CN114960027A - Preparation method of polyvinylidene fluoride piezoelectric nanofiber membrane with branched piezoelectric reinforced nanostructure - Google Patents
Preparation method of polyvinylidene fluoride piezoelectric nanofiber membrane with branched piezoelectric reinforced nanostructure Download PDFInfo
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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
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- D04H1/4318—Fluorine series
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- 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
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- 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
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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
- D04H1/70—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
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Abstract
The invention relates to a preparation method of a polyvinylidene fluoride piezoelectric nanofiber membrane with a branched piezoelectric reinforced nano structure, wherein the piezoelectric nanofiber membrane is obtained by adding organic branched salt into a PVDF spinning solution for electrostatic spinning, and the preparation method is characterized by comprising the following steps: 1) preparing spinning solution, 2) electrostatic spinning. And preparing the polyvinylidene fluoride piezoelectric nanofiber membrane with the branched piezoelectric reinforced nanostructure. The piezoelectric nanofiber membrane prepared by the method has high beta phase content, so that the piezoelectric nanofiber membrane has excellent piezoelectric response performance and has wide application prospects in the fields of energy collection, flexible sensors, intelligent wearable equipment and the like.
Description
Technical Field
The invention relates to the technical field of a preparation method of a nanofiber membrane with a piezoelectric effect, in particular to a polyvinylidene fluoride piezoelectric nanofiber membrane with a branched piezoelectric reinforced nanostructure prepared by an electrostatic spinning technology, and belongs to the technical field of functional polymer fibers.
Background
The intelligent wearable device is based on the Internet of things and has the characteristics of miniaturization, rich functionalization and the like. This puts requirements on the flexibility, integration and ease of maintenance of the energy supply unit. The flexible piezoelectric nano generator can convert mechanical energy with low power density into electric energy, a self-powered power supply unit is constructed in various environments, and development of intelligent wearable equipment is widened.
Polyvinylidene fluoride (PVDF) is a semi-crystalline polymer with piezoelectric effect and can exhibit five different crystalline forms, α, β, γ, δ and ∈. The piezoelectric effect of PVDF is attributed to the presence of the beta crystal form of the trans-TTTT helical structure, in which two fluorine atoms are simultaneously bonded to one carbon atom and the C-F bond has a strong polarity, resulting in a large dipole moment of the PVDF monomer, which gives PVDF a strong piezoelectric property. The gamma phase with TTTGTTTG' conformation is the intermediate polar phase of PVDF, which also contributes significantly to the improvement of piezoelectric performance. In addition, PVDF has the characteristics of good flexibility, small volume, light weight, good processability and the like, and can be processed into a complex shape according to requirements, so that the PVDF is suitable for various applications such as high-precision instruments and the like.
Due to the major contribution of the polar phases (β, γ -phase) to the piezoelectric effect of PVDF, researchers have conducted a great deal of research and research on how to increase the content of the polar phase in PVDF. The main means are high pressure, thermal annealing, mechanical stretching, electric field polarization, and doping of nano-filler. The incorporation of nanofillers is the most common and effective means compared to the stringent conditions of other methods. Currently, the nanofillers that have been demonstrated to improve the piezoelectric properties of PVDF are rich in species, including metallic monomers or ions, carbonaceous materials, piezoelectric ceramic particles, nano-metal oxides, composite nanoparticles, and the like. Among these, some nanofillers containing surface charges, such as quaternary ammonium ion salts, interact with the PVDF dipole, promoting the beta phase content in the PVDF.
The electrospinning technique has the advantages of simple operation and low cost, and can be used for aligning molecular dipole- (CH) along the direction of applied voltage 2 -CF 2 ) Production of PVDF nanofibers with high beta phase content. In the spinning process, PVDF jet flow is drafted and split, and is mechanically stretched and electrically polarized, so that the PVDF jet flow has piezoelectricity, redundant steps of secondary polarization are avoided, and the PVDF jet flow plays a remarkable role in improving the piezoelectric performance of a nano composite material-based nano generator. Therefore, the electrospinning technology has become the first technology for developing the piezoelectricity of the PVDF material. The effective stretching of the jet is the most common cause of the crystallographic transformation of PVDF, as compared to electrical polarization, and is also the key mechanism for the formation of polarized beta crystals. The invention discloses a preparation method of a PVDF piezoelectric nanofiber membrane with a branched piezoelectric enhanced nano structure. The nanofiber membrane prepared by the method splits a large number of branched fibers with the diameter of 5-100nm, has high beta-phase content, and has excellent piezoelectric response performance. The following is a detailed summary of the invention.
Disclosure of Invention
The invention relates to a preparation method of a polyvinylidene fluoride piezoelectric nanofiber membrane with a branched piezoelectric reinforced nanostructure. The PVDF piezoelectric nanofiber membrane prepared by the invention has wide application prospect in the field of intelligent wearable equipment.
The invention relates to a preparation method of a polyvinylidene fluoride piezoelectric nanofiber membrane with a branched piezoelectric reinforced nanostructure, which is characterized by comprising the following steps of:
(1) preparing a spinning solution: adding a certain amount of polyvinylidene fluoride (PVDF) powder into a composite solvent of N, N-Dimethylformamide (DMF) and acetone, and stirring at 40-50 ℃ to completely dissolve the PVDF powder to prepare a PVDF solution with the concentration of 17-19%; and then adding a certain amount of organic branched salt into the solution, and continuously stirring until the organic branched salt is completely dissolved, wherein the organic branched salt accounts for 0.5-3.5% of the spinning solution by mass percent.
(2) Electrostatic spinning: and (3) spinning the spinning solution in the previous step by adopting an electrostatic spinning method, wherein the spinning voltage is 20-30 kV, the receiving distance is 10-15 cm, and the liquid supply rate is 0.3-0.7 mL/h, so as to prepare the polyvinylidene fluoride piezoelectric nanofiber membrane with the branched piezoelectric enhanced nano structure.
The organic branched salt is any one of tetrabutylammonium hexafluorophosphate, tetrabutylammonium chloride, tetrabutylammonium bromide and tetrapropylammonium chloride, and the molecular weight is 200-400.
According to the technical scheme, the PVDF piezoelectric nanofiber membrane with the branched piezoelectric reinforced nanostructure is prepared by adopting an electrostatic spinning method, and the addition of the organic branched salt is a key factor for forming the piezoelectric reinforced nanostructure. The structure of the organic branched salt has relatively longer alkane chains, so that the conductivity of the spinning solution can be increased, and PVDF polymer jet flow is split under the action of a high-voltage electric field to form rich branched structure fibers with the diameters of 5-80 nm. Under the action of strong mechanical tension, beta-phase nucleation and conversion from non-polar phase to polar phase are promoted.
The organic branched salt may also function as a nucleating agent in the present invention, providing conditions for the formation of the beta phase. In addition, the positive charge on the surface of the organic branched salt will react with the CF of PVDF 2 The interaction between the two molecules limits the twisting of PVDF molecular chains to align the PVDF molecular chains, and increases the content of beta phase.
Drawings
FIG. 1 is an electron microscope picture of the morphology of a PVDF nanofiber membrane with branched piezoelectric enhanced nanostructures prepared in example 1 of the present invention and a comparison graph of Fourier infrared spectrum curves of the PVDF nanofiber membrane with branched piezoelectric enhanced nanostructures prepared in example 2 of the present invention and a common PVDF nanofiber membrane;
fig. 2 is a graph of the current and voltage response of a piezoelectric nanogenerator fabricated using a PVDF nanofiber membrane with branched piezoelectric-enhanced nanostructures fabricated in example 5 of the invention.
Detailed Description
Example 1
(1) Preparing a spinning solution: weighing 1.975g of PVDF powder, adding the PVDF powder into 7mL of DMF and 3mL of acetone composite solvent, stirring at 40 ℃ to completely dissolve the PVDF powder, and preparing a PVDF solution with the concentration of 18%; then adding 77.5mg of tetrabutylammonium hexafluorophosphate into the solution, and continuously stirring until the tetrabutylammonium hexafluorophosphate is completely dissolved, wherein the tetrabutylammonium hexafluorophosphate accounts for 0.7 percent of the mass of the spinning solution;
(2) electrostatic spinning: and (3) spinning the spinning solution in the previous step by adopting an electrostatic spinning method, wherein the spinning voltage is 30kV, the receiving distance is 10cm, and the liquid supply rate is 0.5mL/h, so that the PVDF piezoelectric nanofiber membrane with the branched piezoelectric enhanced nano structure is prepared. Fig. 1 is an electron microscope picture of the morphology of the PVDF piezoelectric nanofiber membrane with a branched piezoelectric-enhanced nanostructure prepared in example 1 of the present invention. The diameter of the branched structure fiber was measured between 5 and 80nm using SEM images.
The nanofiber membrane in example 1 was made to 3X 3cm 2 Piezoelectric material of standard is placed on upper and lower copper electrodes (2 × 2 cm) 2 ) And in the middle, keeping tight fit, packaging by using a polyethylene terephthalate (PET) film, and tightly fitting all parts by a hot pressing technology to prepare the piezoelectric nano generator. The nano generator is connected with the signal collecting device by a lead, and the piezoelectric response current of the piezoelectric nano generator is 0.67 muA and the voltage is 2.58V by applying mechanical force in the thickness direction to the piezoelectric nano generator.
Example 2
(1) Preparing a spinning solution: weighing 1.975g of PVDF powder, adding the PVDF powder into 7mL of DMF and 3mL of acetone composite solvent, stirring at 40 ℃ to completely dissolve the PVDF powder, and preparing a PVDF solution with the concentration of 18%; then adding 387mg of tetrabutylammonium hexafluorophosphate into the solution, and continuously stirring until the tetrabutylammonium hexafluorophosphate is completely dissolved, wherein the tetrabutylammonium hexafluorophosphate accounts for 3.5 percent of the mass of the spinning solution;
(2) electrostatic spinning: and (3) spinning the spinning solution in the previous step by adopting an electrostatic spinning method, wherein the spinning voltage is 30kV, the receiving distance is 12cm, and the liquid supply rate is 0.3mL/h, so that the PVDF piezoelectric nanofiber membrane with the branched piezoelectric enhanced nano structure is prepared. FIG. 1 is a view of the utilization of the bookComparison graph of fourier infrared spectrum curves of the PVDF piezoelectric nanofiber membrane with the branched piezoelectric enhanced nano structure prepared in embodiment 2 of the invention and the common PVDF nanofiber membrane. From the figure, it can be seen that the PVDF piezoelectric nanofiber membrane with the branched piezoelectric enhanced nano structure has 840cm in the Fourier infrared spectrum curve -1 The characteristic peaks of beta-phase at the wavelength are obviously enhanced, 490, 532, 613, 763, 796 and 976cm -1 The alpha phase characteristic peak is obviously weakened or even disappears. The PVDF nanofiber membrane with the high polarization branch structure prepared in example 2 is shown to convert more alpha phase into beta phase, so that the content of the polar phase is increased.
The nanofiber membrane of example 2 was used to fabricate a piezoelectric nanogenerator in the same manner as in example 1. The nano generator is connected with the signal collecting device by a lead, and the piezoelectric response current of the piezoelectric nano generator is 2.23 muA and the voltage is 3.53V by applying mechanical force in the thickness direction to the piezoelectric nano generator.
Example 3
(1) Preparing a spinning solution: weighing 1.841g of PVDF powder, adding the PVDF powder into a 7mL DMF and 3mL acetone composite solvent, stirring at 45 ℃ to completely dissolve the PVDF powder, and preparing a 17% PVDF solution; then adding 56mg of tetrabutylammonium chloride into the solution, and continuously stirring until the tetrabutylammonium chloride is completely dissolved, wherein the tetrabutylammonium chloride accounts for 0.5 percent of the mass of the spinning solution;
(2) electrostatic spinning: spinning the spinning solution in the previous step by adopting an electrostatic spinning method, wherein the spinning voltage is 27kV, the receiving distance is 12cm, and the liquid supply rate is 0.7mL/h, so as to prepare the PVDF piezoelectric nanofiber membrane with the branched piezoelectric enhanced nano structure;
(3) preparing a piezoelectric nano generator: the same as in example 1. By applying a mechanical force in the thickness direction to the piezoelectric nanogenerator, a piezoelectric response current of the piezoelectric nanogenerator of 0.37 mua and a voltage of 2.24V were obtained.
Example 4
(1) Preparing a spinning solution: weighing 1.975g of PVDF powder, adding the PVDF powder into 7mL of DMF and 3mL of acetone composite solvent, stirring at 40 ℃ to completely dissolve the PVDF powder, and preparing a PVDF solution with the concentration of 18%; adding 221.81mg of tetrapropylammonium chloride into the solution, and continuously stirring until the tetrapropylammonium chloride is completely dissolved, wherein the tetrapropylammonium chloride accounts for 2% of the mass of the spinning solution;
(2) electrostatic spinning: spinning the spinning solution in the previous step by adopting an electrostatic spinning method, wherein the spinning voltage is 30kV, the receiving distance is 15cm, and the liquid supply rate is 0.3mL/h, so as to prepare the PVDF piezoelectric nanofiber membrane with the branched piezoelectric enhanced nano structure;
(3) preparing a piezoelectric nano generator: the same as in example 1. By applying a mechanical force in the thickness direction to the piezoelectric nanogenerator, a piezoelectric response current of 1.22 mua and a voltage of 2.69V were obtained for the piezoelectric nanogenerator.
Example 5
(1) Preparing a spinning solution: weighing 1.975g of PVDF powder, adding the PVDF powder into 7mL and 3mL of acetone composite solvent, stirring at 50 ℃ to completely dissolve the PVDF powder, and preparing a PVDF solution with the concentration of 18%; then adding 77.5mg of tetrabutylammonium hexafluorophosphate into the solution, and continuously stirring until the tetrabutylammonium hexafluorophosphate is completely dissolved, wherein the tetrabutylammonium hexafluorophosphate accounts for 2.4 percent of the mass of the spinning solution;
(2) electrostatic spinning: spinning the spinning solution in the previous step by adopting an electrostatic spinning method, wherein the spinning voltage is 27kV, the receiving distance is 12cm, and the liquid supply rate is 0.7mL/h, so as to prepare the PVDF piezoelectric nanofiber membrane with the branched piezoelectric enhanced nano structure;
(3) preparing a piezoelectric nano generator: the same as in example 1. By applying a mechanical force in the thickness direction to the piezoelectric nanogenerator, a piezoelectric response current of the piezoelectric nanogenerator of 2.04 mua and a voltage of 4.08V were obtained. Fig. 2 is a graph of the current and voltage response of a piezoelectric nanogenerator fabricated using example 5 of the invention.
Example 6
(1) Preparing a spinning solution: weighing 2.109g of PVDF powder, adding the PVDF powder into 7mL of DMF and 3mL of acetone composite solvent, stirring at 40 ℃ to completely dissolve the PVDF powder, and preparing a PVDF solution with the concentration of 19%; adding 161.185mg of tetrabutylammonium bromide into the solution, and continuously stirring until the tetrabutylammonium bromide is completely dissolved, wherein the tetrabutylammonium bromide accounts for 1.4% of the spinning solution by mass;
(2) electrostatic spinning: spinning the spinning solution in the previous step by adopting an electrostatic spinning method, wherein the spinning voltage is 20kV, the receiving distance is 10cm, and the liquid supply rate is 0.5mL/h, so as to prepare the PVDF piezoelectric nanofiber membrane with the branched piezoelectric enhanced nano structure;
the nanofiber membrane of example 6 was used to fabricate a piezoelectric nanogenerator in the same manner as in example 1. The nano generator is connected with the signal collecting device by a lead, and the piezoelectric response current of the piezoelectric nano generator is 3.68 muA and the voltage is 5.15V by applying mechanical force in the thickness direction to the piezoelectric nano generator.
Table 1 is the piezoelectric response data for PVDF piezoelectric nanofiber film based piezoelectric nanogenerators with branched piezoelectric enhanced nanostructures made in examples 1-6.
TABLE 1
Claims (2)
1. A preparation method of a polyvinylidene fluoride piezoelectric nanofiber membrane with a branched piezoelectric reinforced nanostructure is characterized by comprising the following steps:
(1) preparing a spinning solution: adding a certain amount of polyvinylidene fluoride (PVDF) powder into a composite solvent of N, N-Dimethylformamide (DMF) and acetone, and stirring at 40-50 ℃ to completely dissolve the PVDF powder to prepare a PVDF solution with the concentration of 17-19%; and then adding a certain amount of organic branched salt into the solution, and continuously stirring until the organic branched salt is completely dissolved, wherein the organic branched salt accounts for 0.5-3.5% of the spinning solution by mass percent.
(2) Electrostatic spinning: and (3) spinning the spinning solution in the previous step by adopting an electrostatic spinning method, wherein the spinning voltage is 20-30 kV, the receiving distance is 10-15 cm, and the liquid supply rate is 0.3-0.7 mL/h, so that the polyvinylidene fluoride piezoelectric nanofiber membrane with the branched piezoelectric reinforced nanostructure is prepared.
2. The preparation method of the PVDF piezoelectric nanofiber membrane with the nano piezoelectric enhancement structure as claimed in claim 1, wherein the organic branched salt is any one of tetrabutylammonium hexafluorophosphate, tetrabutylammonium chloride, tetrabutylammonium bromide and tetrapropylammonium chloride.
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| CN115478362A (en) * | 2022-10-10 | 2022-12-16 | 天津工业大学 | Method for preparing polyvinylidene fluoride skin-core structure piezoelectric nanofiber membrane by in-situ growth of ZIF-67 |
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| CN115478362A (en) * | 2022-10-10 | 2022-12-16 | 天津工业大学 | Method for preparing polyvinylidene fluoride skin-core structure piezoelectric nanofiber membrane by in-situ growth of ZIF-67 |
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