WO2024031842A1 - Film élastomère de microstructure et procédé de préparation associé, et capteur de pression flexible et procédé de préparation associé - Google Patents

Film élastomère de microstructure et procédé de préparation associé, et capteur de pression flexible et procédé de préparation associé Download PDF

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WO2024031842A1
WO2024031842A1 PCT/CN2022/128150 CN2022128150W WO2024031842A1 WO 2024031842 A1 WO2024031842 A1 WO 2024031842A1 CN 2022128150 W CN2022128150 W CN 2022128150W WO 2024031842 A1 WO2024031842 A1 WO 2024031842A1
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film
elastomer
microstructure
preparation
microstructured
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PCT/CN2022/128150
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English (en)
Chinese (zh)
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杨小牛
李宗林
张通
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中国科学院长春应用化学研究所
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Publication of WO2024031842A1 publication Critical patent/WO2024031842A1/fr

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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
    • G01L1/18—Measuring force or stress, in general using properties of piezo-resistive materials, i.e. materials of which the ohmic resistance varies according to changes in magnitude or direction of force applied to the material
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61B—DIAGNOSIS; SURGERY; IDENTIFICATION
    • A61B5/00—Measuring for diagnostic purposes; Identification of persons
    • A61B5/02—Detecting, measuring or recording pulse, heart rate, blood pressure or blood flow; Combined pulse/heart-rate/blood pressure determination; Evaluating a cardiovascular condition not otherwise provided for, e.g. using combinations of techniques provided for in this group with electrocardiography or electroauscultation; Heart catheters for measuring blood pressure
    • A61B5/024—Detecting, measuring or recording pulse rate or heart rate
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61B—DIAGNOSIS; SURGERY; IDENTIFICATION
    • A61B5/00—Measuring for diagnostic purposes; Identification of persons
    • A61B5/02—Detecting, measuring or recording pulse, heart rate, blood pressure or blood flow; Combined pulse/heart-rate/blood pressure determination; Evaluating a cardiovascular condition not otherwise provided for, e.g. using combinations of techniques provided for in this group with electrocardiography or electroauscultation; Heart catheters for measuring blood pressure
    • A61B5/024—Detecting, measuring or recording pulse rate or heart rate
    • A61B5/0245—Detecting, measuring or recording pulse rate or heart rate by using sensing means generating electric signals, i.e. ECG signals

Definitions

  • the invention belongs to the technical field of pressure sensors, and in particular relates to a microstructured elastomer film, its preparation method, and a flexible pressure sensor and its preparation method.
  • Piezoresistive flexible pressure sensors are light, thin, and flexible, can be attached to complex-shaped surfaces, and are easy to carry. Therefore, they have broad application prospects in the fields of electronic skin, health monitoring, human-computer interaction, and motion recognition. Piezoresistive flexible pressure sensors have attracted widespread attention due to their simple structure, easy signal reading, and convenient production.
  • the sensing mechanism of piezoresistive flexible pressure sensors can be divided into two types: bulk conductivity and surface conductivity. Bulk conductivity means that the conductive filler is evenly dispersed in the elastomer. However, the sensor with this mechanism is greatly affected by the viscoelasticity and temperature changes of the material itself, so the output signal is unstable.
  • Surface microstructure conductivity is a device structure developed to address the lack of bulk conductivity. When this type of sensor is pressed, the surface microstructure of the elastomer film deforms, and the contact area between the conductive film and the interdigital electrode becomes larger. The resistance is reduced, thereby achieving force-to-electricity conversion.
  • microstructured flexible pressure sensors In recent years, with the efforts of scientific researchers, the performance of microstructured flexible pressure sensors has been greatly improved. At present, most of the microstructures used by researchers use transfer printing methods to obtain them from the microstructure surface. For example, the application number is 202111156003.0, and the invention patent titled "Preparation method and application of a flexible pressure sensor” uses sandpaper as the template, multi-walled carbon nanotubes (MWCNTs) as the conductive material, and polydimethylsiloxane (PDMS). ) obtains a microstructured flexible sensing layer for a flexible substrate, but there is a problem of small linear interval.
  • MWCNTs multi-walled carbon nanotubes
  • PDMS polydimethylsiloxane
  • the invention patent with application number 201910240874.7, titled "An elastomer film and its preparation method and a flexible pressure sensor containing the elastomer film” uses selective laser sintering 3D printing technology to prepare a microstructure template , the obtained microstructure sensing film has a good linear response within the pressure range of 200kPa, which improves the performance of the sensor.
  • the transfer method also has shortcomings that hinder the commercialization of flexible pressure sensors.
  • the transfer printing method is limited by the template size, elastomer leveling requirements, separation of the film and template and other operational aspects, and cannot be used in large areas;
  • the microstructure of the template will wear out during multiple uses, resulting in The production quality is unstable;
  • the processing of the template and the commonly used elastomer material (PDMS) make the cost of the template method high, and the complexity of the transfer operation makes the production efficiency low.
  • PDMS commonly used elastomer material
  • Electrospinning technology can achieve the preparation of microstructured films of a certain area, but it has the problems of low production efficiency and small linear range.
  • development of a non-transferable, large-area, efficient, and low-cost method for preparing high-performance microstructured elastomer films is of great significance to promote the commercial application of flexible pressure sensors.
  • the object of the present invention is to provide a method for preparing a microstructured elastomer film and a method for preparing a flexible pressure sensor.
  • the method for preparing the microstructured elastomer film of the present invention is easy to industrialize, and the flexible pressure sensor prepared based on the microstructured film Its current signal has a good linear relationship with pressure within a wide range of 20MPa, and can be used for radial artery pulse monitoring.
  • the invention provides a microstructured elastomer film, which includes a substrate and a microstructured layer attached to the surface of the substrate;
  • the microstructure layer has a granular microstructure with a small lower end connected to the base, an enlarged upper end, a rough surface, and a fluffy interior; or a mountain-like microstructure with a large lower end connected to the base, a small upper end, a rough surface, and a fluffy interior. structure; or a fabric-like microstructure with interlaced fibers.
  • the substrate is polyethylene terephthalate film, thermoplastic polyurethane elastomer film, polyethylene film, polypropylene film or polyimide film;
  • the thickness of the substrate is 50-100 ⁇ m.
  • the present invention provides a method for preparing the microstructured elastomer film as described above, which includes the following steps:
  • thermoplastic elastomer material Dissolve the thermoplastic elastomer material in the solvent and prepare an elastomer solution with a concentration of 10 to 120 mg/mL;
  • thermoplastic elastomer material is one or more of hydrogenated styrene-butadiene block copolymer and thermoplastic polyurethane;
  • the solvent is tetrahydrofuran, butyl acetate, 1,4-dioxane, cyclohexane One or more of ketone and N,N-dimethylformamide;
  • an air-assisted spray gun is used to spray the elastomer solution onto the substrate surface; the carrier gas pressure of the spraying is 0.1 ⁇ 0.8MPa; the diameter of the nozzle is 0.8 ⁇ 2.5mm; the spraying distance is 20 ⁇ 50cm.
  • the thickness of the microstructured elastomer film is 50-300 ⁇ m.
  • the solvent is removed by heating or evaporation at room temperature.
  • the present invention provides a flexible pressure sensor including the microstructured elastomer film described above.
  • the invention provides a method for preparing a flexible pressure sensor, which includes the following steps:
  • conductive ink is sprayed on the surface of the microstructured elastomer film to form a conductive layer
  • a metal conductive layer is formed on the surface of the microstructured elastomer film by magnetron sputtering or vacuum evaporation.
  • the conductive ink is an organic dispersion of conductive carbon material; the thickness of the conductive layer is 1 to 2 ⁇ m.
  • the invention provides a microstructure elastomer film, which includes a substrate and a microstructure layer attached to the surface of the substrate; the microstructure layer has a small lower end connected to the substrate, an enlarged upper end, a rough surface, and a fluffy granular microstructure inside. structure; or it has a mountain-like microstructure with a large lower end connected to the base, a small upper end, a rough surface, and a fluffy interior; or it has a fabric-like microstructure with interlaced fibers.
  • the invention provides a method for preparing a microstructured elastomer film, which includes the following steps: A) dissolving a thermoplastic elastomer material in a solvent to prepare an elastomer solution with a concentration of 10 to 120 mg/mL; the elastomer material It is one or more of hydrogenated styrene-butadiene block copolymer and thermoplastic polyurethane; the solvent is tetrahydrofuran, butyl acetate, 1,4-dioxane, cyclohexanone, N,N- One or more of dimethylformamide; B) Spray the elastomer solution evenly onto the surface of the substrate, and obtain a microstructured elastomer film after removing the solvent.
  • the preparation method of the elastomer film of the present invention is mainly based on the spraying process. First, select a suitable soluble elastomer polymer material and prepare it into a solution of a certain concentration. Then use an air-assisted spray gun to spray the solution on the temperature-controlled substrate to form a film. After the solution evaporates, a multi-layered surface can be obtained. Microstructured elastomeric films.
  • the flexible pressure sensor prepared with this film has a good linear relationship between the current signal and the pressure within the range of 20MPa, and can be used for radial artery pulse monitoring.
  • Figure 1 is an optical microscope side view of the microstructured elastomer film prepared in Example 1 of the present invention
  • Figure 2 is an SEM image of the microstructured elastomer film prepared in Example 1 of the present invention.
  • Figure 3 is an optical microscope top view of the microstructured elastomer film prepared in Example 2 of the present invention.
  • Figure 4 is an optical microscope top view of the microstructured elastomer film prepared in Example 3 of the present invention.
  • Figure 5 is an SEM image of the microstructured elastomer film prepared in Example 3 of the present invention.
  • Figure 6 is an SEM image of the microstructured elastomer film prepared in Example 4 of the present invention.
  • Figure 7 is a electromechanical test diagram of the flexible pressure sensor in Embodiment 6 of the present invention under a pressure of 0 to 20MPa;
  • Figure 8 is a pulse test chart of the flexible pressure sensor in Embodiment 6 of the present invention.
  • the invention provides a microstructured elastomer film, which includes a substrate and a microstructured layer attached to the surface of the substrate;
  • the microstructure layer has a granular microstructure with a small lower end connected to the base, an enlarged upper end, a rough surface, and a fluffy interior; or a mountain-like microstructure with a large lower end connected to the base, a small upper end, a rough surface, and a fluffy interior. structure; or a fabric-like microstructure with interlaced fibers.
  • the microstructure layer has three morphologies, namely:
  • the invention provides a method for preparing a microstructured elastomer film, which includes the following steps:
  • thermoplastic elastomer material Dissolve the thermoplastic elastomer material in the solvent and prepare an elastomer solution with a concentration of 10 to 120 mg/mL;
  • the elastomer material is one or more of hydrogenated styrene-butadiene block copolymer and thermoplastic polyurethane; the solvent is tetrahydrofuran, butyl acetate, 1,4-dioxane, and cyclohexanone , one or more of N,N-dimethylformamide;
  • the use of spraying method to prepare microstructured elastomer films requires the selection of appropriate elastomer materials.
  • the elastomer materials are preferably hydrogenated styrene-butadiene block copolymer (SEBS) or thermoplastic polyurethane (TPU).
  • SEBS hydrogenated styrene-butadiene block copolymer
  • TPU thermoplastic polyurethane
  • the solvent is preferably one or more of tetrahydrofuran, butyl acetate, 1,4-dioxane, cyclohexanone, N,N-dimethylformamide, more preferably It is a low boiling point solvent, such as tetrahydrofuran (THF).
  • THF tetrahydrofuran
  • the concentration of the elastomer material directly affects the microstructure morphology of the surface of the microstructured elastomer film.
  • the concentration of the elastomer material is preferably 10 to 120 mg/mL, such as 10 mg/mL, 15 mg/mL.
  • mL 20mg/mL, 25mg/mL, 30mg/mL, 35mg/mL, 40mg/mL, 45mg/mL, 50mg/mL, 55mg/mL, 60mg/mL, 65mg/mL, 70mg/mL, 75mg/mL, 80 mg/mL, 85 mg/mL, 90 mg/mL, 95 mg/mL, 100 mg/mL, 105 mg/mL, 110 mg/mL, 115 mg/mL, 120 mg/mL, preferably a range value with any of the above values as the upper limit or lower limit.
  • the droplets sprayed with a low-concentration (10-30 mg/mL) solution can be dispersed well to obtain a broccoli-like microstructure; the viscosity of the medium-concentration (30-70 mg/mL) solution increases during spraying. It cannot be dispersed well, and some stringing appears.
  • the microstructure is like a mountain range, with large bottom and small top, continuous; continue to increase the solution concentration (70 ⁇ 120mg/mL), and the main thing sprayed out at this time is filaments, and we get It has a fabric-like surface with fibrous filaments criss-crossing in a criss-cross pattern, and the overall height of the surface does not fluctuate much.
  • the present invention sprays the elastomer solution evenly onto the surface of the substrate by spraying.
  • the spraying path is a serpentine curve, and the path parameters are adjusted according to the base area and spray width to ensure uniform coverage.
  • the spraying method used in the present invention can quickly and uniformly prepare a variety of elastomer films with different microstructures and morphologies over a large area.
  • the material liquid is affected by gravity or pressure in the storage tank and flows out from the nozzle to form a liquid film.
  • the surface of the liquid film produces unstable fluctuations under the action of the surrounding high-speed gas jets. As the fluctuations develop, the liquid film breaks into liquid lines, liquid rings or larger particles, and at the same time leaves the nozzle and moves forward. The droplets formed by the initial rupture will continue to be affected by the rear airflow in the air.
  • the droplets formed by the initial rupture will undergo secondary rupture, resulting in a finer spray liquid. drop. As these small droplets continue to fly forward, they will also partially collide and merge, and finally hit the substrate and attach to its surface.
  • spraying parameters such as carrier gas flow rate, feed liquid composition, base material, and spraying speed, different atomization and drying effects can be achieved, and surface microstructure films with different morphologies can be obtained.
  • an air-assisted spray gun is preferably used to spray the elastomer solution.
  • the nozzle diameter of the air-assisted spray gun is preferably 0.8 to 2.5 mm, more preferably 1 to 2 mm, and the carrier gas pressure is preferably 0.1 to 0.8 MPa, more preferably 0.3 ⁇ 0.5MPa, such as 0.1MPa, 0.2MPa, 0.3MPa, 0.4MPa, 0.5MPa, 0.6MPa, 0.7MPa, 0.8MPa, preferably a range value with any of the above values as the upper limit or lower limit; the spraying distance is preferably 20-50cm, more preferably 30-40cm.
  • the spraying process can be repeated and sprayed multiple times until the required thickness is reached to ensure the elasticity of the film.
  • the present invention preferably uses a heating method to remove the solvent in the sprayed layer.
  • a temperature-controllable heating device can be provided below the substrate, or an infrared radiation lamp can be used to heat from the top.
  • the purpose of heating in the present invention is to volatilize and remove the solvent. Therefore, the heating temperature needs to be adjusted according to the type of solvent. At the same time, the selection of the heating temperature must also take into account the resistance temperature of the base material and the resistance temperature of the elastomer.
  • the heating temperature is preferably 70 to 150°C, more preferably 90°C.
  • the thickness of the elastomer microstructure layer prepared by the spraying method is preferably 50 to 300 ⁇ m, and more preferably 100 to 200 ⁇ m.
  • the substrate is preferably polyethylene terephthalate (PET) film, TPU film, polyethylene (PE) film, polypropylene (PP) film or polyimide (PI) film,
  • PET polyethylene terephthalate
  • PE polyethylene
  • PP polypropylene
  • PI polyimide
  • the present invention also provides a flexible pressure sensor, which includes the microstructured elastomer film described above.
  • the present invention also provides a preparation method of a flexible pressure sensor, which includes the following steps:
  • the conductive ink can be sprayed on the surface of the microstructured elastomer by air-assisted spraying or ultrasonic spraying to form a conductive layer, or the conductive layer can be formed on the surface of the microstructure by magnetron sputtering or vacuum evaporation. Build a metal conductive layer.
  • the conductive ink preferably includes a conductive carbon material and an organic solvent.
  • a conductive carbon material preferably includes a conductive carbon material and an organic solvent.
  • an N,N-dimethylformamide (DMF) dispersion of multi-walled carbon nanotubes can be used, and the concentration is preferably 1 to 10 mg. /mL, more preferably 3 to 8 mg/mL, most preferably 5 to 6 mg/mL; the metal in the metal conductive layer may be gold or silver.
  • DMF N,N-dimethylformamide
  • the conductive layer side of the sensing film is combined with the interdigital electrode and packaged to obtain a flexible pressure sensor.
  • the interdigital electrode is preferably a PI base and a silver conductive layer.
  • the invention provides a method for preparing a microstructured elastomer film, which includes the following steps: A) Mix the elastomer material with a solvent to prepare an elastomer solution with a concentration of 10 to 120 mg/mL; the elastomer material is hydrogenated One or more of styrene-butadiene block copolymer and thermoplastic polyurethane; the solvent is tetrahydrofuran, butyl acetate, 1,4-dioxane, cyclohexanone, N,N-dimethyl One or more of the base formamides; B) Spray the elastomer solution evenly onto the surface of the substrate, and obtain a microstructured elastomer film after removing the solvent.
  • the preparation method of the elastomer film of the present invention is mainly based on the spraying process. First, select a suitable soluble polymer material and prepare it into a solution with a certain concentration. Then use an air-assisted spray gun to spray the solution on the temperature-controlled substrate to form a film. After the solution evaporates, you can obtain a multi-layered surface microstructure. Structural elastomeric film.
  • the flexible pressure sensor prepared with this film has a good linear relationship between the current signal and the pressure within the range of 20MPa, and can be used for radial artery pulse monitoring.
  • the selected material is SEBS, brand name is Karton G1650, and is dissolved in tetrahydrofuran (THF) to prepare a 20mg/mL solution.
  • the spray gun is Iwata Wider2-25W1G, the carrier gas pressure is 0.25MPa, and the elastomer film with a thickness of about 200 ⁇ m and a granular surface microstructure is sprayed on a 100 ⁇ m thick polyimide (PI) film.
  • PI polyimide
  • the selected material is TPU, the brand name is Estane AlR MC 93A-V, and it is dissolved in tetrahydrofuran (THF) to prepare a 20mg/mL solution.
  • THF tetrahydrofuran
  • the spray gun is Iwata Wider2-25W1G, the carrier gas pressure is 0.25MPa, and an elastomer film with a thickness of about 100 ⁇ m and a granular surface microstructure is sprayed on a 100 ⁇ m thick polyimide (PI) film. Its morphology and examples The appearance is similar to that in 1.
  • Figure 3 is its optical microscope image.
  • the selected material is SEBS, brand name is Karton G1650, and is dissolved in tetrahydrofuran (THF) to prepare a 50mg/mL solution.
  • the spray gun is Iwata Wider2-25W1G, the carrier gas pressure is 0.25MPa, and an elastomer film with a thickness of about 200 ⁇ m and a "mountain"-like surface microstructure is sprayed on an 80 ⁇ m thick ethylene terephthalate (PET) film.
  • Figures 4 to 5 show the optical microscope images and scanning electron microscope images respectively.
  • the selected material is SEBS, brand name is Karton G1652, and is dissolved in tetrahydrofuran (THF) to prepare a 120mg/mL solution.
  • the spray gun is Iwata Wider2-25W1G, the carrier gas pressure is 0.7MPa, and an elastomer film with a thickness of about 200 ⁇ m and a brushed surface microstructure is obtained by spraying on an 80 ⁇ m thick PET film.
  • Figure 6 is its scanning electron microscope image.
  • Conductive ink was sprayed on the surface of the elastomer film prepared in Example 1 using a pneumatic spray gun.
  • the conductive ink is an N,N-dimethylformamide (DMF) dispersion of multi-walled carbon nanotubes (MWCNTs) with a concentration of 2mg/mL; the spraying carrier gas pressure is 0.25MPa, and the thickness of the conductive layer obtained by spraying is 1 ⁇ 2um.
  • a flexible pressure sensor is obtained by combining a microstructured film with a conductive layer and an interdigital electrode (the interdigital electrode is a PI base, a silver conductive layer, a working area of 2cm*2cm, a total of 20 fingers, and a finger gap width of 150 ⁇ m).
  • Conductive ink was ultrasonically sprayed on the surface of the elastomer film prepared in Example 3.
  • the conductive ink is an N,N-dimethylformamide (DMF) solution of multi-walled carbon nanotubes (MWCNTs) with a concentration of 5mg/mL; the ultrasonic spraying carrier gas pressure is 0.4MPa, the ultrasonic power is 3.5W, and the ink flow rate is 0.2mL/min, the thickness of the conductive layer obtained by spraying is 1 ⁇ 2 ⁇ m.
  • DMF N,N-dimethylformamide
  • MWCNTs multi-walled carbon nanotubes
  • a flexible pressure sensor is obtained by combining a microstructured film with a conductive layer and an interdigital electrode (the interdigital electrode is a PI base, a silver conductive layer, a working area of 2cm*2cm, a total of 20 fingers, and a finger gap width of 150 ⁇ m).
  • the selected material is SEBS, brand name is Karton G1650, and is dissolved in tetrahydrofuran (THF) to prepare a solution of 80mg/mL.
  • the spray gun is Iwata Wider2-25W1G, the carrier gas pressure is 0.25MPa, and an elastomer film with a thickness of about 200 ⁇ m and a brushed surface microstructure is obtained by spraying on a 100 ⁇ m thick PI film. Conductive ink is then sprayed on the surface of the film.
  • the conductive ink is a DMF dispersion of MWCNTs with a concentration of 2 mg/mL; a pneumatic-assisted spray gun is used with a carrier gas pressure of 0.25 MPa and a conductive layer thickness of 1 to 2 ⁇ m.
  • a flexible pressure sensor is obtained by combining a microstructured film with a conductive layer and an interdigital electrode (the interdigital electrode is a PI base, a silver conductive layer, a working area of 2cm*2cm, a total of 20 fingers, and a finger gap width of 150 ⁇ m).
  • the pressure sensor prepared in Example 5 is used to test human pulse.
  • the test process is as follows: attach one side of the encapsulated sensor microstructure film to the radial artery of the wrist and fix it with tape. Then the sensor is powered through the source meter and the test data is recorded. The results are shown in Figure 8. It can be seen from Figure 8 that the sensor of the present invention can clearly distinguish the human radial artery pulse and has application potential.

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Abstract

Film élastique de microstructure, comprenant un substrat et une couche de microstructure fixée à la surface du substrat. La couche de microstructure possède une microstructure granulaire reliée au substrat et possédant une petite extrémité inférieure, une extrémité supérieure expansée, une surface rugueuse et un intérieur pelucheux, ou une microstructure de type montagne reliée au substrat et possédant une grande extrémité inférieure, une petite extrémité supérieure, une surface rugueuse et un intérieur pelucheux, ou une microstructure de type tissu formée par décalage vertical et horizontal de fibres. L'invention concerne également un procédé de préparation basé sur un processus de revêtement par pulvérisation pour le film élastomère de microstructure, ainsi qu'un capteur de pression flexible et un procédé de préparation associé. Le signal de courant et la pression du capteur de pression flexible préparé à l'aide du film sont dans une bonne relation linéaire dans la plage de 20 MPa, et le capteur de pression flexible peut être utilisé à des fins de surveillance d'impulsion radiale.
PCT/CN2022/128150 2022-08-09 2022-10-28 Film élastomère de microstructure et procédé de préparation associé, et capteur de pression flexible et procédé de préparation associé WO2024031842A1 (fr)

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CN202210951117.2A CN115290231A (zh) 2022-08-09 2022-08-09 一种微结构弹性体薄膜、其制备方法及柔性压力传感器、其制备方法
CN202210951117.2 2022-08-09

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