CN117230539A - Mechanical sensitive material for resistance type pressure sensor and preparation method and application thereof - Google Patents
Mechanical sensitive material for resistance type pressure sensor and preparation method and application thereof Download PDFInfo
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- CN117230539A CN117230539A CN202311507977.8A CN202311507977A CN117230539A CN 117230539 A CN117230539 A CN 117230539A CN 202311507977 A CN202311507977 A CN 202311507977A CN 117230539 A CN117230539 A CN 117230539A
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- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 239000004372 Polyvinyl alcohol Substances 0.000 claims abstract description 43
- 229920002451 polyvinyl alcohol Polymers 0.000 claims abstract description 43
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 42
- 239000000835 fiber Substances 0.000 claims abstract description 36
- 239000002041 carbon nanotube Substances 0.000 claims abstract description 34
- 229910021393 carbon nanotube Inorganic materials 0.000 claims abstract description 32
- 239000002904 solvent Substances 0.000 claims abstract description 11
- 238000002791 soaking Methods 0.000 claims abstract description 5
- 239000002202 Polyethylene glycol Substances 0.000 claims abstract description 4
- 229920001223 polyethylene glycol Polymers 0.000 claims abstract description 4
- KKEYFWRCBNTPAC-UHFFFAOYSA-L terephthalate(2-) Chemical compound [O-]C(=O)C1=CC=C(C([O-])=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-L 0.000 claims abstract description 4
- 239000010410 layer Substances 0.000 claims description 34
- 229920000139 polyethylene terephthalate Polymers 0.000 claims description 26
- 239000005020 polyethylene terephthalate Substances 0.000 claims description 26
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 25
- 238000000576 coating method Methods 0.000 claims description 24
- 239000000725 suspension Substances 0.000 claims description 24
- 238000000034 method Methods 0.000 claims description 22
- 239000011248 coating agent Substances 0.000 claims description 21
- -1 polyethylene terephthalate Polymers 0.000 claims description 19
- 239000002244 precipitate Substances 0.000 claims description 17
- 239000000203 mixture Substances 0.000 claims description 11
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical group N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 10
- 239000011159 matrix material Substances 0.000 claims description 10
- 238000009210 therapy by ultrasound Methods 0.000 claims description 10
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 8
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- 238000001035 drying Methods 0.000 claims description 6
- 125000000524 functional group Chemical group 0.000 claims description 6
- PQXKHYXIUOZZFA-UHFFFAOYSA-M lithium fluoride Chemical compound [Li+].[F-] PQXKHYXIUOZZFA-UHFFFAOYSA-M 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 6
- 238000006243 chemical reaction Methods 0.000 claims description 5
- 229910052757 nitrogen Chemical group 0.000 claims description 5
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- 150000003624 transition metals Chemical class 0.000 claims description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 4
- 239000011247 coating layer Substances 0.000 claims description 4
- 239000006228 supernatant Substances 0.000 claims description 4
- ISPYQTSUDJAMAB-UHFFFAOYSA-N 2-chlorophenol Chemical compound OC1=CC=CC=C1Cl ISPYQTSUDJAMAB-UHFFFAOYSA-N 0.000 claims description 3
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- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 description 3
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Abstract
The invention discloses a mechanical sensitive material for a resistance type pressure sensor and a preparation method and application thereof, wherein a solvent capable of dissolving polyethylene glycol terephthalate and incapable of dissolving polyvinyl alcohol is adopted to disperse polyethylene glycol terephthalate and carbon nano tubes, then a dispersion liquid is coated on the surface of polyvinyl alcohol fibers, then the polyvinyl alcohol fibers are removed by etching, a hollow structure intermediate is obtained, and an MXene material is arranged on the intermediate in a soaking way.
Description
Technical Field
The invention relates to the field of resistance pressure sensors, in particular to a mechanical sensitive material for a resistance pressure sensor, a preparation method and application thereof.
Background
The principle of the sensor is to convert the external stimulus into an electrical signal, such as a resistive, capacitive, current or voltage signal, which can be collected and analyzed by a computer. For example, a resistive pressure sensor converts a pressure value into a resistance signal through a pressure sensing device so as to realize pressure measurement and control of an object to be measured, in some measurement processes of compressive stress with regular and irregular complex structures, the pressure sensor is required to have not only good pressure-resistance characteristics, but also excellent performances such as flexibility, for example, in the case of a wearable biosensor, theoretically, the pressure sensor can conveniently and noninvasively collect physiological signals, provide sufficient information for health monitoring and even preliminary medical diagnosis, but firstly, needs to have enough flexibility due to the fact that the pressure sensor needs to be worn on the body, otherwise, wearing comfort is seriously affected, and biological structures are difficult to better adapt, secondly, needs to have excellent response sensitivity, otherwise, timely and accurate monitoring is difficult to realize in a small limb movement, thirdly, needs to have better repeated stability performance, because health monitoring is a continuous process, only single use can bring great inconvenience, and is high in cost, and fourthly, it is important for a human body or other organisms that heat insulation performance is important whether electrical signals can be collected for a long time and can be continuously monitored in real time. However, the mechanical sensitive material for the current resistance pressure sensor is basically difficult to achieve the compromise of the performances, and has the problem of losing the compromise.
Disclosure of Invention
The invention aims to overcome one or more defects in the prior art, and provides a novel preparation method of a mechanical sensitive material for a resistance type pressure sensor.
The invention also provides a mechanical sensitive material for the resistance type pressure sensor prepared by the method.
The invention also provides an application of the mechanical sensitive material for the resistance type pressure sensor prepared by the method in preparation of the resistance type pressure sensor.
In order to achieve the above purpose, the invention adopts a technical scheme that:
a preparation method of a mechanical sensitive material for a resistance type pressure sensor comprises the following steps:
dispersing polyethylene glycol terephthalate and carbon nano tubes in a first solvent to obtain a first mixture; wherein the first solvent is capable of dissolving polyethylene terephthalate and is incapable of dissolving polyvinyl alcohol;
uniformly coating the first mixture on the surface of the polyvinyl alcohol fiber in a coating mode to form a coating layer which is coated on the surface of the polyvinyl alcohol fiber and is continuously distributed to obtain a first intermediate, soaking the first intermediate in water to swell, and then raising the water temperature until the polyvinyl alcohol fiber in the first intermediate is completely dissolved in the water to obtain a second intermediate with a hollow structure;
immersing the second intermediate with the hollow structure in MXene suspension, separating and drying to obtain a mechanical sensitive material with the hollow structure for the resistance type pressure sensor; the saidThe MXene suspension is prepared by dispersing an MXene material in water, the MXene material having the formula M n+1 X n T a M is a transition metal, X is carbon and/or nitrogen, and T represents a surface functional group.
The polyester, a polymer obtained by polycondensation of polyalcohol and polybasic acid, is mainly polyethylene terephthalate (PET for short), is an engineering plastic polyester with excellent performance and wide application, is a common resin in life, is a milky white or pale yellow polymer with high crystallization degree, and has smooth and glossy surface. The high-temperature-resistant high-voltage cable has excellent physical and mechanical properties in a wider temperature range, can be used for 120 ℃ for a long time, has excellent electrical insulation property, and has good electrical properties, creep resistance, fatigue resistance, friction resistance and dimensional stability even at high temperature and high frequency. According to some preferred aspects of the invention, the polyethylene terephthalate has a melt viscosity of 1000 to 2000 mPa-s after melting. In the invention, polyethylene terephthalate (PET) is used as a resin base material, so that abrasion can be reduced.
According to some preferred aspects of the invention, the carbon nanotubes (CNTs for short) have a length of 10-30 μm and a diameter of 10-20nm.
According to some preferred aspects of the present invention, the carbon nanotubes are added in an amount of 4% -12% by mass of the total addition amount of the polyethylene terephthalate and the carbon nanotubes. Further, in some embodiments of the present invention, the carbon nanotubes are added in an amount of 6% to 10% by mass of the total addition amount of the polyethylene terephthalate and the carbon nanotubes.
According to some preferred aspects of the invention, the first solvent comprises o-chlorophenol.
According to some preferred aspects of the invention, the polyethylene terephthalate comprises 5% to 10% by mass of the first mixture.
According to some preferred aspects of the invention, the coated embodiment comprises:
coating the surface of the polyvinyl alcohol fiber along a first direction to form a first layer which is continuously distributed;
coating the surface of the polyvinyl alcohol fiber along a second direction to form a second layer which is coated on the first layer and is continuously distributed;
coating the surface of the polyvinyl alcohol fiber in an alternating coating mode along the first direction and the second direction to form a third layer which is coated on the second layer and is continuously distributed;
the first direction intersects the second direction, and the first layer, the second layer, and the third layer constitute the cladding layer. The coating mode can obtain a more compact and dense coating layer and can also enable the carbon nano tubes to be in excellent lap joint.
In some embodiments of the present invention, the first direction may be a transverse direction and the second direction may be a longitudinal direction.
According to some preferred aspects of the invention, the thickness of the first layer, the thickness of the second layer and the thickness of the third layer are each 0.1-0.5mm.
According to some preferred aspects of the invention, during the coating process, the coating of the next layer is performed after the previous layer has dried.
According to some preferred aspects of the invention, the swelling is carried out in water at ambient temperature for a period of 10-60 minutes.
According to some preferred aspects of the invention, the water temperature is raised to 80-95 ℃ after the swelling is performed.
According to some preferred aspects of the invention, the polyvinyl alcohol fibers have a diameter of 0.5 to 8 μm.
Further, the polyvinyl alcohol fiber has a diameter of 1 to 5 μm.
Further, the polyvinyl alcohol fiber has a diameter of 2 to 4 μm.
In some embodiments of the present invention, the method for preparing the polyvinyl alcohol fiber (PVA fiber for short) includes:
the polyvinyl alcohol (the dissolution temperature of the polyvinyl alcohol is 90-120 ℃) is dissolved in hot water (the dissolution time is further controlled to be 0.5-1 h), so that spinning solution with certain viscosity and good spinnability can be obtained; further, the mass percentage of the polyvinyl alcohol in the spinning solution is 10% -20% in terms of mass percentage; further, the mass percentage of the polyvinyl alcohol in the spinning solution is 15% -17% in terms of mass percentage;
delivering the spinning solution to a spinning device through a circulating pipeline, metering and filtering, and delivering the spinning solution into a spinneret to extrude a stock solution trickle, wherein a solvent in the stock solution trickle can diffuse into a coagulating bath, and a coagulating agent permeates into the trickle, so that the stock solution trickle reaches a critical concentration, and is separated out in the coagulating bath to form polyvinyl alcohol fibers; further, the coagulation bath is an aqueous sodium sulfate solution.
The MXene material is a novel two-dimensional crystal material, belongs to a graphene-like material, is considered as a better substitute for graphene and other carbon nano materials, and can be prepared by etching MAX phase through a wet chemical method. MXene material has the general formula M n+1 X n T a M is a transition metal, X is carbon and/or nitrogen, T represents a surface functional group (for example, -O, -F, -OH, etc.), a represents the number of the surface functional group, and n is a natural number greater than 0.
According to some preferred aspects of the invention, the concentration of the MXene material in the MXene suspension is between 0.1 and 1.0mg/L.
According to some preferred aspects of the present invention, in the mechanically sensitive material for a resistive pressure sensor, a ratio of a mass of the MXene material to a total mass of the polyethylene terephthalate and the carbon nanotube is 1:5-20.
According to some preferred aspects of the invention, the MXene material has a thickness of 0.8-1.2nm and a length of 0.5-4 μm.
According to some preferred aspects of the invention, the method of preparing the MXene suspension comprises:
mixing lithium fluoride with hydrochloric acid, adding MAX phase, and reacting, wherein the chemical formula of MAX phase is Ti 3 SiC 2 ；
After the reaction is finished, centrifuging to obtain a first precipitate, mixing with water, performing ultrasonic treatment, centrifuging again, repeating the centrifugation and ultrasonic treatment until a mixture with neutral pH value is obtained, and separating out a second precipitate;
and then dispersing the second precipitate in an alcohol solvent, carrying out ultrasonic treatment and centrifugation to obtain a third precipitate, dispersing the third precipitate in water, carrying out ultrasonic treatment and centrifugation to obtain a supernatant, namely the MXene suspension.
In some embodiments of the invention, the reaction temperature of the reaction is 30-35 ℃ during the preparation of the MXene suspension.
In some embodiments of the invention, the reaction is carried out under stirring conditions during the preparation of the MXene suspension at a rotational speed of 3000 to 10000rpm.
In some embodiments of the invention, the hydrochloric acid may have a concentration of 6-12mol/L.
The invention provides another technical scheme that: the mechanical sensitive material for the resistance type pressure sensor is prepared by the preparation method of the mechanical sensitive material for the resistance type pressure sensor.
The invention provides another technical scheme that: a mechanical sensitive material for a resistance type pressure sensor comprises a hollow structure matrix, carbon nanotubes distributed in the hollow structure matrix, and an MXene material at least distributed on the outer surface of the hollow structure matrix, wherein the general formula of the MXene material is M n+1 X n T a M is transition metal, X is carbon and/or nitrogen, T is a surface functional group, and the material of the hollow structural matrix is polyethylene terephthalate.
The invention provides another technical scheme that: the application of the mechanical sensitive material for the resistance type pressure sensor in preparing the resistance type pressure sensor is provided.
In some embodiments of the present invention, the resistive pressure sensor of the present invention made of mechanically sensitive material exhibits great development potential when used as a monitor for real-time monitoring of human body movements including finger bending and wrist bending.
In some embodiments of the present invention, the resistive pressure sensor may be a wearable biosensor, for example, may be formed into a predetermined shape by a braiding method or the like.
Due to the application of the technical scheme, compared with the prior art, the invention has the following advantages:
based on the problems of the mechanical sensitive material for the resistance type pressure sensor in the prior art, through a great deal of experimental researches, the invention innovatively provides the mechanical sensitive material with a hollow structure, wherein the mechanical sensitive material takes polyethylene terephthalate as a hollow structure resin matrix, carbon nano tubes are dispersed in the hollow structure resin matrix to serve as an internal conductive electronic network, and an MXene material is arranged on the surface of the mechanical sensitive material to form an external conductive electronic network.
Drawings
FIG. 1 is a photograph of an MXene suspension prepared in accordance with the present invention;
FIG. 2 is a schematic structural diagram of a first intermediate;
FIG. 3 is a schematic structural diagram of a mechanical sensitive material for a resistive pressure sensor prepared in example 1 of the present invention;
FIG. 4 is a schematic view of a woven fabric of a mechanically sensitive material for a resistive pressure sensor prepared in example 2 of the present invention;
FIG. 5 is a schematic diagram of a digital source meter for testing the performance of a mechanically sensitive material for a resistive pressure sensor having a hollow structure according to an embodiment of the present invention; in the reference numerals, 1, a mechanical sensitive material; 2. a wire; 3. a digital source table;
FIG. 6 is a graph showing the results of a response repeatability test of the mechanically sensitive material for a resistive pressure sensor prepared in example 1 of the present invention;
FIG. 7 is a graph showing the results of a response repeatability test of the mechanically sensitive material for a resistive pressure sensor prepared in example 2 of the present invention;
FIG. 8 is a graph showing the results of a response repeatability test of the mechanical sensitive material for a resistive pressure sensor prepared in example 3 of the present invention;
FIG. 9 is a graph showing the results of a response repeatability test of the mechanically sensitive material for a resistive pressure sensor prepared according to comparative example 1 of the present invention;
FIG. 10 is a graph showing the results of a response repeatability test of the mechanically sensitive material for a resistive pressure sensor prepared according to comparative example 2 of the present invention;
FIG. 11 is a graph showing the results of a response repeatability test of the mechanically sensitive material for a resistive pressure sensor prepared according to comparative example 3 of the present invention;
FIG. 12 is a graph showing the results of a test for the repeatability of the response of the mechanically sensitive material for a resistive pressure sensor of example 2 at a weight of 50 g;
FIG. 13 is a graph showing the results of a test for the repeatability of the response of the mechanically sensitive material for a resistive pressure sensor of example 2 at a weight of 100 g;
FIG. 14 is a graph showing the results of a test for the repeatability of the response of the mechanically sensitive material for a resistive pressure sensor of example 2 at a weight of 200 g;
fig. 15 is a graph showing the relationship between the change in the relative resistance value of the mechanically sensitive material for the resistive pressure sensor of example 2 and the weight mass.
Detailed Description
The above-described aspects are further described below in conjunction with specific embodiments; it should be understood that these embodiments are provided to illustrate the basic principles, main features and advantages of the present invention, and that the present invention is not limited by the scope of the following embodiments; the implementation conditions employed in the examples may be further adjusted according to specific requirements, and the implementation conditions not specified are generally those in routine experiments.
All starting materials are commercially available or prepared by methods conventional in the art, not specifically described in the examples below.
In the following, the polyvinyl alcohol fiber is prepared by the following method: polyvinyl alcohol (polyvinyl alcohol 088-50 of PVA of Henan Jiapei environmental protection technology Co., ltd., petrochemical grade in China) is dissolved in hot water at 95 ℃ to obtain a solution with the mass percent content of 16% and good spinnability; filtering and defoamating the spinning solution, pouring into a spinning machine, delivering to a spinneret through a metering pump and a filter, extruding from a spinneret orifice to obtain spinning trickle, and obtaining supersaturated Na 2 SO 4 Solidifying the fiber into primary fiber in a coagulating bath, controlling the temperature of the coagulating bath to be 44+/-1 ℃ and stretching the spinneret to be 30%; wherein, by changing the size of the spinneret, the diameter of the polyvinyl alcohol fiber can be controlled.
In the following, an MXene suspension was prepared by the following method: (1) 2g of LiF and 9M 40mL of hydrochloric acid were weighed and stirred in a polytetrafluoroethylene beaker for 30min, and 2g of MAX phase (Ti 3 SiC 2 ) Slowly adding the mixture into the beaker in the step, and continuously stirring the mixture for 24 hours at the temperature of 30 ℃; (2) Centrifuging the obtained reaction liquid, pouring out the supernatant after centrifuging, adding deionized water into the precipitate, shaking uniformly, mixing the precipitate with the deionized water uniformly, putting the precipitate into an ultrasonic machine for ultrasonic treatment, taking out, continuing centrifuging, and repeating for several times until the pH value of the mixture is neutral; (3) Adding ethanol into the precipitate, performing ultrasonic treatment for 1h, centrifuging to obtain precipitate, adding deionized water into the precipitate, shaking, and performing ultrasonic centrifugation to obtain dark green supernatant, namely MXene suspension, wherein the photograph is shown in FIG. 1, and the concentration of the MXene material is measured to be about 0.5mg/L. If not etched, the MAX phase will precipitate to the bottom, after etching, form MXene nanoplatelets which will be stably dispersed in aqueous solution, while as can be seen from FIG. 1, etching has occurred, forming a stable suspension.
Polyethylene terephthalate (PET) was purchased from Shanghai, open-spin under the brand CB651S; carbon Nanotubes (CNT) were purchased from nanjing first-come nanomaterial technologies, inc.
Example 1
The embodiment provides a mechanical sensitive material for a resistance type pressure sensor and a preparation method thereof, and the preparation method of the mechanical sensitive material for the resistance type pressure sensor comprises the following steps:
(1) Dissolving PET in o-chlorophenol, uniformly mixing CNT in the solution, and evaporating part of the solvent to prepare PET/CNT mixed solution; wherein, the CNTs account for 0.8 percent of the CNTPET/CNT mixed solution and the PET accounts for 10 percent of the CNTPET/CNT mixed solution by mass percent;
(2) Coating the PET/CNT mixed solution prepared according to the method in the step (1) on the surface of a polyvinyl alcohol fiber with the diameter of 1 mu m to form a coating layer which is coated on the surface of the polyvinyl alcohol fiber and is continuously distributed, so as to obtain a first intermediate, wherein the structure schematic diagram of the first intermediate is shown in figure 2;
wherein, the coating process is as follows:
coating the surface of the polyvinyl alcohol fiber along the transverse direction to form a first layer which is continuously distributed, drying for about 4 hours, and the thickness of the first layer is about 0.3 mu m; then coating the surface of the polyvinyl alcohol fiber along the longitudinal direction to form a second layer which is coated on the first layer and is continuously distributed, drying for about 4 hours, and the thickness is about 0.3 mu m; coating the surface of the polyvinyl alcohol fiber in an alternating coating mode along the transverse direction and the longitudinal direction to form a third layer which is covered on the second layer and is continuously distributed, drying for about 4 hours, and the thickness is about 0.3 mu m;
then, the first intermediate is soaked in the low-temperature water for swelling for 30min, then the water temperature is increased to 90 ℃, and the temperature is kept until the polyvinyl alcohol fibers in the first intermediate are completely dissolved in the water, and a second intermediate with a hollow structure is separated;
(3) Soaking the second intermediate with the hollow structure, which is prepared in the step (2), in an MXene suspension for 8 hours, separating and drying after the soaking is completed to obtain a mechanical sensitive material for the resistance pressure sensor with the hollow structure, wherein the structural schematic diagram of the mechanical sensitive material is shown in figure 3; wherein, in the mechanical sensitive material for the resistance pressure sensor, the ratio of the mass of the MXene material to the total mass of the polyethylene terephthalate and the carbon nano tube is 1:10.
Example 2
Substantially the same as in example 1, the only difference is that: the polyvinyl alcohol fibers had a diameter of 3. Mu.m.
Example 3
Substantially the same as in example 1, the only difference is that: the polyvinyl alcohol fibers had a diameter of 5. Mu.m.
Comparative example 1
Substantially the same as in example 2, the only difference is that: replacing the "MXene suspension" with a "suspension of flaky molybdenum disulfide";
the flaky molybdenum disulfide suspension is purchased from Nanjing Xianfeng nano materials science and technology Co., ltd, and has the brand XF135 and the concentration of: 5mg/mL.
Comparative example 2
Substantially the same as in example 2, the only difference is that: replacing the MXene suspension with a suspension of graphene oxide in the form of flakes;
the platy graphene oxide suspension is purchased from Nanjing Xianfeng nanomaterial technologies Inc., brand XF224, and has the concentration of: 2mg/mL.
Comparative example 3
Substantially the same as in example 2, the only difference is that: the CNT is located on the surface of the material and the MXene material is located inside the PET, specifically, in step (1), the CNT is replaced with the MXene material, and in step (3), the "MXene suspension" is replaced with the "CNT dispersion", and the CNT dispersion is formed by dispersing the carbon nanotubes in water.
Performance testing
1. The mechanical sensitive material for the resistance type pressure sensor prepared in the embodiment 2 of the invention is knitted, can be knitted into a knitted fabric shown in fig. 4, and has excellent flexibility, so that the mechanical sensitive material for the resistance type pressure sensor can be used in the fields of wearable biosensors and the like.
2. Thermal conductivity testing of the mechanically sensitive materials prepared in examples 1-3 and comparative examples 1-3 of the present invention
The testing method comprises the following steps: the transient plane heat source method is adopted: the probe is placed in the middle of a sample for testing, when current passes through, a certain temperature rise is generated, generated heat is diffused to the samples on two sides of the probe, the heat diffusion speed depends on the heat conduction characteristics of materials, and the heat conductivity coefficient and the heat diffusivity can be directly obtained by a mathematical model by recording the temperature and the response time of the probe.
The test results are shown in table 1.
As can be seen from table 1, the material with the hollow structure of the present invention has a lower thermal conductivity, indicating good heat insulation performance; meanwhile, the mechanical sensitive material prepared by the embodiment of the invention is not lower than that of the comparative example in heat insulation performance, and even is partially and obviously better.
3. The mechanically sensitive materials prepared in examples 1 to 3 and comparative examples 1 to 3 were tested using a digital source meter, the connection structure of which is schematically shown in fig. 5, and two ends of the mechanically sensitive material 1 were connected by a wire 2 and then connected to the digital source meter 3 to form a loop.
(1) Response repeatability tests were carried out on the mechanically sensitive materials prepared in examples 1-3 and comparative examples 1-3 of the present invention, and specific results are shown in fig. 6 to 11;
it can be seen from FIGS. 6 to 8 that the relative resistance change ((R-R) of the mechanically sensitive materials of examples 1 to 3 0 )/ R 0 R is the measured resistance value, R 0 Initial resistance value); compared with the mechanical sensitive material with the diameter of 1 mu m of the hollow structure, the mechanical sensitive material with the diameter of 3 mu m and 5 mu m of the hollow structure has the largest change range, namely has higher response sensitivity, and compared with the mechanical sensitive material with the diameter of 5 mu m of the hollow structure, the mechanical sensitive material with the diameter of 3 mu m of the hollow structure still can return to the vicinity of the initial value even after undergoing a plurality of compression cycles, namely has higher stability.
As can be seen from fig. 9 to 11, the relative resistance change ranges of the mechanically sensitive materials of comparative examples 1 to 3, each of comparative examples 1 to 3 has the same hollow structure as that of example 2 of the present invention, but after the response reproducibility test is performed, it is found that:
the initial resistance of the first and the comparative examples 1-3 is larger, and the relative resistance change is small under the same deformation condition caused by external force, namely the output electric signal is small, namely the response sensitivity is lower;
the mechanically sensitive materials of the second and comparative examples 1-3 hardly return to their original values after undergoing a plurality of compression cycles, and exhibit poor stability; analysis shows that under the structural system of the invention, molybdenum disulfide or graphene oxide of comparative examples 1-2 are difficult to better match other materials; in comparative example 3, however, CNT was present on the surface of the material and MXene was present inside the material, and the conductive network structure was relatively easily damaged by the external force due to the conductive network on the surface of the fiber constructed with one-dimensional CNT, resulting in poor stability of the output signal.
(2) The response repeatability of the mechanical sensitive material for the resistance type pressure sensor of the example 2 under different weight masses (50, 100, 200 and g) is tested, and specific results are shown in fig. 12 to 15;
it can be seen from fig. 12 to 14 that the mechanically sensitive material in embodiment 2 of the present invention has good responsiveness to different pressures; and the relative resistance value change and the weight have good linear relation, and the specific reference can be seen in fig. 15, so that the performance of the device under different application environments can be conveniently mastered.
The above embodiments are provided to illustrate the technical concept and features of the present invention and are intended to enable those skilled in the art to understand the content of the present invention and implement the same, and are not intended to limit the scope of the present invention. All equivalent changes or modifications made in accordance with the spirit of the present invention should be construed to be included in the scope of the present invention.
The endpoints and any values of the ranges disclosed herein are not limited to the precise range or value, and are understood to encompass values approaching those ranges or values. For numerical ranges, one or more new numerical ranges may be found between the endpoints of each range, between the endpoint of each range and the individual point value, and between the individual point value, in combination with each other, and are to be considered as specifically disclosed herein.
Claims (15)
1. The preparation method of the mechanical sensitive material for the resistance type pressure sensor is characterized by comprising the following steps of:
dispersing polyethylene glycol terephthalate and carbon nano tubes in a first solvent to obtain a first mixture; wherein the first solvent is capable of dissolving polyethylene terephthalate and is incapable of dissolving polyvinyl alcohol;
uniformly coating the first mixture on the surface of the polyvinyl alcohol fiber in a coating mode to form a coating layer which is coated on the surface of the polyvinyl alcohol fiber and is continuously distributed to obtain a first intermediate, soaking the first intermediate in water to swell, and then raising the water temperature until the polyvinyl alcohol fiber in the first intermediate is completely dissolved in the water to obtain a second intermediate with a hollow structure;
immersing the second intermediate with the hollow structure in MXene suspension, separating and drying to obtain a mechanical sensitive material with the hollow structure for the resistance type pressure sensor; the MXene suspension is prepared by dispersing an MXene material in water, the MXene material having the formula M n+1 X n T a M is a transition metal, X is carbon and/or nitrogen, and T represents a surface functional group.
2. The method for preparing a mechanically sensitive material for a resistive pressure sensor according to claim 1, wherein the melt viscosity of the polyethylene terephthalate after melting is 1000-2000 mPa-s; and/or the length of the carbon nano tube is 10-30 mu m, and the diameter is 10-20nm.
3. The method for preparing a mechanically sensitive material for a resistive pressure sensor according to claim 1, wherein the carbon nanotubes are added in an amount of 4 to 12% by mass of the total addition of the polyethylene terephthalate and the carbon nanotubes.
4. The method for preparing a mechanically sensitive material for a resistive pressure sensor according to claim 1, wherein the first solvent comprises o-chlorophenol; and/or, the polyethylene terephthalate accounts for 5-10% of the first mixture in percentage by mass.
5. The method of preparing a mechanically sensitive material for a resistive pressure sensor of claim 1, wherein the coating embodiment comprises:
coating the surface of the polyvinyl alcohol fiber along a first direction to form a first layer which is continuously distributed;
coating the surface of the polyvinyl alcohol fiber along a second direction to form a second layer which is coated on the first layer and is continuously distributed;
coating the surface of the polyvinyl alcohol fiber in an alternating coating mode along the first direction and the second direction to form a third layer which is coated on the second layer and is continuously distributed;
the first direction intersects the second direction, and the first layer, the second layer, and the third layer constitute the cladding layer.
6. The method for producing a mechanically sensitive material for a resistive pressure sensor according to claim 5, wherein the thickness of the first layer, the thickness of the second layer, and the thickness of the third layer are each 0.1 to 0.5mm; and/or, in the coating process, the coating of the next layer is performed after the previous layer is dried.
7. The method for preparing a mechanically sensitive material for a resistive pressure sensor according to claim 1, wherein the swelling is performed in normal temperature water for 10-60min; and/or, after the swelling is performed, the water temperature is raised to 80-95 ℃.
8. The method for preparing a mechanically sensitive material for a resistive pressure sensor according to claim 1, wherein the polyvinyl alcohol fiber has a diameter of 0.5 to 8 μm.
9. The method for preparing a mechanically sensitive material for a resistive pressure sensor according to claim 8, wherein the polyvinyl alcohol fiber has a diameter of 1-5 μm.
10. The method for preparing a mechanically sensitive material for a resistive pressure sensor according to claim 9, wherein the polyvinyl alcohol fiber has a diameter of 2-4 μm.
11. The method for preparing a mechanically sensitive material for a resistive pressure sensor according to claim 1, wherein the concentration of the MXene material in the MXene suspension is 0.1-1.0mg/L; and/or, in the mechanical sensitive material for the resistance type pressure sensor, the ratio of the mass of the MXene material to the total mass of the polyethylene terephthalate and the carbon nano tube is 1:5-20.
12. The method for preparing a mechanically sensitive material for a resistive pressure sensor according to claim 1, wherein the MXene material has a thickness of 0.8-1.2nm and a length of 0.5-4 μm; and/or, the preparation method of the MXene suspension comprises the following steps:
mixing lithium fluoride with hydrochloric acid, adding MAX phase, and reacting, wherein the chemical formula of MAX phase is Ti 3 SiC 2 ；
After the reaction is finished, centrifuging to obtain a first precipitate, mixing with water, performing ultrasonic treatment, centrifuging again, repeating the centrifugation and ultrasonic treatment until a mixture with neutral pH value is obtained, and separating out a second precipitate;
and then dispersing the second precipitate in an alcohol solvent, carrying out ultrasonic treatment and centrifugation to obtain a third precipitate, dispersing the third precipitate in water, carrying out ultrasonic treatment and centrifugation to obtain a supernatant, namely the MXene suspension.
13. A mechanically sensitive material for a resistive pressure sensor made by the method of making a mechanically sensitive material for a resistive pressure sensor of any one of claims 1-12.
14. A mechanical sensitive material for a resistance type pressure sensor is characterized by comprising a hollow structure matrix, carbon nanotubes distributed in the hollow structure matrix and an MXene material at least distributed on the outer surface of the hollow structure matrix, wherein the general formula of the MXene material is M n+1 X n T a M is transition metal, X is carbon and/or nitrogen, T is a surface functional group, and the material of the hollow structural matrix is polyethylene terephthalate.
15. Use of a mechanically sensitive material for a resistive pressure sensor according to claim 13 or 14 for the preparation of a resistive pressure sensor.
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