CN113237580A - MXene high-sensitivity piezoresistive sensor and preparation method thereof - Google Patents
MXene high-sensitivity piezoresistive sensor and preparation method thereof Download PDFInfo
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- CN113237580A CN113237580A CN202110545181.6A CN202110545181A CN113237580A CN 113237580 A CN113237580 A CN 113237580A CN 202110545181 A CN202110545181 A CN 202110545181A CN 113237580 A CN113237580 A CN 113237580A
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- 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
Abstract
The invention provides an MXene high-sensitivity piezoresistive sensor and a preparation method thereof, wherein the sensor comprises a conductive material, a flexible interdigital electrode and a flexible sensitive layer, the flexible interdigital electrode is placed on any flexible material by using an interdigital electrode mask and is prepared into the MXene flexible interdigital electrode by a spraying process, the flexible sensitive layer is a flexible sensitive layer with a surface microstructure obtained by using sand paper as a template, and the MXene @ PU sensitive layer is prepared on the microstructure surface of the flexible sensitive layer by the spraying process; the assembly of the above parts together results in an MXene highly sensitive piezoresistive sensor. The conductive materials selected by the invention are MXene, so that the preparation cost is effectively reduced; according to the invention, the PU flexible sensitive layer is prepared by taking sand paper as a template, so that the microstructure flexible sensitive layer with high resilience is effectively obtained, and the sensor has higher sensitivity.
Description
Technical Field
The invention relates to the field of sensors, in particular to an MXene high-sensitivity piezoresistive sensor and a preparation method thereof.
Background
With the rapid development of the intelligent industry, wearable sensor devices are continuously appearing in various aspects of people's life, including human-computer interaction, bionic limbs, health exercise monitoring devices and medical devices, so that healthy life style is compatible with convenience, energy efficiency and intellectualization. At the same time, high performance pressure sensors play a crucial role in wearable sensor devices. According to the working principle, the flexible pressure sensor is generally divided into a piezoresistive type, a capacitive type and a piezoelectric type. The piezoresistive pressure sensor is most widely applied, and mainly has the advantages of simple sensing principle, high signal-to-noise ratio, stable sensing performance and the like compared with a capacitive type pressure sensor and a piezoelectric type pressure sensor.
The problems faced by the flexible piezoresistive sensors at present are mainly divided into two aspects, one is a performance improvement direction, so that the sensors have higher sensitivity, resolution, response speed and good stability; another problem is the development process and cost, and the fabrication of existing flexible piezoresistive sensor electrodes relies mainly on highly complex, high-consumption processes, such as magnetron sputtering, silicon etching, and metal film deposition. Particularly, the experimental conditions of high vacuum and high voltage required by magnetron sputtering have high requirements on equipment, and in addition, precious metals commonly used in magnetron sputtering are expensive. These methods do not allow easy large scale preparation of sensor electrodes, which limits their further applications. Therefore, it is urgent to find an experimental process with simple structure, simple manufacturing process and high sensitivity for preparing the wearable piezoresistive sensor.
Disclosure of Invention
The invention provides an MXene high-sensitivity piezoresistive sensor and a preparation method thereof, and the sensor is very simple in preparation process, energy-saving and environment-friendly, can realize higher sensitivity and has good application prospect.
The technical scheme for realizing the invention is as follows:
a high-sensitivity piezoresistive transducer for MXene comprises a conductive material, a flexible interdigital electrode and a flexible sensitive layer, wherein the conductive material is a novel two-dimensional transition metal carbide, nitride or carbonitride MXene, the flexible interdigital electrode is a flexible interdigital electrode which is prepared by placing an interdigital electrode mask on any flexible material and preparing MXene through a spraying process, the flexible sensitive layer is a Polyurethane (PU) flexible sensitive layer with a surface microstructure by using sand paper as a template, and the MXene @ PU sensitive layer is prepared on the microstructure surface of the flexible PU sensitive layer through the spraying process; the assembly of the above parts together results in an MXene highly sensitive piezoresistive sensor.
The interdigital electrode mask is a stainless steel interdigital electrode mask prepared by a high-precision chemical corrosion method and can be repeatedly used.
The conductive material is novel two-dimensional transition metal carbide, nitride or carbonitride MXene.
The conductive material is Ti2C、V2C、Mo2C、Ti3C2、(V,Cr)3C2、Ti3(C,N)2Or Ti4C3One or more of them.
The flexible sensitive layer comprises at least one of flexible materials such as polyimide, cellulose filter membrane, polyurethane, polydimethylsiloxane or ordinary A4 paper.
Preferably, the flexible material for preparing the interdigital electrode is polyimide.
The preparation method of the MXene high-sensitivity piezoresistive sensor comprises the following steps:
(1) a synthetic conductive material MXene;
the MXene is obtained by selectively etching a precursor MAX phase through hydrochloric acid and lithium fluoride, wherein M is a transition metal, A is mainly a III group element or an IV group element, and X is a C element or an N element in the MAX phase; the precursor MAX phase is more preferably Ti3AlC2MXene is therefore Ti3C2TXNanosheets;
with Ti3AlC2For example, the details are as follows:
0.5g of precursor (Ti) was weighed3AlC2) Slowly adding the solution into a mixed solution of 0.5g LiF and 10ml of 75% HCl, magnetically stirring the solution at room temperature (25 ℃) for reaction for 36 hours, then centrifugally cleaning the reacted mixed solution until the pH value is neutral, and marking the successful synthesis of MXene that the supernatant obtained by the last centrifugation is dark green; dispersing the synthesized MXene into a certain amount of deionized water, and ultrasonically stripping for 1 h while introducing inert gas, wherein the temperature cannot exceed 20 ℃ in the ultrasonic stripping process, and the MXene solution after ultrasonic stripping is subjected to ultrasonic strippingCentrifuging at 3500rpm for 1 h, collecting the supernatant as MXene (Ti)3C2TX) A nanosheet colloidal solution;
(2) preparing an MXene flexible interdigital electrode by a spraying method;
simply fixing an interdigital electrode mask on a polyimide flexible sensitive layer by using an adhesive tape, then placing the polyimide flexible sensitive layer on a heating table, setting the temperature of the heating table at 50-90 ℃, uniformly spraying MXene colloidal solution on the surface of the polyimide flexible sensitive layer, and removing the interdigital electrode mask when the linear resistance of each interdigital electrode per 1 cm is lower than 5 omega to obtain the MXene flexible interdigital electrode;
(3) preparing an MXene @ PU sensitive layer with a surface microstructure by a spraying method;
firstly, using sand paper as a template, respectively casting PU on the rough surfaces of 100, 180, 280, 400, 600 and 800-mesh gauze paper, and after the PU is naturally dried, stripping the PU from the surface of the sand paper to obtain a flexible sensitive layer with a surface microstructure; then placing the micro-structure on a heating table, setting the temperature to be 50-90 ℃, and uniformly spraying MXene colloidal solution on the surface of the micro-structure until the linear resistance of each 1 cm of the surface is 5-30 omega; obtaining MXene @ PU with a surface microstructure;
(4) packaging the MXene @ PU sensitive layer on the surface of the flexible interdigital electrode;
placing the microstructure surface of the MXene @ PU sensitive layer facing the MXene interdigital electrode, and fixing the microstructure surface on the surface of the interdigital electrode by using an adhesive tape;
(5) welding wires at two ends of the interdigital electrode, wherein the wires are copper wires, iron wires or silver wires, and preferably copper wires; the material of the welding electrode is copper foil or conductive silver paste, and more preferably conductive silver paste.
The thickness of the interdigital electrode is 5-5.5 um, the surface microstructure of the MXene @ PU sensitive layer can be adjusted by the mesh number of sand paper, when the interdigital electrode and the MXene @ PU sensitive layer are packaged into a piezoresistive sensor and pressure is applied to the surface of the piezoresistive sensor, conductive paths between the interdigital electrode and the piezoresistive sensor are increased, so that the resistance is reduced, the output current is increased, and finally, the sensitivity is greatly improved. The interdigital electrode takes polyimide as a flexible substrate, and when the mesh number of sand paper is 280 meshes, the prepared piezoresistive sensor is in the range of 0.3346 kPa-5.6369 kPaThe sensitivity in the enclosure is as high as 11812 kPa-1。
The invention has the beneficial effects that:
(1) conductive material: the active conducting layers on the surfaces of the flexible interdigital electrode and the microstructure flexible sensitive layer are made of novel two-dimensional transition metal carbide, nitride or carbonitride MXene lamellar materials, the materials are simple in preparation process, free of pollution to the environment and low in cost, meanwhile, the materials have hydrophilicity and excellent metal conductivity, and the MXene nanosheets are excellent in mechanical property and more suitable for being applied to preparation of flexible piezoresistive sensors.
(2) Microstructure flexible sensitive layer: the flexible sensitive layer with the surface microstructure is prepared by selecting the PU with high resilience and high wear resistance as the flexible sensitive layer and adopting the sand paper as the template, the template method is simple to operate, and the surface microstructure can greatly improve the strain range of the piezoresistive sensor.
(3) Flexible interdigital electrode: the method for preparing the flexible interdigital electrode adopts a simple spraying method, is not only suitable for large-scale production and manufacture, but also solves the problem that the substrate of the interdigital electrode is limited by the traditional preparation method, and has feasibility for preparing the flexible interdigital electrode by any flexible material. The preparation of the flexible interdigital electrode has the advantages of simple operation and universality.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts.
Fig. 1 is a schematic flow chart of a preparation method of an MXene high-sensitivity piezoresistive sensor according to the present invention.
FIG. 2 shows a precursor Ti of the present invention3AlC2And prepared Ti3C2TXXRD pattern of (a).
Fig. 3 is a picture of a flexible interdigital electrode prepared by the spraying method of the present invention.
Fig. 4 is a scanning electron microscope microscopic morphology image of the sensitive layer of MXene @ PU prepared using sandpaper of different roughness according to the present invention.
FIG. 5 is a sensitivity contrast diagram of a flexible piezoresistive sensor prepared by sand paper with different roughness when the flexible interdigital electrode is MXene-polyimide.
FIG. 6 is an I-V diagram of a flexible piezoresistive sensor according to the invention at different pressures.
FIG. 7 is an I-T diagram of a flexible piezoresistive sensor according to the invention at different pressures.
FIG. 8 is a graph of response and recovery time for a flexible piezoresistive sensor according to the present invention.
FIG. 9 is a sensitivity comparison graph of a flexible piezoresistive sensor prepared by sand paper with different roughness when the flexible interdigital electrode is an MXene-cellulose filter membrane.
Detailed Description
The technical solutions of the present invention will be described clearly and completely with reference to the following embodiments of the present invention, and it should be understood that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without any inventive step, are within the scope of the present invention.
Example 1
A schematic diagram of a preparation method of an MXene high-sensitivity piezoresistive sensor specifically comprises the following steps:
(1) a synthetic conductive material MXene; first, 0.5g of precursor (Ti) was weighed3AlC2) Slowly adding the solution into a mixed solution of 0.5g LiF and 10ml 75% HCl, magnetically stirring the solution at room temperature (25 ℃) for reaction for 36 hours, then centrifugally cleaning the reacted mixed solution until the pH value is neutral, wherein the supernatant obtained by the last centrifugation is dark green, which marks the successful synthesis of MXene; dispersing the MXene synthesized in a certain amount of deionized water, and introducingUltrasonic stripping with high purity nitrogen gas for 1 h, wherein the temperature cannot exceed 20 ℃ in the ultrasonic stripping process, MXene solution after ultrasonic stripping is centrifuged at 3500rpm for 1 h, and the collected supernatant is MXene (Ti)3C2TX) A nanosheet colloidal solution;
(2) preparing an MXene flexible interdigital electrode by a spraying method; simply fixing an interdigital electrode mask on a polyimide flexible sensitive layer by using an adhesive tape, then placing the interdigital electrode mask on a heating table, setting the temperature of the heating table at 50-90 ℃, uniformly spraying MXene colloidal solution on the surface of the interdigital electrode mask, and removing the interdigital electrode mask when the linear resistance of each interdigital electrode 1 cm is lower than 5 omega to obtain the MXene-polyimide flexible interdigital electrode;
(3) preparing an MXene @ PU sensitive layer with a surface microstructure by a spraying method; firstly, using sand paper as a template, respectively casting PU on the rough surfaces of 100, 180, 280, 400, 600 and 800-mesh gauze paper, and after the PU is naturally dried, stripping the PU from the surface of the sand paper to obtain a flexible sensitive layer with a surface microstructure; then placing the micro-structure on a heating table, and uniformly spraying MXene colloidal solution on the surface of the micro-structure until the linear resistance of each 1 cm of the surface is between 5 and 30 omega; obtaining MXene @ PU sensitive layer with surface microstructure;
(4) packaging the MXene @ PU sensitive layer on the surface of the flexible interdigital electrode; placing the microstructure surface of the MXene @ PU sensitive layer facing the MXene interdigital electrode, and fixing the microstructure surface on the surface of the interdigital electrode by using an adhesive tape;
(5) welding wires at two ends of the interdigital electrode; the lead is a copper wire, and the material of the welding electrode is conductive silver paste.
In this embodiment, the surface of the sensitive layer intercepting MXene @ PU by the piezoresistive sensor is 1 × 1 cm2。
FIG. 2 shows precursors (Ti) respectively3AlC2) And MXene (Ti)3C2TX) XRD pattern of nanosheet, from which precursor (Ti) can be seen3AlC2) The Al in (b) was successfully etched away.
FIG. 3 (a) is an interdigital electrode mask in an embodiment; fig. 3 (b) and fig. 3 (c) are the front and side surfaces of an MXene flexible interdigital electrode obtained by uniformly spraying MXene on a polyimide substrate by an interdigital electrode reticle in the example, respectively.
FIG. 4 is a Scanning Electron Microscope (SEM) microscopic morphology of MXene @ PU sensitive layers prepared from 100, 180, 280, 400, 600 and 800 mesh tissue papers respectively according to the invention; it can be seen that the protrusions and holes on the surface of the sensitive layer become smaller and smaller as the number of sandpaper used increases.
FIG. 5 is a graph comparing sensitivity of flexible piezoresistive sensors fabricated from sandpaper of different roughness according to the present invention; it can be seen that when the flexible interdigital electrode is MXene-polyimide, the piezoresistive sensor has ultrahigh sensitivity, wherein the sensitivity of the flexible piezoresistive sensor prepared by 280-mesh sand paper is as high as 11812 kPa in the range of 0.3346 kPa to 5.6369 kPa-1。
FIG. 6 is an I-V diagram of a flexible piezoresistive sensor according to the invention at different pressures.
FIG. 7 is an I-T diagram of a flexible piezoresistive sensor according to the invention at different pressures.
FIG. 8 is a graph of response and recovery times for a flexible piezoresistive sensor according to the present invention; the sensor can be seen to have extremely fast response speed, response time 89.6 ms and recovery time 67.2 ms when being stimulated by external pressure.
Example 2
A schematic diagram of a preparation method of an MXene high-sensitivity piezoresistive sensor specifically comprises the following steps:
(1) a synthetic conductive material MXene; first, 0.5g of precursor (Ti) was weighed3AlC2) Slowly adding the mixed solution into a mixed solution of 0.5g LiF and 10ml of 75% HCl, magnetically stirring the mixed solution at 35 ℃ for reaction for 36 hours, then centrifugally cleaning the reacted mixed solution until the pH value is neutral, and marking the successful synthesis of MXene that the supernatant obtained by the last centrifugation is dark green; dispersing the synthesized MXene into a certain amount of deionized water, performing ultrasonic stripping for 1 h while introducing high-purity argon, centrifuging the MXene solution subjected to ultrasonic stripping at 3000rpm for 1 h while paying attention to the fact that the temperature cannot exceed 20 ℃ in the ultrasonic stripping process, and collectingThe supernatant of (A) is MXene (Ti)3C2TX) nanosheet colloidal solution;
(2) preparing an MXene flexible interdigital electrode by a spraying method; simply fixing the interdigital electrode mask on a cellulose filter paper flexible substrate by using an adhesive tape, then placing the substrate on a heating table, setting the temperature of the heating table at 50-90 ℃, uniformly spraying MXene colloidal solution on the surface of the substrate, and removing the interdigital electrode mask when the linear resistance of each interdigital electrode 1 cm is lower than 5 omega to obtain the MXene-cellulose filter membrane flexible interdigital electrode;
(3) preparing an MXene @ PU sensitive layer with a surface microstructure by a spraying method; firstly, using sand paper as a template, respectively casting PU on the rough surfaces of 100, 180, 280, 400, 600 and 800-mesh gauze paper, and peeling off the PU from the surface of the sand paper after the PU is naturally dried to obtain a flexible substrate with a surface microstructure; then placing the micro-structure on a heating table, and uniformly spraying MXene colloidal solution on the surface of the micro-structure until the linear resistance of each 1 cm of the surface is between 5 and 30 omega; obtaining MXene @ PU sensitive layer with surface microstructure;
(4) packaging the MXene @ PU sensitive layer on the surface of the flexible interdigital electrode; placing the microstructure surface of the MXene @ PU sensitive layer facing the MXene interdigital electrode, and fixing the microstructure surface on the surface of the interdigital electrode by using an adhesive tape;
(5) welding wires at two ends of the interdigital electrode; the lead is a copper wire, and the material of the welding electrode is conductive silver paste.
In this embodiment, the surface of the sensitive layer intercepting MXene @ PU by the piezoresistive sensor is 1 × 1 cm2。
FIG. 9 is a graph comparing sensitivity of flexible piezoresistive sensors fabricated from sandpaper of different roughness according to the present invention; it can be seen that when the flexible interdigital electrode is an MXene-cellulose filter membrane, the piezoresistive sensor has ultrahigh sensitivity, wherein the sensitivity of the flexible piezoresistive sensor prepared by 400-mesh sand paper is up to 10213 kPa in the range of 0.2358 Pa-5.7715 kPa-1。
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (10)
1. An MXene's high sensitivity piezoresistive sensor, includes conducting material, flexible interdigital electrode and flexible sensitive layer, its characterized in that: the flexible interdigital electrode is prepared by adopting a spraying process.
2. The MXene high sensitivity piezoresistive sensor according to claim 1, characterized in that: fixing the interdigital electrode mask on the flexible sensitive layer, then placing the interdigital electrode mask on a heating table, setting the temperature of the heating table at 50-90 ℃, uniformly spraying MXene colloidal solution on the surface of the interdigital electrode mask, and removing the interdigital electrode mask when the linear resistance of each 1 cm of the interdigital electrode is lower than 5 omega to obtain the MXene flexible interdigital electrode.
3. The MXene high sensitivity piezoresistive sensor according to claim 1, characterized in that: the conductive material is novel two-dimensional transition metal carbide, nitride or carbonitride MXene.
4. The MXene high sensitivity piezoresistive sensor of claim 3 wherein: the conductive material is Ti2C、V2C、Mo2C、Ti3C2、(V,Cr)3C2、Ti3(C,N)2Or Ti4C3One or more of them.
5. The MXene high sensitivity piezoresistive sensor according to claim 2, characterized in that: the flexible sensitive layer comprises at least one of polyimide, cellulose filter, polyurethane, polydimethylsiloxane or ordinary A4 paper.
6. The method for preparing MXene high sensitivity piezoresistive sensor as claimed in any of claims 1-5, wherein the steps are as follows:
(1) a synthetic conductive material MXene;
(2) preparing an MXene flexible interdigital electrode by a spraying method;
(3) preparing an MXene @ PU sensitive layer with a surface microstructure by a spraying method;
(4) packaging the MXene @ PU sensitive layer on the surface of the flexible interdigital electrode;
(5) and welding wires at two ends of the interdigital electrode.
7. The preparation method according to claim 6, wherein in the step (2), the interdigital electrode mask is fixed on the flexible sensitive layer and then placed on a heating table, the temperature of the heating table is set to be 50-90 ℃, MXene colloid solution is uniformly sprayed on the surface of the interdigital electrode mask, and when the linear resistance of each 1 cm of the interdigital electrode is lower than 5 Ω, the interdigital electrode mask is removed to obtain the MXene flexible interdigital electrode.
8. The method of claim 6, wherein: in the step (3), sand paper is used as a template, PU is cast on the rough surface of the sand paper, and after the PU is naturally dried, the PU is peeled off from the surface of the sand paper to obtain the flexible sensitive layer with the surface microstructure; and then placing the photosensitive layer on a heating table, and uniformly spraying MXene colloidal solution on the surface of the microstructure until the linear resistance of each 1 cm of the surface is between 5 and 30 omega, thus obtaining the MXene @ PU sensitive layer with the surface microstructure.
9. The method of claim 8, wherein: the grit number comprises 100, 180, 280, 400, 600, or 800 grit sandpaper.
10. The method of claim 9, wherein: when the mesh number of the sand paper is 280 meshes, the sensitivity of the prepared piezoresistive sensor is as high as 11812 kPa within the range of 0.3346 kPa-5.6369 kPa-1。
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| CN113237580B (en) | 2023-01-10 |
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