CN109431460B - Flexible high-flexibility nanofiber core-spun yarn stress sensor with fold structure and preparation method thereof - Google Patents
Flexible high-flexibility nanofiber core-spun yarn stress sensor with fold structure and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a flexible high-flexibility nanofiber core-spun yarn stress sensor with a folded structure and a preparation method thereof. The high-performance elastic filament is used as a core yarn as a high-flexibility elastic matrix, and then the surface of the elastic filament pre-stretched to a certain length is coated with electrostatic spinning nano-fibers through a conjugated electrostatic spinning technology to prepare the continuous nano-fiber core-spun yarn. A layer of conductive polymer polypyrrole is polymerized and coated on the surface of the shell layer nanofiber of the core-spun yarn through an in-situ liquid phase polymerization method, and finally a layer of gel film with conductive copper wires is coated on the surface of the yarn to obtain the stress sensor, and the stress sensor is applied to wearable electronic skin. When the nanofiber yarn stress sensor is subjected to external stimuli such as stretching, bending and pressure, the nanofiber yarn stress sensor has good mechanical adaptability, and shows ultrahigh sensitivity and a wide sensing range. In a human body monitoring system, limb movement monitoring of monitoring large stress changes from a heart rate of weak stress changes can be achieved.
Description
Technical Field
The invention belongs to the technical field of flexible sensors, and relates to a flexible high-flexibility nanofiber core-spun yarn stress sensor with a fold structure and a preparation method thereof, in particular to a flexible high-flexibility nanofiber core-spun yarn sensor with a fold structure, which is prepared by an electrostatic spinning technology and a liquid deposition polymerization technology and is applied to a human health monitoring system.
Background
Human skin is capable of transmitting various mechanical stimuli from the external environment to the brain. Achieving this function in artificial skin is key to creating advanced humanoid robots, biomedical prostheses, surgical electronic gloves and wearable health monitoring devices. In order to mimic the properties of human skin, artificial skin should have the ability to measure the spatial distribution of stress caused by a variety of mechanical stimuli such as normal pressure, lateral strain and flexion, in order to be able to master control and record body movements, secondly, scalability is an important property of artificial skin, ensuring that it adaptively covers surfaces that are arbitrarily curved and moving, such as the joints of a robotic arm, and is subject to repeated and prolonged mechanical deformations, such as bending and twisting, and thirdly, in order to achieve a wide range of applications of artificial skin in daily life, artificial skin should be compatible with large area preparation, and low material costs. In the last decade, the development of artificial skin based on pressure sensor arrays on flexible substrates has been greatly advanced, with high sensitivity, fast response speed and resolution of tactile mapping, but at a large distance from human skin, these pressure sensor arrays lack stretchability and can only provide the function of spatial pressure distribution information. In order to solve the problems, the selection of a new structural design sensor of an intrinsically stretchable material is an effective strategy for manufacturing a sensor with multiple mechanical force sensitivity and stretching mechanical property, so that the design of an ultrasensitive nanofiber core spun yarn stress sensor with small volume, good flexibility and high stretching property is the key for solving the problems.
Electrostatic spinning is a simple, highly efficient, and most attractive nanotechnology. Nanofibers prepared by electrospinning have shown good applicability in many fields due to their small size, high void fraction and large specific surface area. Therefore, the invention adopts high-performance elastic filament as core yarn as high-elasticity elastic matrix, firstly coats the surface of the elastic filament pre-stretched to a certain length with electrostatic spinning nano-fiber to prepare continuous nano-fiber core-spun yarn by a conjugated electrostatic spinning technology, and releases the pre-stretched elastic filament (core yarn) to obtain the nano-fiber core-spun yarn with a fold structure. And then grafting a layer of conductive polymer on the surface of the nanofiber of the core-spun yarn, and finally compounding a gel film with a conductive copper wire on the surface of the yarn to obtain the flexible high-flexibility nanofiber core-spun yarn stress sensor with a corrugated structure, and applying the sensor to wearable electronic skin.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides a preparation method of a yarn stress sensor with high flexibility and high elasticity and a fold structure. The high-performance elastic filament is used as a core yarn as a high-flexibility elastic matrix, and then the surface of the elastic filament pre-stretched to a certain length is coated with electrostatic spinning nano-fibers through a conjugated electrostatic spinning technology to prepare the continuous nano-fiber core-spun yarn. Due to the stiffness mismatch between the nanofibers and the highly elastic filaments, releasing the pre-stretched elastic filaments can result in a nanofiber core spun yarn with a periodic crimp structure. On the basis, a layer of conductive polymer is polymerized and coated on the surface of the shell layer nanofiber of the core-spun yarn through an in-situ liquid phase polymerization method, and finally a layer of gel film with conductive copper wires is coated on the surface of the yarn, so that the flexible high-flexibility nanofiber core-spun yarn stress sensor with a fold structure is obtained and is applied to wearable electronic skin. When the nanofiber yarn stress sensor is subjected to external stimuli such as stretching, bending and pressure, the nanofiber yarn stress sensor not only has good mechanical adaptability, but also shows ultrahigh stress sensitivity and a wider sensing range. In a human body monitoring system, limb movement monitoring of monitoring large stress changes from a heart rate of weak stress changes can be achieved.
In order to solve the technical problems, the invention adopts the following technical scheme:
a flexible high-flexibility nanofiber core-spun yarn sensor with a fold structure is a nanofiber core-spun yarn with the fold structure, which is formed by coating electrostatic spinning nanofibers on the surface of a high-flexibility elastic filament. The method specifically comprises the steps of using high-performance elastic filaments as core yarns as high-elasticity elastic matrixes, and then coating electrospun nano-fibers on the surfaces of the elastic filaments pre-stretched to a certain length by a conjugated electrostatic spinning technology to prepare the continuous nano-fiber core-spun yarns. Due to the stiffness mismatch between the nanofibers and the highly elastic filaments, releasing the pre-stretched elastic filaments can result in a nanofiber core spun yarn with a periodic crimp structure. On the basis, a layer of conductive polymer is polymerized and coated on the surface of the shell layer nanofiber of the core-spun yarn by an in-situ liquid phase polymerization method, and finally a layer of gel film with conductive copper wires is coated on the surface of the yarn to obtain the flexible high-flexibility nanofiber core-spun yarn stress sensor with a folded structure.
The elongation of the high-elasticity elastic filament is more than or equal to 100 percent, and the diameter of the elastic filament is 60-500 mu m.
The nano-fiber is composed of high molecular polymer, and the diameter of the nano-fiber is 100-900 nm.
The polymer is one or more of polyvinylidene fluoride (PVDF), Polyurethane (PU) and Polyacrylonitrile (PAN), and the molecular weight of the polymer is larger than or equal to 100000.
The diameter of the nanofiber core-spun yarn is 60-500 mu m, and the elongation is more than or equal to 0.01%. The gel film is a Polydimethylsiloxane (PDMS) film with the thickness of 0.01-10 mm. The diameter of the copper wire is 0.1-10 mm.
The invention discloses a flexible high-flexibility nanofiber covering yarn stress sensor with a fold structure, which comprises the following steps:
(1) dissolving a high molecular polymer in N, N Dimethylformamide (DMF) or a mixed solvent of N, N Dimethylformamide (DMF) and tetrahydrofuran, and stirring for 1-10 h at 30-100 ℃ to obtain a polymer solution with the mass fraction of 8-30%;
(2) an electrospinning apparatus was set up as shown in fig. 1, and the elastic filaments were first unwound from an unwinding device and wound through a metal bell mouth onto a winding device. The ratio of the unwinding speed of the unwinding device to the winding speed of the winding device is 0-1. And (2) adding the spinning solution obtained in the step (1) into a syringe pump to prepare a continuous nanofiber core-spun yarn. The electrostatic spinning voltage is 14-22 kV, the total flow of spinning solution is 0.5-0.9 mL/h, the diameter of a metal horn is 10-20cm, the vertical distance between the metal horn and a winding device is 40-60cm, the vertical distance between a spray head and the metal horn is 4-8cm, the horizontal distance between the spray head and the metal horn is 3-5cm, the number of the spray heads is 2-16, the inner diameter of the spray head is 0.26-0.86 mm, the flow ratio of positive and negative spray head solution is 1:0.5-1, the distance between the positive and negative spray heads is 13-17.5 cm, and the winding speed is 10-1000 mm/min.
(3) And (3) unwinding the nanofiber core-spun yarn prepared in the step (2) from a winding device and rewinding the nanofiber core-spun yarn to another winding device. The ratio of the winding speed of the winding device to the unwinding speed of the unwinding device is 0-1, ensuring that the core yarn (elastic filament) in the nanofiber core-spun yarn prepared during unwinding is restored to the original unstretched state, thereby forming the nanofiber core-spun yarn having a wrinkled structure.
(4) Soaking the nanofiber core-spun yarn with the folded structure prepared in the step (3) in ferric chloride (FeCl) with the concentration of 30-100 mol/L3) Dissolving in the solution for 30-100 min;
(5) soaking the nanofiber core-spun yarn in the step (4) in pyrrole (Py) solution with the concentration of 30-100 mol/L for 1-5 h at low temperature (0-4 ℃), taking out, washing with deionized water, and then drying in a vacuum oven at 30-90 ℃;
(6) and (5) coating a gel film Polydimethylsiloxane (PDMS) film with a conductive copper wire on the surface of the nanofiber core-spun yarn in the step (5) to obtain the nanofiber yarn stress sensor.
The invention has the beneficial effects that: (1) according to the invention, the nanofiber core-spun yarn with a folded structure is prepared by coating nanofiber on the surface of an elastic filament with high elasticity by using an electrostatic spinning technology, so that the nanofiber core-spun yarn with higher elongation is obtained. (2) The nanofiber core-spun yarn stress sensor prepared by the invention has the performance of being sensitive to pressure, tension and bending multi-force, and has the characteristics of high sensitivity, high response speed, high conductivity, wide bearable strain range, good stability and the like. (3) The prepared nanofiber core-spun yarn stress sensor has good mechanical adaptability, and can realize a wearable sensor in a real sense.
Drawings
FIG. 1 is a schematic diagram of an electrostatic spinning apparatus, including a winding device 1, a spray head 2, an injection pump 3, a metal horn 4, a high voltage generator 5, a positive electrode 51, and a negative electrode 52;
FIG. 2 is a schematic structural diagram of a nanofiber core spun yarn stress sensor, 6 copper wires, 7 PDMS elastic membranes and 8 nanofiber core spun yarns;
FIG. 3 SEM pictures of nanofiber core spun yarns with a pleated structure and single fibers;
figure 4 sensitivity of nanofiber core spun yarn stress sensor at different pressures in example 1.
Detailed Description
The present invention will be further described with reference to the following examples. It is to be understood that the following examples are illustrative only and are not intended to limit the scope of the invention, which is to be given numerous insubstantial modifications and adaptations by those skilled in the art based on the teachings set forth above.
Example 1
The preparation method of the flexible high-flexibility nanofiber core-spun yarn stress sensor with the corrugated structure comprises the following steps:
(1) dissolving Polyacrylonitrile (PAN) in N, N Dimethylformamide (DMF) solvent, and stirring at 80 ℃ for 6 h to obtain PAN solution with the mass fraction of 8%;
(2) building an electrostatic spinning device according to the diagram 1, adding the PAN solution in the step (1) into an injection pump to prepare continuous nanofiber yarns, wherein the elongation of elastic filaments is equal to 100%, the electrostatic spinning voltage is 17.5 kV, the total flow of the spinning solution is 0.6 mL/h, the diameter of a metal horn is 10 cm, the vertical distance between the metal horn and a winding device is 50 cm, the vertical distance between a spray head and the metal horn is 4 cm, the horizontal distance between the spray head and the metal horn is 3 cm, the number of the spray heads is 4, the inner diameter of each spray head is 0.4 mm, the flow ratio of positive and negative spray head solutions is 2:1, the distance between the positive and negative spray heads is 17 cm, and the winding speed is 50 mm/min;
(3) soaking the nanofiber core-spun yarn prepared in the step (2) in ferric chloride (FeCl) with the concentration of 50 mol/L3) Soaking in the solution for 30 min;
(4) soaking the nanofiber core-spun yarn in the step (3) in 50 mol/L pyrrole (Py) solution at low temperature (0-4 ℃) for 3 hours, taking out, washing with deionized water, and then drying in a vacuum oven at 60 ℃ to obtain the nanofiber core-spun yarn of PPy @ PAN;
(5) and (4) compounding a Polydimethylsiloxane (PDMS) film with a conductive copper wire on the surface of the nanofiber core-spun yarn in the step (4) to obtain the PPy @ PAN nanofiber yarn stress sensor.
(6) The PPy @ PAN nanofiber yarn stress sensors prepared in step (5) were stretched to different lengths to obtain corresponding stretch sensitivities, which, as shown in the figure, showed higher sensitivity and a wider range of stretch sensitivities.
Example 2
The preparation method of the flexible high-flexibility nanofiber core-spun yarn stress sensor with the corrugated structure comprises the following steps:
(1) dissolving polyvinylidene fluoride (PVDF) in a mixed solvent of N, N Dimethylformamide (DMF) and tetrahydrofuran (mass ratio is 1: 1), and stirring for 6 hours at 80 ℃ to obtain a PVDF solution with the mass fraction of 16.5%;
(2) building an electrostatic spinning device according to the diagram 1, adding the spinning solution in the step (1) into an injection pump to prepare continuous nanofiber yarns, wherein the elongation of elastic filaments is equal to 150%, the electrostatic spinning voltage is 17.5 kV, the total flow of the spinning solution is 0.6 mL/h, the diameter of a metal horn is 10 cm, the vertical distance between the metal horn and a winding device is 50 cm, the vertical distance between a spray head and the metal horn is 4 cm, the horizontal distance between the spray head and the metal horn is 3 cm, the number of the spray heads is 4, the inner diameter of each spray head is 0.4 mm, the flow ratio of positive and negative spray head solutions is 2:1, the distance between the positive and negative spray heads is 17 cm, and the winding speed is 50 mm/min;
(3) soaking the nanofiber core-spun yarn prepared in the step (2) in ferric chloride (FeCl) with the concentration of 30 mol/L3) Soaking in the solution for 50 min;
(4) soaking the nanofiber core-spun yarn in the step (3) in a pyrrole (Py) solution with the concentration of 30 mol/L at a low temperature (0-4 ℃) for 4 hours, taking out, washing with deionized water, and then drying in a vacuum oven at 60 ℃ to obtain the PVDF @ PPy nanofiber core-spun yarn;
(5) and (4) compounding a Polydimethylsiloxane (PDMS) film with a conductive copper wire on the surface of the nanofiber core-spun yarn in the step (4) to obtain the PVDF @ PPy nanofiber yarn stress sensor.
Example 3
The preparation method of the flexible high-flexibility nanofiber core-spun yarn stress sensor with the corrugated structure comprises the following steps:
(1) dissolving Polyurethane (PU) in a mixed solvent of N, N Dimethylformamide (DMF) and tetrahydrofuran (mass ratio is 1: 1), and stirring for 8 hours at normal temperature to obtain a PU solution with the mass fraction of 12%;
(2) building an electrostatic spinning device according to the diagram 1, adding the spinning solution in the step (1) into an injection pump to prepare continuous nanofiber yarns, wherein the elongation of elastic filaments is equal to 200%, the electrostatic spinning voltage is 20 kV, the total flow of the spinning solution is 0.6 mL/h, the diameter of a metal horn is 10 cm, the vertical distance between the metal horn and a winding device is 50 cm, the vertical distance between a spray head and the metal horn is 4 cm, the horizontal distance between the spray head and the metal horn is 3 cm, the number of the spray heads is 4, the inner diameter of the spray head is 0.4 mm, the flow ratio of a positive spray head solution to a negative spray head solution is 2:1, the distance between the positive spray head and the negative spray head is 17 cm, and the winding speed is 50 mm/min;
(3) soaking the nanofiber core-spun yarn prepared in the step (2) in ferric chloride (FeCl) with the concentration of 75 mol/L3) Soaking in the solution for 70 min;
(4) soaking the nanofiber core-spun yarn in the step (3) in 75 mol/L pyrrole (Py) solution at low temperature (0-4 ℃) for 1 h, taking out, washing with deionized water, and then drying in a vacuum oven at 60 ℃ to obtain the nanofiber core-spun yarn of PU @ PPy;
(5) and (4) compounding a Polydimethylsiloxane (PDMS) film with a conductive copper wire on the surface of the nanofiber core-spun yarn in the step (4) to obtain the PU @ PPy nanofiber yarn stress sensor.
(6) And (3) weaving the PPy @ PAN nanofiber yarn stress sensor prepared in the step (5) into a fabric, and applying different pressures to obtain corresponding pressure sensitivity.
Example 4
The preparation method of the flexible high-flexibility nanofiber core-spun yarn stress sensor with the corrugated structure comprises the following steps:
(1) dissolving Polyurethane (PU) in a mixed solvent of N, N Dimethylformamide (DMF) and tetrahydrofuran (mass ratio is 1: 1), and stirring for 8 hours at normal temperature to obtain a PU solution with the mass fraction of 12%;
(2) building an electrostatic spinning device according to the diagram 1, adding the spinning solution in the step (1) into an injection pump to prepare continuous nanofiber yarns, wherein the elongation of elastic filaments is equal to 200%, the electrostatic spinning voltage is 20 kV, the total flow of the spinning solution is 0.6 mL/h, the diameter of a metal horn is 10 cm, the vertical distance between the metal horn and a winding device is 50 cm, the vertical distance between a spray head and the metal horn is 4 cm, the horizontal distance between the spray head and the metal horn is 3 cm, the number of the spray heads is 4, the inner diameter of the spray head is 0.4 mm, the flow ratio of a positive spray head solution to a negative spray head solution is 2:1, the distance between the positive spray head and the negative spray head is 17 cm, and the winding speed is 50 mm/min;
(3) soaking the nanofiber core-spun yarn prepared in the step (2) in ferric chloride (FeCl) with the concentration of 75 mol/L3) Soaking in the solution for 70 min;
(4) soaking the nanofiber core-spun yarn in the step (3) in 75 mol/L pyrrole (Py) solution at low temperature (0-4 ℃) for 1 h, taking out, washing with deionized water, and then drying in a vacuum oven at 60 ℃ to obtain the nanofiber core-spun yarn of PU @ PPy;
(5) and (4) compounding a Polydimethylsiloxane (PDMS) film with a conductive copper wire on the surface of the nanofiber core-spun yarn in the step (4) to obtain the PU @ PPy nanofiber yarn stress sensor.
(6) And (4) bending the PPy @ PAN nanofiber yarn stress sensor prepared in the step (5) to different angles to obtain corresponding bending sensitivity.
Therefore, the flexible high-flexibility nanofiber yarn stress sensor prepared by the invention shows ultrahigh sensitivity and a wider sensing range when being stimulated by external force based on the characteristics of larger specific surface area of nanofibers and excellent performance of materials. In a human body monitoring system, limb movement monitoring from a weak pressure heart rate to a large pressure can be realized. In addition, the preparation process is simple and convenient, the cost is low, and the development towards large-scale commercialization is facilitated.
The foregoing shows and describes the general principles and features of the present invention, together with the advantages thereof. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are described in the specification and illustrated only to illustrate the principle of the present invention, but that various changes and modifications may be made therein without departing from the spirit and scope of the present invention, which fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (7)
1. A preparation method of a flexible high-flexibility nanofiber covering yarn stress sensor with a fold structure is characterized by comprising the following steps of: the method comprises the following steps of adopting a high-performance elastic filament as a core yarn as a high-flexibility elastic matrix, then coating electrospun nano-fibers on the surface of the elastic filament pre-stretched to a certain length by a conjugated electrostatic spinning technology to prepare continuous nano-fiber core-spun yarn, on the basis, polymerizing and coating a layer of conductive polymer on the surface of the nano-fibers of a shell layer of the core-spun yarn by an in-situ liquid phase polymerization method, and finally coating a layer of gel film with conductive copper wires on the surface of the yarn to obtain the flexible high-flexibility nano-fiber core-spun yarn stress sensor with a folded structure; the preparation method comprises the following steps:
(1) dissolving a high molecular polymer in N, N dimethylformamide or a mixed solvent of N, N dimethylformamide and tetrahydrofuran, and stirring for 1-10 h at 30-100 ℃ to obtain a spinning solution with the mass fraction of 8% -30%;
(2) building an electrostatic spinning device, firstly unwinding an elastic filament from an unwinding device, winding the elastic filament on a winding device through a metal bell mouth, then adding the spinning solution obtained in the step (1) into an injection pump, and preparing continuous nanofiber core-spun yarns by taking the elastic filament as a high-elasticity elastic matrix; wherein the ratio of the unwinding speed of the unwinding device to the winding speed of the winding device is 0-1, and the elongation of the elastic filament is more than or equal to 100 percent;
(3) unwinding the nanofiber core-spun yarn prepared in the step (2) from a winding device and rewinding the nanofiber core-spun yarn on another winding device, wherein the ratio of the winding speed of the winding device to the unwinding speed of the unwinding device is 0-1, so that the elastic filament in the nanofiber core-spun yarn prepared in the unwinding process is ensured to be restored to the original non-elongated state, and the nanofiber core-spun yarn with a corrugated structure is formed;
(4) soaking the nanofiber core-spun yarn with the folded structure prepared in the step (3) in ferric chloride (FeCl) with the concentration of 30-100 mol/L3) Dissolving in the solution for 30-100 min;
(5) soaking the nanofiber core-spun yarn treated in the step (4) in a pyrrole (Py) solution with the concentration of 30-100 mol/L for 1-5 h at 0-4 ℃, taking out, washing with deionized water, and then drying in a vacuum oven at 30-90 ℃;
(6) and (5) coating a gel film with a conductive copper wire on the surface of the nanofiber core-spun yarn dried in the step (5) to obtain the nanofiber core-spun yarn stress sensor.
2. The method of claim 1, wherein: the nanofiber is composed of high molecular polymer, and the diameter of the nanofiber is 100-900 nm.
3. The method of claim 2, wherein: the high molecular polymer is polyvinylidene fluoride, polyurethane and polyacrylonitrile, and the molecular weight of the polymer is more than or equal to 100000.
4. The method of claim 1, wherein: the diameter of the nanofiber core-spun yarn is 60-500 mu m.
5. The method of claim 1, wherein: the gel film is polydimethylsiloxane film with the thickness of 0.01-10 mm.
6. The method of claim 1, wherein: the diameter of the copper wire is 0.1-10 mm.
7. The method of claim 1, wherein: when the continuous nanofiber core-spun yarn is prepared in the step (2), the electrostatic spinning voltage is 14-22 kV, the total flow rate of a spinning solution is 0.5-0.9 mL/h, the diameter of a metal horn is 10-20cm, the vertical distance between the metal horn and a winding device is 40-60cm, the vertical distance between a spray head and the metal horn is 4-8cm, the horizontal distance between the spray head and the metal horn is 3-5cm, the number of the spray heads is 2-16, the inner diameter of the spray head is 0.26-0.86 mm, the flow rate ratio of a positive spray head solution to a negative spray head solution is 1:0.5-1, the distance between the positive spray head and the negative spray head is 13-17.5 cm, and the winding speed is 40-53 mm/min.
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| CN113981552B (en) * | 2021-11-19 | 2023-04-11 | 嘉兴学院 | Preparation method of elastic nanofiber yarn |
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