CN113340478A - Preparation method of flexible stress sensor - Google Patents
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- CN113340478A CN113340478A CN202110621353.3A CN202110621353A CN113340478A CN 113340478 A CN113340478 A CN 113340478A CN 202110621353 A CN202110621353 A CN 202110621353A CN 113340478 A CN113340478 A CN 113340478A
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- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims abstract description 61
- 239000002042 Silver nanowire Substances 0.000 claims abstract description 60
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 47
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- CXQXSVUQTKDNFP-UHFFFAOYSA-N octamethyltrisiloxane Chemical compound C[Si](C)(C)O[Si](C)(C)O[Si](C)(C)C CXQXSVUQTKDNFP-UHFFFAOYSA-N 0.000 description 1
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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
- G01L1/14—Measuring force or stress, in general by measuring variations in capacitance or inductance of electrical elements, e.g. by measuring variations of frequency of electrical oscillators
- G01L1/142—Measuring force or stress, in general by measuring variations in capacitance or inductance of electrical elements, e.g. by measuring variations of frequency of electrical oscillators using capacitors
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Abstract
The invention belongs to the technical field of electronic materials and the field of sensors, and discloses a preparation method of a flexible stress sensor. The method comprises the steps of cleaning conductive sponge, preparing a silver nanowire ethanol solution, dripping and coating, and packaging the sensor. The inherent three-dimensional porous loose structure of the conductive sponge is fully utilized, and the conductive sponge can deform when the stress changes slightly, so that the change of the stress is sensitively sensed, and the sensitivity of the sensor is enhanced; meanwhile, the silver nanowires are combined with the sponge structure, so that the conductivity is enhanced, and the silver nanowires and the porous loose structure of the conductive sponge generate a synergistic effect to enhance the sensitivity of the sensor.
Description
Technical Field
The invention belongs to the technical field of electronic materials and the field of sensors, and particularly relates to a preparation method of a flexible stress sensor.
Background
In recent years, flexible stress sensors based on flexible conductive materials have been widely studied and applied in the thermal fields of electronic mobile terminals, medical health monitoring devices, intelligent robots, and the like. Conventional stress sensing devices are mostly based on metal and semiconductor materials, and their stretchability and sensitivity are greatly limited. The flexible stress sensor not only has the advantages of the traditional sensor, but also has good stretchability and sensing characteristics, so that the flexible stress sensor can be attached to the surface of the skin of a human body and the surface of an object with a complex structure.
A flexible stress sensor typically includes several portions, a base layer, a dielectric layer, an active layer, and electrodes. For flexible stress sensors, the substrate material is the key factor in determining its elastic deformation properties, and generally requires high flexibility and relatively low roughness. The dielectric material is typically an electrically insulating material, and the dielectric material of the flexible electronic field effect transistor is typically a conventional elastomeric material, such as PDMS. The active layer is one of the most important components of the flexible stress sensor, so that the active layer material with excellent mechanical properties and electronic properties is the key to determine the performance of the flexible stress sensor. The electrodes are two end electrodes for continuously inputting and outputting micro current from the flexible stress sensor, and in the process of preparing the flexible stress sensor, the conductivity of the electrode material is also an important factor influencing the sensitivity and stability of the sensor.
The flexible stress sensor has many defects in the aspects of preparation and application, such as poor force-sensitive characteristics, incapability of combining flexibility and high sensitivity, complex preparation process and the like, and further development of the flexible stress sensor is still seriously hindered. At present, the development of new materials is a very good development opportunity of the flexible stress sensor, for example, continuous research and development of materials such as novel graphene, novel carbon nanotubes and novel silver nanowires, and the like, and a new development opportunity of the functional composite flexible material is provided. Researchers at home and abroad are actively researching and preparing flexible stress sensors based on composite materials such as graphene, carbon nanotubes and silver nanowires, and the like, and hopefully, the flexible stress sensors have great potential in the aspects of strain and stress monitoring by virtue of the excellent properties of the novel materials. The flexible stress sensor with high sensitivity and quick response time is still difficult to prepare by adopting a simple and low-cost method, and the assembly, arrangement, acquisition and packaging technology of the flexible stress sensor still needs to be further improved. Therefore, the flexible stress sensor which has simple research process, low cost, high sensitivity and quick response time has important research significance and application prospect.
Disclosure of Invention
In order to overcome the defects of the existing flexible stress sensor, the invention provides a preparation method of the flexible stress sensor, and the preparation method has the advantages of low cost, simplicity in preparation and easiness in large-scale production. The flexible stress sensor is based on the combination of conductive sponge and silver nanowires as a substrate layer and an active layer. The conductive sponge and the silver nanowires are directly purchased and obtained in the market. The conductive sponge is made of polyurethane foam sponge as a matrix, and is subjected to PVD (physical vapor deposition) conductive treatment and electro-deposition of metal nickel, copper and other thickening treatments, so that the sponge is conductive in all directions, has the characteristics of good conductivity, strong bonding force, high shielding efficiency, good rebound resilience, stable performance and the like, and is an EMI/ESD (electro-magnetic interference/static discharge) material widely applied at present.
The above purpose of the invention is realized by the following technical scheme: a method for preparing a flexible stress sensor comprises the following steps:
1) cleaning the conductive sponge: and placing the conductive sponge in deionized water and absolute ethyl alcohol for ultrasonic cleaning, and then airing or drying at low temperature for later use.
2) Preparing an ethanol solution of silver nanowires: preparing a uniform silver nanowire ethanol solution with the concentration range of 0.1mg/ml-10 mg/ml.
3) And (3) dripping: and uniformly dripping the dispersed silver nanowire ethanol solution on clean conductive sponge, and dripping multiple layers. The silver nanowire composite conductive sponge generates a synergistic effect, and the sensitivity of the sensor is enhanced in the force application process.
4) Packaging of the sensor: the flexible stress sensor is prepared by packaging a conductive sponge attached with silver nanowires as an electrode and a polyurethane sponge, a polyethylene film or a polytetrafluoroethylene film as a dielectric layer.
Further, the number of the drop coating layers in the step 3) is 2-10.
Compared with the prior art, the invention has the beneficial effects that: 1) the inherent three-dimensional porous loose structure of the conductive sponge is fully utilized, and the conductive sponge can deform when the stress changes slightly, so that the change of the stress is sensed sensitively, and the sensitivity of the sensor is enhanced. The sponge is directly purchased from the market, so that the preparation process of the sensor is greatly simplified, the cost is low, and the large-scale production is facilitated. 2) The silver nanowires are combined with the sponge structure, the conductivity is enhanced, the silver nanowires and the porous loose structure of the conductive sponge generate a synergistic effect, the sponge deforms to cause capacitance change in the force application process, and the silver nanowires can further form capacitance change along with deformation, so that the sensitivity of the sensor is enhanced.
Drawings
FIG. 1 is a block diagram of a packaged flexible stress sensor made in accordance with the present invention;
FIG. 2 is a scanning electron microscope image of the conductive sponge after dropping silver nanowires, magnified 250 times;
FIG. 3 is a scanning electron microscope image of the conductive sponge with 20000 times magnification after dropping silver nanowires;
FIG. 4 shows sensitivity curves for different dielectric material sensors in an embodiment of the invention.
In the figure, 1 is a conducting wire, 2 is a metal sponge, 3 is a dielectric layer, and 4 is a double-sided adhesive tape.
Detailed Description
The invention is described in more detail below with reference to specific examples, without limiting the scope of the invention. Unless otherwise specified, the experimental methods adopted by the invention are all conventional methods, and experimental equipment, materials, reagents and the like used in the experimental method can be obtained from commercial sources.
A flexible stress sensor comprising a conductive sponge and a layer of silver nanowires attached to its surface. The preparation method of the flexible stress sensor provided by the embodiment of the invention comprises the following steps:
firstly, cleaning the conductive sponge. Cutting the conductive sponge into a sample with a certain size, firstly placing the sample in deionized water for ultrasonic cleaning for 20 minutes, then placing the sample in absolute ethyl alcohol for ultrasonic cleaning for 20 minutes, placing the cleaned conductive sponge in a culture dish for natural airing or placing the cleaned conductive sponge in a vacuum oven for 1 hour at 50 ℃.
And step two, preparing an ethanol solution of the silver nanowires. Preparing ethanol solution (0.01-5 mg/ml) of silver nanowires with a certain concentration, and performing ultrasonic treatment for 10 minutes after preparation to fully disperse the silver nanowires in the ethanol to obtain uniform solution.
And thirdly, dripping. And uniformly dripping the dispersed silver nanowire ethanol solution on clean conductive sponge, wherein 2-10 layers can be dripped, and after one layer is dripped, the silver nanowire ethanol solution is placed in a cool and dry place to be naturally dried and then dripped one layer. The silver nanowire composite conductive sponge is expected to produce a synergistic effect, and the sensitivity of the sensor is enhanced in the force application process.
And fourthly, packaging the sensor. Spreading the prepared conductive sponge electrode on a glass slide with one side facing upwards, and attaching double-sided adhesive tapes to the peripheral edge of the side facing downwards of the conductive sponge electrode. One end of the copper wire is inserted into the gap between the conductive sponge and the double-sided tape. The side of the dielectric layer (such as polyurethane sponge, PE film or PTFE film) facing upwards is attached to the side of the conductive sponge electrode facing downwards. And attaching the other conductive sponge electrode with the double-sided adhesive tape and the copper wire adhered to the periphery of the other conductive sponge electrode to the other surface of the dielectric layer to form the sensor with the five-layer structure of the conductive sponge electrode/adhesive tape/dielectric layer/adhesive tape/conductive sponge electrode. And (4) carrying out surface packaging on the prepared flexible stress sensor by using a preservative film. The packaged sensor structure is shown in fig. 1.
Some flexible stress sensors are fabricated by designing nano conductive materials to form a three-dimensional network structure within an elastomer. The mechanism of stress sensing is that the resistance or capacitance is changed due to the change of the nano conductive network structure in the stress process. The uniformity of the nano conductive network and the microstructure change of the nano conductive network are important influencing factors influencing the sensitivity of the sensor. The uniformity of the nano-conductive network is particularly poorly controlled. The conductive sponge adopted by the invention adopts polyurethane foam sponge as a substrate, and all directions of the sponge are conductive through PVD conductive treatment and thickening treatment of electrodeposited metal nickel, copper and the like, and the three-dimensional network structure is stable and uniform. The conductive sponge has excellent flexibility because of the close arrangement of the pores. And when the silver nanowires are uniformly attached to the foam network of the conductive sponge and stressed, the silver nanowire structure also generates secondary deformation in a microscopic mode along with the large deformation of the sponge foam structure, and the change of the multi-level conductive network structure is beneficial to enhancing the sensitivity of the stress sensor.
Example 1
And immersing the conductive sponge cut into 13mm multiplied by 13mm into deionized water, and ultrasonically cleaning for 20min to clean impurities on the surface of the conductive sponge. And after the deionized water cleaning is finished, soaking the glass substrate in absolute ethyl alcohol for ultrasonic cleaning for 20 min. And taking out the conductive sponge after the ultrasonic cleaning from the absolute ethyl alcohol, and drying in a vacuum drying oven at 50 ℃ for 20 min. And taking out after drying, standing and cooling. Using 200 mul pipette to transfer 0.05ml silver nano-wire solution with concentration of 10mg/ml into 1.5ml micro centrifuge tube, then using 1000 mul pipette to transfer 0.95ml deionized water into the same micro centrifuge tube, and oscillating the micro centrifuge tube to prepare 1ml silver nano-wire solution with concentration of 0.5 mg/ml. And (3) uniformly dripping and coating the silver nanowire solution with the concentration of 0.5mg/ml on one surface of the dried and cooled conductive sponge by using a liquid transfer gun from the micro centrifugal tube, standing and drying to obtain the conductive sponge electrode dripping and coating a layer of silver nanowire ethanol solution. And after the sample is dried, turning over the conductive sponge, transferring the silver nanowire solution with the concentration of 0.5mg/ml from the micro centrifugal tube by using a liquid transfer gun, uniformly dripping the silver nanowire solution on the other surface, and standing and drying. To this end the conductive sponge has been drop coated with 2 layers of silver nanowire solution with a concentration of 0.5 mg/ml. The above operation was repeated to prepare a conductive sponge with 6 layers of silver nanowires drop-coated. The microstructure of the conductive sponge for preparing the 6-layer silver nanowire drop coating is shown in fig. 2 and 3. The porous structure of the conductive sponge can be observed from fig. 2, and fig. 3 is a microscopic morphology of silver nanowires attached to the conductive sponge after 2 ten thousand times of amplification.
Spreading and placing the prepared conductive sponge flexible electrode on a glass slide with the front side facing upwards, and tightly attaching a double-sided adhesive tape with the width of 5mm and the length of 5mm to the periphery of the downward reverse side of the conductive sponge flexible electrode. One end of a copper wire with the length of 10cm, which is exposed out of the copper wire, is tightly inserted into a gap between the conductive flexible sponge and the double-sided adhesive. And (3) attaching the upward front surface of the tiled flexible polyurethane sponge with the thickness of 0.5cm to the downward back surface of the conductive sponge electrode. And attaching the other conductive flexible sponge electrode with the double-sided adhesive tape and the copper wire adhered to the periphery of the other conductive flexible sponge electrode to the other surface of the polyurethane sponge to form the sensor with the five-layer structure of the conductive sponge electrode/adhesive tape/polyurethane sponge/adhesive tape/conductive sponge electrode. And (4) carrying out surface packaging on the prepared flexible stress sensor by using a preservative film. The dielectric layer is Polyurethane (PU) sponge, and the electrode material is a flexible stress sensor of conductive sponge with 6 layers of silver nanowires in a dripping mode. The red curve in fig. 4 is the sensitivity curve of this embodiment.
Example 2
And immersing the conductive sponge cut into 13mm multiplied by 13mm into deionized water, and ultrasonically cleaning for 20min to clean impurities on the surface of the conductive sponge. And after the deionized water cleaning is finished, soaking the glass substrate in absolute ethyl alcohol for ultrasonic cleaning for 20 min. And taking out the conductive sponge after the ultrasonic cleaning from the absolute ethyl alcohol, and drying in a vacuum drying oven at 50 ℃ for 20 min. And taking out after drying, standing and cooling. Using 200 mul pipette to transfer 0.05ml silver nano-wire solution with concentration of 10mg/ml into 1.5ml micro centrifuge tube, then using 1000 mul pipette to transfer 0.95ml deionized water into the same micro centrifuge tube, and oscillating the micro centrifuge tube to prepare 1ml silver nano-wire solution with concentration of 0.5 mg/ml. And (3) transferring the silver nanowire solution with the concentration of 0.5mg/ml from the micro centrifugal tube by using a liquid transfer gun, uniformly dripping and coating one surface of the dried and cooled conductive sponge, standing and drying, and thus finishing dripping and coating 1 layer of the sample. And after the sample is dried, turning over the conductive sponge, transferring the silver nanowire solution with the concentration of 0.5mg/ml from the micro centrifugal tube by using a liquid transfer gun, uniformly dripping the silver nanowire solution on the other surface, and standing and drying. To this end the conductive sponge has been drop coated with 2 layers of silver nanowire solution with a concentration of 0.5 mg/ml. The above operation was repeated to prepare a conductive sponge with 6 layers of silver nanowires drop-coated. The microstructure of the conductive sponge for preparing the 6-layer silver nanowires by drop coating is shown in fig. 2 and 3. The porous structure of the conductive sponge can be observed from fig. 2, and fig. 3 is a microscopic morphology of silver nanowires attached to the conductive sponge after 2 ten thousand times of amplification.
Spreading and placing the prepared conductive sponge flexible electrode on a glass slide with the front side facing upwards, and tightly attaching a double-sided adhesive tape with the width of 5mm and the length of 5mm to the periphery of the downward reverse side of the conductive sponge flexible electrode. One end of a copper wire with the length of 10cm, which is exposed out of the copper wire, is tightly inserted into a gap between the conductive flexible sponge and the double-sided adhesive. And attaching the upward front side of the PE film to the downward back side of the conductive sponge electrode. And attaching the other conductive flexible sponge electrode with the double-sided adhesive tape and the copper wire adhered to the periphery of the other conductive flexible sponge electrode to the other side of the PE film to form the sensor with the five-layer structure of conductive sponge electrode/adhesive tape/PE film/adhesive tape/conductive sponge electrode. And (4) carrying out surface packaging on the prepared flexible stress sensor by using a preservative film. The dielectric layer is a Polyethylene (PE) film, and the electrode material is a flexible stress sensor of conductive sponge with 6 layers of silver nanowires in a dropping mode. The blue curve in fig. 4 is the sensitivity curve of this embodiment.
Example 3
And immersing the conductive sponge cut into 13mm multiplied by 13mm into deionized water, and ultrasonically cleaning for 20min to clean impurities on the surface of the conductive sponge. And after the deionized water cleaning is finished, soaking the glass substrate in absolute ethyl alcohol for ultrasonic cleaning for 20 min. And taking out the conductive sponge after the ultrasonic cleaning from the absolute ethyl alcohol, and drying in a vacuum drying oven at 50 ℃ for 20 min. And taking out after drying, standing and cooling. Using 200 mul pipette to transfer 0.05ml silver nano-wire solution with concentration of 10mg/ml into 1.5ml micro centrifuge tube, then using 1000 mul pipette to transfer 0.95ml deionized water into the same micro centrifuge tube, and oscillating the micro centrifuge tube to prepare 1ml silver nano-wire solution with concentration of 0.5 mg/ml. And (3) transferring the silver nanowire solution with the concentration of 0.5mg/ml from the micro centrifugal tube by using a liquid transfer gun, uniformly dripping and coating one surface of the dried and cooled conductive sponge, standing and drying, and thus finishing dripping and coating 1 layer of the sample. And after the sample is dried, turning over the conductive sponge, transferring the silver nanowire solution with the concentration of 0.5mg/ml from the micro centrifugal tube by using a liquid transfer gun, uniformly dripping the silver nanowire solution on the other surface, and standing and drying. To this end the conductive sponge has been drop coated with 2 layers of silver nanowire solution with a concentration of 0.5 mg/ml. The above operation was repeated to prepare a conductive sponge with 6 layers of silver nanowires drop-coated. The microstructure of the conductive sponge for preparing the 6-layer silver nanowires by drop coating is shown in fig. 2 and 3. The porous structure of the conductive sponge can be observed from fig. 2, and fig. 3 is a microscopic morphology of silver nanowires attached to the conductive sponge after 2 ten thousand times of amplification.
Spreading and placing the prepared conductive sponge flexible electrode on a glass slide with the front side facing upwards, and tightly attaching a double-sided adhesive tape with the width of 5mm and the length of 5mm to the periphery of the downward reverse side of the conductive sponge flexible electrode. One end of a copper wire with the length of 10cm, which is exposed out of the copper wire, is tightly inserted into a gap between the conductive flexible sponge and the double-sided adhesive. And attaching the upward front surface of the Polytetrafluoroethylene (PTFE) film to the downward back surface of the conductive sponge electrode. And attaching the other conductive flexible sponge electrode with the double-sided adhesive tape and the copper wire adhered to the periphery of the other conductive flexible sponge electrode to the other surface of the PTFE film to form the sensor with the five-layer structure of the conductive sponge electrode/adhesive tape/PTFE film/adhesive tape/conductive sponge electrode. And (4) carrying out surface packaging on the prepared flexible stress sensor by using a preservative film. The dielectric layer is a tetrafluoroethylene (PTFE) film, and the electrode material is a flexible stress sensor of conductive sponge with 6 layers of silver nanowires in a dropping mode. The black curve in fig. 4 is the sensitivity curve of this embodiment.
The embodiments described above are merely preferred embodiments of the invention, rather than all possible embodiments of the invention. Any obvious modifications to the above would be obvious to those of ordinary skill in the art, but would not bring the invention so modified beyond the spirit and scope of the present invention.
Claims (3)
1. A preparation method of a flexible stress sensor is characterized by comprising the following steps:
1) cleaning the conductive sponge: placing the conductive sponge in deionized water and absolute ethyl alcohol for ultrasonic cleaning, and then airing or drying at low temperature for later use;
2) preparing an ethanol solution of silver nanowires: preparing a uniform silver nanowire ethanol solution with the concentration range of 0.1mg/ml-10 mg/ml;
3) and (3) dripping: uniformly dripping the dispersed silver nanowire ethanol solution on clean conductive sponge, wherein multiple layers can be dripped;
4) packaging of the sensor: and (3) packaging the conductive sponge attached with the silver nanowires with a dielectric layer to prepare the flexible stress sensor.
2. The method for preparing a flexible stress sensor according to claim 1, wherein the number of the dropping layers in the step 3) is 2-10.
3. The method of claim 1, wherein the dielectric layer of step 4) is one of a polyurethane sponge, a polyethylene film, or a teflon film.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114486013A (en) * | 2022-02-14 | 2022-05-13 | 东南大学 | Pressure sensor based on capacitance-resistance conversion principle and preparation method thereof |
| CN115302902A (en) * | 2022-07-06 | 2022-11-08 | 河南工业大学 | Flexible magnetic sensor and preparation method thereof |
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