CN115096483A - Preparation method and application of shape-programmable flexible pressure sensor - Google Patents
Preparation method and application of shape-programmable flexible pressure sensor Download PDFInfo
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Abstract
A manufacturing method and application of a programmable-shape flexible pressure sensor comprise the following steps: preparing a polyethylene glycol diacrylate aqueous solution; adding the dispersion liquid of the material with the function of supplying electric conduction into the aqueous solution of the polyethylene glycol diacrylate, and carrying out ice bath; adding an ammonium persulfate solution and a tetramethyl ethylenediamine solution into the final liquid to obtain a precursor solution, and quickly moving the precursor solution to a mold; moving the mold onto a copper column, and contacting the bottom of the copper column with liquid nitrogen until the precursor solution is completely frozen; finally, carrying out freeze polymerization on the reaction system, and after the freeze polymerization is finished, carrying out freeze drying to obtain anisotropic aerogel; and coating conductive silver paste on the upper surface and the lower surface of the aerogel, and connecting the aerogel with a digital multimeter probe by using a lead to obtain the shape-programmable flexible pressure sensor. By introducing the shape memory performance into the design of the flexible pressure sensing material, the wearable pressure sensor with the shape programmable function is prepared, so that the wearable pressure sensor can be self-adaptive to the detection part with the complex curvature surface.
Description
Technical Field
The invention relates to the technical field of sensor preparation, in particular to a preparation method and application of a programmable-shape flexible pressure sensor.
Background
With the development of flexible technology, intelligent wearable devices based on pressure sensors are rapidly increased, and the intelligent wearable devices are widely applied to emerging fields such as medical care, human-computer interfaces, wearable electronic equipment, robots and the Internet of things and have high economic and scientific values.
However, the materials for preparing the pressure sensor are basically metal materials, and they are generally planar and rigid, so that the sensor lacks shape deformability, and cannot be applied to a detection part with a curved surface, thereby severely limiting the application scene of the wearable pressure sensor.
At present, deformable pressure sensors can be prepared by preparing flexible soft functional materials to reduce the thickness of electronic devices or designing stretchable physical structures, however, such deformation cannot be sustained continuously and needs to be fixed on a detection position under the action of large external force. And the sensing performance of the sensor is affected when the sensor has a reversible deformation function.
Disclosure of Invention
Shape memory polymers are naturally inspired stimuli responsive materials that can be carefully programmed into any temporary shape and return to their original shape under specific external stimuli (e.g., heat, light, chemical environmental changes, etc.). Therefore, the shape memory performance is introduced into the design of the flexible pressure sensing material, and the research and development of the wearable pressure sensor with the shape programmable function are very important.
Aiming at the problem that the conventional wearable pressure sensor lacks deformability, the wearable pressure sensor is endowed with a shape programmable function by introducing shape memory performance in material design, so that the wearable pressure sensor can adapt to the detection part with a complex curvature surface in a shape self-adaption mode, and the accuracy of a detection signal of the device is improved. A shape programmable flexible pressure sensor takes polyethylene glycol diacrylate (PEGDA) and aminated carbon nanotubes (A-CNTs) as examples, which are respectively used as two functional units of a shape memory aerogel to respectively provide shape memory performance and conductivity, and then an anisotropic aerogel is prepared by adopting a method of combining directional freeze polymerization and freeze drying. The wearable pressure sensor has the advantages that the shape memory performance is introduced, the device has a shape programmable function, the shape of the wearable pressure sensor can be adjusted through shape programming and shape recovery according to the surface shape of the target wearing position, and the self-adaptive wearing and accurate detection of the target part are realized. The method specifically comprises the following steps:
s11, preparing a polyethylene glycol diacrylate aqueous solution;
s12, adding the dispersion liquid of the material with the function of conductivity into the aqueous solution of the polyethylene glycol diacrylate to obtain reaction liquid of the material with the function of conductivity, and carrying out ice-bath on the reaction liquid;
s13, adding an ammonium persulfate solution and a tetramethyl ethylene diamine solution into the final liquid obtained in the step S12 to obtain a precursor solution, and quickly moving the precursor solution to a mold;
s14, moving the mold to a copper column, and contacting the bottom of the copper column with liquid nitrogen until the precursor solution is completely frozen;
s15, carrying out freeze polymerization on the S14 final reaction system, and after the freeze polymerization is finished, carrying out freeze drying to obtain anisotropic aerogel;
and S16, coating conductive silver paste on the upper surface and the lower surface of the aerogel, and connecting the aerogel and a digital multimeter probe by using a lead to obtain the shape-programmable flexible pressure sensor.
Preferably, the aqueous solution of polyethylene glycol diacrylate is prepared from PEGDA 4000 、PEGDA 600 Prepared by the PEGDA 4000 、PEGDA 600 The mass ratio is 1.5-2.5: 1.
preferably, the conductive functional material is selected from one or more of aminated carbon nanotubes, titanium carbide, graphene oxide, liquid metal and conductive carbon black.
Preferably, the concentration of the conductive functional material dispersion liquid is 1 wt% to 5 wt%.
Preferably, the mass fraction of the conductive functional material in the whole system is 0.1 wt% to 3 wt%.
Preferably, the step S12 is further carried out by ultrasonically dispersing the functional material for supplying electricity and the shape memory polymer reaction solution by using an ultrasonic cell disruptor, wherein the dispersion time is longer than 1h, and the ice bath temperature is 0-8 ℃.
Preferably, the concentration of the ammonium persulfate solution is 2-6 wt%.
Preferably, the volume ratio of the ammonium persulfate solution to the tetramethylethylenediamine solution to the electrically functional material dispersion liquid is as follows: 5: 0.5: 70-100.
Preferably, the temperature of the freezing polymerization reaction is between 20 ℃ below zero and 10 ℃ below zero, the reaction time is between 40 and 60 hours, and the freezing drying time is more than 48 hours.
Use of a flexible pressure sensor prepared by any of the above methods, comprising:
s17, setting the flexible pressure sensor to a target shape state;
s18, changing the target shape state to obtain a temporary shape state;
s19, under the application scene, the target shape state is restored through external stimulation, and the flexible pressure sensor is worn on the specific wearing position in a self-adaptive mode.
The flexible pressure sensing material with the shape memory function has one-way and two-way shape memory effects or single, double, triple and multiple shape memory effects.
The flexible pressure sensing device returns to a permanent shape by an external stimulus of temperature, light, pH or humidity. The preparation method of the target shape state comprises cutting, direct molding of a mold and 3D printing. The shape programmable flexible pressure sensor is adaptive to fit objects with complex surfaces. Such as certain wearing locations including human skin, organ tissue surfaces, and other objects having complex surfaces. The shape programmable flexible pressure sensor deforms from a 2D plane shape to a 3D shape, and the application of cooperative deformation with different wearing positions is realized.
Advantageous effects
1. According to the invention, the shape memory performance is introduced into the design of the flexible pressure sensing material to prepare the wearable pressure sensor with the shape programmable function, so that the wearable pressure sensor can adapt to the detection part with the complex curvature surface in a shape self-adaption mode, and the long-term accuracy of the detection signal of the device is improved.
2. The problem that the current rigid pressure sensor is not deformable is solved from the perspective of material structure design.
3. Aiming at the problem that the existing wearable pressure sensor lacks of deformability, the shape memory performance is introduced into the material design, and the device is endowed with a shape programmable function, so that the wearable pressure sensor can be self-adaptive to the detection part with the complex curvature surface in shape, and the accuracy of the detection signal of the device is improved.
4. The shape memory performance is introduced in the design of the wearable electronic material, the shape programmable function is given to the device, so that the wearable pressure sensor can adapt to the detection part with the complex curvature surface in a shape self-adaption mode, and the design idea of the accuracy of the detection signal of the device is improved.
Drawings
Fig. 1 is a diagram showing detection signals of a pressing rubber head dropper.
Fig. 2 is a diagram of detection signals of a pressed finger.
Fig. 3 is a schematic diagram of self-adaptive wearing on a wrist by using a shape recovery technology.
Fig. 4 is a schematic diagram of adaptive wearing on a wrist by using an optical response shape recovery technique.
Detailed Description
In order to better embody the technical effects of the present invention, the following further description is made on the embodiments of the present invention, and the examples are only for explaining the present invention and are not intended to limit the scope of the present invention.
The basic information of the reagent and the instrument used in the invention is as follows:
TABLE 1 chemical reagents used in the preparation of the materials
Example 1
1. Preparation of shape memory conductive aerogel
(1) Mixing PEGDA 4000 (2.1g)、PEGDA 600 (0.9g) dissolved in deionized water (6mL) at room temperature with stirring to give an aqueous solution of PEGDA;
(2) adding a predetermined amount of 3 wt% A-CNTs dispersion (9mL) to the PEGDA aqueous solution, ultrasonically dispersing for more than 1h by using an ultrasonic cell disruptor (SM-900D, Shunhima instruments and Equipment Co., Ltd., Nanjing), and then transferring the reaction system to a refrigerator at 4 ℃ for precooling;
(3) APS solution (2 wt%, 1mL) and TEMED solution (50. mu.L) were added with slow stirring in an ice bath and quickly transferred to a mold (20 mm. times.10 mm. times.5 mm);
(4) rapidly transferring the mold onto a copper column (the bottom of the copper column is always in contact with liquid nitrogen), and guiding ice crystals to directionally grow from the bottom to the top until the precursor solution is completely frozen;
(5) and finally, placing the reaction system in a refrigerator at the temperature of-15 ℃ for reaction for 40 hours. And after freezing polymerization is finished, freeze-drying for more than 48 hours to obtain the anisotropic conductive aerogel.
2. Assembly of a flexible pressure sensor
The aerogel with the upper and lower surfaces coated with the conductive silver paste is connected with a test probe of a digital multimeter (DMM 6500, Giaxle instruments, Inc.) by using a copper wire as a lead, so that the resistance change of the aerogel under pressure can be tested.
3. Application of shape programmable flexible pressure sensor (wearing on rubber head dropper with small curvature surface)
Placing strip-shaped pressure sensor in oven and heating to T high (set at 70 ℃) and kept for 10min to eliminate the thermal history, and then cooled againCooling to room temperature; then again placed in the oven and held for 10min (T) high 70 deg.C, applying external force to bend and deform the sensor by a certain angle (basically consistent with the curved surface shape of the rubber head dropper), transferring the whole into a refrigerator, and cooling to T low (set to 4 ℃) for 10min to fix the temporary shape; removing the external force, and continuously placing the sensor in the refrigerator until the shape is not changed; a sample is worn on a rubber head dropper, the rubber head dropper can be attached to a complex curved surface in a self-adaptive manner, and the size of the pressing pressure of the rubber head dropper can be detected after the rubber head dropper is connected with a digital multimeter (figure 1); finally, the sample in the temporary shape is placed back into the 70 ℃ oven again to be heated for 10min, and then the pressure sensor in the strip shape is recovered.
Example 2
1. Preparation of shape memory conductive aerogel
(1) Mixing PEGDA 4000 (1.575g)、PEGDA 600 (0.675g) was dissolved in deionized water (13mL) at room temperature with stirring to give an aqueous solution of PEGDA;
(2) adding a predetermined amount of 1 wt% MXene dispersion (2mL) to the aqueous PEGDA solution, ultrasonically dispersing for more than 1h by using an ultrasonic cell disrupter (SM-900D, Shunhima instruments Co., Ltd.) and then transferring the reaction system to a refrigerator at 4 ℃ for precooling;
(3) APS solution (4 wt%, 500. mu.L) and TEMED solution (50. mu.L) were added with slow stirring in an ice bath and quickly transferred to a mold (20 mm. times.10 mm. times.5 mm);
(4) rapidly transferring the mold onto a copper column (the bottom of the copper column is always in contact with liquid nitrogen), and guiding ice crystals to directionally grow from the bottom to the top until the precursor solution is completely frozen;
(5) and finally, placing the reaction system in a refrigerator at the temperature of-10 ℃ for reaction for 50 hours. And after freezing polymerization is finished, freeze-drying for more than 48 hours to obtain the anisotropic conductive aerogel.
2. Assembly of a flexible pressure sensor
The aerogel with the upper and lower surfaces coated with the conductive silver paste is connected with a test probe of a digital multimeter (DMM 6500, Giaxle instruments, Inc.) by using a copper wire as a lead, so that the resistance change of the aerogel under pressure can be tested.
3. Application of shape programmable flexible pressure sensor (wearing on finger with large curvature surface)
The temporary shape of the strip-shaped pressure sensor is changed by utilizing the shape memory effect, the shape is fixed, the curvature shape which is almost the same as that of a finger is formed, the strip-shaped pressure sensor is attached to the finger, and the shape of the strip-shaped pressure sensor is adaptively changed through the shape memory effect, so that the strip-shaped pressure sensor is not required to be additionally provided with external force to deform, and the detection of the sensor is prevented from being influenced. The annular sensor can be self-adaptively worn on the finger through the assistance of the adhesive tape, and sensitively detects a resistance change signal pressed by the finger, as shown in fig. 2.
Example 3
1. Preparation of shape memory conductive aerogel
(1) Mixing PEGDA 4000 (1.68g)、PEGDA 600 (0.72g) dissolved in deionized water (13mL) at room temperature with stirring to give an aqueous solution of PEGDA;
(2) adding a predetermined amount of 1 wt% graphene oxide dispersion (2mL) to the aqueous PEGDA solution, ultrasonically dispersing for more than 1h with an ultrasonic cell disruption apparatus (SM-900D, Shunmar instruments, Inc., Nanjing), and then transferring the reaction system to a refrigerator at 4 ℃ for precooling;
(3) APS solution (6 wt%, 334 μ L) and TEMED solution (60 μ L) were added with slow stirring in an ice bath and quickly transferred to a circular ring mold;
(4) rapidly transferring the mold onto a copper column (the bottom of the copper column is always contacted with liquid nitrogen), and guiding the ice crystals to directionally grow from the bottom to the top until the precursor solution is completely frozen;
(5) and finally, placing the reaction system in a refrigerator at the temperature of-20 ℃ for reaction for 60 hours. And after freezing polymerization is finished, freeze-drying for more than 48 hours to obtain the anisotropic conductive aerogel.
2. Assembly of a flexible pressure sensor
The aerogel with the upper and lower surfaces coated with the conductive silver paste is connected with a test probe of a digital multimeter (DMM 6500, Giaxle instruments, Inc.) by using a copper wire as a lead, so that the resistance change of the aerogel under pressure can be tested.
3. Application of a shape programmable flexible pressure sensor (self-adaptive wearing on the wrist using shape recovery technology). Placing annular pressure sensor in oven, and heating to T high (set at 70 ℃) and held for 10min to eliminate the thermal history, and then cooled to room temperature again; then again placed in the oven and held for 10min (T) high At 70 deg.C, and applying external force to fix the sensor into planar sheet shape, transferring the whole body into refrigerator to cool to T low (set to 4 ℃) for 10min to fix the temporary shape; removing the external force, and continuously placing the sensor in the refrigerator until the shape is not changed; the sample was placed on the wrist and allowed to return to the circular ring shape by heating to fit snugly on the wrist as shown in fig. 3.
Example 4
1. Preparation of shape memory conductive aerogel
(1) Mixing PEGDA 4000 (2.625g)、PEGDA 600 (1.125g) was dissolved in deionized water (6mL) with stirring at room temperature to give an aqueous solution of PEGDA;
(2) adding a predetermined amount of 2 wt% carbon black dispersion (9mL) to the aqueous PEGDA solution, ultrasonically dispersing for more than 1h by using an ultrasonic cell disruptor (SM-900D, Shunhamer instruments Co., Ltd., Nanjing), and then transferring the reaction system to a refrigerator at 4 ℃ for precooling;
(3) APS solution (4 wt%, 500. mu.L) and TEMED solution (50. mu.L) were added with slow stirring in an ice bath and quickly transferred to a circular ring mold;
(4) rapidly transferring the mold onto a copper column (the bottom of the copper column is always in contact with liquid nitrogen), and guiding ice crystals to directionally grow from the bottom to the top until the precursor solution is completely frozen;
(5) and finally, placing the reaction system in a refrigerator at the temperature of-15 ℃ for reaction for 50 hours. And after freezing polymerization is finished, freeze-drying for more than 48 hours to obtain the anisotropic conductive aerogel.
2. Assembly of a flexible pressure sensor
The aerogel with the upper and lower surfaces coated with the conductive silver paste is connected with a test probe of a digital multimeter (DMM 6500, Giaxle instruments, Inc.) by using a copper wire as a lead, so that the resistance change of the aerogel under pressure can be tested.
3. Application of shape programmable flexible pressure sensor (self-adaptive wearing on wrist by using light response shape recovery technology)
Placing annular pressure sensor in oven, and heating to T high (set at 70 ℃) and held for 10min to eliminate the thermal history, and then cooled to room temperature again; then again placed in the oven and held for 10min (T) high At 70 deg.C, and applying external force to fix the sensor into planar sheet shape, transferring the whole body into refrigerator to cool to T low (set to 4 ℃) for 10min to fix the temporary shape; removing the external force, and continuously placing the sensor in the refrigerator until the shape is not changed; the sample was placed on the wrist and indirectly heated under irradiation of near infrared light to return to a circular ring shape to be adaptively worn on the wrist (fig. 4).
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and should not be taken as limiting the scope of the present invention, which is intended to cover any modifications, equivalents, improvements, etc. within the spirit and scope of the present invention.
Claims (10)
1. A method of making a programmable shape flexible pressure sensor, comprising:
s11, preparing a polyethylene glycol diacrylate aqueous solution;
s12, adding the dispersion liquid of the material with the function of conductivity into the aqueous solution of the polyethylene glycol diacrylate to obtain reaction liquid of the material with the function of conductivity, and carrying out ice-bath on the reaction liquid;
s13, adding an ammonium persulfate solution and a tetramethyl ethylene diamine solution into the final liquid obtained in the step S12 to obtain a precursor solution, and quickly moving the precursor solution to a mold;
s14, moving the mold to a copper column, and contacting the bottom of the copper column with liquid nitrogen until the precursor solution is completely frozen;
s15, carrying out freeze polymerization on the S14 final reaction system, and after the freeze polymerization is finished, carrying out freeze drying to obtain anisotropic aerogel;
and S16, coating conductive silver paste on the upper surface and the lower surface of the aerogel, and connecting the aerogel and a digital multimeter probe by using a lead to obtain the shape-programmable flexible pressure sensor.
2. The method of claim, wherein the aqueous solution of polyethylene glycol diacrylate is PEGDA 4000 、PEGDA 600 Prepared by the PEGDA 4000 、PEGDA 600 The mass ratio is 1.5-2.5: 1.
3. a method for manufacturing a programmable flexible pressure sensor in shape according to claim 1, wherein the conductive functional material is selected from one or more of aminated carbon nanotube, titanium carbide, graphene oxide, liquid metal, and conductive carbon black.
4. A method of making a flexible shape programmable pressure sensor as in claim 1 wherein said conductive functional material dispersion has a concentration of 1 wt% to 5 wt%.
5. A method of making a flexible shape programmable pressure sensor as in claim 1 wherein the mass fraction of the conductive functional material throughout the system is between 0.1 wt% and 3 wt%.
6. The method of claim 1, wherein the step S12 further comprises the step of ultrasonically dispersing the conductive functional material and the shape memory polymer reaction solution by an ultrasonic cell disruptor, wherein the dispersion time is longer than 1 hour, and the ice bath temperature is 0-8 ℃.
7. A method of making a flexible shape programmable pressure sensor as in claim 1 wherein the ammonium persulfate solution concentration is in the range of 2 wt% to 6 wt%.
8. The method of claim 1, wherein the volume ratio of the ammonium persulfate solution, the tetramethylethylenediamine solution and the conductive functional material dispersion is 5: 0.5: 70-100.
9. A method of making a flexible shape programmable pressure sensor according to claim 1, wherein said freeze polymerization is carried out at a temperature of-20 ℃ to-10 ℃ for a time of 40h to 60h and a freeze drying time of greater than 48 h.
10. Use of a flexible pressure sensor prepared according to any one of claims 1 to 9, comprising:
s17, setting the flexible pressure sensor to a target shape state;
s18, changing the target shape state to obtain a temporary shape state;
and S19, restoring the target shape state through external stimulation in the application scene, and the flexible pressure sensor is worn on a specific wearing position in a self-adaptive mode.
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| CN115975411A (en) * | 2023-01-03 | 2023-04-18 | 山东大学 | Liquid metal conductive coating with cooperative deformability and preparation method thereof |
| CN117537699A (en) * | 2024-01-09 | 2024-02-09 | 西南交通大学 | Flexible strain sensor and preparation method thereof |
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