CN113203505A - Pressure/strain bimodal sensor based on low-dimensional nano composite material and preparation method thereof - Google Patents
Pressure/strain bimodal sensor based on low-dimensional nano composite material and preparation method thereof Download PDFInfo
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- CN113203505A CN113203505A CN202110526887.8A CN202110526887A CN113203505A CN 113203505 A CN113203505 A CN 113203505A CN 202110526887 A CN202110526887 A CN 202110526887A CN 113203505 A CN113203505 A CN 113203505A
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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
- G01L1/20—Measuring force or stress, in general by measuring variations in ohmic resistance of solid materials or of electrically-conductive fluids; by making use of electrokinetic cells, i.e. liquid-containing cells wherein an electrical potential is produced or varied upon the application of stress
- G01L1/22—Measuring force or stress, in general by measuring variations in ohmic resistance of solid materials or of electrically-conductive fluids; by making use of electrokinetic cells, i.e. liquid-containing cells wherein an electrical potential is produced or varied upon the application of stress using resistance strain gauges
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01B—MEASURING LENGTH, THICKNESS OR SIMILAR LINEAR DIMENSIONS; MEASURING ANGLES; MEASURING AREAS; MEASURING IRREGULARITIES OF SURFACES OR CONTOURS
- G01B7/00—Measuring arrangements characterised by the use of electric or magnetic techniques
- G01B7/16—Measuring arrangements characterised by the use of electric or magnetic techniques for measuring the deformation in a solid, e.g. by resistance strain gauge
- G01B7/18—Measuring arrangements characterised by the use of electric or magnetic techniques for measuring the deformation in a solid, e.g. by resistance strain gauge using change in resistance
Abstract
The invention discloses a pressure/strain bimodal sensor based on a low-dimensional nano composite material and a preparation method thereof, wherein the pressure sensor comprises a lower electrode, a resistance sensitive layer, a TPU sponge framework and an upper electrode; the resistance sensitive layer is compounded by one-dimensional and two-dimensional conductive materials, takes the 3D porous structure of TPU sponge as a framework, and is uniformly deposited on the surface of the framework to form a film. The composite material forms a microscopic cross-linked conductive network consisting of point contact, surface-to-surface contact and point-to-surface contact of a one-dimensional conductive material and a two-dimensional conductive material on a microscopic material structure. The conductive network of the resistance sensitive layer deforms or is disconnected under the action of strain, the output resistance is increased along with the increase of the strain, and the strain detection mode is realized; under the pressure action, the pores of the 3D porous structure of the resistance sensitive layer are closed, the resistance sensitive layers deposited on the surfaces of the upper wall and the lower wall of each pore are contacted, the conductive paths are increased, the output resistance is reduced along with the increase of the pressure, and the pressure detection is realized. The flexible sensor can realize bimodal detection of pressure and strain signals, and the preparation method is simple and easy to implement and high in feasibility.
Description
Technical Field
The invention relates to a flexible sensor, in particular to a pressure/strain bimodal sensor based on a low-dimensional nano composite material and a preparation method thereof.
Background
With the rapid development of wearable electronic devices, flexible mechanical sensors have received much attention due to their potential applications in motion detection, biomedical monitoring, human-computer interaction, and the like. Sensors are generally classified into four main types, piezoelectric, capacitive, frictional, and resistive, depending on the operating mechanism. Among various sensing types, the resistive sensor can convert applied pressure into changes of current or resistance, and has the advantages of high sensitivity, quick response, simple manufacturing process, low energy consumption and the like. Microstructural designs, such as porous structures, hollow sphere structures, micro-pyramid array structures, etc., are generally considered to be effective methods of fabricating pressure sensors. However, the manufacturing processes for these microstructure designs are mostly expensive and complex. Therefore, it remains a challenge to produce flexible mechanical sensors with high sensitivity at low cost and on a large scale, especially to produce flexible sensors that can be used for strain and pressure bimodal detection.
Sponge is widely applied to daily life of people as a low-cost porous material. The material has the advantages of good water absorption, good elasticity, high porosity, large internal surface area and the like. Generally, the interaction between the sponge and the one-dimensional conductive material or the nano-particles is not strong enough, which results in an unstable sensor. Although additional processing techniques, such as layer-by-layer assembly and multiple dip coating, can overcome the above disadvantages, the manufacturing process of the sensor becomes more complex.
Disclosure of Invention
The technical problem is as follows: the technical problem to be solved by the invention is as follows: the pressure/strain bimodal sensor based on the low-dimensional nano composite material is provided, and strain and pressure double-parameter detection is realized. Also provides a preparation method of the material and the structure of the sensor.
The technical scheme is as follows: in order to solve the problems, the invention provides a pressure/strain bimodal sensor based on a low-dimensional nano composite material, which comprises a lower electrode, a TPU sponge framework, an upper electrode and a resistance sensitive layer;
the resistance sensitive layer is positioned in the TPU sponge framework and coated on the surface of the porous structure of the TPU sponge framework, the upper electrode is positioned on the upper surface of the TPU sponge framework, and the lower electrode is positioned on the lower surface of the TPU sponge framework.
Further, the resistance sensitive layer is a composite of a one-dimensional conductive material and a two-dimensional conductive material. The composite material forms a microscopic cross-linked conductive network consisting of point contact, surface-to-surface contact and point-to-surface contact of a one-dimensional conductive material and a two-dimensional conductive material on a microscopic material structure.
Further, the two-dimensional conductive material is MXene nanosheets, and the one-dimensional material is multi-walled carbon nanotubes.
Furthermore, the upper electrode and the lower electrode are both metal conductive adhesive tapes and are respectively attached to the upper surface and the lower surface of the TPU sponge framework.
The one-dimensional conductive material and the two-dimensional conductive material are mutually crosslinked in the TPU sponge framework to form a conductive network. The conductive network of the resistance sensitive layer deforms or is disconnected under the action of strain, the resistance is increased along with the increase of the strain, and the strain detection mode is realized; the TPU sponge framework porous structure with the resistance sensitive layer is closed in the pores under the action of pressure, the resistance sensitive layers positioned on the upper wall and the lower wall of the pores are contacted, the conductive path is increased, the resistance is reduced along with the increase of the pressure, and the pressure detection is realized. The flexible sensor can realize bimodal detection of pressure and strain signals, and the preparation method is simple and easy to implement and high in feasibility.
On the other hand, the invention also provides a preparation method of the pressure/strain bimodal sensor based on the low-dimensional nano composite material, which comprises the following steps:
the first step is as follows: soaking TPU polyurethane sponge into ethanol solution for ultrasonic treatment to remove impurities on the surface of the TPU polyurethane sponge, and using the TPU polyurethane sponge as a TPU sponge framework;
the second step is that: mixing a two-dimensional conductive material and a one-dimensional conductive material in water and performing ultrasonic treatment to completely disperse the two materials, and stirring by using a magnetic stirrer to form a uniformly mixed aqueous solution of the two-dimensional conductive material and the one-dimensional conductive material;
the third step: soaking the TPU sponge framework into a mixed aqueous solution of a two-dimensional conductive material and a one-dimensional conductive material and carrying out ultrasonic treatment to enable the TPU sponge framework to fully absorb the solution;
the fourth step: putting the TPU sponge framework which absorbs the mixed solution of the two-dimensional conductive material and the one-dimensional conductive material into a vacuum drying oven for drying, so that the two-dimensional conductive material and the one-dimensional conductive material are uniformly deposited on the surface of the TPU sponge framework to form a conductive network which is a resistance composite sensitive layer and is crosslinked with each other;
the fifth step: repeating the third step and the fourth step until the resistance value of the resistance sensitive layer on the surface of the TPU sponge framework tends to be stable;
and a sixth step: and adhering an upper electrode to the upper surface of the TPU sponge framework coated with the resistance sensitive layer, and adhering a lower electrode to the lower surface of the TPU sponge framework to obtain the flexible pressure sensor.
Further, in the second step, the two-dimensional conductive material is an MXene nanosheet, the one-dimensional conductive material is a multiwall carbon nanotube, and the MXene nanosheet and the multiwall carbon nanotube are mixed according to a mass ratio of 1: 5 mixing in water.
Has the advantages that:
compared with the prior art, the invention uses MXene nano-sheets and multi-walled carbon nano-tubes to compound as a sensitive layer, and the sensitive layer is uniformly deposited on the surface of the TPU sponge framework, and has the following beneficial effects,
first, the reliability and stability of the sensor is improved. The MXene nanosheets are two-dimensional flaky, can be in large-area contact with the sponge framework, are stably and firmly attached to the surface of the framework, and increase the attachment capacity of the resistance sensitive layer on the surface of the framework, so that the reliability and the stability of sensing detection are improved;
and secondly, the detection range of the sensor during strain test is improved. As the MXene nanosheets and the multi-walled carbon nanotubes are compounded with the conductive network, when the MXene nanosheets are subjected to tensile strain, the MXene nanosheets are firstly separated, so that the conductive network is partially disconnected, and the resistance value is increased; with the increase of external force, the resistance value is continuously increased due to more separation of MXene nano sheets, and a conductive network formed by one-dimensional nano tubes is arranged at the edge of the disconnection between the surfaces of the nano sheets;
and thirdly, the sensitivity of the sensor is improved, and MXene serving as a two-dimensional nano material with ultrahigh conductivity in the existing report can provide a large number of low-resistance conductive paths. The surface-to-surface contact of the MXene nanosheets is damaged under the action of strain, so that the resistance can be increased rapidly, and the device has higher sensitivity;
fourthly, as the multi-walled carbon nano tube is insoluble in water and easy to agglomerate, the MXene nano sheet is ultrasonically mixed with the multi-walled carbon nano tube, so that the uniform dispersion of the multi-walled carbon nano tube in an aqueous solution is facilitated, the uniform distribution of the nano material on the surface of the framework in the dip coating process is further ensured, and the stability of the device is improved on the other hand;
in addition, by adopting the preparation scheme of the invention, the sensing detection of different modes of pressure and strain can be realized. The preparation method is simple and feasible and has high feasibility.
Drawings
FIG. 1 is a schematic diagram and cross-sectional view of a sensor in an embodiment of the invention;
FIG. 2 is a cross-sectional view of a first step in a method of making a sensor according to an embodiment of the present invention;
FIG. 3 is a structural sectional view of a second step of the sensor manufacturing method in the embodiment of the present invention;
FIG. 4 is a sectional view showing the structure of the third step of the sensor manufacturing method in the embodiment of the present invention;
FIG. 5 is an SEM image of the surface microtopography of a sensor in an embodiment of the invention;
FIG. 6 is a schematic diagram of a strain sensing mode detection of a sensor in an embodiment of the invention;
FIG. 6(a) is a cross-sectional view in the direction of stretching of a sensor of the present invention when unstrained;
FIG. 6(b) is a cross-sectional view of the sensor of the present invention taken along the direction of elongation with a slight strain;
FIG. 6(c) is a cross-sectional view of the sensor of the present invention taken along the direction of elongation at high strain;
FIG. 7 is a schematic diagram of a pressure sensing mode detection of a sensor in an embodiment of the present invention;
FIG. 7(a) is a cross-sectional view and a partially enlarged view of the sensor of the present invention in the absence of external pressure;
FIG. 7(b) is a cross-sectional view and a partially enlarged view of the sensor of the present invention when subjected to a slight pressure;
FIG. 7(c) is a cross-sectional view and a partially enlarged view of the sensor of the present invention under slight pressure;
fig. 7(d) is a cross-sectional view and a partial enlargement of the sensor of the present invention with the aperture fully closed.
The figure shows that: 1. a lower electrode; 2. a resistance sensitive layer; 3. a TPU sponge framework; 4. an upper electrode; 201. MXene nanosheets; 202. multi-walled carbon nanotubes.
Detailed Description
As shown in fig. 1, a pressure/strain bimodal sensor based on a low-dimensional nanocomposite material comprises a lower electrode 1, a TPU sponge framework 3, an upper electrode 4 and a resistance sensitive layer 2.
The resistance sensitive layer is positioned in the TPU sponge framework 3 and is coated on the surface of the porous structure of the TPU sponge framework 3, the upper electrode 4 is positioned on the upper surface of the TPU sponge framework 3, and the lower electrode 1 is positioned on the lower surface of the TPU sponge framework 3. The upper electrode 4 and the lower electrode 1 are respectively connected with lead wires for leading out.
The resistance sensitive layer 2 is a composite material of a one-dimensional conductive material and a two-dimensional conductive material; the two-dimensional conductive material is MXene nanosheet 201; the one-dimensional material is multi-walled carbon nanotubes 202.
The upper electrode 4 and the lower electrode 1 are made of the same structure and material, and the upper electrode 4 and the lower electrode 1 are made of metal conductive adhesive tapes which are respectively attached to the upper surface and the lower surface of the TPU sponge framework 3.
The embodiment of the invention also provides a preparation method of the pressure/strain bimodal sensor based on the low-dimensional nano composite material, and the preparation flow comprises the following steps:
the first step is as follows: cutting TPU polyurethane sponge into regular sizes, immersing the TPU polyurethane sponge into an ethanol solution for 30 minutes of ultrasonic treatment, removing impurities on the surface of the sponge, and using the sponge as a TPU sponge framework 3 as shown in figure 2;
the second step is that: mixing MXene nano-sheets 201 and multi-wall carbon nano-tubes 202 according to the mass ratio of 1: 5 mixing in water and sonicating for 2 hours to completely disperse the two materials. Stirring for 30 minutes by using a magnetic stirrer to ensure that the MXene nanosheets 201 and the multi-walled carbon nanotubes 202 form a uniformly mixed aqueous solution; wherein, the performance of the sensor is influenced by the mass ratio of the MXene nano-sheets 201 to the multi-wall carbon nano-tubes 202.
The third step: immersing the TPU sponge framework 3 into a mixed aqueous solution of MXene nanosheets 201 and multi-walled carbon nanotubes 202, and performing ultrasonic treatment for 2 hours to enable the TPU sponge framework 3 to fully absorb the solution;
the fourth step: putting the TPU sponge framework 3 absorbing the mixed solution of the MXene nanosheets 201 and the multi-walled carbon nanotubes 202 into a vacuum drying oven, and drying at 70 ℃ for 12 hours to ensure that the MXene nanosheets 201 and the multi-walled carbon nanotubes 202 are uniformly deposited on the surface of the TPU sponge framework 3 to form a conductive network which is mutually crosslinked to form a resistance composite sensitive layer, as shown in FIG. 3;
the fifth step: repeating the third step and the fourth step until the resistance value of the resistance sensitive layer 2 on the surface of the TPU sponge framework 3 tends to be stable;
and a sixth step: and adhering an upper electrode 4 to the upper surface of the TPU sponge framework 3 coated with the resistance sensitive layer 2, and adhering a lower electrode 1 to the lower surface of the TPU sponge framework to obtain the pressure sensor based on the low-dimensional nano composite material-polyurethane sponge, as shown in FIG. 4.
The SEM image of the surface microtopography of the prepared sensor is shown in FIG. 5, wherein the situation that the MXene nanosheet 201 and the multi-wall carbon nanotube 202 composite material is deposited on a sponge framework, the MXene nanosheet 201 coats the framework, the multi-wall carbon nanotube 202 is uniformly distributed between the surface of the MXene nanosheet 201 and the adjacent MXene nanosheets 201, and the situation that the multi-wall carbon nanotubes are still connected at the surface disconnection part of the MXene nanosheet 201 can be observed.
When the flexible sensor in the above embodiment operates in the strain detection mode, the operating mechanism of the flexible sensor is shown in fig. 6, fig. 6(a) is a structural diagram of the sensor in the absence of strain, and under the action of an external strain, as shown in fig. 6(b), for a conductive network formed by crosslinking of MXene nanosheets 201 and multi-walled carbon nanotubes 202, overlapping portions of the MXene nanosheets 201 are firstly separated under a slight strain, the resistance increases with the increase of the strain, and the conductive network at this time mainly depends on the crosslinking of the multi-walled carbon nanotubes 202 distributed among the MXene nanosheets 201; with the further increase of the strain, as shown in fig. 6(c), the multi-walled carbon nanotubes 202 originally distributed between the MXene nanosheets 201 and constituting the conductive path for the same are pulled apart, so that effective point contact cannot be formed, the conductive path is greatly reduced, and the resistance is greatly increased with the increase of the strain. On the basis of the principle, the strain is converted into the change of the resistance, and the strain detection mode is realized.
When the flexible sensor of the above embodiment works in the pressure detection mode, the working mechanism is shown in fig. 7, and the resistance sensitive layer 2 is uniformly deposited on the porous structure in the TPU sponge skeleton 3, such as the 3D porous structure shown in fig. 7 (a). Under the action of a slight pressure, as shown in fig. 7(b), the initial stress is mainly concentrated at the intersection of the frameworks, the intersection is slightly deformed under the action of the pressure, the resistance sensitive layer 2 on the surface cracks, and the resistance is increased along with the increase of the pressure; as the pressure increases, the multi-walled carbon nanotubes 202 of the surface resistance sensitive layer 2 generate more cross-linking under the action of extrusion, the negative effect of cracks at the beginning is gradually inhibited, and the resistance decreases along with the increase of the pressure; under the further action of pressure, as shown in fig. 7(c), the MXene nanosheets 201 in the resistance sensitive layer 2 begin to overlap with each other to form more surface contacts, and the resistance continues to decrease with the increase of the pressure; when the pressure is increased to a certain degree, as shown in fig. 7(d), the pores of the porous structure begin to close, the resistance sensitive layers 2 on the upper and lower walls of the pores form a large amount of surface contact, the conductive paths are increased, and the resistance is greatly reduced along with the increase of the pressure; when the pore is completely closed, the pressure is continuously applied, the sensor reaches the detection limit, and the resistance is hardly changed. On the basis of the principle, pressure is converted into resistance change, and a pressure detection mode is realized.
The foregoing illustrates and describes the principles, general features, and advantages of the present invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are intended to further illustrate the principles of the invention, and that various changes and modifications may be made without departing from the spirit and scope of the invention, which is also intended to be covered by the appended claims. The scope of the invention is defined by the claims and their equivalents.
Claims (6)
1. A pressure/strain bimodal sensor based on a low-dimensional nano composite material is characterized by comprising a lower electrode, a TPU sponge framework, an upper electrode and a resistance sensitive layer;
the resistance sensitive layer is positioned in the TPU sponge framework and coated on the surface of the porous structure of the TPU sponge framework, the upper electrode is positioned on the upper surface of the TPU sponge framework, and the lower electrode is positioned on the lower surface of the TPU sponge framework.
2. The low dimensional nanocomposite based pressure/strain bimodal sensor according to claim 1, wherein said resistive sensitive layer is a composite of one-dimensional conductive material and two-dimensional conductive material.
3. The low dimensional nanocomposite based pressure/strain bimodal sensor according to claim 2, wherein the two dimensional conductive material is MXene nanoplatelets and the one dimensional material is multiwall carbon nanotubes.
4. The low-dimensional nanocomposite material-based pressure/strain bimodal sensor as claimed in claim 2, wherein the upper electrode and the lower electrode are both metal conductive tapes, respectively attached to the upper surface and the lower surface of the TPU sponge skeleton.
5. A method for preparing a high-sensitivity flexible pressure sensor based on a multilayer composite film according to any one of claims 1 to 4, comprising the following steps:
the first step is as follows: soaking TPU polyurethane sponge into ethanol solution for ultrasonic treatment to remove impurities on the surface of the TPU polyurethane sponge, and using the TPU polyurethane sponge as a TPU sponge framework;
the second step is that: mixing a two-dimensional conductive material and a one-dimensional conductive material in water and performing ultrasonic treatment to completely disperse the two materials, and stirring by using a magnetic stirrer to form a uniformly mixed aqueous solution of the two-dimensional conductive material and the one-dimensional conductive material;
the third step: soaking the TPU sponge framework into a mixed aqueous solution of a two-dimensional conductive material and a one-dimensional conductive material and carrying out ultrasonic treatment to enable the TPU sponge framework to fully absorb the solution;
the fourth step: putting the TPU sponge framework which absorbs the mixed solution of the two-dimensional conductive material and the one-dimensional conductive material into a vacuum drying oven for drying, so that the two-dimensional conductive material and the one-dimensional conductive material are uniformly deposited on the surface of the TPU sponge framework to form a conductive network which is a resistance composite sensitive layer and is crosslinked with each other;
the fifth step: repeating the third step and the fourth step until the resistance value of the resistance sensitive layer on the surface of the TPU sponge framework tends to be stable;
and a sixth step: and adhering an upper electrode to the upper surface of the TPU sponge framework coated with the resistance sensitive layer, and adhering a lower electrode to the lower surface of the TPU sponge framework to obtain the flexible pressure sensor.
6. The method for preparing the high-sensitivity flexible pressure sensor based on the multilayer composite film as claimed in claim 5, wherein in the second step, the two-dimensional conductive material is MXene nanosheets, the one-dimensional conductive material is multiwall carbon nanotubes, and the MXene nanosheets and the multiwall carbon nanotubes are mixed in a mass ratio of 1: 5 mixing in water.
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Application publication date: 20210803 |