CN114235212A - Flexible temperature sensing material, sensor and preparation method thereof - Google Patents
Flexible temperature sensing material, sensor and preparation method thereof Download PDFInfo
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01K—MEASURING TEMPERATURE; MEASURING QUANTITY OF HEAT; THERMALLY-SENSITIVE ELEMENTS NOT OTHERWISE PROVIDED FOR
- G01K13/00—Thermometers specially adapted for specific purposes
- G01K13/20—Clinical contact thermometers for use with humans or animals
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01K—MEASURING TEMPERATURE; MEASURING QUANTITY OF HEAT; THERMALLY-SENSITIVE ELEMENTS NOT OTHERWISE PROVIDED FOR
- G01K5/00—Measuring temperature based on the expansion or contraction of a material
- G01K5/48—Measuring temperature based on the expansion or contraction of a material the material being a solid
- G01K5/486—Measuring temperature based on the expansion or contraction of a material the material being a solid using microstructures, e.g. made of silicon
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01K—MEASURING TEMPERATURE; MEASURING QUANTITY OF HEAT; THERMALLY-SENSITIVE ELEMENTS NOT OTHERWISE PROVIDED FOR
- G01K5/00—Measuring temperature based on the expansion or contraction of a material
- G01K5/48—Measuring temperature based on the expansion or contraction of a material the material being a solid
- G01K5/50—Measuring temperature based on the expansion or contraction of a material the material being a solid arranged for free expansion or contraction
- G01K5/52—Measuring temperature based on the expansion or contraction of a material the material being a solid arranged for free expansion or contraction with electrical conversion means for final indication
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- General Physics & Mathematics (AREA)
- Chemical & Material Sciences (AREA)
- Crystallography & Structural Chemistry (AREA)
- Measuring Temperature Or Quantity Of Heat (AREA)
Abstract
The invention discloses a flexible temperature sensing material, a sensor and a preparation method thereof. The flexible temperature sensor comprises a substrate layer and a temperature sensing layer attached to the substrate layer. The substrate layer comprises a polymer fiber film and interdigital electrodes growing on the polymer fiber film, and one surface of the substrate layer, which is provided with the interdigital electrodes, faces the temperature sensing layer. The materials of the temperature sensing layer include: the three-dimensional fiber material and the conductive substance and the hydrophobic substance attached to the fiber surface of the three-dimensional fiber material; wherein the conductive material may include carbon nanotubes, and the hydrophobic material may include reduced graphene oxide. The flexible temperature sensing layer and the substrate layer of the flexible temperature sensor provided by the invention are made of fiber materials, so that the flexible temperature sensor has good air permeability, and meanwhile, the flexible temperature sensing layer has a waterproof function, so that the measurement precision of the flexible temperature sensor cannot be influenced by sweat.
Description
Technical Field
The invention relates to a flexible temperature sensing material, a sensor and a preparation method thereof.
Background
With the continuous progress of the living standard of human beings and modern high-temperature living style, the health monitoring equipment is more and more popular with people. As a flexible health monitoring device, the flexible temperature sensor is usually worn on a user and monitors the body temperature of the user. At present, on one hand, the existing flexible temperature sensing device has poor air permeability, so that the wearing discomfort is caused; on the other hand, sweat generated from the skin affects the accuracy of its temperature measurement.
Disclosure of Invention
The invention aims to provide a flexible temperature sensing material with good air permeability and no influence of sweat, a flexible temperature sensor and a preparation method thereof.
In order to achieve the purpose, the invention provides the following scheme:
a flexible temperature sensing material comprising: the three-dimensional fiber material comprises a three-dimensional fiber material and a conductive substance and a hydrophobic substance which are attached to the fiber surface of the three-dimensional fiber material.
Optionally, the conductive substance includes carbon nanotubes.
Optionally, the hydrophobic substance comprises reduced graphene oxide.
Optionally, the three-dimensional fibrous material comprises cotton flakes.
The present invention also provides a flexible temperature sensor comprising: the temperature sensing device comprises a substrate layer and a temperature sensing layer attached to the substrate layer;
the material of the temperature sensing layer is the flexible temperature sensing material provided by the invention;
the substrate layer comprises a polymer fiber film and interdigital electrodes grown on the polymer fiber film, and one surface of the substrate layer, which is provided with the interdigital electrodes, faces the temperature sensing layer.
The invention also provides a preparation method of the flexible temperature sensing material, which comprises the following steps:
soaking the three-dimensional fiber material in the hydrophobic treatment material dispersion liquid and then carrying out first drying; the hydrophobic treatment material dispersion liquid is prepared by dissolving a hydrophobic treatment material in a first organic solvent;
soaking the three-dimensional fiber material subjected to the first drying in a conductive material dispersion liquid, and then carrying out second drying to obtain a flexible temperature sensing material; the conductive material dispersion liquid is prepared by dissolving a conductive material in a first organic solvent.
Optionally, the hydrophobic processing material includes graphene oxide, and the preparation method of the flexible temperature sensing material further includes:
and placing the flexible temperature sensing material in a vacuum environment for thermal reduction.
The invention also provides a preparation method of the flexible temperature sensor, which comprises the following steps:
the flexible temperature sensing material provided by the invention is used for preparing a flexible temperature sensing layer;
carrying out electrostatic spinning by adopting a polymer fiber solution to obtain a polymer fiber membrane; the polymer fiber solution is prepared by dissolving a polymer in a second organic solvent;
growing an interdigital electrode on the surface of the polymer fiber membrane to obtain a substrate layer;
and attaching the flexible temperature sensing layer to one side of the substrate layer with the interdigital electrodes.
According to the specific embodiment provided by the invention, the following technical effects are disclosed: the flexible temperature sensing material provided by the embodiment of the invention comprises a three-dimensional fiber material, and a conductive substance and a hydrophobic substance which are attached to the surface of the fiber of the three-dimensional fiber material. As the three-dimensional fiber material expands when heated, the conductive material on the three-dimensional fiber material is dispersed, so that the conductivity is reduced, the three-dimensional fiber material is shrunk when cooled, and the conductive material on the three-dimensional fiber material is gathered, so that the conductivity is improved. That is, the flexible temperature sensing material used in the embodiments of the present invention has a temperature sensitive characteristic. Based on this principle, the flexible temperature sensing material described above can be used for temperature measurement.
The flexible temperature sensing material prepared by the method is a fiber material, so that the air permeability is good, and meanwhile, the hydrophobic substance attached to the three-dimensional fiber material enables the flexible temperature sensing material to have a waterproof function, so that the temperature measurement precision cannot be influenced by sweat.
The flexible temperature sensor provided by the embodiment of the invention comprises a substrate layer and a temperature sensing layer prepared from the flexible temperature sensing material, wherein the substrate layer comprises a polymer fiber film made of polymer fibers and an electrode growing on the polymer fiber film. Because the flexible temperature sensing layer and the substrate layer of the flexible temperature sensor are made of the fiber materials, the flexible temperature sensor has good air permeability, and meanwhile, the flexible temperature sensor has a waterproof function, so that the measuring precision of the flexible temperature sensor cannot be influenced by sweat.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings needed to be used in the embodiments will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings without inventive exercise.
FIG. 1 is a schematic structural diagram of a flexible temperature sensor in an embodiment of the invention;
fig. 2 is a schematic diagram of a constituent module of a wireless transmission system constructed in an embodiment of the present invention;
FIG. 3 is a Field Emission Scanning Electron Microscope (FESEM) image of electrospun P (VDF-HFP) porous film according to an embodiment of the present invention;
FIG. 4 is a flow chart of a method for manufacturing a flexible temperature sensing material according to an embodiment of the present invention;
FIG. 5 is a flow chart of a method for manufacturing a flexible temperature sensor according to an embodiment of the present invention;
FIG. 6 is another flow chart of a method of making a flexible temperature sensor in an embodiment of the invention;
FIG. 7 is a FESEM image of the temperature sensing layer of the Cotton/rGO/CNT structure and a close-up view of a single Cotton fiber thereof in an embodiment of the invention;
FIG. 8 is a schematic contact angle diagram of the Cotton/rGO/CNT structure in an embodiment of the invention;
FIG. 9 is a schematic contact angle diagram of electrospun P (VDF-HFP) porous film in accordance with an example of the present invention;
FIG. 10 is a bar graph showing the comparison of air permeability of a sealed container containing 10 g of water under four conditions of I) completely sealing a cover, II) sealing a common cotton piece, III) sealing a flexible temperature sensor with a completely air permeable structure, and IV) completely unsealing, respectively, in accordance with an embodiment of the present invention;
FIG. 11 is a graph illustrating the response of a flexible temperature sensor to different temperatures in an embodiment of the present invention;
FIG. 12 is a graph of the recovery time of the temperature response of a flexible temperature sensor in an embodiment of the present invention;
FIG. 13 is a graph of temperature response stability of a flexible temperature sensor in an embodiment of the present invention.
The labels in the figure are: 1. a flexible temperature sensing layer; 2. a polymer fiber film; 3. an interdigital electrode; 4. and (4) conducting wires.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious 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 making any creative effort, shall fall within the protection scope of the present invention.
The invention aims to provide a flexible temperature sensing material with good air permeability and no influence of sweat, a flexible temperature sensor and a preparation method thereof.
The flexible temperature sensor can be applied in the health monitoring field, such as monitoring the body temperature of a human body.
Referring to fig. 1, the flexible temperature sensor includes: the temperature sensing device comprises a substrate layer and a temperature sensing layer attached to the substrate layer. The substrate layer comprises a polymer fiber film 2 and interdigital electrodes 3 growing on the polymer fiber film 2, and one surface of the substrate layer with the interdigital electrodes 3 faces the temperature sensing layer. The material of the temperature sensing layer is the flexible temperature sensing material.
The above-mentioned flexible temperature sensor can be in the same place with measuring circuit and wireless communication module integration, establish wireless communication system (can be called and gather the side), see fig. 2, measuring circuit includes divider resistance, acquisition circuit, MCU and power supply circuit, wherein, divider resistance and above-mentioned flexible temperature sensor establish ties, power supply circuit is the return circuit power supply that divider resistance and above-mentioned flexible temperature sensor constitute, acquisition circuit is connected with above-mentioned flexible temperature sensor's interdigital electrode 3 electricity, gather the voltage at above-mentioned flexible temperature sensor both ends through interdigital electrode 3, and simultaneously, acquisition circuit still is used for gathering the voltage at divider resistance both ends, MCU passes through wireless communication module with the resistance signal that acquisition circuit gathered in real time, for example bluetooth communication module, transmit to terminal equipment (can be called terminal side). The terminal device can exemplarily comprise a terminal data processing and management module and a display module, and the terminal data processing and management module can perform table look-up processing according to the resistance signals to obtain temperature values corresponding to the resistance signals and display the temperature values on the display module, so that real-time acquisition and display of temperature measurement data can be realized.
It should be noted that the terminal devices herein include, but are not limited to: desktop, mobile terminal (e.g., smart watch, smart bracelet, smart phone), ipad, and the like.
In one example, the above-mentioned "terminal data processing and management module" may be applied to the above-mentioned electronic device in the form of software or hardware.
When the method is applied to an electronic device in the form of software, in an example, the "terminal data processing and management module" may be stand-alone software (for example, APP deployed on a terminal), or may also be a component of a terminal operating system or some APP, and the like.
The display module may be a terminal user interface, and in terms of hardware, the terminal user interface may be presented through a display screen of the electronic device.
As will be described in more detail below
Example 1
The present embodiment describes a flexible temperature sensing material used for the flexible temperature sensing layer 1.
The flexible temperature sensing material includes: the three-dimensional fiber material and the conductive substance and the hydrophobic substance attached to the fiber surface of the three-dimensional fiber material. The conductive substance can be carbon nanotubes, the hydrophobic substance can be reduced graphene oxide, and the three-dimensional fiber material can be cotton sheets.
The carbon nano tubes are attached to the fiber surface of the cotton sheet to form a conductive path in the cotton sheet structure, so that the traditional cotton sheet structure is endowed with the conductive characteristic which is not available.
The reduced graphene oxide has both hydrophobicity and conductivity, is attached to the fiber surface of the cotton sheet, and can form a conductive path in the cotton sheet structure together with the carbon nanotube.
When the temperature rises or falls, the volume of the flexible temperature sensing material is increased or reduced, and the density of the conductive paths is reduced or increased because the quantity of the conductive substance is constant, so that the conductivity of the flexible temperature sensing material is reduced or increased. In addition, the hydrophobic property of the reduced graphene oxide also endows the flexible temperature sensing material with the characteristics of hydrophobicity and water resistance. And because the flexible temperature sensing material has a natural three-dimensional reticular structure of the cotton sheet, the flexible temperature sensing material also has excellent air permeability.
In other embodiments of the present invention, the conductive material may be a carbon nanotube, or may be Ag nanowire, poly (3, 4-ethylenedioxythiophene) (PEDOT), Polyaniline (PANI), or the like. The conductive material is only required, and the skilled person can make a flexible choice.
The above hydrophobic substance may be reduced graphene oxide, or may be hydrophobic materials such as SEBS, PFA, FEP, etc., as long as the materials have hydrophobic properties and do not affect conductivity, which is not described herein again.
The three-dimensional fiber material can be selected from cotton sheets, and also can be selected from three-dimensional network structures such as sericin (SS), Zein (Zein), polylactic acid (PLA), Cellulose Nanocrystals (CNC), Cellulose (Cellulose), Chitosan (CS) and the like. As long as the network structure is used. Different combinations of the conductive substance, the hydrophobic substance and the three-dimensional fiber material can obtain a plurality of flexible temperature sensing materials with good air permeability and without being influenced by sweat.
Example 2
The present embodiment provides a flexible temperature sensor, referring to fig. 1, including: the temperature sensing device comprises a substrate layer and a temperature sensing layer attached to the substrate layer.
The substrate layer comprises a polymer fiber film 2 and interdigital electrodes 3 growing on the polymer fiber film 2, and one surface of the substrate layer with the interdigital electrodes 3 faces the temperature sensing layer. The material of the temperature sensing layer can be any one of the flexible temperature sensing materials described above. The interdigital electrode 3 is connected to a lead wire 4 to output a current.
The anode and the cathode of the interdigital electrode are respectively connected with the two wires 4.
The interdigital electrode 3 has a thin thickness, which can be exemplified by 100-500 nm. Therefore, the interdigital electrode 3 has certain bending performance, can be bent along with the bending of the temperature sensing layer, and cannot influence the flexibility of the flexible temperature sensor.
The thickness range of the temperature sensing layer is illustratively 0.5 mm. The thickness of the substrate layer is illustratively 100 um.
The shape of the flexible temperature sensing layer 1 can be circular, oval, square, etc., and those skilled in the art can flexibly design the shape as required, which is not described herein.
Referring to fig. 3, the polymer fiber membrane 2 in the substrate layer is a porous membrane, and thus has a characteristic of strong air permeability.
The polymer fiber membrane 2 in the substrate layer is made of polyvinylidene fluoride-co-hexafluoropropylene P (VDF-HFP) which is hydrophobic and waterproof, and the substrate layer is hydrophobic and waterproof. In addition to P (VDF-HFP), poly (vinylidene fluoride-trifluoroethylene) (P (VDF-TrFE), poly (vinylidene fluoride-trifluoroethylene-chlorotrifluoroethylene) (P (VDF-TrFE-CTFE)), Polycaprolactone (PCL), Polyimide (PI), lactide-caprolactone random copolymer (P (LLA-co-CL)), Polytetrafluoroethylene (PTFE) and other materials can be used to prepare the polymer fiber membrane 2.
The interdigital electrode 3 in the substrate layer is formed by magnetron sputtering, but may be formed by other methods, such as inkjet printing, electron beam evaporation, thermal evaporation, atomic layer deposition, pulsed laser deposition, etc.
The material of the interdigital electrode 3 may be, for example, Ag, and may be, for example, gold (Au), copper (Cu), aluminum (Al), titanium (Ti), tungsten (W), or the like. As long as it is a flexible conductive material having ductility.
In summary, the flexible temperature sensor provided in this embodiment adopts a three-dimensional fiber material to prepare the temperature sensing layer, and adopts a polymer fiber to prepare the substrate layer. The three-dimensional fiber material and the polymer fiber have softness and good air permeability, so that the flexible temperature sensor prepared by adopting the three-dimensional fiber material and the polymer fiber also has flexibility and good air permeability, and can meet the requirement of a wearer on comfort.
In one example, the flexible temperature sensor and the wireless communication module are integrated together to build a wireless flexible communication system, so that the functions of collecting, transmitting, displaying and the like of external temperature information of a human body are completed. For a detailed description, refer to the above description, which is not repeated herein.
Example 3
Referring to fig. 4, the present embodiment provides an exemplary method of preparing a flexible temperature sensing material, the method including the steps of:
step 11: soaking the three-dimensional fiber material in the hydrophobic treatment material dispersion liquid and then carrying out first drying; the hydrophobic treatment material dispersion liquid is prepared by dissolving a hydrophobic treatment material in a first organic solvent;
step 12: soaking the three-dimensional fiber material subjected to the first drying in a conductive material dispersion liquid, and then carrying out second drying to obtain a flexible temperature sensing material; the conductive material dispersion liquid is prepared by dissolving a conductive material in a first organic solvent.
The foregoing mentions that the hydrophobic substance of the flexible temperature sensing material may be reduced graphene oxide. In this case, the hydrophobic treatment material described in step 11 may specifically include graphene oxide. In order to obtain the reduced graphene oxide, after step 12, the flexible temperature sensing material prepared in step 12 is placed in a vacuum environment for thermal reduction, and the graphene oxide on the surface of the flexible temperature sensing material fiber is reduced to the reduced graphene oxide, so that the temperature sensing material has hydrophobic characteristics.
In the following, taking the example that the hydrophobic processing material includes graphene oxide and the conductive substance includes carbon nanotubes, the preparation method of the flexible temperature sensing material is described as follows:
1) respectively dissolving graphene oxide and carbon nanotubes (multi-walled carbon nanotubes) in a first organic solvent to respectively prepare a graphene oxide dispersion liquid and a carbon nanotube dispersion liquid, wherein the concentration of the graphene oxide dispersion liquid is 3-12mg/ml, and the concentration of the carbon nanotube dispersion liquid is 0.1-0.5 mg/ml.
The first organic solvent is preferably any one of N-methylpyrrolidone (NMP), N-Dimethylformamide (DMF), Dimethylsulfide (DMS), and ethanol.
2) Soaking a clean Cotton piece (Cotton) in the graphene oxide dispersion liquid obtained in the step 1) for 3-6 hours, drying for 2-3 hours, and soaking in the carbon nanotube dispersion liquid obtained in the step 1) for 3-6 hours, and drying for 2-3 hours.
3) Placing the cotton piece dried in the step 2) in a vacuum drying oven, wherein the thermal reduction temperature is 160-240 ℃ under the vacuum condition (under the condition that the vacuum degree is 0 Pa), and the reduction time is 2-6h, so as to obtain the temperature sensing material.
Example 4
Referring to fig. 5, the present embodiment provides an exemplary method for manufacturing a flexible temperature sensor, which, based on the method for manufacturing a flexible temperature sensing material according to the above embodiment, further includes the following steps:
step 21: the flexible temperature sensing layer 1 is prepared by using the flexible temperature sensing material in the above embodiment;
step 22: carrying out electrostatic spinning by adopting a polymer solution to obtain a polymer fiber membrane; the polymer solution is prepared by dissolving a polymer in a second organic solvent;
step 23: growing an interdigital electrode on the surface of the polymer fiber membrane to obtain a substrate layer;
step 24: and attaching the flexible temperature sensing layer 1 to one surface of the substrate layer with the interdigital electrode.
Further, referring to fig. 6, taking the example that the hydrophobic processing material includes graphene oxide and the conductive substance includes carbon nanotubes, a specific preparation method of the flexible temperature sensor may be as follows: 1) respectively preparing a Graphene Oxide (GO) dispersion liquid and a dispersion liquid of Carbon Nano Tubes (CNT); 2) washing Cotton sheets Cotton, respectively and sequentially soaking the Cotton in GO and CNT dispersion liquid, and drying, wherein the relevant description and drying time can be referred to the description in the previous embodiment, which is not described herein; 3) placing the dried Cotton sheets in a vacuum drying oven, and performing thermal reduction under a vacuum condition to obtain a temperature sensing layer of Cotton/rGO/CNT, wherein the relevant description and drying time can be referred to the description in the previous embodiment, which is not described herein; 4) preparing a P (VDF-HFP) solution; 5) spinning the P (VDF-HFP) solution by using an electrostatic spinning process to obtain a porous film of the P (VDF-HFP); 6) placing a porous film of P (VDF-HFP) in a cavity of a magnetron sputtering system, and utilizing a metal mask to assist in magnetron sputtering an interdigital electrode of Ag on the surface of the porous film of P (VDF-HFP) to obtain a P (VDF-HFP) substrate layer with the interdigital electrode of Ag; 7) a flexible temperature sensor is formed by a temperature sensing layer structure of Cotton/rGO/CNT and a P (VDF-HFP) substrate layer structure with Ag interdigital electrodes. 8) And a Bluetooth wireless transmission system is built to finish the acquisition and real-time display of the temperature signal of the external environment by the flexible temperature sensor, and the related description and the drying time can be referred to the introduction of the previous embodiment and are not repeated herein.
The above preparation process is described in more detail below:
1) respectively dissolving GO and CNT in a first organic solvent to prepare a GO dispersion liquid and a CNT dispersion liquid, wherein the concentration of the GO dispersion liquid is 3-12mg/ml, and the concentration of the CNT dispersion liquid is 0.1-0.5 mg/ml.
The first organic solvent is preferably any one of N-methylpyrrolidone (NMP), N-Dimethylformamide (DMF), Dimethylsulfide (DMS), and ethanol.
2) Soaking clean Cotton in the GO dispersion liquid obtained in the step 1) for 3-6h, drying for 2-3h, soaking in the CNT dispersion liquid obtained in the step 1) for 3-6h, and drying for 2-3 h.
3) Placing the Cotton sheet dried in the step 2) in a vacuum drying oven, wherein the thermal reduction temperature is 160-240 ℃ and the reduction time is 2-6h under the vacuum condition, so as to obtain the temperature sensing layer structure of the Cotton/rGO/CNT.
4) Dissolving the P (VDF-HFP) polymer in a second solvent, and magnetically stirring for 1000-1600r/min for 16-24h to obtain a solution with the solubility of 10-20 wt%.
The second solvent is preferably any one of acetone (acetone), N-methylpyrrolidone (NMP), dimethylacetamide (DMAc), N-Dimethylformamide (DMF), triethyl phosphate (TEP), Methyl Ethyl Ketone (MEK), and dimethyl sulfide (DMS).
5) Spinning the P (VDF-HFP) solution obtained in the step 4) by using an electrostatic spinning process, wherein the spinning voltage is 15-22kV, the feeding speed of the polymer solution is 1-3ml/h, the distance from an injection needle to a collecting paper is 12-18cm, and collecting on the collecting paper for 2-4h to obtain the porous film of the P (VDF-HFP).
6) And (3) placing the porous film of P (VDF-HFP) obtained in the step (5) in a cavity of a magnetron sputtering system, and carrying out magnetron sputtering on the surface of the porous film of P (VDF-HFP) by using a metal mask to assist an interdigital electrode of Ag, wherein the magnetron sputtering power is 60-100W, and the sputtering time is 10-40min, so as to obtain the substrate layer structure of P (VDF-HFP) with the interdigital electrode of Ag.
7) And (3) forming a flexible temperature sensor by using the obtained temperature sensing layer structure of Cotton/rGO/CNT and 6) the obtained P (VDF-HFP) substrate layer structure with Ag interdigital electrodes.
The specific operation mode of the steps is as follows:
1) and respectively dissolving GO and CNT in DMF (dimethyl formamide) and ethanol solvent to prepare GO and CNT dispersion liquid, wherein the concentration of the GO dispersion liquid is 9mg/ml, and the concentration of the CNT dispersion liquid is 0.1 mg/ml.
2) Soaking clean Cotton in the GO dispersion liquid obtained in the step 1) for 3 hours, drying for 3 hours, and soaking in the CNT dispersion liquid obtained in the step 1) for 3 hours, and drying for 3 hours.
3) And (3) placing the Cotton sheet dried in the step (2) in a vacuum drying oven, and obtaining the material of the temperature sensing layer of the Cotton/rGO/CNT, wherein the thermal reduction temperature is 180 ℃ and the reduction time is 3h under the vacuum condition. From fig. 7, it can be seen that the carbon nanotubes and the reduced graphene oxide are uniformly coated on the surface of the Cotton fiber. From FIG. 8, it can be seen that the contact angle of the temperature sensing layer of the Cotton/rGO/CNT structure is 120.01 degrees, which is much larger than 90 degrees, demonstrating good hydrophobic properties.
4) Dissolving P (VDF-HFP) polymer in acetone, and magnetically stirring for 1000r/min for 24h to obtain a solution with a solubility of 10 wt%.
5) Spinning the P (VDF-HFP) solution obtained in the step 4) by using an electrostatic spinning process, wherein the spinning voltage is 20kV, the feeding rate of the polymer solution is 2ml/h, the distance from an injection needle to a collecting paper is 14cm, and collecting on the collecting paper for 4h to obtain a porous film of the P (VDF-HFP). From fig. 9, it can be seen that the contact angle of the P (VDF-HFP) porous film is 115.56 ° and greater than 90 °, demonstrating its good hydrophobic properties.
6) And (3) placing the porous film of P (VDF-HFP) obtained in the step (5) in a cavity of a magnetron sputtering system, and carrying out magnetron sputtering on an interdigital electrode of Ag on the surface of the porous film of P (VDF-HFP) by utilizing the assistance of a metal mask, wherein the magnetron sputtering power is 100W, and the sputtering time is 10min, so that the substrate layer structure of P (VDF-HFP) with the interdigital electrode of Ag is obtained.
7) And (3) forming a flexible temperature sensor by using the obtained temperature sensing layer structure of Cotton/rGO/CNT and 6) the obtained P (VDF-HFP) substrate layer structure with Ag interdigital electrodes.
8) In the lower computer part (the lower computer part comprises the acquisition side, a voltage division circuit, an analog-to-digital converter, a Bluetooth module and the like), a voltage division circuit is built, a corresponding voltage value can be obtained by using a resistance value measured by the flexible temperature sensor, then, AD conversion is carried out through the analog-to-digital converter (ADC), and the main control unit finishes the reading of the resistance value of the sensor, the AD conversion and the data sending and other commands of the Bluetooth module.
Specifically, the voltage dividing circuit is a series circuit, comprises a standard resistor and a flexible temperature sensor which are connected in series, and can apply preset voltage to the series circuit. According to the voltage division principle, in the series circuit, the currents on the resistors are equal, and the sum of the voltages at the two ends of each resistor is equal to the total voltage of the circuit. The formula of the partial pressure principle is R1, R2 and U1: u2. The voltage across the R1 is U1, and the voltage across the R2 is U2. R1 and R2 represent two resistors in a series circuit. Since the total voltage (preset voltage) of the circuit is known and the resistance value of the standard resistor in the voltage dividing circuit is known, the current resistance value of the flexible temperature sensor can be calculated according to the formula.
The ADC can perform AD conversion on voltage values at two ends of the flexible temperature sensor, the main control unit calculates the current resistance value of the flexible temperature sensor according to the voltage value after the AD conversion, and then the current resistance value of the flexible temperature sensor is sent to an upper computer end through the Bluetooth module.
Or, the main control unit may further calculate a current temperature value according to the current resistance value of the flexible temperature sensor, and send the current temperature value to the upper computer.
In the upper computer part (the upper computer part comprises the terminal side, the Bluetooth module and the like), the Bluetooth module receives data, and the terminal completes the calculation of the temperature value in a table look-up or interpolation mode and the like according to the calibration relation of the resistance value and the temperature value and displays the temperature value.
In one example, the current temperature value may be calculated by the terminal according to the received current resistance value. And the main control unit at the lower computer end can further calculate the current temperature value according to the current resistance value of the flexible temperature sensor and send the current temperature value to the upper computer end. And the terminal correspondingly processes, manages and displays the received temperature value.
More specifically, the terminal or the main control unit may complete the calculation of the temperature value by looking up a table or interpolating or the like according to the calibration relationship (calibration relationship table) between the resistance value and the temperature value.
The interpolation method can be the existing or future foreseeable method, and is not described herein.
Fig. 10 is a bar graph showing comparison of air permeability of a sealed container containing 10 g of water in the embodiment of the present invention under four conditions of I) completely sealing a lid, II) sealing a common cotton piece, III) sealing a flexible temperature sensor provided in the embodiment of the present invention, and IV) completely unsealing, respectively. In the experiment, 4 closed containers (I-IV) containing 10 g of water are placed at 60 ℃, and the amount of the water left in the four containers is measured at 0 th, 8 th, 28 th, 35 th and 48 th hours, so that the weight of the water left in the container in which III) the flexible temperature sensor provided by the embodiment of the invention is sealed is basically equivalent to that of the water left in the container in which IV) is not sealed at all, and the flexible temperature sensor provided by the embodiment of the invention has better air permeability.
FIG. 11 is a graph illustrating the response of a flexible temperature sensor to different temperatures in an embodiment of the present invention. The temperature of the environment where the flexible temperature sensor is located is changed, and meanwhile, the resistances at two ends of the flexible temperature sensor are measured by adopting a source meter (model is Gishili 2602B), as shown in FIG. 11, as the temperature is increased from 30 ℃ to 40 ℃, the resistance value of the flexible temperature sensor in the embodiment of the invention is continuously increased, and is increased from 3200 ohm to 7000 ohm.
FIG. 12 is a graph of the recovery time of the temperature response of a flexible temperature sensor in an embodiment of the present invention. The temperature of the environment where the flexible temperature sensor is located is changed, and meanwhile, the resistances at two ends of the flexible temperature sensor are measured by adopting a source meter (model is Gishly 2602B), as shown in fig. 11, when the temperature is increased from 31 ℃ to 39 ℃, the resistance value of the flexible temperature sensor in the embodiment of the invention is increased from 3500 ohm to 6400 ohm, the response time is 20s, when the temperature is decreased to 31 ℃ again, the resistance value of the flexible temperature sensor in the embodiment of the invention is decreased from 6400 ohm to 3500 ohm, and the recovery time is 80 s.
Fig. 13 is a graph of temperature response stability of the flexible temperature sensor in the embodiment of the present invention, where the temperature of the environment where the flexible temperature sensor is located is changed, and the resistance at both ends of the flexible temperature sensor is measured by using the source meter (model number gishley 2602B), as shown in fig. 11, when the temperature is increased from 31 ℃ to 39 ℃ and then decreased to 31 ℃ for many times, the resistance value of the flexible temperature sensor can also be increased from 3500 ohm to 6400 ohm and then decreased to 3500 ohm for many times, which indicates that the device has good stability.
The invention has the following effects:
(1) the method for preparing the temperature sensing material by the solution infiltration method enables the traditional cotton piece structure to have the characteristics of hydrophobicity, waterproofness and conductivity at the same time, and is simple, easy to operate and lower and low in cost.
(2) From the preparation of a temperature sensing material by a solution infiltration method to the preparation of a P (VDF-HFP) hydrophobic and waterproof substrate layer structure by electrostatic spinning, the whole flexible temperature sensing not only can be waterproof, but also has a full-breathable structure, and can meet the requirements of human skin on wearable comfort.
(3) Based on the temperature sensing material, the material not only has the natural three-dimensional net structure of the traditional cotton sheet structure, but also has the conductive characteristics of rGO and CNT. Therefore, when the temperature of the external environment changes, the three-dimensional network structure deforms, i.e., expands and contracts with heat, thereby resulting in an increase and decrease in the volume of the device. Because the volume of the rGO and CNT conductive filler is unchanged, the resistance value of the device can be increased and decreased along with the increase and decrease of the volume of the device, and the monitoring of an external environment temperature signal is realized.
(4) The real-time response and display system of the flexible temperature sensor to the temperature signal is built, the breathing state of the human body can be monitored in real time, and the system has important significance for the development of wearable medical care systems.
The embodiments in the present description are described in a progressive manner, each embodiment focuses on differences from other embodiments, and the same and similar parts among the embodiments are referred to each other.
The principles and embodiments of the present invention have been described herein using specific examples, which are provided only to help understand the method and the core concept of the present invention; meanwhile, for a person skilled in the art, according to the idea of the present invention, the specific embodiments and the application range may be changed. In view of the above, the present disclosure should not be construed as limiting the invention.
Claims (8)
1. A flexible temperature sensing material, comprising: the three-dimensional fiber material comprises a three-dimensional fiber material and a conductive substance and a hydrophobic substance which are attached to the fiber surface of the three-dimensional fiber material.
2. The flexible temperature sensing material of claim 1, wherein the conductive substance comprises carbon nanotubes.
3. The flexible temperature sensing material of claim 1, wherein the hydrophobic substance comprises reduced graphene oxide.
4. A flexible temperature sensing material according to claim 1, wherein said three-dimensional fibrous material comprises cotton flakes.
5. A flexible temperature sensor, comprising: the temperature sensing device comprises a substrate layer and a temperature sensing layer attached to the substrate layer;
the material of the temperature sensing layer is the flexible temperature sensing material according to any one of claims 1 to 4;
the substrate layer comprises a polymer fiber film and interdigital electrodes grown on the polymer fiber film, and one surface of the substrate layer, which is provided with the interdigital electrodes, faces the temperature sensing layer.
6. A preparation method of a flexible temperature sensing material is characterized by comprising the following steps:
soaking the three-dimensional fiber material in the hydrophobic treatment material dispersion liquid and then carrying out first drying; the hydrophobic treatment material dispersion liquid is prepared by dissolving a hydrophobic treatment material in a first organic solvent;
soaking the three-dimensional fiber material subjected to the first drying in a conductive material dispersion liquid, and then carrying out second drying to obtain a flexible temperature sensing material; the conductive material dispersion liquid is prepared by dissolving a conductive material in a first organic solvent.
7. The method of claim 6, wherein the hydrophobic treatment material comprises graphene oxide, and the method further comprises:
and placing the flexible temperature sensing material in a vacuum environment for thermal reduction.
8. A method for manufacturing a flexible temperature sensor, comprising:
preparing a flexible temperature sensing layer using the flexible temperature sensing material according to any one of claims 1 to 4;
carrying out electrostatic spinning by adopting a polymer solution to obtain a polymer fiber membrane; the polymer solution is prepared by dissolving a polymer in a second organic solvent;
growing an interdigital electrode on the surface of the polymer fiber membrane to obtain a substrate layer;
and attaching the flexible temperature sensing layer to one side of the substrate layer with the interdigital electrodes.
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