CN113150371A - PDMS sponge-based strain sensor and preparation method thereof - Google Patents
PDMS sponge-based strain sensor and preparation method thereof Download PDFInfo
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- CN113150371A CN113150371A CN202110383061.0A CN202110383061A CN113150371A CN 113150371 A CN113150371 A CN 113150371A CN 202110383061 A CN202110383061 A CN 202110383061A CN 113150371 A CN113150371 A CN 113150371A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/36—After-treatment
- C08J9/40—Impregnation
- C08J9/42—Impregnation with macromolecular compounds
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/28—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof by elimination of a liquid phase from a macromolecular composition or article, e.g. drying of coagulum
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/36—After-treatment
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01L—MEASURING FORCE, STRESS, TORQUE, WORK, MECHANICAL POWER, MECHANICAL EFFICIENCY, OR FLUID PRESSURE
- G01L1/00—Measuring force or stress, in general
- G01L1/20—Measuring force or stress, in general by measuring variations in ohmic resistance of solid materials or of electrically-conductive fluids; by making use of electrokinetic cells, i.e. liquid-containing cells wherein an electrical potential is produced or varied upon the application of stress
- G01L1/22—Measuring force or stress, in general by measuring variations in ohmic resistance of solid materials or of electrically-conductive fluids; by making use of electrokinetic cells, i.e. liquid-containing cells wherein an electrical potential is produced or varied upon the application of stress using resistance strain gauges
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2383/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen, or carbon only; Derivatives of such polymers
- C08J2383/04—Polysiloxanes
Abstract
The invention belongs to the field of flexible electronic materials, and particularly relates to a PDMS sponge-based strain sensor and a preparation method thereof, wherein the preparation process comprises the following steps: preparing PDMS sponge by taking monosaccharide as a sacrificial template, carrying out plasma treatment modification on the surface of PDMS, immersing the PDMS sponge into a polyvinyl alcohol-acid aqueous solution, squeezing out excess solution, curing, drying to obtain a conductive modified PDMS sponge strain sensor material, and clamping between two flexible electrodes to prepare the strain sensor. The strain sensor disclosed by the invention has the advantages that the resistance can obviously change in tiny compressive strain, meanwhile, the stability of cyclic compression release is good, the tiny deformation generated by the pulse can be responded, the preparation process is simple, the operation is easy, and the strain sensor has a wide application prospect in the field of flexible strain sensors.
Description
Technical Field
The invention belongs to the field of flexible electronic materials, relates to preparation of a strain sensor material, and more particularly relates to a preparation method of a PDMS sponge-based strain sensor material.
Background
The growing interest in artificial intelligence, human-machine interfaces and electronic skins has driven the development of flexible electronic technology. Flexible electronics technology includes two important components: electronic skins and flexible wearable devices. The key to implementing electronic skin and flexible wearable devices is a high performance flexible sensor. The traditional strain sensor material is generally made of metal or inorganic material, has the defects of high hysteresis, small detection range, easy influence of environmental noise and the like, and can not meet the material requirement of a high-strain sensor. Therefore, the development of the flexible strain sensor with multifunction, high sensitivity, quick response and low cost has important practical significance. The conductive composite material assembled by the flexible elastomer and the proton polymer can generate high deformation and can be applied to flexible strain sensors and wearable equipment.
Disclosure of Invention
The invention aims to provide a novel method for preparing a strain sensor material with a sponge structure aiming at the defects of the existing sensing material. Firstly, the PDMS sponge is prepared by taking the cubic sugar as a sacrificial template. To conductively modify the PDMS sponge, the surface was activated using an oxygen plasma treatment of the PDMS sponge to effectively attach the proton polymer to the PDMS sponge. Finally, the modified PDMS is clamped between two flexible electrodes to prepare the flexible strain sensor.
The specific technical scheme for realizing the purpose of the invention is as follows:
a preparation method of a PDMS sponge-based strain sensor comprises the following steps:
(1) soaking different specifications of square sugar into a mixture of polydimethylsiloxane PDMS prepolymer and curing agent with the mass ratio of 9-11:1, vacuum degassing for 1-2h to form a PDMS-square sugar mixture, heating and curing the PDMS-square sugar mixture at 90-100 ℃ for 2h, heating in deionized water at 60-70 ℃ for 6h after complete curing to completely dissolve the water-soluble sacrificial template square sugar, and drying at 60-80 ℃ for 2h to obtain PDMS sponge;
(2) treating PDMS sponge for 10-15 minutes by adopting oxygen plasma to activate the surface, then soaking the PDMS sponge into a polyvinyl alcohol-acid aqueous solution for 10-20min, wherein the mass fraction of polyvinyl alcohol in the aqueous solution is 8-10%, the mass fraction of acid is 5-20%, taking out the sponge, extruding the excess solution, repeating the soaking-extruding process for 3-4 times, and then curing for 24 hours at the constant temperature of 25 ℃ to obtain the PDMS sponge attached with the proton polymer;
(3) and clamping PDMS sponge attached with the proton polymer between the two flexible electrodes to obtain the PDMS sponge-based strain sensor.
In the step (1), the mixture of the polydimethylsiloxane PDMS prepolymer and the curing agent is placed into a beaker to be uniformly stirred after the PDMS prepolymer and the curing agent are weighed according to the mass ratio of 9-11:1, and bubbles generated by stirring are removed by ultrasonic.
In the step (2), the preparation method of the polyvinyl alcohol-acid aqueous solution comprises the following steps: magnetically stirring 8-10 wt% of polyvinyl alcohol aqueous solution at 90 deg.C for 2h to completely dissolve polyvinyl alcohol, cooling to room temperature, adding 5-20 wt% of acid, magnetically stirring for 2h, and mixing to obtain polyvinyl alcohol-acid aqueous solution.
The acid is one of phosphoric acid, acetic acid and hydrochloric acid.
The flexible electrode includes: one of a conductive tape, a conductive fabric, and a paper-based/PET screen printed silver electrode.
A PDMS sponge-based strain sensor prepared by the method.
Compared with the prior art, the invention has the following advantages:
(1) according to the invention, PDMS sponge with a developed void structure is prepared by using the common sugar cube in life as a water-soluble sacrificial template, so that the deformation capability of the material is greatly improved.
(2) Because PDMS has high hydrophobicity, the invention firstly carries out plasma treatment on PDMS sponge to activate the surface, and effectively attaches the proton polymer to the PDMS sponge.
(3) The proton polymer is attached to the PDMS sponge, so that the non-conductive PDMS sponge is subjected to conductive modification.
The PDMS sponge-based strain sensor provided by the invention has the advantages that the resistance can be obviously changed when the PDMS sponge-based strain sensor is subjected to compression deformation, the PDMS sponge-based strain sensor has excellent compression response stability, the preparation process is simple, the operation is convenient, and the PDMS sponge-based strain sensor has a wide application prospect in the field of flexible strain sensors.
Drawings
FIG. 1 is a photograph of the compression and recovery of a PDMS sponge based strain sensor made in example 1;
FIG. 2 is a schematic diagram of the change of resistance of the PDMS sponge-based strain sensor prepared in example 1 under 10% cyclic compressive strain;
FIG. 3 is a schematic diagram of the resistance change of the PDMS sponge-based strain sensor prepared in example 1 under 60% cyclic compressive strain;
FIG. 4 is a photograph of a PDMS sponge-based strain sensor prepared in example 1 for pulse measurement;
FIG. 5 is a graph of the resistance response of pulse measurement of the PDMS sponge based strain sensor made in example 1;
FIG. 6 is a graph of a single pulse response of pulse measurement of the PDMS sponge-based strain sensor made in example 1.
Detailed Description
In order to make the present invention easier to understand, the present invention is further illustrated by the following examples, but the scope of the present invention is not limited to these examples.
The invention measures the resistance variation performance of the conductive composite material along with different compression deformation quantities through the spiral testing machine frame with the distance measuring function and the LCR instrument.
Example 1
Weighing a certain amount of PDMS prepolymer and curing agent according to a ratio of 10:1, placing the PDMS prepolymer and the curing agent in a beaker, stirring for 10min, then carrying out ultrasonic treatment for 5min to remove bubbles generated by stirring, then immersing a cube sugar with the thickness of 1cm in the cube sugar, placing the cube sugar in a vacuum drying oven for 1h, removing bubbles generated when PDMS mixed liquid is immersed in the cube sugar, taking out the cube sugar, placing the cube sugar in an oven for curing for 2h at 60 ℃, then placing the cured cube sugar in deionized water, heating to dissolve the cube sugar at 70 ℃, and finally placing the PDMS sponge completely dissolved in the drying oven for drying for 2h at 70 ℃ to obtain the PDMS sponge.
And (2) magnetically stirring 10% polyvinyl alcohol aqueous solution at 90 ℃ for 2h to completely dissolve the polyvinyl alcohol, cooling to room temperature, adding 1000 mu L phosphoric acid, magnetically stirring for 2h again, and uniformly mixing to obtain the polyvinyl alcohol-phosphoric acid aqueous solution.
And (3) carrying out plasma treatment on the PDMS sponge prepared in the step (1), activating the surface, then immersing into the polyvinyl alcohol-phosphoric acid aqueous solution prepared in the step (2) for 10-15min, squeezing the solution, repeating the immersion process for 3-4 times, and then curing at a constant temperature of 24.5 ℃ for 24h to crosslink and cure the polyvinyl alcohol to obtain the proton polymer modified polydimethylsiloxane PDMS sponge.
And (4) clamping the proton polymer modified polydimethylsiloxane PDMS sponge prepared in the step (3) between two pieces of conductive fabric, and fixing the periphery by using an adhesive tape to prepare the strain sensor.
FIG. 1 is a photograph of a proton polymer modified PDMS sponge based strain sensor material, wherein a is compressed rapidly by finger pressure and b is released and returns to its original shape. FIG. 2 shows that the strain sensor responds to 80% under 10% deformation cycle compression-release, and the sponge has high response speed and high sensitivity in the 10% compression-release process; and the resistance change trend remained well stable and repeatable over 13 compression-release cycles. FIG. 3 shows that the strain sensor response changes up to 94.5% with a significant change in resistance at 60% deformation cycle compression-release; and the resistance change trend can still keep good stability and repeatability in 15 compression-release cycles. Fig. 4 is a photograph of the sensor used for pulse measurement, fig. 5 is a sensor response curve, it can be seen that there are 9 pulse responses within 6.5s, that is, 83 pulse beats within 1 minute, which is consistent with the pulse frequency of a healthy adult, and fig. 6 is a section of intercepted resistance response curve, which can clearly see the pulse head wave, the tidal wave and the heavy pulse wave, which shows that the sensor can respond well to the tiny deformation such as the pulse beats. These show that the PDMS sponge based strain sensor material has obvious resistance change in compressive strain, simultaneously shows excellent compressive cycle stability, and can detect pulse beat micro deformation, thus being applicable to high-performance flexible strain sensors.
The above description is only a preferred embodiment of the present invention, and all equivalent changes and modifications made in accordance with the claims of the present invention should be covered by the present invention.
Claims (6)
1. A preparation method of a PDMS sponge-based strain sensor is characterized by comprising the following steps:
(1) soaking the square sugar into a mixture of polydimethylsiloxane PDMS prepolymer and a curing agent in a mass ratio of 9-11:1, vacuum degassing for 1-2h to form a PDMS-square sugar mixture, heating and curing the PDMS-square sugar mixture at 90-100 ℃ for 2h, heating in deionized water at 60-70 ℃ for 6h after complete curing to completely dissolve the water-soluble sacrificial template square sugar, and drying at 60-80 ℃ for 2h to obtain PDMS sponge;
(2) treating PDMS sponge for 10-15 minutes by adopting oxygen plasma to activate the surface, then soaking the PDMS sponge into a polyvinyl alcohol-acid aqueous solution for 10-20min, wherein the mass fraction of polyvinyl alcohol in the aqueous solution is 8-10%, the mass fraction of acid is 5-20%, taking out the PDMS sponge, extruding the excess solution, repeating the soaking-extruding process for 3-4 times, and then curing at the constant temperature of 25 ℃ for 24 hours to obtain the PDMS sponge attached with the proton polymer;
(3) and clamping PDMS sponge attached with the proton polymer between the two flexible electrodes to obtain the PDMS sponge-based strain sensor.
2. The method for preparing a PDMS sponge-based strain sensor according to claim 1, wherein in the step (1), the mixture of polydimethylsiloxane PDMS prepolymer and the curing agent is placed in a beaker to be stirred uniformly after the PDMS prepolymer and the curing agent are weighed according to the mass ratio, and bubbles generated by stirring are removed by ultrasound.
3. A method for preparing a PDMS sponge-based strain sensor according to claim 1, wherein in step (2), the method for preparing the polyvinyl alcohol-acid aqueous solution is: magnetically stirring 8-10 wt% of polyvinyl alcohol aqueous solution at 90 deg.C for 2h to completely dissolve polyvinyl alcohol, cooling to room temperature, adding 5-20 wt% of acid, magnetically stirring for 2h, and mixing to obtain polyvinyl alcohol-acid aqueous solution.
4. A method for preparing a PDMS sponge-based strain sensor according to claim 1 or 3, wherein: the acid is one of phosphoric acid, acetic acid or hydrochloric acid.
5. A method for preparing a PDMS sponge-based strain sensor according to claim 1, wherein in step (3), the flexible electrode is: one of a conductive tape, a conductive fabric, and a paper-based/PET screen printed silver electrode.
6. A PDMS sponge-based strain sensor made according to the method of claim 1.
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| CN202110383061.0A CN113150371A (en) | 2021-04-09 | 2021-04-09 | PDMS sponge-based strain sensor and preparation method thereof |
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Cited By (5)
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| CN114196066A (en) * | 2021-12-06 | 2022-03-18 | 南京林业大学 | Thermal response type intelligent sponge and preparation method and application thereof |
| CN114381124A (en) * | 2022-03-03 | 2022-04-22 | 安徽大学 | Three-dimensional porous carbon nanotube-graphene/PDMS composite material, flexible strain sensor and preparation |
| CN114674346A (en) * | 2022-03-24 | 2022-06-28 | 福建工程学院 | Preparation method of sensor and sensor |
| CN115353661A (en) * | 2022-07-29 | 2022-11-18 | 华中科技大学 | Hard magnetic porous material and preparation method and application thereof |
| WO2023104049A1 (en) * | 2021-12-07 | 2023-06-15 | 深圳先进技术研究院 | Elastic dry electrode, and preparation method therefor and use thereof |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114196066A (en) * | 2021-12-06 | 2022-03-18 | 南京林业大学 | Thermal response type intelligent sponge and preparation method and application thereof |
| WO2023104049A1 (en) * | 2021-12-07 | 2023-06-15 | 深圳先进技术研究院 | Elastic dry electrode, and preparation method therefor and use thereof |
| CN114381124A (en) * | 2022-03-03 | 2022-04-22 | 安徽大学 | Three-dimensional porous carbon nanotube-graphene/PDMS composite material, flexible strain sensor and preparation |
| CN114674346A (en) * | 2022-03-24 | 2022-06-28 | 福建工程学院 | Preparation method of sensor and sensor |
| CN115353661A (en) * | 2022-07-29 | 2022-11-18 | 华中科技大学 | Hard magnetic porous material and preparation method and application thereof |
| CN115353661B (en) * | 2022-07-29 | 2023-09-01 | 华中科技大学 | Hard magnetic porous material and preparation method and application thereof |
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