CN111122674A - Photo-thermal double-stimulus response type fibrous sensing device and preparation and application thereof - Google Patents
Photo-thermal double-stimulus response type fibrous sensing device and preparation and application thereof Download PDFInfo
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Abstract
The invention relates to a photo-thermal double-stimulus response type fibrous sensing device and preparation and application thereof. The sensing device includes: the fiber comprises a sheath-core structure fiber, electrodes and an outermost polymer coating layer, wherein the sheath-core structure fiber takes a fiber substrate as a core and a semiconductor functional layer as a sheath, the electrodes are arranged on two sides of the sheath-core structure fiber, and the outermost polymer coating layer is arranged on the outermost polymer coating layer. The method comprises the following steps: dripping vanadium pentoxide nanowire dispersion liquid into a salt solution to form a nanowire flocculating constituent, winding and assembling the nanowire flocculating constituent on a substrate by twisting and weaving wires, and removing moisture to obtain a skin-core structure fiber; electrodes were placed on both sides of the core-sheath fiber and then polymer cladding layers were prepared by extrusion. The method solves the problem that the resistance of the functional fiber increases along with the increase of the length, and is beneficial to the long-range preparation of the functional fiber.
Description
Technical Field
The invention belongs to the field of intelligent fiber materials and preparation and application thereof, and particularly relates to a photo-thermal double-stimulus response type fibrous sensing device and a preparation method and application thereof.
Background
Smart fibers, which are fibers capable of sensing environmental changes or stimuli (e.g., light, electricity, force, humidity, temperature, pH, etc.) and responding thereto, are important constituent structural units of smart wearable systems. In the face of complex environments such as human-computer interaction, how to realize multiple stimulation responses by the intelligent fiber is still a significant challenge and is also a key research object for the development of multifunctional intelligent wearable systems.
One-dimensional nano semiconductor materials (nanowires, nanobelts, nanorods and the like) have surface effects, small-size effects, quantum size effects and the like, and are widely applied to the fields of energy, sensing and the like due to abundant mechanical, electrical and optical characteristics. Growing or wrapping a functional layer of a nanomaterial on a fiber substrate is one of methods for preparing a fibrous responsive device, for example, chinese patent CN201810252172.6 combines atomic layer deposition, liquid-phase laser ablation and a solvothermal method, and prepares a fibrous ultraviolet detector by using a flexible fibrous thin metal wire as a substrate. However, there are some problems with such methods: (1) loading nanowires or nanorods on a fiber substrate generally adopts a hydrothermal or solvothermal method, the reaction conditions need high temperature and high pressure, and the reaction conditions are not mild; (2) the long-range preparation of the fiber cannot be realized by a hydrothermal method or a solvothermal method; (3) the fiber-shaped sensing device structure is usually a skin-core structure, the resistance of the fiber increases with the increase of the length, and the fiber-shaped sensing device structure has obstacles in intelligent clothing application.
Vanadium pentoxide is a transition metal oxide, widely used in the fields of sensing, energy and the like, and is a semiconductor material having important influence on the development of modern society.
Disclosure of Invention
The invention aims to solve the technical problem of providing a photo-thermal double-stimulation response type fibrous sensing device and preparation and application thereof, so as to overcome the defects that nanowires in intelligent fibers cannot be uniformly loaded on a fiber substrate and the like in the prior art.
The invention provides a photo-thermal dual-stimulus responsive fibrous sensing device, comprising: the fiber comprises a fiber substrate, a semiconductor functional layer, electrodes and an outermost polymer coating layer, wherein the fiber substrate is used as a core, the semiconductor functional layer is used as a skin-core structure fiber, the electrodes are arranged on two sides of the skin-core structure fiber, and the outermost polymer coating layer is arranged on the outermost polymer coating layer;
the semiconductor functional layer is a vanadium pentoxide nanowire, the skin-core structure fiber is obtained by forming a nanowire flocculating constituent from the vanadium pentoxide nanowire in a salt solution and then twisting the fiber substrate to enable the nanowire flocculating constituent to be wound and assembled on the substrate.
The fiber substrate is a braided wire with the diameter of 0.2-0.4 mm.
The braided wire is cotton wire, aramid fiber wire or nylon wire.
The thickness of the semiconductor functional layer is 5-20 μm.
The diameter of the vanadium pentoxide nanowire is 30-100 nm, and the length of the vanadium pentoxide nanowire is 0.1-6 mm.
The electrodes arranged on two sides of the skin-core structure fiber are arranged in parallel.
The electrode is a metal copper wire with a diameter of 100 μm.
The polymer coating layer is made of polyvinyl chloride and has a thickness of 0.15-0.25 mm.
The invention also provides a preparation method of the photo-thermal double-stimulation response type fibrous sensing device, which comprises the following steps:
(1) dispersing vanadium pentoxide nanowires in water, and performing ultrasonic treatment to obtain vanadium pentoxide nanowire dispersion liquid;
(2) dripping the vanadium pentoxide nanowire dispersion liquid obtained in the step (1) into a salt solution to form a nanowire flocculating constituent, winding and assembling the obtained nanowire flocculating constituent on a substrate by using a braided wire as the substrate through twisting the braided wire, and removing moisture to obtain a skin-core structure fiber;
(3) and (3) placing electrodes on two sides of the skin-core structure fiber in the step (2), and then preparing a polymer coating layer through extrusion to obtain the photo-thermal double-stimulation response type fibrous sensing device.
The preparation method of the vanadium pentoxide nanowire in the step (1) comprises the following steps: mixing vanadium pentoxide particles with a mixed solvent of hydrogen peroxide and water, stirring, and carrying out hydrothermal reaction at 200-230 ℃ for 72-120 h to obtain vanadium pentoxide nanowires with uniform dimensions, wherein the molar ratio of vanadium pentoxide to hydrogen peroxide is 1: 0.25-0.35, and the volume ratio of hydrogen peroxide to water is 1: 5-8.
The volume fraction of hydrogen peroxide was 30%.
The stirring time is 0.5-1.5 h.
The ultrasonic treatment time in the step (1) is 0.3-2 min.
In the step (2), the vanadium pentoxide nanowire dispersion liquid in the step (1) is dripped into a salt solution to form a nanowire flocculating constituent: slowly dropping the vanadium pentoxide nanowire uniform dispersion liquid obtained in the step (1) into a square container containing a salt solution (with the concentration of 0.1-3 mol/L), wherein the nanowire is provided with a certain charge and is combined with ions with opposite charges in the solution to form aggregation, and macroscopically, the aggregation is expressed as forming a floccule, wherein the volume ratio of the vanadium pentoxide nanowire uniform dispersion liquid to the salt solution is 1: 10-30.
And (3) in the step (2), the salt is sodium chloride, potassium chloride, magnesium chloride or calcium chloride.
The concentration of the salt solution in the step (2) is 0.1-3 mol/L.
And (3) heating to remove water in the step (2), wherein the heating temperature is 60-80 ℃, and the heating time is 8-10 h.
In the step (3), electrodes are arranged on two sides of the skin-core structure fiber in the step (2), and then polymer coating layers are prepared by extrusion: two metal wire external electrodes are parallelly placed on two sides of the skin-core structure fiber, and pass through an extruder together to prepare a polyvinyl chloride protective layer on the outer layer of the skin-core structure fiber.
The invention also provides application of the photo-thermal double-stimulation response type fibrous sensing device. For example, for smart apparel.
According to the invention, vanadium pentoxide forms a flocculating constituent in a salt solution, and the nanowire flocculating constituent is wound and assembled on the substrate by twisting the fiber substrate, so that uniform loading of nanowires on the fiber substrate is realized.
Advantageous effects
(1) The invention adopts the mode that the nanowires with large length-diameter ratio are assembled on the fiber substrate in a flocculation way in solution to prepare the functional fiber, the process is simple, the preparation condition is mild, the functional material is coated on the fiber substrate and is not easy to fall off, and the invention is beneficial to the large-scale preparation of the functional fiber.
(2) The invention solves the problem that the resistance of the functional fiber is increased along with the increase of the length by applying the parallel external electrode, because the fiber resistance is related to the thickness of the loaded functional layer, and is beneficial to the long-range preparation of the functional fiber.
Drawings
Fig. 1 is a schematic structural view of a photothermal double stimulus responsive fibrous sensor device in example 1; wherein 1 is a braided wire substrate, 2 is a vanadium pentoxide functional layer, 3 is an outer parallel double electrode, and 4 is a polyvinyl chloride protective layer.
FIG. 2 is a scanning electron microscope image of the vanadium pentoxide nanowire prepared in example 1;
FIG. 3 is a scanning electron micrograph of a core-sheath structured fiber prepared in example 1;
fig. 4 is a digital photograph of the photothermal dual stimulus responsive fibrous sensor device prepared in example 1: wherein (a) is a prepared ten-meter long fibrous device; (b) a bracelet woven from fibrous devices;
FIG. 5 is a graph illustrating the measurement of the photo-sensitive performance of the photo-thermal dual stimulus responsive fibrous sensor device prepared in example 1;
FIG. 6 is a temperature-sensitive performance test chart of the photothermal dual stimulus responsive fibrous sensing device prepared in example 1;
fig. 7 is a photograph of flocs of vanadium pentoxide nanowires in a salt solution: wherein (a) is a photograph of the flocs in the sodium chloride solution of example 1; (b) is a photograph of the flocs in the magnesium chloride solution in example 3;
fig. 8 is a photograph of a flocculation state of the vanadium pentoxide nanowire prepared after the ultrasonic treatment for 10min in comparative example 1 in a salt solution.
Detailed Description
The invention will be further illustrated with reference to the following specific examples. It should be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present invention. Further, it should be understood that various changes or modifications of the present invention may be made by those skilled in the art after reading the teaching of the present invention, and such equivalents may fall within the scope of the present invention as defined in the appended claims.
Example 1
(1) At room temperature, 0.364g of vanadium pentoxide particles (analytically pure, national medicine) was weighed into a 100mL reagent bottle, then 30mL of deionized water was added, 5mL of hydrogen peroxide (30%) (analytically pure, Hu test) was slowly added, and then magnetic stirring was performed at room temperature for 0.5h to obtain a clear and transparent orange solution. Pouring 35mL of orange solution into a 50mL hydrothermal kettle liner, and heating in an oven at 205 ℃ for 96h to obtain yellow vanadium pentoxide nanowires.
(2) And (2) washing the vanadium pentoxide nanowires in the step (1) for multiple times to prepare 1mg/ml of aqueous dispersion, and performing ultrasonic treatment for 30s to obtain the uniform aqueous dispersion of the vanadium pentoxide nanowires.
(3) And (3) taking the vanadium pentoxide nanowire uniform dispersion liquid (with the volume of 2ml) obtained in the step (2), dripping the vanadium pentoxide nanowire uniform dispersion liquid into 1mol/L sodium chloride solution (with the volume of 40ml), flocculating, taking the aramid yarn as a substrate, winding and assembling the nanowire floccule on the substrate by twisting the braided wire, and heating at 80 ℃ for 6 hours to remove water to obtain the skin-core structure fiber.
(4) And (3) taking the skin-core structure fiber obtained in the step (3), placing two metal copper wires on two sides of the fiber in parallel, enabling the two metal copper wires to pass through an extruder together, preparing a polyvinyl chloride protective layer on the outer layer of the fiber, controlling the thickness of the protective layer to be 0.15mm, and finally obtaining the photo-thermal double-stimulus response type fibrous sensing device, wherein the resistance of the fiber can be changed under the irradiation of 460nm light and under different temperature changes.
Fig. 2 is a scanning electron microscope image of the vanadium pentoxide nanowire prepared in this embodiment, which shows that the vanadium pentoxide nanowire has a large length-diameter ratio and a uniform size distribution.
Fig. 1 is a schematic structural diagram of a photothermal dual stimulus response type fibrous sensing device prepared in this embodiment. Wherein 1 is a braided wire substrate, 2 is a vanadium pentoxide functional layer, 3 is an outer parallel double electrode, and 4 is a polyvinyl chloride protective layer.
Fig. 3 is a scanning electron microscope image of the skin-core structure fiber prepared in this embodiment, where the skin layer is vanadium pentoxide, it can be known that vanadium pentoxide nanowires are tightly and uniformly coated on the braided wire, and the fiber resistance is related to the thickness of the loaded nanowire layer.
Fig. 4 is a digital photograph of the photothermal dual stimulus response type fibrous sensor device prepared in this example, and the fibers can be woven into different shapes.
Fig. 5 is a photosensitive performance test of the photothermal dual stimulus response type fiber sensor device prepared in this example, and it can be seen that the resistance of the fiber is reduced under the irradiation of blue light (wavelength 460nm), and the response time is about 20 s.
Fig. 6 is a temperature-sensitive performance test of the photothermal dual stimulus response type fibrous sensor device prepared in this embodiment, and it can be known that the resistance of the fiber decreases with the increase of temperature.
Example 2
According to the embodiment 1, the step (1) ' heating in an oven at 205 ℃ for 96h ' is changed into the step "heating in an oven at 220 ℃ for 84h ', the rest is the same as the embodiment 1, the vanadium pentoxide nanowire with larger length-diameter ratio can also be obtained, and the photosensitive and temperature-sensitive performance of the assembled fibrous device is the same as the embodiment 1.
Example 3
According to the embodiment 1, the step (3) 'dropping into 1mol/L sodium chloride solution' is changed into 'dropping into 1mol/L magnesium chloride solution', the rest is the same as the embodiment 1, the vanadium pentoxide nanowire flocculating body is obtained, and the photosensitive and temperature-sensitive performance of the assembled fibrous device is the same as the embodiment 1.
Fig. 7 is a photograph of flocs of vanadium pentoxide nanowires in a salt solution: wherein (a) is a photograph of the flocs in the sodium chloride solution in example 1, and (b) is a photograph of the flocs in the magnesium chloride solution in example 3. It is known that vanadium pentoxide can also form flocs in magnesium chloride solution for further device assembly.
Comparative example 1
According to the example 1, the ultrasonic treatment in the step (2) for 30s is changed into ultrasonic treatment for 10min, and the rest is the same as the example 1, as shown in FIG. 8, the length of the nanowire is shortened along with the increase of the ultrasonic time, and the floccule can not be formed in the salt solution.
Chinese patent (CN 108411614A) prepares the flexible sensing fiber by growing a zinc oxide nano structure on a cotton wire through a hydrothermal reaction, but the length of the zinc oxide nano wire on the surface of the cotton wire is short (1-2 mu m), the bonding force between the nano wire networks is weak, the breakage is easy to occur, and the practical use is limited to a certain extent. In Chinese patent (CN 110306260A), vanadium pentoxide nanowires are assembled through a three-phase interface to prepare macroscopic inorganic fibers, which have temperature-sensitive performance, but the macroscopic inorganic fibers are composed of pure inorganic nanowires and have poor flexibility.
Claims (9)
1. A photothermal dual stimulus responsive fibrous sensor device, said sensor device comprising: the fiber comprises a fiber substrate, a semiconductor functional layer, electrodes and an outermost polymer coating layer, wherein the fiber substrate is used as a core, the semiconductor functional layer is used as a skin-core structure fiber, the electrodes are arranged on two sides of the skin-core structure fiber, and the outermost polymer coating layer is arranged on the outermost polymer coating layer;
the semiconductor functional layer is a vanadium pentoxide nanowire, the skin-core structure fiber is obtained by forming a nanowire flocculating constituent from the vanadium pentoxide nanowire in a salt solution and then twisting the fiber substrate to enable the nanowire flocculating constituent to be wound and assembled on the substrate.
2. The sensor device of claim 1, wherein the fiber substrate is a braided wire, and the braided wire has a diameter of 0.2-0.4 mm.
3. The sensor device according to claim 1, wherein the thickness of the semiconductor functional layer is 5 to 20 μm; the diameter of the vanadium pentoxide nanowire is 30-100 nm, and the length of the vanadium pentoxide nanowire is 0.1-6 mm.
4. The sensing device of claim 1, wherein the electrodes disposed on both sides of the core-sheath structured fiber are arranged in parallel; the electrode is a metallic copper wire with a diameter of 100 μm.
5. The sensor device of claim 1, wherein the polymer coating is polyvinyl chloride and has a thickness of 0.15mm to 0.25 mm.
6. A preparation method of a photo-thermal double-stimulation response type fibrous sensing device comprises the following steps:
(1) dispersing vanadium pentoxide nanowires in water, and performing ultrasonic treatment to obtain vanadium pentoxide nanowire dispersion liquid;
(2) dripping the vanadium pentoxide nanowire dispersion liquid obtained in the step (1) into a salt solution to form a nanowire flocculating constituent, winding and assembling the obtained nanowire flocculating constituent on a substrate by using a braided wire as the substrate through twisting the braided wire, and removing moisture to obtain a skin-core structure fiber;
(3) and (3) placing electrodes on two sides of the skin-core structure fiber in the step (2), and then preparing a polymer coating layer through extrusion to obtain the photo-thermal double-stimulation response type fibrous sensing device.
7. The method according to claim 6, wherein the preparation method of the vanadium pentoxide nanowires in the step (1) comprises the following steps: mixing vanadium pentoxide particles with a mixed solvent of hydrogen peroxide and water, stirring, and carrying out hydrothermal reaction at 200-230 ℃ for 72-120 h to obtain the catalyst, wherein the molar ratio of the vanadium pentoxide to the hydrogen peroxide is 1: 0.25-0.35, and the volume ratio of the hydrogen peroxide to the water is 1: 5-8; the ultrasonic treatment time is 0.3-2 min.
8. The method according to claim 6, wherein the salt in the step (2) is sodium chloride, potassium chloride, magnesium chloride or calcium chloride; the concentration of the salt solution is 0.1-3 mol/L.
9. Use of a sensor device according to claim 1.
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Cited By (1)
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| CN114199816A (en) * | 2021-11-22 | 2022-03-18 | 湖北大学 | Near-infrared light excitation-based photo-thermal sensor for detecting biomarker, preparation method thereof and application thereof in marker detection |
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