CN113733697B - High-sensitivity flexible composite film with wide sensing range and application thereof - Google Patents

High-sensitivity flexible composite film with wide sensing range and application thereof Download PDF

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CN113733697B
CN113733697B CN202110919946.8A CN202110919946A CN113733697B CN 113733697 B CN113733697 B CN 113733697B CN 202110919946 A CN202110919946 A CN 202110919946A CN 113733697 B CN113733697 B CN 113733697B
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mxene
tpu
film
composite film
pdms
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CN113733697A (en
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翁凌
张振楠
关丽珠
王小明
郭科
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Harbin University of Science and Technology
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B27/00—Layered products comprising a layer of synthetic resin
    • B32B27/28—Layered products comprising a layer of synthetic resin comprising synthetic resins not wholly covered by any one of the sub-groups B32B27/30 - B32B27/42
    • B32B27/283—Layered products comprising a layer of synthetic resin comprising synthetic resins not wholly covered by any one of the sub-groups B32B27/30 - B32B27/42 comprising polysiloxanes
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29D—PRODUCING PARTICULAR ARTICLES FROM PLASTICS OR FROM SUBSTANCES IN A PLASTIC STATE
    • B29D7/00—Producing flat articles, e.g. films or sheets
    • B29D7/01—Films or sheets
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B27/00—Layered products comprising a layer of synthetic resin
    • B32B27/06—Layered products comprising a layer of synthetic resin as the main or only constituent of a layer, which is next to another layer of the same or of a different material
    • B32B27/08—Layered products comprising a layer of synthetic resin as the main or only constituent of a layer, which is next to another layer of the same or of a different material of synthetic resin
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B27/00—Layered products comprising a layer of synthetic resin
    • B32B27/40—Layered products comprising a layer of synthetic resin comprising polyurethanes
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B3/00—Layered products comprising a layer with external or internal discontinuities or unevennesses, or a layer of non-planar form; Layered products having particular features of form
    • B32B3/02—Layered products comprising a layer with external or internal discontinuities or unevennesses, or a layer of non-planar form; Layered products having particular features of form characterised by features of form at particular places, e.g. in edge regions
    • B32B3/08—Layered products comprising a layer with external or internal discontinuities or unevennesses, or a layer of non-planar form; Layered products having particular features of form characterised by features of form at particular places, e.g. in edge regions characterised by added members at particular parts
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B33/00—Layered products characterised by particular properties or particular surface features, e.g. particular surface coatings; Layered products designed for particular purposes not covered by another single class
    • 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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2255/00—Coating on the layer surface
    • B32B2255/10—Coating on the layer surface on synthetic resin layer or on natural or synthetic rubber layer
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2255/00—Coating on the layer surface
    • B32B2255/20—Inorganic coating

Abstract

The invention discloses a flexible composite film with high sensitivity and wide sensing range and application thereof, belonging to the application fields of wearable sensors, electronic skin and the like. The invention aims to solve the technical problems of weak binding force between the flexible substrate and the active material, weak durability of the material and insufficient sensing range. The flexible composite film comprises an MXene/TPU composite film and a PDMS film, wherein the PDMS film is arranged at two sides of the MXene/TPU composite film and is bonded with the MXene/TPU composite film into a whole; wherein the MXene/TPU composite film is prepared by adopting a coating method, and then spraying 2D Ti 3 C 2 And (3) drying the aqueous solution of the colloid prepared by the MXene nano-sheets. The invention is suitable for a series of applications such as health detection, motion signals, robot motion detection, wearable electronic equipment and the like.

Description

High-sensitivity flexible composite film with wide sensing range and application thereof
Technical Field
The invention belongs to the application fields of wearable sensors, electronic skin and the like; in particular to a flexible composite film with high sensitivity and wide sensing range and application thereof; a preparation method of a PDMS-MXene/TPU flexible stress sensor.
Background
In recent years, with the rapid development of flexible sensors, flexible, thin, light, low-cost, wearable, mass-produced flexible sensors have become a big research hotspot. High sensitivity, fast response, wide sensing range flexible stress sensors are key to human-machine interaction and wearable electronics. The sensor has great application potential in the aspects of human activity monitoring, biomedical research and the like. However, there are still significant challenges in low cost, high sensitivity, mass-produced flexible sensors.
MXnes as 2D transition metal carbides, nitrides and carbonitrides with adjustable interlayer spacing, high specific surface area, metallic conductivity and controllable radical properties are the best choice as an active material for wearable flexible sensors. But MXene has poor stability when exposed to water-oxygen environments and also poor ability to interact with the polymer matrix, limiting the further development of flexibility and durability that MXenes expect in flexible sensors.
Chinese patent CN201811477438.3 adopts TPU flexible fiber membrane as substrate, MXene as conductive layer, and leads are connected at two ends of the film, and the invention is a flexible polyurethane fiber membrane strain sensor based on MXene. The invention improves the strain sensitivity of the sensor and enlarges the strain sensing range of the sensor.
Chinese patent CN202110307158.3 is composed of two layers of mxene@ap fabric structure and two sheets of medical semipermeable polyurethane film. The top layer and the bottom layer of the two-layer MXene@AP fabric structure are adhered with copper foil electrodes through silver paste; the copper foil electrode is connected with a copper wire; the top layer and the bottom layer of the two-layer MXene@AP fabric structure are encapsulated between two medical semipermeable polyurethane films; the MXene@AP fabric structure and the medical semipermeable polyurethane film are provided with a polyester film. The MXene stress sensor is flexible, waterproof, permeable, and wearable.
The above patent documents prepare flexible sensors by using a flexible substrate and an active substance MXene, and improve the melt strength of polypropylene by introducing long-chain branches, but the two technical schemes have the disadvantages of complex preparation process, weak bonding capability between interfaces and low durability.
The wearable sensor material with the wide sensing range is a technical problem to be solved by those skilled in the art.
Disclosure of Invention
The invention aims to solve the technical problems of weak binding force between the flexible substrate and the active material, weak durability of the material and insufficient sensing range; and provides a flexible composite film with high sensitivity and wide sensing range and application thereof.
According to the invention, through adopting PDMS encapsulation, the interaction of interfaces is improved, the durability of materials is enhanced, and the sensing range is enlarged by adopting a multi-spraying technology.
The flexible composite film with high sensitivity and wide sensing range comprises an MXene/TPU composite film and a PDMS film, wherein the PDMS film is arranged at two sides of the MXene/TPU composite film and is bonded with the MXene/TPU composite film into a whole; wherein the MXene/TPU composite film is prepared by adopting a coating method, and then spraying 2D Ti 3 C 2 And (3) drying the aqueous solution of the colloid prepared by the MXene nano-sheets.
Further, the Ti is 3 C 2 The average diameter of the MXene nanoplatelets was 1 μm.
The flexible composite film is used for manufacturing wearable sensors or electronic skins.
The preparation method of the PDMS-MXene/TPU flexible stress sensor is carried out according to the following steps:
dissolving 4-5 g of polyurethane (TPU) granules in 20mL-50mLN, N-Dimethylformamide (DMF) solution, stirring at 120-140 ℃ while condensing and refluxing, heating and reacting for 1 hour to obtain TPU glue solution, vacuumizing to remove bubbles, laying a film on a film laying machine, and drying at 80-100 ℃ for 1-2 hours to obtain a TPU film;
step two, 2D Ti 3 C 2 Adding the MXene nano-sheets into deionized water, and performing ultrasonic treatment for 30 minutes to obtain Ti 3 C 2 Spraying an MXene colloid aqueous solution onto the TPU film obtained in the step one, spraying for 1 to 5 times, and drying at the temperature of between 80 and 100 ℃ for 2 hours to obtain an MXene/TPU composite film;
step three, placing the MXene/TPU composite film into a die, enabling the MXene to face upwards, and placing an upper electrode on the surface of the MXene;
pouring the cured glue solution into a vacuum drying oven, vacuumizing, curing at 80-100 ℃ for 1-2 h, and taking out and demolding to obtain the PDMS-MXene/TPU flexible stress sensor;
the preparation method of the curing glue solution in the fourth step comprises the steps of mixing a curing agent and Polydimethylsiloxane (PDMS) according to the mass ratio of 1:8-12, fully stirring, and then performing ultrasonic treatment for 30 minutes to remove bubbles to obtain the curing glue solution.
According to the method, after the fourth treatment, the obtained composite film is turned over and placed in a die, and the fourth operation is performed, so that the thickness of the PDMS film at two sides of the MXene/TPU composite film can be kept consistent.
Further, the curing agent is dakangnin 184.
Further, the concentration of the colloid aqueous solution is 5mg/mL-20mg/mL.
The invention adopts a method of multiple spraying to change the distribution density of the sensing layer.
The invention uses PDMS for encapsulation treatment, which increases the relative action capability of the active surface and the flexible substrate.
The invention adopts encapsulation, can improve the service life of the material and strengthen the durability.
The flexible composite film with high sensitivity and wide sensing range is used for manufacturing raw materials of a wearable sensor, electronic skin and the like, can effectively improve the sensing performance, linearity and durability of the sensor, and can keep lower use loss.
The flexible composite film with high sensitivity and wide sensing range prepared by the invention uses Ti 3 C 2 The MXene nano-sheet is used as an active material, so that the sensing performance of the composite material is greatly improved.
The flexible composite film with high sensitivity and wide sensing range prepared by the invention has the advantages that the Thermoplastic Polyurethane (TPU) is used as a flexible matrix, the flexibility and the rebound resilience are good, the mechanical property of the sensor is maintained, and the sensing range is further improved. The requirement of the material on the mechanical property in the application field is ensured.
The PDMS-MXene/TPU flexible stress sensor has low detection limit (less than 0.005 percent, 0.5 mu m), wide sensing range (0-90 percent), short response time (120.1 ms) and excellent durability (> 3000 cycles). The high-sensitivity flexible strain sensor can be applied to a series of applications such as health detection, motion signals, robot motion detection, wearable electronic equipment and the like.
The flexible composite film with high sensitivity and wide sensing range prepared by the invention has the advantages of simple preparation process, no pollution, low energy consumption and high safety coefficient, and is suitable for industrial production.
Drawings
FIG. 1 is a schematic diagram of a sensor; in the figure, 1 is PDMS film, 2 is Ti 3 C 2 MXene, 3-TPU film, 4-electrode;
FIG. 2 is a scanning electron microscope image of an MXene/TPU composite film;
FIG. 3 shows ΔR/R of the flexible sensor at a stretch change of 10% -50% 0 A value map;
FIG. 4 shows the flexible sensor attached to a finger and the finger bending ΔR/R 0 A value map;
FIG. 5 shows the flexible sensor attached to the elbow, and the elbow being flexed by ΔR/R 0 A value map;
FIG. 6 is a graph of sensing performance of the flexible sensor under small shock;
FIG. 7 is a graph of sensing performance of a flexible sensor under small deformations;
FIG. 8 is a sensing performance of a flexible sensor stretched at a constant velocity;
FIG. 9 is a sensing performance of a flexible sensor under 40% elongation at speed change;
FIG. 10 is a response time of a flexible sensor;
FIG. 11 is a mechanical property of a flexible sensor in tension deformation;
fig. 12 is a sensing performance of the flexible sensor at 3000 stretch releasing cycles.
Detailed Description
Example 1: the preparation method of the PDMS-MXene/TPU flexible stress sensor comprises the following steps:
step 1, preparing a flexible substrate by a film coating method, firstly weighing 5g of polyurethane (TPU) granules, adding 40ml of N, N-Dimethylformamide (DMF) solution which is weighed in the same amount into a three-mouth bottle together, heating and stirring, and introducing water for condensation and reflux for about one hour to obtain TPU glue solution. Pouring the glue solution into a beaker, and vacuumizing to remove bubbles. The transparent glass plate is then washed and baked. Taking out the treated glue solution, uniformly pouring the glue solution on a glass plate, placing the glass plate on an automatic film coating machine for coating, placing the glass plate in a vacuum drying oven for drying after film laying is completed, and obtaining the TPU film after drying for 1h at 100 ℃ and demoulding.
Step 2, ti of 2D 3 C 2 Adding MXene nano-sheets into deionized water, and performing ultrasonic treatment for 30 minutes to obtain Ti with the concentration of 15mg/ml 3 C 2 MXene colloidal aqueous solution of Ti 3 C 2 The MXene colloid aqueous solution is treated by ultrasonic for 30 minutes, so that the MXene colloid aqueous solution is uniformly dispersed and has no agglomeration phenomenon. Thereafter Ti is added 3 C 2 And uniformly spraying the Mxene colloid aqueous solution on the TPU film, putting the TPU film in a drying oven for drying, drying at 80 ℃ for 2 hours, and taking out to obtain the MXene/TPU composite film.
And 3, placing the MXene/TPU composite film into a die, wherein the MXene faces upwards, copper foil electrodes are placed at two ends of the surface of the MXene, and the copper foil electrodes are connected with copper wires.
Step 4, preparing PDMS glue solution, and mixing Polydimethylsiloxane (PDMS) and a curing agent (dakangning 184) according to a weight ratio of 12:1, fully stirring, removing bubbles by ultrasonic for 30 minutes, pouring the glue solution into a mold stably, placing into a vacuum drying oven, vacuumizing, curing for one hour at 80 ℃, taking out and demolding to obtain the PDMS-MXene/TPU flexible stress sensor.
Example 2: the preparation method of the PDMS-MXene/TPU flexible stress sensor comprises the following steps:
step 1, a flexible substrate is prepared by a coating method. Firstly, 4g of polyurethane (TPU) granules are weighed, 30ml of N, N-Dimethylformamide (DMF) solution which is weighed together are added into a three-mouth bottle, and the mixture is heated and stirred while water is introduced for condensation reflux, so that TPU glue solution is obtained for about one hour. Pouring the glue solution into a beaker, and vacuumizing to remove bubbles. The transparent glass plate is then washed and baked. Taking out the treated glue solution, uniformly pouring the glue solution on a glass plate, placing the glass plate on an automatic film coating machine for coating, placing the glass plate in a vacuum drying oven for drying after film laying is completed, and obtaining the TPU film after drying at 80 ℃ for 2 hours and demoulding.
Step 2, ti of 2D 3 C 2 Adding MXene nano-sheets into deionized water, and performing ultrasonic treatment for 30 minutes to obtain Ti with the concentration of 10mg/ml 3 C 2 MXene colloidal aqueous solution of Ti 3 C 2 The MXene colloid aqueous solution is treated by ultrasonic for 30 minutes, so that the MXene colloid aqueous solution is uniformly dispersed and has no agglomeration phenomenon. Thereafter Ti is added 3 C 2 And uniformly spraying the Mxene colloid aqueous solution on the TPU film, drying the TPU film in a drying oven, drying the TPU film at 100 ℃ for 2 hours, continuously spraying the TPU film after drying, spraying the TPU film twice, and taking out the TPU film to obtain the MXene/TPU composite film.
And 3, placing the MXene/TPU composite film into a die, enabling the MXene to face upwards, placing copper foil electrodes at two ends of the surface of the MXene, and connecting copper wires with the copper foil electrodes.
Step 4, preparing PDMS glue solution, and mixing Polydimethylsiloxane (PDMS) and a curing agent (specifically, dakangning 184) according to a weight ratio of 9:1, fully stirring, removing bubbles by ultrasonic for 30 minutes, pouring the glue solution into a mold stably, placing into a vacuum drying oven, vacuumizing, curing at 100 ℃ for one hour, and taking out to obtain the PDMS-MXene/TPU flexible stress sensor (see figure 1).
As can be seen from FIG. 2, the scanning electron microscope image of the MXene/TPU composite film shows that the MXene nano-sheets are uniformly distributed on the TPU film.
As can be seen from fig. 3, the flexible sensor has stable sensitivity and linearity under 10% -50% deformation.
As can be seen from fig. 4, the flexible sensor has good sensitivity and sensing performance in finger bending motion. As a sensing element for electronic skin.
As can be seen from fig. 5, the flexible sensor has good sensitivity and sensing performance in elbow bending motion. As a sensing element for electronic skin.
The sensing performance of the flexible sensor under small vibrations is shown by fig. 6, which can be as small as 0.5 μm.
The sensing performance of the flexible sensor under small deformation is shown by fig. 7, which shows good linearity.
The sensing performance of the flexible sensor stretched at constant speed is illustrated by fig. 8.
The sensing performance of the flexible sensor under 40% of stretching speed is shown in fig. 9, so that different speeds can be obtained, the sensor is hardly affected, and the sensor stability is high.
The short response time of the flexible sensor, 120.1ms, is demonstrated by fig. 10.
The mechanical properties of the flexible sensor in tensile deformation are shown in fig. 11, and it is known that only very small creep occurs, basically no influence is caused on the properties, the mechanical properties are good, and the service life is good.
The sensing performance of the flexible sensor at 3000 stretch re-release cycles is illustrated by fig. 12. From the values, ΔR/R after 3000 times 0 The value is not changed greatly, the performance is not changed, and the durability and durability are good.

Claims (8)

1. The flexible composite film with high sensitivity and wide sensing range is characterized by comprising an MXene/TPU composite film and a PDMS film, wherein the PDMS film is arranged at two sides of the MXene/TPU composite film and is bonded with the MXene/TPU composite film into a whole; wherein the MXene/TPU composite film is prepared by adopting a coating method, and then spraying 2D Ti 3 C 2 The MXene nano-sheet prepared colloid aqueous solution is dried;
the preparation method comprises the following steps:
dissolving 4g-5g of polyurethane (TPU) granules in 20mL-50mLN, N-Dimethylformamide (DMF) solution, stirring at 120-140 ℃ while condensing and refluxing water, heating and reacting for 1 hour to obtain TPU glue solution, vacuumizing to remove bubbles, laying a film on a film laying machine, and drying at 80-100 ℃ for 1h-2h to obtain a TPU film;
step two, 2D Ti 3 C 2 Adding the MXene nano-sheets into deionized water, and performing ultrasonic treatment for 30 minutes to obtain Ti 3 C 2 Spraying an MXene colloid aqueous solution onto the TPU film obtained in the step one, spraying for 1 to 5 times, and drying at the temperature of between 80 and 100 ℃ for 2 hours to obtain an MXene/TPU composite film;
step three, placing the MXene/TPU composite film into a die, enabling the MXene to face upwards, and placing an upper electrode on the surface of the MXene;
pouring the cured glue solution into a vacuum drying oven, vacuumizing, curing at 80-100 ℃ for 1-2 h, and taking out and demolding to obtain the PDMS-MXene/TPU flexible stress sensor;
the preparation method of the curing glue solution in the fourth step comprises the steps of mixing a curing agent and Polydimethylsiloxane (PDMS) according to the mass ratio of 1:8-12, fully stirring, and then performing ultrasonic treatment for 30 minutes to remove bubbles to obtain the curing glue solution.
2. A flexible composite film according to claim 1, characterized in that said Ti 3 C 2 The average diameter of the MXene nanoplatelets was 1 μm.
3. The flexible composite film according to claim 1, wherein the concentration of the aqueous colloidal solution is 5mg/mL to 20mg/mL.
4. The flexible composite film of claim 1 for use in making wearable sensors or electronic skin.
5. The preparation method of the PDMS-MXene/TPU flexible stress sensor is characterized by comprising the following steps:
dissolving 4g-5g of polyurethane (TPU) granules in 20mL-50mLN, N-Dimethylformamide (DMF) solution, stirring at 120-140 ℃ while condensing and refluxing water, heating and reacting for 1 hour to obtain TPU glue solution, vacuumizing to remove bubbles, laying a film on a film laying machine, and drying at 80-100 ℃ for 1h-2h to obtain a TPU film;
step two, 2D Ti 3 C 2 Adding the MXene nano-sheets into deionized water, and performing ultrasonic treatment for 30 minutes to obtain Ti 3 C 2 Spraying an MXene colloid aqueous solution onto the TPU film obtained in the step one, spraying for 1 to 5 times, and drying at the temperature of between 80 and 100 ℃ for 2 hours to obtain an MXene/TPU composite film;
step three, placing the MXene/TPU composite film into a die, enabling the MXene to face upwards, and placing an upper electrode on the surface of the MXene;
pouring the cured glue solution into a vacuum drying oven, vacuumizing, curing at 80-100 ℃ for 1-2 h, and taking out and demolding to obtain the PDMS-MXene/TPU flexible stress sensor;
the preparation method of the curing glue solution in the fourth step comprises the steps of mixing a curing agent and Polydimethylsiloxane (PDMS) according to the mass ratio of 1:8-12, fully stirring, and then performing ultrasonic treatment for 30 minutes to remove bubbles to obtain the curing glue solution.
6. The method for manufacturing the PDMS-MXene/TPU flexible stress sensor according to claim 5, wherein after the fourth treatment, the obtained composite membrane is turned over and placed in a mold, and then the operation of the fourth treatment is performed.
7. The method for manufacturing a PDMS-MXene/TPU flexible stress sensor according to claim 5 or 6 wherein the curing agent is Dow Corning 184.
8. The method for manufacturing the PDMS-MXene/TPU flexible stress sensor according to claim 5 or 6, wherein the concentration of the aqueous colloidal solution in the second step is 5mg/mL-20mg/mL.
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CN113203505A (en) * 2021-05-14 2021-08-03 东南大学 Pressure/strain bimodal sensor based on low-dimensional nano composite material and preparation method thereof

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