CN115491815A - Enhanced flexible polyvinylidene fluoride nanofiber material and friction nano generator - Google Patents

Enhanced flexible polyvinylidene fluoride nanofiber material and friction nano generator Download PDF

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CN115491815A
CN115491815A CN202211288188.5A CN202211288188A CN115491815A CN 115491815 A CN115491815 A CN 115491815A CN 202211288188 A CN202211288188 A CN 202211288188A CN 115491815 A CN115491815 A CN 115491815A
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polyvinylidene fluoride
layer
friction
metal electrode
nanofiber material
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张析
杨专青
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Puli New Material Technology Suzhou Co ltd
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Puli New Material Technology Suzhou Co ltd
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    • D—TEXTILES; PAPER
    • D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
    • D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
    • D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
    • D04H1/40—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties
    • D04H1/42—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties characterised by the use of certain kinds of fibres insofar as this use has no preponderant influence on the consolidation of the fleece
    • D04H1/4282—Addition polymers
    • D04H1/4318—Fluorine series
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D5/00—Formation of filaments, threads, or the like
    • D01D5/0007—Electro-spinning
    • D01D5/0015—Electro-spinning characterised by the initial state of the material
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F1/00—General methods for the manufacture of artificial filaments or the like
    • D01F1/02—Addition of substances to the spinning solution or to the melt
    • D01F1/10—Other agents for modifying properties
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
    • D01F6/44—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds as major constituent with other polymers or low-molecular-weight compounds
    • D01F6/48—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds as major constituent with other polymers or low-molecular-weight compounds of polymers of halogenated hydrocarbons
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
    • D01F6/88—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds
    • D01F6/90—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds of polyamides
    • D—TEXTILES; PAPER
    • D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
    • D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
    • D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
    • D04H1/70—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres
    • D04H1/72—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres the fibres being randomly arranged
    • D04H1/728—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres the fibres being randomly arranged by electro-spinning
    • H—ELECTRICITY
    • H02—GENERATION; CONVERSION OR DISTRIBUTION OF ELECTRIC POWER
    • H02N—ELECTRIC MACHINES NOT OTHERWISE PROVIDED FOR
    • H02N1/00—Electrostatic generators or motors using a solid moving electrostatic charge carrier
    • H02N1/04—Friction generators

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  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Manufacturing & Machinery (AREA)
  • Mechanical Engineering (AREA)
  • Laminated Bodies (AREA)

Abstract

The invention provides an enhanced flexible polyvinylidene fluoride nano-fiber material and a friction nano-generator, and relates to the technical field of nano-energy. The material can be used as a negative electricity layer material of a friction nano generator, the manufacturing process is simple, the cost is low, and the manufactured friction nano generator has excellent output performance. The invention prepares the enhanced flexible polyvinylidene fluoride nano-fiber material by an expandable electrostatic spinning method, and has the advantages of quick manufacture, high yield and the like.

Description

Enhanced flexible polyvinylidene fluoride nanofiber material and friction nano generator
Technical Field
The invention relates to the technical field of nano energy, in particular to an enhanced flexible polyvinylidene fluoride nano fiber material and a friction nano generator.
Background
With the increasing use of discrete intelligent electronic devices, there is an urgent need to find convenient, sustainable, and clean power sources for portable and wearable electronic devices. In recent years, triboelectric nano-generators (TENG) have been explored and developed as one of promising candidates due to their simplicity of manufacture, flexibility in material selection, and high efficiency of energy conversion. The friction nano generator is an energy conversion device which converts mechanical energy into electric energy by utilizing friction electrification and electrostatic induction effects. When two friction material layers are in contact with each other, charge movement will occur between the layers to maintain charge balance. Through contact and separation, TENG can collect mechanical energy in the environment and convert the mechanical energy into electric energy, and has great application potential in the fields of mechanical energy collection and self-driven sensing.
In order to achieve high performance TENG, many efforts have been made to develop various triboelectric layer materials, such as nylon-11, a triboelectric positive layer of cellulose, and a triboelectric negative layer of polyvinylidene fluoride (PVDF), polydimethylsiloxane. Among them, β -phase PVDF is the best choice for the triboelectric layer because it has excellent electronegativity and piezoelectricity. There are several different methods for enhancing the piezoelectricity of PVDF-based triboelectric layers, such as mechanical stretching, electrospinning, electric field polarization, and the incorporation of piezoelectric fillers including lead zirconate titanate (PZT) particles, baTiO 3 Particles and MoS 2 A sheet. However, the piezoelectric fillers currently incorporated are generally toxic. For the practical application of TENG, the piezoelectricity as well as the cost effect and environmental friendliness of PVDF-based materials need to be further improved. Therefore, processes that use low cost electrospinning fabrication methods and processes that use cheaper, less toxic materials are more desirable. In the context of flexible electronic applications, such as human body-based wearable applications, there is a need to develop a flexible triboelectric layer material that has excellent output performance and is environmentally friendly.
Disclosure of Invention
The invention aims to provide an enhanced flexible polyvinylidene fluoride nano-fiber material and a friction nano-generator. The technical effects that can be produced by the preferred technical scheme in the technical schemes provided by the invention are described in detail in the following.
In order to realize the purpose, the invention provides the following technical scheme:
the invention provides an enhanced flexible polyvinylidene fluoride nano-fiber material, which is prepared by taking a two-dimensional hexagonal boron nitride nanosheet as a filler through an electrostatic spinning method, wherein the preparation method of the polyvinylidene fluoride nano-fiber material comprises the following steps:
mixing N, N-dimethylformamide and acetone according to a mass ratio of 6:4, uniformly mixing to prepare a mixed solution;
adding a two-dimensional hexagonal boron nitride nanosheet in an amount of 0.2-0.8wt.% based on the mass of the mixed solution into the mixed solution, and performing ultrasonic dispersion for 2 hours;
continuously adding 10wt.% of polyvinylidene fluoride powder in the mass ratio of the mixed solution, and heating in an oil bath at 60 ℃ and stirring for dissolving;
and after the added polyvinylidene fluoride is completely dissolved, carrying out electrostatic spinning to prepare the polyvinylidene fluoride nano-fiber material.
According to a preferred embodiment, the preparation method further comprises:
after the electrostatic spinning is finished, the prepared polyvinylidene fluoride nano-fiber material is placed in an oven to be dried for 6 hours at the temperature of 120 ℃ to remove the solvent.
According to a preferred embodiment, the preparation method further comprises:
and in the electrostatic spinning process, collecting the nanofibers by using a roller collecting device covered by an aluminum foil, and after the electrostatic spinning is finished, taking down the aluminum foil to obtain the polyvinylidene fluoride nanofiber material.
According to a preferred embodiment, the electrospinning preparation parameters are as follows: the method adopts 21G needle spinning single-needle single-solution spinning, the distance between a needle and a roller collecting device is 17cm, the solution flow rate is 1ml/h, the voltage is 21kV, the roller speed is 1500rpm, the temperature is room temperature, and the spinning time is 2 hours and 10 minutes.
According to a preferred embodiment, the two-dimensional hexagonal boron nitride nanosheets are added in an amount of 0.5wt.% based on the mass of the mixed solution.
Based on the technical scheme, the reinforced flexible polyvinylidene fluoride nanofiber material disclosed by the invention at least has the following technical effects:
the enhanced flexible polyvinylidene fluoride nano-fiber material prepared by the electrostatic spinning method has the characteristics of convenient preparation process and simple equipment. Van der Waals force exists between the interfaces of the two-dimensional hexagonal boron nitride nanosheets and the polyvinylidene fluoride nanofibers, when the polyvinylidene fluoride nanofibers are subjected to external force, external load can be transmitted to the internal two-dimensional hexagonal boron nitride, the electromechanical conversion capacity of the polyvinylidene fluoride nanofibers can be promoted due to the excellent piezoelectric property of the two-dimensional hexagonal boron nitride, and therefore the output performance can be correspondingly improved. The polyvinylidene fluoride nanofiber material takes the two-dimensional hexagonal boron nitride nanosheets as the filler, the two-dimensional hexagonal boron nitride nanosheets have strong piezoelectric performance, and the two-dimensional hexagonal boron nitride nanosheets can effectively enhance the overall piezoelectric performance of the material as the nanofiller, so that the electromechanical conversion capacity can be promoted when external force is added, and the output performance of the friction nano-generator is improved. The two-dimensional hexagonal boron nitride nanosheet is non-toxic and has excellent chemical inertness, and the material comprises strong oxidation resistance, can be used for preparing an environment-friendly negative friction layer material, and can be widely applied to a friction nano-generator.
The invention also provides a friction nano generator which comprises a friction positive electricity layer, a first metal electrode, a first supporting structure, a friction negative electricity layer, a second metal electrode, a second supporting structure and a PET film, wherein the friction negative electricity layer is made of the polyvinylidene fluoride nano fiber material, the friction positive electricity layer is made of nylon-11 nano fiber,
the PET film comprises a first metal electrode, a friction positive layer, a friction negative layer, a second metal electrode, a friction negative layer, a PET film and a PET film, wherein the friction positive layer is covered on the first metal electrode, one side of the first metal electrode, which is far away from the friction positive layer, is pasted on a first supporting structure, the friction negative layer is covered on a second metal electrode, one side of the second metal electrode, which is far away from the friction negative layer, is pasted on a second supporting structure, the friction negative layer and the friction positive layer are oppositely arranged face to face, and the PET film is respectively pasted on the side surfaces of the oppositely arranged first supporting structure and the second supporting structure.
According to a preferred embodiment, the PET film is in an arc structure, and the length of the PET film ensures that the gap between the positive friction layer and the negative friction layer is 1cm.
According to a preferred embodiment, the preparation method of the nylon-11 nanofiber comprises the following steps:
adding 10wt.% of nylon-11 particles into 10g of hexafluoroisopropanol, and dissolving under magnetic stirring to prepare a solution; then electrostatic spinning is carried out to prepare the nylon-11 nano fiber.
According to a preferred embodiment, the first metal electrode and the second metal electrode are both aluminum foils, and both the first metal electrode and the second metal electrode are adhered with conducting wires for connecting an external circuit.
According to a preferred embodiment, the thickness of the PET film is between 0.5 and 2mm.
Based on the technical scheme, the friction nano generator at least has the following technical effects:
the friction nano-generator is obviously improved in output performance by taking flexible polyvinylidene fluoride nano-fibers enhanced by two-dimensional hexagonal boron nitride nano-sheets as a friction negative electric layer and taking nylon-11 NFs as a friction positive electric layer, and is tested to be 3.13W/m in power density 2 Compared with the friction nanometer generator without any piezoelectric filler in the prior art, the friction nanometer generator has the advantages that the open-circuit voltage is improved by 350%, the short-circuit current is improved by 404%, and the transfer charge quantity is improved by 466%. Is the highest record of the current nanometer generator based on the piezoelectricity enhanced polyvinylidene fluoride nanometer fiberAnd (5) recording the value. And the triboelectric nanogenerators of the present application are easily integrated into flexible electronics, such as human-based wearable applications.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 (a) is an X-ray diffraction spectrum spectrogram of polyvinylidene fluoride nanofibers (hBNNSs-PVDFNFs) prepared under different mass ratios of two-dimensional hexagonal boron nitride nanosheets; (b) Is a flexible display of reinforced polyvinylidene fluoride nanofibers and nylon-11 nanofibers;
fig. 2 is (a) open circuit voltage, (b) short circuit current, (c) transferred charge, (d) power density of tribo-nanogenerators based on polyvinylidene fluoride nanofibers (PVDFNF) prepared at different two-dimensional hexagonal boron nitride nanosheet mass ratios.
Fig. 3 is a schematic structural diagram of a triboelectric nanogenerator based on two-dimensional hexagonal boron nitride nanosheet polyvinylidene fluoride nanofibers (hbnss-PVDF) of the present invention.
Fig. 4 is (a) a flexible sensor and (b) a wearable application of a triboelectric nanogenerator based on polyvinylidene fluoride Polynanofibers (PVDFNF) prepared from 0.5wt.% two-dimensional hexagonal boron nitride nanosheets.
In the figure: 1-triboelectric positive layer; 2-a first metal electrode; 3-a first support structure; 4-rubbing the negative electric layer; 5-a second metal electrode; 6-a second support structure; 7-PET film.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the technical solutions of the present invention will be described in detail below. It should be apparent that the described embodiments are only some embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the examples given herein without any inventive step, are within the scope of the present invention.
Example 1
The embodiment 1 provides a reinforced flexible polyvinylidene fluoride nanofiber material, and the specific preparation process is as follows:
(1) 6g of N, N-Dimethylformamide (DMF) and 4g of acetone were mixed to obtain a mixed solution;
(2) Adding 0.027g (0.2 wt.%) of two-dimensional hexagonal boron nitride nanosheet to the mixed solution, and ultrasonically dispersing for 2 hours;
(3) Continuously adding 10wt.% polyvinylidene fluoride (PVDF) powder, and stirring the mixture under the heating of an oil bath at 60 ℃ until the solution is uniform;
(4) And (3) carrying out electrostatic spinning on the prepared solution by using an electrostatic spinning machine:
10ml of the solution was drawn by a disposable syringe at a flow rate of 1ml/h, and an aluminum foil wound around a drum at 1500rpm for collecting nanofibers was attached to a drum collecting device at a receiving distance of 17cm, a voltage of 21kv, a relative humidity of 40 ± 5%, and an electrospinning time of 2 hours and 10 minutes.
(5) After the electrostatic spinning is finished, the nanofibers collected on the aluminum foil are taken down together with the aluminum foil and are transferred into a drying oven at the temperature of 120 ℃ for drying for 6 hours, the reinforced flexible polyvinylidene fluoride nanofiber material can be obtained, and the nanofiber membrane is deposited on the aluminum foil.
This example also provides a preparation method of nylon-11 nanofibers, which comprises the following steps:
(1) 10wt.% nylon-11 particles were added to 10g hexafluoroisopropanol and magnetically stirred for 2 hours to prepare a 10wt.% solution;
(2) The prepared solution was electrospun using an electrospinning machine, comprising:
10ml of the solution was drawn by a disposable syringe at a flow rate of 1ml/h, and an aluminum foil wound around a drum at 1500rpm for collecting nanofibers was attached to a drum collecting device at a receiving distance of 17cm, a voltage of 21kv, a relative humidity of 40 ± 5%, and an electrospinning time of 2 hours and 10 minutes.
(3) And after the electrostatic spinning is finished, taking down the nanofibers collected on the aluminum foil together with the aluminum foil to obtain the flexible nylon-11 nanofiber material, wherein the nanofiber membrane is deposited on the aluminum foil.
Application example one:
in the present application example, polyvinylidene fluoride nanofibers of 0.2wt.% hexagonal boron nitride nanosheets prepared in example 1 are used as a material of a negative friction layer, and nylon-11 nanofiber material is used as a material of a positive friction layer to prepare a friction nanogenerator, and the specific process thereof comprises the following steps:
step 1, cutting the reinforced polyvinylidene fluoride nanofiber negative electrode layer material prepared in the above example 1 into 4 × 4cm 2 The aluminum foil is used as an electrode of a negative electrode layer material; the enameled wire is used as a lead and is pasted on an aluminum foil and connected to an external circuit;
step 2, cutting the acrylic plate into 4 multiplied by 4cm 2 The square shape is used as a supporting material of the friction nano generator, and the material in the step 1 is attached to one side of an acrylic plate;
step 3, cutting the nylon-11 nano-fiber electropositive layer material into 4 multiplied by 4cm 2 An electrode which takes aluminum foil as a positive electrode layer material; the enameled wire is used as a lead and is pasted on an aluminum foil and connected to an external circuit;
step 4, cutting the acrylic plate into 4 multiplied by 4cm 2 The square is used as a supporting material of the friction nano generator, and the material in the step 3 is attached to one side of a square acrylic plate; adjusting the positions of the positive electric layer and the negative electric layer to enable the positive electric layer and the negative electric layer to be placed face to face;
step 5, taking a rectangle 4 multiplied by 12cm with the thickness of 1.5mm 2 The PET film is attached to the back surface of the acrylic plate with the positive electric layer and the negative electric layer and is used as a separation and contact material for assisting the positive electric layer and the negative electric layer;
and 6, adjusting the length of the PET film to enable the gap between the friction positive/negative electric layers to be 1cm.
Experimental tests have shown that the open-circuit voltage and the short-circuit current of the triboelectric nanogenerator with polyvinylidene fluoride nanofibers of two-dimensional hexagonal boron nitride nanosheets prepared according to application example one correspond to 0.2wt.% in the graph, as shown by the curves in fig. 2 (a-c). The open circuit voltage of the friction nanogenerator prepared from 0.2wt.% of polyvinylidene fluoride nano-fibers of two-dimensional hexagonal boron nitride nanosheets was 180V, the short circuit current was 8.4 μ a, and the transfer charge amount was 66nC.
Example 2
The embodiment 2 provides a reinforced flexible polyvinylidene fluoride nanofiber material, and the specific preparation process is as follows:
(1) 6g of N, N-Dimethylformamide (DMF) and 4g of acetone were mixed to obtain a mixed solution;
(2) Adding 0.036g (0.3 wt.%) of two-dimensional hexagonal boron nitride nanosheets to the mixed solution, and ultrasonically dispersing for 2 hours;
(3) Continuously adding 10wt.% polyvinylidene fluoride (PVDF) powder, and stirring the mixture under the heating of an oil bath at 60 ℃ until the solution is uniform;
(4) And (3) carrying out electrostatic spinning on the prepared solution by using an electrostatic spinning machine:
10ml of the solution was taken out of a disposable syringe with a flow rate of 1ml/h, and an aluminum foil wound around a drum for collecting nanofibers was attached to a drum collecting device with a speed of 1500rpm, a take-up distance of 17cm, a voltage of 21kV, a relative humidity of 40. + -. 5%, and an electrospinning time of 2 hours and 10 minutes.
(5) After the electrostatic spinning is finished, the nanofibers collected on the aluminum foil are taken down together with the aluminum foil and are transferred into a drying oven at the temperature of 120 ℃ for drying for 6 hours, the reinforced flexible polyvinylidene fluoride nanofiber material can be obtained, and the nanofiber membrane is deposited on the aluminum foil.
This example 2 further provides a preparation method of nylon-11 nanofibers, which comprises the following steps:
(1) 10wt.% nylon-11 particles were added to 10g hexafluoroisopropanol and magnetically stirred for 2 hours to prepare a 10wt.% solution;
(2) And (3) carrying out electrostatic spinning on the prepared solution by using an electrostatic spinning machine:
10ml of the solution was taken out of a disposable syringe with a flow rate of 1ml/h, and an aluminum foil wound around a drum for collecting nanofibers was attached to a drum collecting device with a speed of 1500rpm, a take-up distance of 17cm, a voltage of 21kV, a relative humidity of 40. + -. 5%, and an electrospinning time of 2 hours and 10 minutes.
(3) And after the electrostatic spinning is finished, taking down the nanofibers collected on the aluminum foil together with the aluminum foil to obtain the flexible nylon-11 nanofiber material, wherein the nanofiber membrane is deposited on the aluminum foil.
Application example two:
in the present application example, polyvinylidene fluoride nanofibers of 0.3wt.% hexagonal boron nitride nanosheets prepared in example 2 were used as a material of a negative friction layer, and nylon-11 nanofiber material was used as a material of a positive friction layer to prepare a friction nanogenerator, and the specific process thereof includes the following steps:
step 1, cutting the enhanced polyvinylidene fluoride nano-fiber negative electrode layer material into 4 x 4cm 2 The aluminum foil is used as an electrode of a negative electrode layer material; the enameled wire is used as a lead and is stuck to the aluminum foil by a copper adhesive tape and connected to an external circuit;
step 2, cutting the acrylic plate into 4 multiplied by 4cm 2 The square shape is used as a supporting material of the friction nano generator, and the material in the step 1 is attached to one side of an acrylic plate;
step 3, cutting the nylon-11 nano-fiber electropositive layer material into 4 multiplied by 4cm 2 An electrode which takes aluminum foil as a positive electrode layer material; the enameled wire is used as a lead and is pasted on an aluminum foil and connected to an external circuit;
step 4, cutting the acrylic plate into 4 multiplied by 4cm 2 The square is used as a supporting material of the friction nano generator, and the material in the step 3 is attached to one side of a square acrylic plate; adjusting the positions of the positive electric layer and the negative electric layer to enable the positive electric layer and the negative electric layer to be placed face to face;
step 5, taking a rectangle 4 multiplied by 12cm with the thickness of 1.5mm 2 The PET film is attached to the back surface of the acrylic plate with the positive electric layer and the negative electric layer and is used as a separation and contact material for assisting the positive electric layer and the negative electric layer;
and 6, adjusting the length of the PET film to enable the gap between the friction positive/negative electric layers to be 1cm.
Experimental tests show that the open-circuit voltage and the short-circuit current of the friction nanogenerator of the polyvinylidene fluoride nanofiber prepared according to the two-dimensional hexagonal boron nitride nanosheet of application example two correspond to 0.3wt.% in the graph, as shown by the curves in fig. 2 (a-c). The open circuit voltage of the friction nanogenerator prepared from 0.3wt.% of polyvinylidene fluoride nano-fibers of two-dimensional hexagonal boron nitride nanosheets was 221V, the short circuit current was 11.5 μ a, and the transfer charge amount was 83nC.
Example 3
The embodiment 3 provides a reinforced flexible polyvinylidene fluoride nanofiber material, which is prepared by the following specific steps:
(1) 6g of N, N-Dimethylformamide (DMF) and 4g of acetone were mixed to obtain a mixed solution;
(2) Adding 0.055g (0.5 wt.%) of two-dimensional hexagonal boron nitride nanosheets to the mixed solution, and ultrasonically dispersing for 2 hours;
(3) Continuously adding 10wt.% polyvinylidene fluoride (PVDF) powder, and stirring the mixture under the heating of an oil bath at 60 ℃ until the solution is uniform;
(4) And (3) carrying out electrostatic spinning on the prepared solution by using an electrostatic spinning machine:
10ml of the solution was drawn by a disposable syringe at a flow rate of 1ml/h, and an aluminum foil wound around a drum at 1500rpm was attached to a drum collecting device for collecting nanofibers at a receiving distance of 17cm, a voltage of 21kv, a relative humidity of 40 ± 5%, and an electrospinning time of 2 hours and 10 minutes.
(5) After the electrostatic spinning is finished, the nanofibers collected on the aluminum foil are taken down together with the aluminum foil and are transferred into a drying oven at the temperature of 120 ℃ for drying for 6 hours, the reinforced flexible polyvinylidene fluoride nanofiber material can be obtained, and the nanofiber membrane is deposited on the aluminum foil.
This example 3 further provides a preparation method of nylon-11 nanofibers, which comprises the following steps:
(1) 10wt.% nylon-11 particles were added to 10g hexafluoroisopropanol and magnetically stirred for 2 hours to prepare a 10wt.% solution;
(2) And (3) carrying out electrostatic spinning on the prepared solution by using an electrostatic spinning machine:
10ml of solution is extracted by a disposable syringe, the flow rate is set to be 1ml/h, aluminum foil which is wound around a roller for one circle is attached to a roller collecting device and is used for collecting the nano fibers, the speed of the roller is set to be 1500rpm, the receiving distance is 17cm, the voltage is 21kV, the relative humidity is 40 +/-5%, and the electrostatic spinning time is set to be 2 hours and 10 minutes.
(3) And after the electrostatic spinning is finished, taking down the nanofibers collected on the aluminum foil together with the aluminum foil to obtain the flexible nylon-11 nanofiber material, wherein the nanofiber membrane is deposited on the aluminum foil.
Application example three:
in the present application example, polyvinylidene fluoride nanofibers of 0.5wt.% hexagonal boron nitride nanosheets prepared in example 3 were used as a material of a negative friction layer, and nylon-11 nanofiber material was used as a material of a positive friction layer to prepare a friction nanogenerator, and the specific process thereof includes the following steps:
step 1, cutting the reinforced polyvinylidene fluoride nano-fiber negative electrode layer material into 4 multiplied by 4cm 2 The aluminum foil is used as an electrode of a negative electrode layer material; the enameled wire is used as a lead and is pasted on an aluminum foil and connected to an external circuit;
step 2, cutting the acrylic plate into 4 multiplied by 4cm 2 The square shape is used as a supporting material of the friction nano generator, and the material in the step 1 is attached to one side of an acrylic plate;
step 3, cutting the nylon-11 nano-fiber positive electricity layer material into 4 multiplied by 4cm 2 Taking aluminum foil as an electrode of a positive electrode material; the enameled wire is used as a lead and is pasted on an aluminum foil and connected to an external circuit;
step 4, cutting the acrylic plate into 4 multiplied by 4cm 2 The square is used as a supporting material of the friction nano generator, and the material in the step 3 is attached to one side of a square acrylic plate; adjusting the positions of the positive electric layer and the negative electric layer to enable the positive electric layer and the negative electric layer to be placed face to face;
step 5, taking a rectangle 4 multiplied by 12cm with the thickness of 1.5mm 2 PET film, laminated on acrylic sheet having positive and negative electric layersOn the reverse side, it is used as the separation and contact material of the auxiliary positive layer and negative layer;
and 6, adjusting the length of the PET film to enable the gap between the friction positive/negative electric layers to be 1cm.
Through experimental tests, the open-circuit voltage, the short-circuit current, the transfer charge and the power density of the friction nano-generator of the polyvinylidene fluoride nano-fiber of the two-dimensional hexagonal boron nitride nanosheet prepared according to application example three correspond to 0.5wt.% in the figure and respectively correspond to curves in fig. 2 (a-d). The open-circuit voltage of the friction nano-generator prepared by using 0.5wt.% of polyvinylidene fluoride nano-fibers of two-dimensional hexagonal boron nitride nanosheets is 500V, the short-circuit current is 25.2 muA, the transferred charge amount is 183nC, and the output power reaches 3.13W/m 2 。
Example 4
The embodiment 4 provides a reinforced flexible polyvinylidene fluoride nanofiber material, which is prepared by the following specific steps:
(1) 6g of N, N-Dimethylformamide (DMF) and 4g of acetone were mixed to obtain a mixed solution;
(2) Adding 0.089g (0.8 wt.%) of two-dimensional hexagonal boron nitride nanosheet to the mixed solution, and ultrasonically dispersing for 2 hours;
(3) Continuously adding 10wt.% polyvinylidene fluoride (PVDF) powder, and stirring the mixture under the heating of an oil bath at 60 ℃ until the solution is uniform;
(4) And (3) carrying out electrostatic spinning on the prepared solution by using an electrostatic spinning machine:
10ml of the solution was taken out of a disposable syringe with a flow rate of 1ml/h, and an aluminum foil wound around a drum for collecting nanofibers was attached to a drum collecting device with a speed of 1500rpm, a take-up distance of 17cm, a voltage of 21kV, a relative humidity of 40. + -. 5%, and an electrospinning time of 2 hours and 10 minutes.
(5) After the electrostatic spinning is finished, the nanofibers collected on the aluminum foil are taken down together with the aluminum foil and are transferred into a drying oven at the temperature of 120 ℃ for drying for 6 hours, the reinforced flexible polyvinylidene fluoride nanofiber material can be obtained, and the nanofiber membrane is deposited on the aluminum foil.
This example 4 further provides a preparation method of nylon-11 nanofibers, which comprises the following steps:
(1) 10wt.% nylon-11 particles were added to 10g hexafluoroisopropanol and magnetically stirred for 2 hours to prepare a 10wt.% solution;
(2) And (3) carrying out electrostatic spinning on the prepared solution by using an electrostatic spinning machine:
10ml of solution is extracted by a disposable syringe, the flow rate is set to be 1ml/h, aluminum foil which is wound around a roller for one circle is attached to a roller collecting device and is used for collecting the nano fibers, the speed of the roller is set to be 1500rpm, the receiving distance is 17cm, the voltage is 21kV, the relative humidity is 40 +/-5%, and the electrostatic spinning time is set to be 2 hours and 10 minutes.
(3) And after the electrostatic spinning is finished, taking down the nanofibers collected on the aluminum foil together with the aluminum foil to obtain the flexible nylon-11 nanofiber material, wherein the nanofiber membrane is deposited on the aluminum foil.
Application example four:
in the present application example, polyvinylidene fluoride nanofibers of 0.8wt.% hexagonal boron nitride nanosheets prepared in example four were used as a material of a negative friction layer, and nylon-11 nanofiber material was used as a material of a positive friction layer to prepare a friction nanogenerator, and the specific process thereof includes the following steps:
step 1, cutting the enhanced polyvinylidene fluoride nano-fiber negative electrode layer material into 4 x 4cm 2 Taking aluminum foil as an electrode of a negative electrode layer material; the enameled wire is used as a lead and is pasted on an aluminum foil and connected to an external circuit;
step 2, cutting the acrylic plate into 4 multiplied by 4cm 2 The square shape is used as a supporting material of the friction nano generator, and the material in the step 1 is attached to one side of an acrylic plate;
step 3, cutting the nylon-11 nano-fiber positive electricity layer material into 4 multiplied by 4cm 2 An electrode which takes aluminum foil as a positive electrode layer material; the enameled wire is used as a lead and is stuck to the aluminum foil by a copper adhesive tape and connected to an external circuit;
step 4, cutting the acrylic plate into 4 multiplied by 4cm 2 The square is used as the supporting material of the friction nanometer generator, and the material in the step 3 is pasted on the squareOne side of the gram force plate; adjusting the positions of the positive electric layer and the negative electric layer to enable the positive electric layer and the negative electric layer to be placed face to face;
step 5, taking a rectangle 4 multiplied by 12cm with the thickness of 1.5mm 2 The PET film is attached to the reverse side of the acrylic plate with the positive electric layer and the negative electric layer and is used as a separation and contact material for assisting the positive electric layer and the negative electric layer;
and 6, adjusting the length of the PET film to enable the gap between the friction positive/negative electric layers to be 1cm.
Through experimental tests, the open-circuit voltage and the short-circuit current of the friction nano-generator of the polyvinylidene fluoride nano-fiber of the two-dimensional hexagonal boron nitride nanosheet prepared according to application example four correspond to 0.8wt.% in the graph and are respectively shown in the curves in fig. 2 (a-c). The open circuit voltage of the triboelectric nanogenerator prepared from 0.8wt.% of polyvinylidene fluoride nanofibers of two-dimensional hexagonal boron nitride nanosheets was 372V, the short circuit current was 20.6 μ a, and the amount of transferred charge was 165nC.
As shown in fig. 1, fig. 1 (a) shows XRD spectra of PVDFNFs for different wt.% hBNNSs, with the peak at 20.4 ° corresponding to the β -phase (110) of the PVDFNFs, and the two peaks at 26.6 ° (002) and 41.6 ° corresponding to hBNNSs. Illustrating the successful introduction of hBNNSs into PVDF nanofibers, since the piezoelectric response is generated at (110) and (002), hBNNSs and PVDF with piezoelectric properties are known to improve the overall piezoelectric performance.
Example 5
As shown in fig. 3, fig. 3 shows a structural schematic diagram of the triboelectric nanogenerator based on two-dimensional hexagonal boron nitride nanosheet polyvinylidene fluoride nanofibers according to the present invention. The embodiment provides a triboelectric nanogenerator, which comprises a triboelectric positive layer 1, a first metal electrode 2, a first support structure 3, a triboelectric negative layer 4, a second metal electrode 5, a second support structure 6 and a PET film 7.
Wherein, the negative friction layer 4 is the polyvinylidene fluoride nanofiber material prepared in the examples 1 to 4, and the positive friction layer 1 is the nylon-11 nanofiber prepared in the examples 1 to 4.
The friction positive electricity layer 1 covers the first metal electrode 2, the first metal electrode 2 is an aluminum foil, and one side of the first metal electrode 2, which is far away from the friction positive electricity layer 1, is attached to the first support structure 3. First bearing structure 3 is the ya keli board, and the negative electricity layer of friction 4 covers on second metal electrode 5, and second metal electrode 5 deviates from one side subsides of the negative electricity layer of friction on second bearing structure 6, and negative electricity layer of friction 4 sets up with the positive electricity layer of friction 1 is relative face-to-face, has pasted PET film 7 respectively in the side of relative first bearing structure 3 that sets up and second bearing structure 6. For assisting in separating the contacts. The PET film 7 is of an arc-shaped structure, the thickness of the PET film is 0.5-2mm, and the length of the PET film 7 ensures that the gap between the positive friction layer 1 and the negative friction layer 4 is 1cm. Preferably, the first metal electrode 2 and the second metal electrode 5 are both adhered with wires through copper tapes to connect with an external circuit. The wire may be an enameled wire.
As shown in fig. 4, fig. 4 illustrates (a) flexible sensors and (b) wearable applications of the triboelectric nanogenerator of example 3 based on polyvinylidene fluoride Polynanofibers (PVDFNF) prepared from 0.5wt.% two-dimensional hexagonal boron nitride nanoplates. As can be seen from fig. 4, the triboelectric nanogenerator prepared by the present application exhibits excellent flexibility when applied to a flexible sensor. As shown in fig. 4 (b), when the knee flexion angle is increased from 30 ° to 90 °, the open circuit voltage rises from 1.8V to 2.4V. The results show that the friction nano-generator based on the reinforced polyvinylidene fluoride nano-fiber has huge potential in practical application. The negative electrical layer made of hBNNSs-PVDFNFs prepared according to the invention was assembled with the positive electrical layer made of nylon-11 NFs to obtain TENG, showing excellent flexibility due to the all-fiber layer. The flexible TENG can be applied to power supplies and flexible wearable sensors for real-time human motion monitoring.
The above description is only for the specific embodiments of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art can easily conceive of the changes or substitutions within the technical scope of the present invention, and all the changes or substitutions should be covered within the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the appended claims.

Claims (10)

1. The reinforced flexible polyvinylidene fluoride nanofiber material is characterized in that the polyvinylidene fluoride nanofiber material is prepared by taking a two-dimensional hexagonal boron nitride nanosheet as a filler through an electrostatic spinning method, and the preparation method of the polyvinylidene fluoride nanofiber material comprises the following steps:
mixing N, N-dimethylformamide and acetone according to a mass ratio of 6:4, uniformly mixing to prepare a mixed solution;
adding a two-dimensional hexagonal boron nitride nanosheet in an amount of 0.2-0.8wt.% based on the mass of the mixed solution into the mixed solution, and performing ultrasonic dispersion for 2 hours;
continuously adding 10wt.% of polyvinylidene fluoride powder in the mass ratio of the mixed solution, and heating in an oil bath at 60 ℃ and stirring for dissolving;
and after the added polyvinylidene fluoride is completely dissolved, carrying out electrostatic spinning to prepare the polyvinylidene fluoride nano-fiber material.
2. The polyvinylidene fluoride nanofiber material of claim 1, wherein the preparation method further comprises:
after the electrostatic spinning is finished, the prepared polyvinylidene fluoride nanofiber material is placed in an oven to be dried for 6 hours at the temperature of 120 ℃ to remove the solvent.
3. The polyvinylidene fluoride nanofiber material of claim 1, wherein the preparation method further comprises:
and in the electrostatic spinning process, collecting the nanofibers by using a roller collecting device covered by an aluminum foil, and after the electrostatic spinning is finished, taking down the aluminum foil to obtain the polyvinylidene fluoride nanofiber material.
4. The polyvinylidene fluoride nanofiber material of claim 1, wherein the electrospinning preparation parameters are as follows: the method adopts 21G needle spinning single-needle single-solution spinning, the distance between a needle and a roller collecting device is 17cm, the solution flow rate is 1ml/h, the voltage is 21kV, the roller speed is 1500rpm, the temperature is room temperature, and the spinning time is 2 hours and 10 minutes.
5. The polyvinylidene fluoride nanofiber material of claim 1, wherein the two-dimensional hexagonal boron nitride nanosheets are added in an amount of 0.5wt.% based on the mass of the mixed solution.
6. Triboelectric nanogenerator, comprising a triboelectric positive layer (1), a first metal electrode (2), a first support structure (3), a triboelectric negative layer (4), a second metal electrode (5), a second support structure (6) and a PET film (7), wherein the triboelectric negative layer (4) is a polyvinylidene fluoride nanofiber material according to any of claims 1 to 5, the triboelectric positive layer (1) is nylon-11 nanofiber,
the friction positive electricity layer (1) is covered on a first metal electrode (2), one side of the first metal electrode (2) departing from the friction positive electricity layer (1) is attached to a first supporting structure (3), the friction negative electricity layer (4) is covered on a second metal electrode (5), one side of the second metal electrode (5) departing from the friction negative electricity layer is attached to a second supporting structure (6), the friction negative electricity layer (4) and the friction positive electricity layer (1) are oppositely arranged face to face, and PET thin films (7) are respectively attached to the side faces of the first supporting structure (3) and the second supporting structure (6) which are oppositely arranged.
7. Tribo nanogenerator according to claim 6, characterized in that the PET film (7) is in an arc-shaped structure and the length of the PET film (7) ensures a gap of 1cm between the tribo-positive layer (1) and the tribo-negative layer (4).
8. The triboelectric nanogenerator according to claim 6, wherein the preparation method of the nylon-11 nanofibers comprises:
adding 10wt.% of nylon-11 particles into 10g of hexafluoroisopropanol, and dissolving under magnetic stirring to prepare a solution; then electrostatic spinning is carried out to prepare the nylon-11 nano fiber.
9. The triboelectric nanogenerator according to claim 6, wherein the first metal electrode (2) and the second metal electrode (5) are both aluminum foils, and wires are adhered to the first metal electrode (2) and the second metal electrode (5) to connect to an external circuit.
10. The triboelectric nanogenerator according to claim 6, wherein the thickness of the PET film is 0.5-2mm.
CN202211288188.5A 2022-10-20 2022-10-20 Enhanced flexible polyvinylidene fluoride nanofiber material and friction nano generator Pending CN115491815A (en)

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