CN114396869B - Preparation method of extreme environment tolerance type high-sensitivity strain sensor - Google Patents
Preparation method of extreme environment tolerance type high-sensitivity strain sensor Download PDFInfo
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- CN114396869B CN114396869B CN202210056557.1A CN202210056557A CN114396869B CN 114396869 B CN114396869 B CN 114396869B CN 202210056557 A CN202210056557 A CN 202210056557A CN 114396869 B CN114396869 B CN 114396869B
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01B—MEASURING LENGTH, THICKNESS OR SIMILAR LINEAR DIMENSIONS; MEASURING ANGLES; MEASURING AREAS; MEASURING IRREGULARITIES OF SURFACES OR CONTOURS
- G01B7/00—Measuring arrangements characterised by the use of electric or magnetic techniques
- G01B7/16—Measuring arrangements characterised by the use of electric or magnetic techniques for measuring the deformation in a solid, e.g. by resistance strain gauge
- G01B7/18—Measuring arrangements characterised by the use of electric or magnetic techniques for measuring the deformation in a solid, e.g. by resistance strain gauge using change in resistance
Abstract
The invention relates to a preparation method of an extreme environment tolerance type high-sensitivity strain sensor, which comprises the following steps: adding distilled water into polyvinyl alcohol, swelling, stirring and heating until the polyvinyl alcohol is completely dissolved, preparing polyvinyl alcohol gel, and cooling to room temperature for standby; dropwise adding the glycerol solution into the polyvinyl alcohol solution, and uniformly stirring to obtain a polyvinyl alcohol/glycerol mixed solution; dropping PEDOT/PSS water solution into polyvinyl alcohol/glycerin solution, and rapidly and uniformly stirring to obtain poly (3, 4-ethylenedioxythiophene): a mixed solution of polystyrene sulfonic acid/polyvinyl alcohol/glycerin; and (3) rapidly injecting the obtained mixed solution into a capillary tube by using an injector, repeatedly freezing and thawing at low temperature, taking out the gel fiber from the glass capillary tube, and airing at room temperature to obtain the PEDOT: PSS@PVA hydrogel fiber, namely the extremely environment-tolerant high-sensitivity strain sensor. The preparation method of the extreme environment tolerance type high-sensitivity strain sensor has the advantages of simple process, low cost and good extreme environment tolerance.
Description
Technical Field
The invention relates to the technical field of strain sensors, in particular to a preparation method of an extreme environment tolerance type high-sensitivity strain sensor.
Background
The rapid development of flexible wearable electronics has led to a hot interest in flexible sensors, which are of great interest due to their ultra-high stretchability, biocompatibility and high plasticity. However, most of the flexible sensors commonly used at present can only work under room temperature conditions and are difficult to adapt to extremely cold or dry environments.
If the sensor is to be operated normally in extremely cold and dry environments, it is desirable that such sensors still have high stretchability and mechanical strength at extremely low temperatures, while also ensuring high sensitivity. The lowest withstand temperature of the sensor can be lowered by adding inorganic salts or organic solvents (CN 202110838025.9; adv. Funct. Mater.2021, 2101696), but such sensors have the disadvantages of low mechanical strength, poor withstand temperature, low sensitivity, etc. The lowest temperature tolerance of the sensor is reduced by multicomponent crosslinking while the mechanical strength is increased (Biomacromolecules, 2021, 22, 1220-1230; chemEngJ,2021, 403, 126431-126445; acsappl. Mater. Interfaces,2019, 11, 9405-9414.), but such sensors have limited sensitivity and are difficult to use for fine physiological signal detection, and high sensitivity strain sensors currently available for extreme environments still have drawbacks.
Disclosure of Invention
The invention aims to solve the defects of the prior art and provide a preparation method of a high-sensitivity strain sensor with simple process, low cost and extreme environmental tolerance.
In order to achieve the above purpose, the present invention adopts the following technical scheme:
a preparation method of an extreme environment tolerance type high-sensitivity strain sensor comprises the following steps:
step 1, adding distilled water into polyvinyl alcohol, swelling, stirring and heating until the polyvinyl alcohol is completely dissolved, preparing polyvinyl alcohol gel, and cooling to room temperature for standby;
step 2, dropwise adding the glycerol solution into the polyvinyl alcohol gel prepared in the step 1, and uniformly stirring to prepare a polyvinyl alcohol/glycerol mixed solution;
step 3, poly (3, 4-ethylenedioxythiophene): and (2) dropwise adding the aqueous solution of polystyrene sulfonic acid, namely the aqueous solution of PEDOT and PSS into the mixed solution of polyvinyl alcohol and glycerol prepared in the step (2), and rapidly and uniformly stirring to obtain poly (3, 4-ethylenedioxythiophene): a mixed solution of polystyrene sulfonic acid/polyvinyl alcohol/glycerol (PEDOT: PSS/PVA/GL);
step 4, rapidly injecting the mixed solution obtained in the step 3 into a glass capillary by using a syringe, repeatedly freezing and thawing at low temperature, taking out the prepared gel fiber from the glass capillary, and airing at room temperature to obtain the PEDOT: PSS@PVA hydrogel fiber, namely the extremely environment-tolerant high-sensitivity strain sensor
Further, in the step 1, the mass ratio of the distilled water to the polyvinyl alcohol is 5-10:1. The polyvinyl alcohol gel prepared under the condition has high stretchability and strong breaking strength, and can meet various application scenes.
Further, the swelling temperature in the step 1 is 55-65 ℃ and the time is 60-70 min; the temperature of stirring and heating is 80-95 ℃ and the time is 1-3 h. Under these conditions, the polyvinyl alcohol can be sufficiently dissolved in a short period of time.
Further, the glycerol solution in the step 2 is prepared by adding 0.05-0.3 g of glycerol into 0.2mL of deionized water; the mass ratio of the glycerol to the polyvinyl alcohol is 1-4: 10. the PEDOT prepared under the condition forms a dynamic hydrogen bond between the glycerin in PSS@PVA and the polyvinyl alcohol and between the glycerin and water molecules, so that the minimum tolerance temperature of the hydrogel can be improved, and the water retention of the hydrogel can be improved.
Further, the volume of the PEDOT/PSS aqueous solution in the step 3 is 0.5-1.5 mL. PEDOT: PSS is added to the PEDOT: PSS@PVA gel as a conductive agent, and the resistance of the hydrogel is controlled by controlling the addition amount of PEDOT: PSS, so that the sensitivity of the sensor is further controlled.
Further, in the step 4, the mixed solution is quickly injected into the glass capillary tube with the inner diameter of 1mm by using the injector, so that the mixed solution can be quickly transferred, and the glass capillary tube plays a role of a die. The diameter of the gel fiber can be controlled by the method, and the surface of the dried gel can be ensured to be smoother.
Further, the freezing temperature in the step 4 is-20 ℃, and the number of freeze-thawing cycles is 5-10. The conditions can ensure that PEDOT PSS/PVA/GL precursor solution can be frozen rapidly. In the repeated freezing-thawing process, water serving as a solvent is rapidly crystallized, and the formed ice crystals serve as templates to repeatedly squeeze the crosslinked polyvinyl alcohol molecular chains, so that the formation of a crystallization area is promoted, and the mechanical strength of the fiber is further enhanced. The PEDOT-PSS conductive particles are wrapped by water, glycerol and polyvinyl alcohol to form a three-dimensional network structure through the action of dynamic hydrogen bonds in the PEDOT-PSS/PVA/GL conductive hydrogel prepared under the condition, so that a conductive network is formed, the PEDOT-PSS conductive hydrogel has excellent tensile property and high sensitivity, can resist extremely cold conditions of minus 60 ℃, and has good flexibility after being placed for half a year at room temperature.
Compared with the prior art, the invention has the following advantages:
1. in the invention, polyvinyl alcohol is used as an elastic substrate, and the addition amount of the crosslinking agent can be controlled to regulate and control the poly (3, 4-ethylenedioxythiophene): tensile length mechanical strength of polystyrene sulfonic acid @ polyvinyl alcohol hydrogel fibers.
2. The glycerol is used as a cross-linking agent to enhance the flexibility of the polyvinyl alcohol substrate, and can be used as an anti-freezing agent and a water-retaining agent, so that the prepared sensor can still keep good flexibility at the extremely low temperature of 60 ℃ below zero, and still has flexibility after being placed for half a year at room temperature.
3. The poly (3, 4-ethylenedioxythiophene) prepared by the invention: the polystyrene sulfonic acid@polyvinyl alcohol hydrogel fiber can be used as a high-sensitivity strain sensor, can respond to 0.01% of tiny strain in time, and can detect 10% of strain at the extremely low air temperature of minus 60 ℃.
Drawings
FIG. 1 is a schematic diagram of poly (3, 4-ethylenedioxythiophene) prepared in example 3: a surface scanning electron microscope image of the polystyrene sulfonic acid@polyvinyl alcohol composite fiber;
FIG. 2 is a schematic representation of poly (3, 4-ethylenedioxythiophene) prepared in example 3: a cross-section scanning electron microscope image of the polystyrene sulfonic acid@polyvinyl alcohol composite fiber;
FIG. 3 is a schematic representation of poly (3, 4-ethylenedioxythiophene) prepared in example 3: stress-strain curve of polystyrene sulfonic acid @ polyvinyl alcohol composite fiber;
FIG. 4 is a schematic representation of poly 3, 4-ethylenedioxythiophene prepared in example 3: the polystyrene sulfonic acid@polyvinyl alcohol strain sensor responds to an electric signal with 0.01% -1% strain;
FIG. 5 is a schematic diagram of poly (3, 4-ethylenedioxythiophene) prepared in example 3: polystyrene sulfonic acid @ polyvinyl alcohol strain sensor test curve for 10% large strain stability at very low temperatures of-60 ℃.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1
A preparation method of a high-sensitivity piezoresistive strain sensor comprises the following steps:
(1) 10g of distilled water is added into 2.0g of polyvinyl alcohol powder, swelling is carried out for 60min at 55 ℃, stirring and heating are carried out for 1h at 80 ℃ until the polymer is completely dissolved, thus obtaining polyvinyl alcohol solution, and cooling to room temperature for standby.
(2) 0.05g of glycerol is added into 0.2mL of deionized water, and after uniform stirring, the mixture is rapidly added into 0.5g of polyvinyl alcohol gel in a dropwise manner, and the mixture is rapidly and uniformly stirred, so that a polyvinyl alcohol/glycerol solution is prepared.
(3) 0.5mL of poly 3, 4-ethylenedioxythiophene: dripping aqueous solution of polystyrene sulfonic acid (PEDOT: PSS) into polyvinyl alcohol/glycerol solution, and rapidly and uniformly stirring to obtain poly (3, 4-ethylenedioxythiophene): polystyrene sulfonic acid/polyvinyl alcohol/glycerin.
(4) Using a syringe, poly 3, 4-ethylenedioxythiophene: the polystyrene sulfonic acid/polyvinyl alcohol/glycerin mixed solution was rapidly injected into a glass capillary tube having an inner diameter of 1mm, and then frozen at a low temperature of-20 ℃ for one night, thawed at room temperature, and the number of freeze-thaw cycles was 5. Taking out the gel fiber from the glass capillary tube, and airing at room temperature to obtain the poly (3, 4-ethylenedioxythiophene): polystyrene sulfonic acid@polyvinyl alcohol (PEDOT: PSS@PVA) hydrogel fibers are the extremely environment-tolerant high-sensitivity strain sensor.
Example 2
A preparation method of a high-sensitivity piezoresistive strain sensor comprises the following steps:
1) 10g of distilled water is added into 1.2g of polyvinyl alcohol powder, swelling is carried out for 60min at 60 ℃, stirring and heating are carried out for 2h at 85 ℃ until the polymer is completely dissolved, thus obtaining polyvinyl alcohol solution, and cooling to room temperature for standby.
(2) 0.08g of glycerol is added into 0.2mL of deionized water, and after uniform stirring, the mixture is rapidly added into 0.5g of polyvinyl alcohol gel in a dropwise manner, and the mixture is rapidly and uniformly stirred, so that a polyvinyl alcohol/glycerol solution is prepared.
(3) 0.8mL of poly 3, 4-ethylenedioxythiophene: dripping aqueous solution of polystyrene sulfonic acid (PEDOT: PSS) into polyvinyl alcohol/glycerol solution, and rapidly and uniformly stirring to obtain poly (3, 4-ethylenedioxythiophene): polystyrene sulfonic acid/polyvinyl alcohol/glycerin.
(4) Using a syringe, poly 3, 4-ethylenedioxythiophene: the polystyrene sulfonic acid/polyvinyl alcohol/glycerin mixed solution was rapidly injected into a glass capillary tube having an inner diameter of 1mm, and then frozen at a low temperature of-20 ℃ for one night, thawed at room temperature, and the number of freeze-thaw cycles was 5. Taking out the gel fiber from the glass capillary tube, and airing at room temperature to obtain the poly (3, 4-ethylenedioxythiophene): polystyrene sulfonic acid@polyvinyl alcohol (PEDOT: PSS@PVA) hydrogel fibers are the extremely environment-tolerant high-sensitivity strain sensor.
Example 3
A preparation method of a high-sensitivity piezoresistive strain sensor comprises the following steps:
(1) 10g of distilled water is added into 1.0g of polyvinyl alcohol powder, swelling is carried out for 60min at 60 ℃, stirring and heating are carried out for 1h at 90 ℃ until the polymer is completely dissolved, thus obtaining polyvinyl alcohol gel, and cooling to room temperature for standby.
(2) 0.20g of glycerol is added into 0.2mL of deionized water, and after uniform stirring, the mixture is rapidly added into 0.5g of polyvinyl alcohol gel in a dropwise manner, and the mixture is rapidly and uniformly stirred, so that a polyvinyl alcohol/glycerol solution is prepared.
(3) 1.0mL of poly 3, 4-ethylenedioxythiophene: dripping aqueous solution of polystyrene sulfonic acid (PEDOT: PSS) into polyvinyl alcohol/glycerol solution, and rapidly and uniformly stirring to obtain poly (3, 4-ethylenedioxythiophene): polystyrene sulfonic acid/polyvinyl alcohol/glycerin.
(4) Using a syringe, poly 3, 4-ethylenedioxythiophene: the polystyrene sulfonic acid/polyvinyl alcohol/glycerin mixed solution was rapidly injected into a glass capillary tube having an inner diameter of 1mm, and then frozen at a low temperature of-20 ℃ for one night, thawed at room temperature, and the number of freeze-thaw cycles was 5. Taking out the gel fiber from the glass capillary tube, and airing at room temperature to obtain the poly (3, 4-ethylenedioxythiophene): polystyrene sulfonic acid@polyvinyl alcohol (PEDOT: PSS@PVA) hydrogel fibers are the extremely environment-tolerant high-sensitivity strain sensor.
FIGS. 1 and 2 are flexible, stretchable poly 3, 4-ethylenedioxythiophene prepared in example 3 of the present invention: the surface and cross section scanning electron microscope images of the polystyrene sulfonic acid@polyethylene hydrogel fiber show that the fiber surface is smoother, and the poly 3, 4-ethylenedioxythiophene: polystyrene sulfonic acid can be uniformly wrapped in a polyvinyl alcohol three-dimensional network structure, and when the breaking elongation is 519.9%, the breaking strength is 13.8MPa (figure 3). As can be seen from fig. 4, the polypyrrole/polyvinyl alcohol sensor can detect 0.01% of minute strain, and can stably detect 10% of large strain at an extremely low temperature of-60 ℃ and respond to an electric signal in time (fig. 5).
Example 4
A preparation method of a high-sensitivity piezoresistive strain sensor comprises the following steps:
(1) 10g of distilled water is added into 1.0g of polyvinyl alcohol powder, swelling is carried out for 60min at 60 ℃, stirring and heating are carried out for 2h at 90 ℃ until the polymer is completely dissolved, thus obtaining polyvinyl alcohol gel, and cooling to room temperature for standby.
(2) 0.1g of glycerol is added into 0.2mL of deionized water, and after uniform stirring, the mixture is rapidly added into 0.5g of polyvinyl alcohol gel in a dropwise manner, and the mixture is rapidly and uniformly stirred, so that a polyvinyl alcohol/glycerol solution is prepared.
(3) 1.2mL of poly 3, 4-ethylenedioxythiophene: dripping aqueous solution of polystyrene sulfonic acid (PEDOT: PSS) into polyvinyl alcohol/glycerol solution, and rapidly and uniformly stirring to obtain poly (3, 4-ethylenedioxythiophene): polystyrene sulfonic acid/polyvinyl alcohol/glycerin.
(4) Using a syringe, poly 3, 4-ethylenedioxythiophene: the polystyrene sulfonic acid/polyvinyl alcohol/glycerin mixed solution was rapidly injected into a glass capillary having an inner diameter of 1mm, and then frozen at a low temperature of-20 ℃ for one night, thawed at room temperature, and the number of freeze-thaw cycles was 7. Taking out the gel fiber from the glass capillary tube, and airing at room temperature to obtain the poly (3, 4-ethylenedioxythiophene): polystyrene sulfonic acid@polyvinyl alcohol (PEDOT: PSS@PVA) hydrogel fibers are the extremely environment-tolerant high-sensitivity strain sensor.
Example 5
A preparation method of a high-sensitivity piezoresistive strain sensor comprises the following steps:
(1) 10g of distilled water is added into 1.0g of polyvinyl alcohol powder, swelling is carried out for 70min at 65 ℃, stirring and heating are carried out for 3h at 95 ℃ until the polymer is completely dissolved, thus obtaining polyvinyl alcohol gel, and cooling to room temperature for standby.
(2) 0.30g of glycerol is added into 0.2mL of deionized water, and after uniform stirring, the mixture is rapidly added into 0.5g of polyvinyl alcohol gel in a dropwise manner, and the mixture is rapidly and uniformly stirred, so that a polyvinyl alcohol/glycerol solution is prepared.
(3) 1.5mL of poly 3, 4-ethylenedioxythiophene: dripping aqueous solution of polystyrene sulfonic acid (PEDOT: PSS) into polyvinyl alcohol/glycerol solution, and rapidly and uniformly stirring to obtain poly (3, 4-ethylenedioxythiophene): polystyrene sulfonic acid/polyvinyl alcohol/glycerin.
(4) Using a syringe, poly 3, 4-ethylenedioxythiophene: the polystyrene sulfonic acid/polyvinyl alcohol/glycerin mixed solution was rapidly injected into a glass capillary tube having an inner diameter of 1mm, and then frozen at a low temperature of-20 ℃ for one night, thawed at room temperature, and the number of freeze-thaw cycles was 10. Taking out the gel fiber from the glass capillary tube, and airing at room temperature to obtain the poly (3, 4-ethylenedioxythiophene): polystyrene sulfonic acid@polyvinyl alcohol (PEDOT: PSS@PVA) hydrogel fibers are the extremely environment-tolerant high-sensitivity strain sensor.
Claims (6)
1. The preparation method of the extreme environment tolerance type high-sensitivity strain sensor comprises the following steps:
step 1, adding distilled water into polyvinyl alcohol, swelling, stirring and heating until the polyvinyl alcohol is completely dissolved, preparing polyvinyl alcohol gel, and cooling to room temperature for standby;
step 2, dropwise adding a glycerol solution into the polyvinyl alcohol gel prepared in the step 1, and uniformly stirring to prepare a polyvinyl alcohol/glycerol mixed solution, wherein the glycerol solution is prepared by adding 0.05-0.3 g of glycerol into 0.2mL of deionized water; the mass ratio of the glycerol to the polyvinyl alcohol is 1-4: 10;
step 3, poly (3, 4-ethylenedioxythiophene): and (2) dropwise adding the aqueous solution of polystyrene sulfonic acid, namely the aqueous solution of PEDOT and PSS into the mixed solution of polyvinyl alcohol and glycerol prepared in the step (2), and rapidly and uniformly stirring to obtain poly (3, 4-ethylenedioxythiophene): a mixed solution of polystyrene sulfonic acid/polyvinyl alcohol/glycerin;
and 4, rapidly injecting the mixed solution obtained in the step 3 into a glass capillary by using a syringe, repeatedly freezing and thawing at low temperature, taking out the prepared gel fiber from the glass capillary, and airing at room temperature to obtain the PEDOT: PSS@PVA hydrogel fiber, namely the extremely environment-tolerant high-sensitivity strain sensor.
2. The method for manufacturing an extreme environment tolerant high sensitivity strain sensor according to claim 1, wherein: in the step 1, the mass ratio of distilled water to polyvinyl alcohol is 5-10:1.
3. The method for manufacturing an extreme environment tolerant high sensitivity strain sensor according to claim 1, wherein: the swelling temperature in the step 1 is 55-65 ℃ and the swelling time is 60-70 min; the temperature of stirring and heating is 80-95 ℃ and the time is 1-3 h.
4. The method for manufacturing an extreme environment tolerant high sensitivity strain sensor according to claim 1, wherein: in the step 3, the volume of the PEDOT/PSS aqueous solution is 0.5-1.5 mL.
5. The method for manufacturing an extreme environment tolerant high sensitivity strain sensor according to claim 1, wherein: in the step 4, the mixed solution is quickly injected into a glass capillary tube with an inner diameter of 1mm by a syringe.
6. The method for manufacturing an extreme environment tolerant high sensitivity strain sensor according to claim 1, wherein: the freezing temperature in the step 4 is-20 ℃, and the times of freezing-thawing cycles are 5-10 times.
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| CN115993086B (en) * | 2023-01-10 | 2023-06-06 | 合肥工业大学 | PEDOT (polymer electrolyte oxygen) PSS (power system stabilizer) based flexible strain sensor and preparation method thereof |
| CN116239799A (en) * | 2023-03-15 | 2023-06-09 | 昆明理工大学 | Double-network toughened hydrogel and preparation method thereof |
| CN117050370A (en) * | 2023-07-10 | 2023-11-14 | 浙江大学 | Polymer-based electromagnetic shielding material with shielding effect of terahertz wave band and preparation method and application thereof |
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