowire dispersion liquid is 1-10 mg/mL.
In the scheme, the solvent adopted in the metal nanowire dispersion liquid can be one or more of methanol, ethanol, acetone, isopropanol, ethylene glycol, glycerol, deionized water and the like.
In the scheme, the mass ratio of the introduced metal nanowire dispersion liquid to the polyvinyl alcohol solution is 1 (1-50).
In the scheme, the metal nanowires are required to be uniformly spread on the surface of the polyvinyl alcohol.
In the scheme, the temperature of the natural evaporation film forming is 10-30 ℃; the time is 12-36 h.
The stress sensor prepared according to the scheme comprises a polyvinyl alcohol flexible substrate and metal nanowires distributed in the polyvinyl alcohol flexible substrate and on the surface of the polyvinyl alcohol flexible substrate, wherein most of the metal nanowires are coated on the upper part of the polyvinyl alcohol flexible substrate to form a uniformly distributed and communicated conductive network, so that the long-term stability of a conductive material is ensured; part of the composite material is exposed on the upper surface of the polyvinyl alcohol substrate, so that the surface contact resistance of the obtained composite material is provided, and a layered composite semi-coating structure is further formed.
The invention also provides a method for recovering the conductive material metal nanowire in the stress sensor, which comprises the following steps:
and (3) putting the stress sensor into water, heating and dissolving, removing supernatant, adding water, heating and dissolving, repeating the operation for a plurality of times, adding a proper amount of solvent (water, ethanol and the like) for ultrasonic dispersion, and obtaining the dispersion liquid of the metal nanowires again.
In the scheme, the ultrasonic dispersion time is 10-300 s.
In the scheme, the solvent adopted by the ultrasonic treatment comprises one or more of methanol, ethanol, acetone, isopropanol, glycol, glycerol, deionized water and the like.
In the scheme, the heating and dissolving temperature is 40-150 ℃.
The principle of the invention is as follows:
1) the invention firstly proposes that a metal nanowire dispersion liquid is introduced into viscous polyvinyl alcohol, and then synchronous drying and film forming are carried out to prepare the nano composite material with a layered semi-coating structure, wherein the polyvinyl alcohol forms a semi-coating structure for the metal nanowire, a polyvinyl alcohol substrate provides mechanical support for a sensor, and the upper polyvinyl alcohol/metal nanowire (most of which is coated in the polyvinyl alcohol and a small amount of which is exposed on the surface of the polyvinyl alcohol to form a communicated conductive network) provides conductive strain capacity and is beneficial to improving the long-term stability of the conductivity of the metal nanowire; the metal nanowires form a conductive network in polyvinyl alcohol, effective connection can be established among the nanowires, contact points among the nanowires are regularly reduced after the nanowires are subjected to regular strain, a stable resistance change trend is formed, and then stress signals are converted into visible electric signals;
2) the invention can realize the quick and high-efficiency recycling of the core conductive material metal nanowire in the sensor: before absorbing water, the polyvinyl alcohol is an elastic body capable of stretching and straining, molecular chains of the elastic body are mutually wound and bent, and a three-dimensional network-shaped cross-linking structure is formed between the chains; in aqueous solution, hydroxyl on the main chain is dissociated out of the network, and other charged groups are mutually exclusive and are very easy to dissolve; the polyvinyl alcohol component in the precipitate is removed by repeated washing, the purity of the recovered metal nanowires can be effectively improved, and then the dispersibility of the metal nanowires in the solvent can be further improved by optimizing the ultrasonic time and selecting different solvents, so that the cyclic utilization of the metal nanowires is realized.
Compared with the prior art, the invention has the beneficial effects that:
1) the stress sensor provided by the invention is a half-coating structure formed by layering and compounding polyvinyl alcohol and metal nanowires; the metal nanowires can form a good conductive network on the surface of the stress sensor, provide excellent conductive performance, and have the advantages of wide range, high sensitivity and the like on electric signals generated by stress; the polyvinyl alcohol can effectively improve the environmental stability of the metal nanowire and the repeatability of the sensor by well coating the metal nanowire; in addition, the polyvinyl alcohol used as the base material is nontoxic to human bodies and the environment, has good biocompatibility and biodegradability, excellent film forming property and mechanical flexibility and is suitable for being used for green and environment-friendly flexible base materials;
2) the recovery process of the stress sensor provided by the invention utilizes the characteristic that polyvinyl alcohol is easily dissolved in water; the semi-coating structure sensor is dissolved in water, and the dissolution of polyvinyl alcohol is promoted by repeated heating, so that the purity of the recovered metal nanowires can be effectively improved; aiming at different metal nanowires, the form and the performance of the metal nanowires can not be obviously changed by adjusting the types of solvents, ultrasonic power and ultrasonic time, and the metal nanowires can be efficiently recycled.
Drawings
FIG. 1 is a schematic diagram of a process for preparing the stress sensor of example 1;
FIG. 2 is a scanning electron microscope photograph of (a) the surface and (b) the brittle fracture section of the sensor obtained in example 1;
FIG. 3 is the response of the sensor obtained in example 1 to the bending motion of a finger;
FIG. 4 is the response of the 3-sensor obtained in example 2 to the bending motion of the elbow;
FIG. 5 is a schematic view showing a process for recovering silver nanowires from the sensor obtained in example 2;
fig. 6 is an XRD pattern of the silver nanowires recovered in example 2.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
In the following embodiments, the metal nanowires used are silver nanowires, the diameter of the metal nanowires is 30 to 120nm, and the length of the metal nanowires is 30 to 200 μm; specific reference is made to the preparation of "facility synthesis of very-long silver nanowires for transparent electrodes".
In the following examples, polyvinyl alcohol pellets having an average degree of polymerization of 1750. + -. 50 and a molecular weight of about 77000 were used as commercially available products.
Example 1
A semi-coating structure stress sensor is shown in a schematic diagram of a preparation process of the semi-coating structure stress sensor in figure 1, and a specific preparation method comprises the following steps:
1) dissolving 1.0g of polyvinyl alcohol particles in 50ml of deionized water, controlling the temperature at 100 ℃, pouring the polyvinyl alcohol particles into a mold (room temperature 25 ℃) after the polyvinyl alcohol is completely dissolved, and naturally evaporating the polyvinyl alcohol particles at the room temperature (25 ℃) for later use;
2) preparing 8ml of silver nanowire ethanol dispersion liquid with the concentration of 4.0 mg/ml;
3) after natural evaporation for 5min, the polyvinyl alcohol solution in the mould is highly viscous, and the silver nanowire ethanol dispersion liquid obtained in the step 2) is uniformly dripped into the highly viscous polyvinyl alcohol;
4) naturally evaporating the polyvinyl alcohol/silver nanowire complex system obtained in the step 3) for 24 hours at room temperature to form a film, and obtaining a polyvinyl alcohol and silver nanowire layered composite semi-cladding structure stress sensor;
5) respectively cutting the stress sensor in the step 4) by using scissors to obtain a strip-shaped sensor with the width of 10mm for later use.
FIG. 2 is a Scanning Electron Microscope (SEM) image of (a) the surface and (b) the brittle fracture cross-section of the sensor prepared in this example; it can be seen that: in the obtained product, most of the silver nanowires are uniformly coated on the upper part of the polyvinyl alcohol matrix (see figure (b)), and a small amount of silver nanowires are exposed on the surface of the polyvinyl alcohol matrix (see the brighter part marked by the box of figure (a)); the introduced silver nanowires have ultrahigh length-diameter ratio, a conductive network can be built in polyvinyl alcohol, and after the silver nanowires are subjected to stretchability, the contact points among the silver nanowires are reduced, so that the resistance is increased; when the contact points between the silver nanowires recover after the stretching recovery, the resistance recovers.
FIG. 3 is a graph of the response of a stress sensor having a width of 10mm to a finger bending motion (finger bending 90); the results show that: the resulting sensor is also responsive to slight finger bending, exhibits high sensitivity, and is also highly repeatable.
Example 2
A semi-coating structure stress sensor is shown in a schematic diagram of a preparation process of the semi-coating structure stress sensor in figure 1, and a specific preparation method comprises the following steps:
1) dissolving 1.0g of polyvinyl alcohol particles in 50ml of deionized water, controlling the temperature at 100 ℃, pouring the polyvinyl alcohol particles into a mould (room temperature is 20 ℃) after the polyvinyl alcohol is completely dissolved, and naturally evaporating the polyvinyl alcohol particles at the room temperature (20 ℃) for later use;
2) preparing 8ml of silver nanowire ethanol dispersion liquid with the concentration of 4.8 mg/ml;
3) after natural evaporation for 5min, the polyvinyl alcohol solution in the mould is highly viscous, and the silver nanowire ethanol dispersion liquid obtained in the step 2) is uniformly dripped into the highly viscous polyvinyl alcohol;
4) naturally evaporating the polyvinyl alcohol/silver nanowire complex system obtained in the step 3) to form a film at room temperature to obtain a polyvinyl alcohol and silver nanowire layered composite semi-cladding structure stress sensor;
5) respectively cutting the stress sensor in the step 4) by using scissors to obtain a strip-shaped sensor with the width of 10mm for later use.
Figure 4 is a graph of the response of a stress sensor of 10mm width to elbow finger bending.
The invention also provides a recovery method of the semi-coating structure stress sensor, 2.0g of the stress sensor is placed in water and heated to 90 ℃ for dissolution, supernatant fluid is removed, ethanol is added, the supernatant fluid is removed after standing and layering, a proper amount of ethanol is added for ultrasonic 30s dispersion, and the concentration of the dispersion liquid of the newly obtained silver nanowires is measured to be 4.4 mg/ml; the specific recovery process is schematically shown in FIG. 5; XRD of the recovered silver nanowires is shown in fig. 6. The results show that: the chemical composition of the recovered silver nanowires is the same as that of the original silver nanowires. In addition, the scanning electron microscope result of the recovered silver nanowires shows that the morphology of the silver nanowires obtained by the recovery method is basically not changed.
The above embodiments are merely examples for clearly illustrating the present invention and do not limit the present invention. Other variants and modifications of the invention, which are obvious to those skilled in the art and can be made on the basis of the above description, are not necessary or exhaustive for all embodiments, and are therefore within the scope of the invention.
Claims (10)
1. The preparation method of the stress sensor is characterized by comprising the following steps of:
1) heating polyvinyl alcohol to dissolve in water, then adding the polyvinyl alcohol into a mould, and evaporating at room temperature to obtain viscous polyvinyl alcohol;
2) and (3) dripping the metal nanowire dispersion liquid on the surface of viscous polyvinyl alcohol, and performing natural evaporation to form a film to form the stress sensor with a layered composite structure and a half-coating structure.
2. The preparation method according to claim 1, wherein the dosage ratio of the polyvinyl alcohol to the water is 1g: 20-200 mL.
3. The method according to claim 1, wherein the room temperature evaporation temperature is 10 to 30 ℃ and the time is 1 to 30 min.
4. The method according to claim 1, wherein the metal nanowires have a diameter of 30 to 120nm and a length of 30 to 200 μm.
5. The preparation method according to claim 1, wherein the metal nanowires are one or more of silver nanowires, copper nanowires, and gold nanowires.
6. The method according to claim 1, wherein the concentration of the metal nanowire dispersion is 1 to 10 mg/mL.
7. The preparation method according to claim 1, wherein the natural evaporation temperature is 10-30 ℃ and the time is 12-36 h.
8. The stress sensor prepared by the preparation method of any one of claims 1 to 7, which comprises a polyvinyl alcohol flexible substrate and metal nanowires distributed in the polyvinyl alcohol flexible substrate and on the surface of the polyvinyl alcohol flexible substrate, wherein the metal nanowires are partially coated in the polyvinyl alcohol flexible substrate and partially exposed on the surface of the polyvinyl alcohol flexible substrate to form a layered composite semi-coating structure.
9. A method for recovering metal nanowires of conductive material in the stress sensor according to claim 8, comprising the steps of: and (3) putting the stress sensor into water, heating and dissolving, removing supernatant, repeating the steps, adding a solvent for ultrasonic dispersion, and obtaining the dispersion liquid of the metal nanowires again.
10. The recycling method according to claim 9, wherein the ultrasonic dispersion time is 10 to 300 s.
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| JP2017014621A (en) * | 2015-07-01 | 2017-01-19 | 昭和電工株式会社 | Production method of metal nanowire dispersion and production method of metal nanowire ink |
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| WO2020174223A1 (en) * | 2019-02-25 | 2020-09-03 | Oxford University Innovation Limited | Sensor |
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2021
- 2021-11-22 CN CN202111388511.1A patent/CN114136506A/en active Pending
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| Publication number | Priority date | Publication date | Assignee | Title |
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| WO2015049067A2 (en) * | 2013-10-02 | 2015-04-09 | The Provost, Fellows, Foundation Scholars, And The Other Members Of Board, Of The College Of The Holy And Undivided Trinity Of Queen Elizabeth, Near Dublin | Sensitive, high-strain, high-rate, bodily motion sensors based on conductive nano-material-rubber composites |
| CN104021840A (en) * | 2014-06-18 | 2014-09-03 | 中南大学 | Low-temperature curing high-conductive silver paste, preparation method of low-temperature curing high-conductive silver paste, conductive film and preparation method of conductive film |
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| CN109387307A (en) * | 2018-12-12 | 2019-02-26 | 深圳大学 | A kind of flexibility stress sensor and preparation method thereof |
| WO2020174223A1 (en) * | 2019-02-25 | 2020-09-03 | Oxford University Innovation Limited | Sensor |
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