CN113686469A - Preparation method of high-sensitivity pressure sensing device - Google Patents

Preparation method of high-sensitivity pressure sensing device Download PDF

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Publication number
CN113686469A
CN113686469A CN202111053673.XA CN202111053673A CN113686469A CN 113686469 A CN113686469 A CN 113686469A CN 202111053673 A CN202111053673 A CN 202111053673A CN 113686469 A CN113686469 A CN 113686469A
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sensing device
amount
pressure sensing
sponge
sensitivity
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李秋瑾
孙月静
张健飞
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Tiangong University
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Tianjin Polytechnic University
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01LMEASURING FORCE, STRESS, TORQUE, WORK, MECHANICAL POWER, MECHANICAL EFFICIENCY, OR FLUID PRESSURE
    • G01L1/00Measuring force or stress, in general
    • G01L1/20Measuring 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
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J9/00Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
    • C08J9/36After-treatment
    • C08J9/40Impregnation
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J9/00Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
    • C08J9/36After-treatment
    • C08J9/40Impregnation
    • C08J9/42Impregnation with macromolecular compounds

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  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • General Physics & Mathematics (AREA)
  • Measuring Fluid Pressure (AREA)

Abstract

The invention relates to a preparation method of a high-sensitivity pressure sensor, belonging to the field of composite materials. With the development of scientific technology and the demand of human beings for good life, the smart sensor is receiving attention as an emerging device. The invention adopts an ultraviolet in-situ polymerization method to combine double-network ionic gel with sponge and utilizes the micropore structure of the sea surface to prepare a high-sensitivity pressure sensing device. The pressure sensing device prepared by the method has the characteristics of high sensitivity, high flexibility, low viscosity and the like, and has wide application prospect in the field of composite materials. The method has important positive significance in the fields of medical treatment, health, sports, diagnosis and the like in the future.

Description

Preparation method of high-sensitivity pressure sensing device
Technical Field
The invention relates to a preparation method of a high-sensitivity pressure sensor, belonging to the field of composite materials.
Background
With the development of scientific technology and the demand of human beings for good life, the smart sensor is receiving attention as an emerging device. The invention adopts an ultraviolet in-situ polymerization method to combine double-network ionic gel with sponge and utilizes the micropore structure of the sea surface to prepare a high-sensitivity pressure sensing device. The pressure sensing device prepared by the method has the characteristics of high sensitivity, high flexibility, low viscosity and the like, and has wide application prospect in the field of composite materials. The method has important positive significance in the fields of medical treatment, health, sports, diagnosis and the like in the future.
Disclosure of Invention
The invention uses ionic liquid and two monomers of N, N-dimethylacrylamide, tetraethyl orthosilicate and other raw materials to mix and react to obtain uniform solution, and then the pretreated sponge is dipped in prepolymerization liquid. The pressure sensing device prepared by the invention has the characteristics of high sensitivity, high flexibility, low viscosity and the like, and has wide application prospect in the field of composite materials.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
(1) measuring a certain amount of ionic liquid 1-butyl-3-methylimidazole bistrifluoromethylsulfonyl imide salt, anhydrous formic acid and tetraethyl orthosilicate according to the concentration required in the reaction, and blending and stirring under the protection of nitrogen;
(2) weighing a certain amount of alpha-ketoglutaric acid, N' -methylene bisacrylamide and N, N-dimethylacrylamide according to the required concentration, and continuing blending and stirring;
(3) putting the pretreated sponge into the prepared pre-polymerization solution, adopting a supersaturated impregnation method, putting the sponge into a sealed container after reaching adsorption balance, and putting the sealed container into an oven for heating;
(4) placing the soaked sponge under an ultraviolet light source for irradiation and then carrying out vacuum drying;
(5) and carrying out piezoresistive test analysis on the pressure sensing device.
The dosage of the ionic liquid 1-butyl-3-methylimidazole bistrifluoromethanesulfonylimide salt in the step (1) is 1-100g, the dosage of the anhydrous formic acid is 0.1-10mL, and the dosage of the tetraethyl orthosilicate is 0.1-10 mL;
the time for mixing and stirring in the step (1) is 1-10 h;
in the step (2), the dosage of the alpha-ketoglutaric acid is 0.001-0.01g, the dosage of the N, N' -methylene bisacrylamide is 0.001-0.01g, and the dosage of the N, N-dimethylacrylamide is 0.2-20 mL;
the time for mixing and stirring in the step (2) is 1-10 h;
in the step (3), the length, width and height of the sponge are all 0-100cm, the impregnation ratio is 10-500%, and the calculation formula is as follows:
Figure BSA0000251502490000021
w0is the weight of the sponge,. l0Is the mass of the impregnating solution;
the heating temperature of the oven in the step (3) is 10-100 ℃, and the heating time is 24-72 h;
the wavelength of the ultraviolet light source in the step (4) is 300-400nm, the irradiation time is 1-10h, and the vacuum drying time is 1-10 h;
the test in the step (5) comprises the steps of comparing the microscopic appearance of the electron microscope and detecting the signal change of the compression sensing resistor by a sensing test detection system;
the resistance data processing formula of the electrical property test in the step (5) is as follows:
Figure BSA0000251502490000022
R0r is the initial resistance and the dynamic resistance.
The invention has the advantages that:
the invention adopts an ultraviolet in-situ polymerization method to combine double-network ionic gel with sponge and utilizes the micropore structure of the sea surface to prepare a high-sensitivity pressure sensing device. The excellent flexibility and the high sensitivity of this pressure sensing device possess fabulous signal conversion and transmission ability, can assemble into the pressure sensor of high conductivity, but design after the equipment wide application in high and new technology fields such as intelligent wearing fabrics, flexible sensing device, flexible electrode.
Drawings
The drawings are only for purposes of illustrating and explaining the present invention and are not to be construed as limiting the scope of the present invention. Wherein:
FIG. 1: is a graph showing the results of example 1 of the present invention.
FIG. 2: is a graph showing the results of example 2 of the present invention.
Detailed Description
The invention is described below in connection with specific embodiments with the attached figures. Unless otherwise specified, the technical means used in the present invention are well known to those skilled in the art. In addition, the embodiments should be considered illustrative, and not restrictive, of the scope of the invention, which is defined solely by the claims. It will be apparent to those skilled in the art that various changes or modifications in the components and amounts of the materials used in these embodiments can be made without departing from the spirit and scope of the invention.
Example 1: the high-sensitivity flexible pressure sensing device prepared by experiments according to the technical scheme of the invention is shown in figure 1, wherein (a) is a cold field scanning electron microscope image of pretreated sponge; (b) is a cold field scanning electron microscope picture of the pre-polymerization liquid after in-situ polymerization. Comparison of the two figures shows successful polymerization of the ionic gel in the internal pores of the sponge.
Example 2: the pressure sensing device prepared by the invention is used for pressure sensing to realize the purposes of man-machine interaction and the like, a sensing test machine is used for detecting the compression resistance of the pressure sensing device, as shown in figure 2, the resistance change rate can reach 45% at most by a resistance change rate curve of repeated loading-unloading circulation within the load range of 0-50cN and the time of 800 seconds, and two small graphs of two time periods selected in the graph can better prove the stability and better repeatability of the sensing device.

Claims (6)

1. A preparation method of a high-sensitivity pressure sensing device comprises the following steps:
(1) measuring a certain amount of ionic liquid 1-butyl-3-methylimidazole bistrifluoromethylsulfonyl imide salt, anhydrous formic acid and tetraethyl orthosilicate according to the concentration required in the reaction, and blending and stirring under the protection of nitrogen;
(2) weighing a certain amount of alpha-ketoglutaric acid, N' -methylene bisacrylamide and N, N-dimethylacrylamide according to the required concentration, and continuing blending and stirring;
(3) putting the pretreated sponge into the prepared pre-polymerization solution, adopting a supersaturated impregnation method, putting the sponge into a sealed container after reaching adsorption balance, and putting the sealed container into an oven for heating;
(4) placing the soaked sponge under an ultraviolet light source for irradiation and then carrying out vacuum drying;
(5) and carrying out piezoresistive test analysis on the pressure sensing device.
2. The method for preparing a high-sensitivity pressure sensing device according to claim 1, wherein the ionic liquid 1-butyl-3-methylimidazole bistrifluoromethanesulfonylimide salt in the step (1) is used in an amount of 1-100g, the anhydrous formic acid is used in an amount of 0.1-10mL, the tetraethyl orthosilicate is used in an amount of 0.1-10mL, and the blending and stirring time is 1-10 h.
3. The method of claim 1, wherein the α -ketoglutaric acid is used in an amount of 0.001 to 0.01g, the N, N '-methylenebisacrylamide is used in an amount of 0.001 to 0.01g, the N, N' -dimethylacrylamide is used in an amount of 0.2 to 20mL, and the blending and stirring time is 1 to 10 hours in the step (2).
4. The method for preparing a high-sensitivity pressure sensor according to claim 1, wherein the length, width and height of the sponge in the step (3) are all 0-100cm, the dipping ratio is 10% -500%, and the calculation formula is as follows:
Figure FSA0000251502480000011
w0is the mass of the raw fiber rope,. l0Is the mass of the impregnating solution; the heating temperature of the oven in the step (3) is 10-100 ℃, and the heating time is 24-72 h.
5. The method as claimed in claim 1, wherein the wavelength of the ultraviolet light source in step (4) is 300-400nm, the irradiation time is 1-10h, and the vacuum drying time is 1-10 h.
6. The method for manufacturing a high-sensitivity pressure sensor device according to claim 1, wherein the testing in the step (5) includes comparing the micro-topography of the cold-field scanning electron microscope, and detecting the signal change of the compressive sensing resistor by a sensing test detection system. The resistance data processing formula of the electrical property test is as follows:
Figure FSA0000251502480000012
R0r is the initial resistance and the dynamic resistance.
CN202111053673.XA 2021-09-09 2021-09-09 Preparation method of high-sensitivity pressure sensing device Pending CN113686469A (en)

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Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110527112A (en) * 2019-08-01 2019-12-03 同济大学 Ionic conduction double-network hydrogel and its preparation method and application
CN111094361A (en) * 2017-11-21 2020-05-01 日东电工株式会社 Method for producing structure containing ionic liquid, and structure containing ionic liquid
CN111548513A (en) * 2020-05-25 2020-08-18 郑州大学 Telescopic anti-freezing full-physical cross-linked hydrogel material for multi-mode flexible sensor and preparation method thereof
CN112201386A (en) * 2020-09-30 2021-01-08 南京工业大学 Flexible transparent high-stability ion conductive electrode, preparation method and application thereof
CN112341573A (en) * 2020-12-18 2021-02-09 郑州大学 Preparation method and application of multifunctional composite hydrogel
CN112599863A (en) * 2020-12-12 2021-04-02 同济大学 Repairable ionic gel electrolyte and preparation method and application thereof

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111094361A (en) * 2017-11-21 2020-05-01 日东电工株式会社 Method for producing structure containing ionic liquid, and structure containing ionic liquid
CN110527112A (en) * 2019-08-01 2019-12-03 同济大学 Ionic conduction double-network hydrogel and its preparation method and application
CN111548513A (en) * 2020-05-25 2020-08-18 郑州大学 Telescopic anti-freezing full-physical cross-linked hydrogel material for multi-mode flexible sensor and preparation method thereof
CN112201386A (en) * 2020-09-30 2021-01-08 南京工业大学 Flexible transparent high-stability ion conductive electrode, preparation method and application thereof
CN112599863A (en) * 2020-12-12 2021-04-02 同济大学 Repairable ionic gel electrolyte and preparation method and application thereof
CN112341573A (en) * 2020-12-18 2021-02-09 郑州大学 Preparation method and application of multifunctional composite hydrogel

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* Cited by examiner, † Cited by third party
Title
JUN YANG: "In situ synthesis of poly(acrylic acid) physical hydrogels from silica nanoparticles" *
李小康: "基于聚合物凝胶的柔性传感器制备及性能研究" *

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Application publication date: 20211123