CN114396869A - 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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- CN114396869A CN114396869A CN202210056557.1A CN202210056557A CN114396869A CN 114396869 A CN114396869 A CN 114396869A CN 202210056557 A CN202210056557 A CN 202210056557A CN 114396869 A CN114396869 A CN 114396869A
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- 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 discloses a preparation method of an extreme environment tolerance type high-sensitivity strain sensor, which comprises the following steps: adding distilled water into polyvinyl alcohol, firstly swelling, then stirring and heating until the polyvinyl alcohol is completely dissolved to prepare polyvinyl alcohol gel, and cooling to room temperature for later use; dripping a glycerol solution into a polyvinyl alcohol solution, and uniformly stirring to prepare a polyvinyl alcohol/glycerol mixed solution; dripping a PEDOT (PSS) water solution into a polyvinyl alcohol/glycerol solution, and quickly and uniformly stirring to obtain poly (3, 4-ethylenedioxythiophene): a mixed solution of polystyrene sulfonic acid/polyvinyl alcohol/glycerin; and (3) quickly injecting the obtained mixed solution into a capillary tube by using an injector, repeatedly freezing and unfreezing at a low temperature, taking out the gel fiber from the glass capillary tube, and airing at room temperature to prepare the PEDOT (PSS) @ PVA hydrogel fiber, namely the extreme environment tolerance type high-sensitivity strain sensor. The preparation method of the extreme environment tolerance type high-sensitivity strain sensor is simple in process, low in cost and good in 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 electronic devices has brought about a hot trend in the research of flexible sensors, and flexible polymer-based flexible sensors are receiving attention due to the ultrahigh stretchability, biocompatibility and high plasticity. However, most of the currently common flexible sensors can only work under the condition of room temperature, and are difficult to adapt to the extremely cold or dry environment.
If the sensor is required to work normally in an extremely cold and dry environment, the sensor still has high stretchability and mechanical strength at an extremely low temperature, and high sensitivity is ensured. The lowest temperature resistance of the sensor can be reduced by adding inorganic salts or organic solvents (CN 202110838025.9; adv. Funct. Mater.2021, 2101696), but the sensor has the defects of low mechanical strength, poor temperature resistance, low sensitivity and the like. The lowest resistance temperature of the sensor is reduced by multi-component crosslinking, and the mechanical strength is improved (Biomacromolecules, 2021, 22, 1220-.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a preparation method of a high-sensitivity strain sensor with simple process, low cost and extreme environment tolerance.
In order to achieve the purpose, the 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, firstly swelling, then stirring and heating until the polyvinyl alcohol is completely dissolved to prepare polyvinyl alcohol gel, and cooling to room temperature for later use;
step 2, dripping a 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 (3) dropwise adding a polystyrene sulfonic acid aqueous solution, namely a PEDOT (PolyEthylenedioxy Ethanoic acid) PSS aqueous solution into the polyvinyl alcohol/glycerol mixed solution prepared in the step 2, and quickly and uniformly stirring to obtain the poly (3, 4-ethylenedioxythiophene): a mixed solution of polystyrenesulfonic acid/polyvinyl alcohol/glycerin (PEDOT: PSS/PVA/GL);
and 4, quickly injecting the mixed solution obtained in the step 3 into a glass capillary by using an injector, repeatedly freezing and unfreezing at a low temperature, taking the prepared gel fiber out of the glass capillary, and airing at room temperature to prepare the PEDOT (PSS) @ PVA hydrogel fiber which is the extreme environment tolerance type high-sensitivity strain sensor
Further, the mass ratio of the distilled water to the polyvinyl alcohol in the step 1 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 swelling time is 60-70 min; the stirring and heating temperature is 80-95 ℃, and the time is 1-3 h. Under the condition, the polyvinyl alcohol can be fully dissolved in a short 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. PSS @ PVA glycerin prepared under the condition forms dynamic hydrogen bonds with polyvinyl alcohol and water molecules, so that the lowest tolerance temperature of the hydrogel can be improved, and the water retention of the hydrogel can be improved.
Furthermore, the volume of the PEDOT/PSS aqueous solution in the step 3 is 0.5-1.5 mL. And the PEDOT PSS is added into the PEDOT PSS @ PVA gel as a conductive agent, and the resistance of the hydrogel is controlled by controlling the addition amount of the PEDOT PSS, so that the sensitivity of the sensor is further controlled.
Further, in the step 4, the mixed solution is quickly injected into a glass capillary tube with an inner diameter of 1mm by using a syringe, so that the mixed solution can be quickly transferred, and the glass capillary tube plays a role of a mold. The method can control the diameter of the gel fiber and ensure that the surface of the dried gel is smooth.
Further, the freezing temperature in the step 4 is-20 ℃, and the number of freezing-unfreezing cycles is 5-10. The conditions can ensure that the PEDOT/PSS/PVA/GL precursor solution can be frozen quickly. In the repeated freezing-unfreezing process, water as a solvent is rapidly crystallized, and formed ice crystals are used as templates to repeatedly extrude cross-linked polyvinyl alcohol molecular chains, so that the formation of a crystallization area is promoted, and the mechanical strength of the fiber is further enhanced. In the PEDOT/PSS/PVA/GL conductive hydrogel prepared under the condition, water, glycerol and polyvinyl alcohol form a three-dimensional net structure under the action of dynamic hydrogen bonds, and PEDOT/PSS conductive particles are wrapped to form a conductive network, so that the PEDOT/PVA conductive hydrogel has excellent tensile property and high sensitivity, can resist an extremely cold condition of 60 ℃ below zero, and still has good flexibility after being placed at room temperature for half a year.
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 content of the poly-3, 4-ethylenedioxythiophene: tensile length mechanical strength of polystyrene sulfonic acid @ polyvinyl alcohol hydrogel fiber.
2. The glycerol is used as a cross-linking agent to enhance the flexibility of the polyvinyl alcohol substrate, and can also be used as a freezing-resistant agent and a water-retaining agent, so that the prepared sensor still keeps good flexibility at the extremely low temperature of 60 ℃ below zero, and still has flexibility after being placed at room temperature for half a year.
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 micro strain in time, and can detect 10% of strain at the extremely low temperature of minus 60 ℃.
Drawings
FIG. 1 is a graph of poly 3, 4-ethylenedioxythiophene prepared in example 3: scanning electron microscope images of the surfaces of the polystyrene sulfonic acid @ polyvinyl alcohol composite fibers;
FIG. 2 is a graph 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 graph of poly 3, 4-ethylenedioxythiophene prepared in example 3: the stress-strain curve of the polystyrene sulfonic acid @ polyvinyl alcohol composite fiber;
FIG. 4 is a graph 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 graph of poly 3, 4-ethylenedioxythiophene prepared in example 3: the polystyrene sulfonic acid @ polyvinyl alcohol strain sensor has a test curve for large strain stability of 10% at an extremely low temperature of-60 ℃.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
A preparation method of a high-sensitivity piezoresistive strain sensor comprises the following steps:
(1) adding 10g of distilled water into 2.0g of polyvinyl alcohol powder, swelling for 60min at 55 ℃, stirring and heating for 1h at 80 ℃ until the polymer is completely dissolved to obtain a polyvinyl alcohol solution, and cooling to room temperature for later use.
(2) 0.05g of glycerol is added into 0.2mL of deionized water, and after being uniformly stirred, the mixture is quickly dripped into 0.5g of polyvinyl alcohol gel and is quickly 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 the polyvinyl alcohol/glycerol solution, and quickly and uniformly stirring to obtain poly (3, 4-ethylenedioxythiophene): mixed solution of polystyrene sulfonic acid/polyvinyl alcohol/glycerin.
(4) Using a syringe, mixing the poly 3, 4-ethylenedioxythiophene: quickly injecting the mixed solution of polystyrene sulfonic acid/polyvinyl alcohol/glycerol into a glass capillary tube with the inner diameter of 1mm, freezing for one night at the low temperature of-20 ℃, and unfreezing at room temperature, wherein the cycle number of freezing-unfreezing is 5. Taking out the gel fiber from the glass capillary, and airing at room temperature to prepare poly 3, 4-ethylenedioxythiophene: polystyrene sulfonic acid @ polyvinyl alcohol (PEDOT: PSS @ PVA) hydrogel fiber is the extreme environment tolerance type high-sensitivity strain sensor.
Example 2
A preparation method of a high-sensitivity piezoresistive strain sensor comprises the following steps:
1) adding 10g of distilled water into 1.2g of polyvinyl alcohol powder, swelling for 60min at 60 ℃, stirring and heating for 2h at 85 ℃ until the polymer is completely dissolved to obtain a polyvinyl alcohol solution, and cooling to room temperature for later use.
(2) 0.08g of glycerol is added into 0.2mL of deionized water, and after being uniformly stirred, the mixture is quickly dripped into 0.5g of polyvinyl alcohol gel and is quickly 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 the polyvinyl alcohol/glycerol solution, and quickly and uniformly stirring to obtain poly (3, 4-ethylenedioxythiophene): mixed solution of polystyrene sulfonic acid/polyvinyl alcohol/glycerin.
(4) Using a syringe, mixing the poly 3, 4-ethylenedioxythiophene: quickly injecting the mixed solution of polystyrene sulfonic acid/polyvinyl alcohol/glycerol into a glass capillary tube with the inner diameter of 1mm, freezing for one night at the low temperature of-20 ℃, and unfreezing at room temperature, wherein the cycle number of freezing-unfreezing is 5. Taking out the gel fiber from the glass capillary, and airing at room temperature to prepare poly 3, 4-ethylenedioxythiophene: polystyrene sulfonic acid @ polyvinyl alcohol (PEDOT: PSS @ PVA) hydrogel fiber is the extreme environment tolerance type high-sensitivity strain sensor.
Example 3
A preparation method of a high-sensitivity piezoresistive strain sensor comprises the following steps:
(1) adding 10g of distilled water into 1.0g of polyvinyl alcohol powder, swelling for 60min at 60 ℃, stirring and heating for 1h at 90 ℃ until the polymer is completely dissolved to obtain polyvinyl alcohol gel, and cooling to room temperature for later use.
(2) 0.20g of glycerol is added into 0.2mL of deionized water, and after being uniformly stirred, the mixture is quickly dripped into 0.5g of polyvinyl alcohol gel and is quickly and uniformly stirred, so as to prepare a polyvinyl alcohol/glycerol solution.
(3) 1.0mL of poly 3, 4-ethylenedioxythiophene: dripping aqueous solution of polystyrene sulfonic acid (PEDOT: PSS) into the polyvinyl alcohol/glycerol solution, and quickly and uniformly stirring to obtain poly (3, 4-ethylenedioxythiophene): mixed solution of polystyrene sulfonic acid/polyvinyl alcohol/glycerin.
(4) Using a syringe, mixing the poly 3, 4-ethylenedioxythiophene: quickly injecting the mixed solution of polystyrene sulfonic acid/polyvinyl alcohol/glycerol into a glass capillary tube with the inner diameter of 1mm, freezing for one night at the low temperature of-20 ℃, and unfreezing at room temperature, wherein the cycle number of freezing-unfreezing is 5. Taking out the gel fiber from the glass capillary, and airing at room temperature to prepare poly 3, 4-ethylenedioxythiophene: polystyrene sulfonic acid @ polyvinyl alcohol (PEDOT: PSS @ PVA) hydrogel fiber is the extreme environment tolerance type high-sensitivity strain sensor.
Fig. 1 and 2 are flexible and stretchable poly 3, 4-ethylenedioxythiophene prepared in embodiment 3 of the present invention: scanning electron micrographs of the surface and the cross section of the polystyrene sulfonic acid @ polyethylene hydrogel fiber show that the fiber surface is relatively smooth, and the ratio of poly (3, 4-ethylenedioxythiophene): the polystyrene sulfonic acid can be uniformly wrapped in a polyvinyl alcohol three-dimensional network structure, and the breaking strength is 13.8MPa when the breaking elongation is 519.9% (figure 3). As can be seen from fig. 4, the polypyrrole/polyvinyl alcohol sensor can detect a small strain of 0.01%, can stably detect a large strain of 10% at an extremely low temperature of-60 ℃, and can respond with an electrical signal in time (fig. 5).
Example 4
A preparation method of a high-sensitivity piezoresistive strain sensor comprises the following steps:
(1) adding 10g of distilled water into 1.0g of polyvinyl alcohol powder, swelling for 60min at 60 ℃, stirring and heating for 2h at 90 ℃ until the polymer is completely dissolved to obtain polyvinyl alcohol gel, and cooling to room temperature for later use.
(2) 0.1g of glycerol is added into 0.2mL of deionized water, and after being uniformly stirred, the mixture is quickly dripped into 0.5g of polyvinyl alcohol gel and is quickly and uniformly stirred, so as to prepare a polyvinyl alcohol/glycerol solution.
(3) 1.2mL of poly 3, 4-ethylenedioxythiophene: dripping aqueous solution of polystyrene sulfonic acid (PEDOT: PSS) into the polyvinyl alcohol/glycerol solution, and quickly and uniformly stirring to obtain poly (3, 4-ethylenedioxythiophene): mixed solution of polystyrene sulfonic acid/polyvinyl alcohol/glycerin.
(4) Using a syringe, mixing the poly 3, 4-ethylenedioxythiophene: quickly injecting the mixed solution of polystyrene sulfonic acid/polyvinyl alcohol/glycerol into a glass capillary tube with the inner diameter of 1mm, freezing for one night at the low temperature of-20 ℃, and unfreezing at room temperature, wherein the number of freezing-unfreezing cycles is 7. Taking out the gel fiber from the glass capillary, and airing at room temperature to prepare poly 3, 4-ethylenedioxythiophene: polystyrene sulfonic acid @ polyvinyl alcohol (PEDOT: PSS @ PVA) hydrogel fiber is the extreme environment tolerance type high-sensitivity strain sensor.
Example 5
A preparation method of a high-sensitivity piezoresistive strain sensor comprises the following steps:
(1) adding 10g of distilled water into 1.0g of polyvinyl alcohol powder, swelling for 70min at 65 ℃, stirring and heating for 3h at 95 ℃ until the polymer is completely dissolved to obtain polyvinyl alcohol gel, and cooling to room temperature for later use.
(2) 0.30g of glycerol is added into 0.2mL of deionized water, and after being uniformly stirred, the mixture is quickly dripped into 0.5g of polyvinyl alcohol gel and is quickly and uniformly stirred, so as to prepare a polyvinyl alcohol/glycerol solution.
(3) 1.5mL of poly 3, 4-ethylenedioxythiophene: dripping aqueous solution of polystyrene sulfonic acid (PEDOT: PSS) into the polyvinyl alcohol/glycerol solution, and quickly and uniformly stirring to obtain poly (3, 4-ethylenedioxythiophene): mixed solution of polystyrene sulfonic acid/polyvinyl alcohol/glycerin.
(4) Using a syringe, mixing the poly 3, 4-ethylenedioxythiophene: quickly injecting the mixed solution of polystyrene sulfonic acid/polyvinyl alcohol/glycerol into a glass capillary tube with the inner diameter of 1mm, freezing for one night at the low temperature of minus 20 ℃, and unfreezing at room temperature, wherein the cycle number of freezing-unfreezing is 10. Taking out the gel fiber from the glass capillary, and airing at room temperature to prepare poly 3, 4-ethylenedioxythiophene: polystyrene sulfonic acid @ polyvinyl alcohol (PEDOT: PSS @ PVA) hydrogel fiber is the extreme environment tolerance type high-sensitivity strain sensor.
Claims (7)
1. 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, firstly swelling, then stirring and heating until the polyvinyl alcohol is completely dissolved to prepare polyvinyl alcohol gel, and cooling to room temperature for later use;
step 2, dripping a 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 (3) dropwise adding a polystyrene sulfonic acid aqueous solution, namely a PEDOT (PolyEthylenedioxy Ethanoic acid) PSS aqueous solution into the polyvinyl alcohol/glycerol mixed solution prepared in the step 2, and quickly and uniformly stirring to obtain the poly (3, 4-ethylenedioxythiophene): a mixed solution of polystyrene sulfonic acid/polyvinyl alcohol/glycerin;
and 4, quickly injecting the mixed solution obtained in the step 3 into a glass capillary by using an injector, repeatedly freezing and unfreezing at a low temperature, taking the prepared gel fiber out of the glass capillary, and airing at room temperature to obtain the PEDOT (PSS) @ PVA hydrogel fiber, namely the extreme environment tolerance type high-sensitivity strain sensor.
2. The method for preparing an extreme environment tolerant high sensitivity strain sensor according to claim 1, wherein: the mass ratio of the distilled water to the polyvinyl alcohol in the step 1 is 5-10: 1.
3. The method for preparing 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 stirring and heating temperature is 80-95 ℃, and the time is 1-3 h.
4. The method for preparing an extreme environment tolerant high sensitivity strain sensor according to claim 1, wherein: 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.
5. the method for preparing 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.
6. The method for preparing an extreme environment tolerant high sensitivity strain sensor according to claim 1, wherein: in the step 4, the mixed solution is rapidly injected into a glass capillary tube with an inner diameter of 1mm by using a syringe.
7. The method for preparing an extreme environment tolerant high sensitivity strain sensor according to claim 1, wherein: the freezing temperature in the step 4 is-20 ℃, and the freezing-unfreezing cycle times are 5-10.
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