CN115045044A - Method for preparing composite piezoelectric material based on electrostatic spinning process - Google Patents
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- 238000000034 method Methods 0.000 title claims abstract description 41
- 239000000463 material Substances 0.000 title claims abstract description 35
- 238000010041 electrostatic spinning Methods 0.000 title claims abstract description 33
- 239000002131 composite material Substances 0.000 title claims abstract description 24
- 230000008569 process Effects 0.000 title claims abstract description 22
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims abstract description 48
- JRPBQTZRNDNNOP-UHFFFAOYSA-N barium titanate Chemical compound [Ba+2].[Ba+2].[O-][Ti]([O-])([O-])[O-] JRPBQTZRNDNNOP-UHFFFAOYSA-N 0.000 claims abstract description 41
- 238000009987 spinning Methods 0.000 claims abstract description 41
- 239000000835 fiber Substances 0.000 claims abstract description 40
- 239000002033 PVDF binder Substances 0.000 claims abstract description 38
- 229920002981 polyvinylidene fluoride Polymers 0.000 claims abstract description 38
- 239000012528 membrane Substances 0.000 claims abstract description 29
- 239000002245 particle Substances 0.000 claims abstract description 29
- 229910002113 barium titanate Inorganic materials 0.000 claims abstract description 28
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 26
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 26
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims abstract description 23
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 20
- 229910020763 KH570 Inorganic materials 0.000 claims abstract description 20
- 238000002360 preparation method Methods 0.000 claims abstract description 20
- 239000002904 solvent Substances 0.000 claims abstract description 17
- 239000008367 deionised water Substances 0.000 claims abstract description 10
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000003756 stirring Methods 0.000 claims description 12
- 239000000843 powder Substances 0.000 claims description 9
- 239000002994 raw material Substances 0.000 claims description 7
- 238000012935 Averaging Methods 0.000 claims description 6
- ATHHXGZTWNVVOU-UHFFFAOYSA-N N-methylformamide Chemical compound CNC=O ATHHXGZTWNVVOU-UHFFFAOYSA-N 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 6
- 238000007789 sealing Methods 0.000 claims description 6
- 238000005303 weighing Methods 0.000 claims description 6
- 230000004048 modification Effects 0.000 claims description 4
- 238000012986 modification Methods 0.000 claims description 4
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 3
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 3
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 3
- 238000001523 electrospinning Methods 0.000 claims 2
- 239000000919 ceramic Substances 0.000 abstract description 3
- 238000004519 manufacturing process Methods 0.000 abstract 1
- 229920000620 organic polymer Polymers 0.000 abstract 1
- 239000002861 polymer material Substances 0.000 abstract 1
- 239000013078 crystal Substances 0.000 description 5
- 230000007613 environmental effect Effects 0.000 description 4
- 238000001878 scanning electron micrograph Methods 0.000 description 4
- 230000005684 electric field Effects 0.000 description 3
- 239000002121 nanofiber Substances 0.000 description 3
- 230000010287 polarization Effects 0.000 description 3
- 229920000642 polymer Polymers 0.000 description 3
- 230000032683 aging Effects 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
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- 238000012545 processing Methods 0.000 description 2
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- 230000008020 evaporation Effects 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 229910052451 lead zirconate titanate Inorganic materials 0.000 description 1
- HFGPZNIAWCZYJU-UHFFFAOYSA-N lead zirconate titanate Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Ti+4].[Zr+4].[Pb+2] HFGPZNIAWCZYJU-UHFFFAOYSA-N 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
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- 238000002844 melting Methods 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 238000004528 spin coating Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000010345 tape casting Methods 0.000 description 1
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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
-
- 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
- D01D5/003—Electro-spinning characterised by the initial state of the material the material being a polymer solution or dispersion
-
- 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
- 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
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- Engineering & Computer Science (AREA)
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
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- Mechanical Engineering (AREA)
- Inorganic Fibers (AREA)
Abstract
The invention discloses a method for preparing a composite piezoelectric material based on an electrostatic spinning process, which comprises the following steps: s1: preparation of materials: the composite material comprises PVDF, barium titanate, graphene, ethanol, deionized water, KH570, barium titanate particles, dimethylformamide, acetone and graphene oxide; s2: preparing modified barium titanate particles; s4: preparing a solvent for electrostatic spinning; s5: preparing a spinning solution; s6: preparing the material by an electrostatic spinning process; s7: the piezoelectric strain constant of the fiber membrane was calculated. The method for preparing the composite piezoelectric material based on the electrostatic spinning process has the flexibility of an organic polymer material and the strong piezoelectricity of inorganic ceramic, is simple in preparation method and low in cost, is easy to prepare a film with any shape and large area, is suitable for mass production and preparation, avoids lead pollution due to the adoption of lead-free barium titanate, and can be applied to underwater sound, electroacoustic, medical treatment and the like.
Description
Technical Field
The invention relates to a preparation method of a high-voltage electric functional film, in particular to a method for preparing a composite piezoelectric material based on an electrostatic spinning process.
Background
Polyvinylidene fluoride has the advantages of excellent piezoelectric property, softness, light weight, high toughness, high sensitivity, wide frequency range, low price and the like, is an ideal material for preparing a flexible sensor, is rapidly developed along with the deep research of people on the piezoelectric effect theory of polyvinylidene fluoride, is increasingly wide and almost relates to various aspects in life.
PVDF is a polycrystalline polymer, at least five crystal forms are found, namely an alpha phase, a beta phase, a gamma phase, a delta phase and an epsilon phase, wherein the beta crystal form has the best piezoelectric effect, the preparation method of the PVDF piezoelectric film comprises a tape casting method, a melting method, an electrostatic spinning method, a spin coating method and the like, the alpha phase is converted into the beta phase, the beta phase can be converted only by adopting high-temperature treatment or stretching or high-voltage polarization conventionally, the energy requirement is extremely high, the process is complex, the yield is not high, and the electrostatic spinning method is concerned due to strong controllability and high beta crystal form content of the prepared spinning film.
The electrostatic spinning process can form PVDF nano-fiber with beta crystal form, and the mechanism of the PVDF nano-fiber is probably as follows: (1) the formation of the beta phase structure is a stretching of the electric field force in the electrostatic field by the polymer jet, this electric field force directed stretching can be equivalent to the mechanical stretching of the PVDF film; (2) the electrostatic spinning process of PVDF is carried out in a strong electric field, and is equivalent to the polarization process to a certain extent; (3) the rapid evaporation of the solvent and the solidification and molding of the PVDF nanofiber can promote the formation of beta crystal form.
Although PVDF has the advantages of light weight, good formability and the like, but has the problems of low piezoelectric strain constant d33, large voltage required during polarization and the like, modification treatment is often required, the most common modified piezoelectric ceramic is lead zirconate titanate, but because of environmental protection consideration, how to remove Pb element from piezoelectric materials becomes a research hotspot, and how to retain the excellent properties of piezoelectric PVDF polymer and introduce the good high-temperature resistance of piezoelectric ceramic is a problem to be solved urgently at present.
Disclosure of Invention
The invention mainly aims to provide a method for preparing a composite piezoelectric material based on an electrostatic spinning process, which can effectively solve the problems in the background art.
In order to achieve the purpose, the invention adopts the technical scheme that:
a method for preparing a composite piezoelectric material based on an electrostatic spinning process comprises the following operation steps:
s1: preparation of materials: the composite material comprises PVDF, barium titanate, graphene, ethanol, deionized water, KH570, barium titanate particles, dimethylformamide, acetone and graphene oxide, wherein the PVDF accounts for 100 percent, the barium titanate accounts for 5-20 percent, the graphene accounts for 0.05-0.20 percent, the ethanol accounts for 10ml, the deionized water accounts for 190ml, the KH570 accounts for 0.2g, the barium titanate particles accounts for 2g, the methyl formamide accounts for 6g, the acetone accounts for 4g, and the graphene oxide accounts for 0.0005-0.0020 g;
s2: preparation of modified barium titanate particles: respectively adding 10ml of ethanol, 190ml of deionized water and 0.2g of KH570 into a beaker, adjusting the pH value of the solution to 10 by using ammonia water, mechanically stirring for 10min, then adding 2g of barium titanate particles, ultrasonically oscillating, mechanically stirring for 1 hour respectively, centrifuging, and drying at 120 ℃ to obtain KH570 modified barium titanate particles;
s4: preparation of solvent for electrostatic spinning: the solvent for electrostatic spinning is a Dimethylformamide (DMF) -acetone system, 6g of DMF (DMF) and 4g of acetone are weighed and stirred and mixed uniformly to obtain the solvent for spinning;
s5: preparation of spinning solution: weighing 1g of PVDF powder, 0.05-0.20 g of KH570 modified barium titanate particles prepared in S2, 0.0005-0.0020 g of graphene oxide and 10g of solvent for electrostatic spinning prepared in S4, mixing, sealing, heating in an oil bath at 50 ℃, and stirring for 2 hours to obtain a spinning solution;
s6: preparing the material by an electrostatic spinning process: limiting parameters of electrostatic spinning equipment, wherein the spinning voltage is 10-16 kV; the spinning speed is 0.5-2 ml/h; the spinning distance is 9-15 cm; the inner diameter of the needle is 0.50-0.80 mm, the temperature in the spinning process is 20 ℃, and the ambient humidity is 30% -50%, so that the composite piezoelectric material containing nano barium titanate, graphene oxide and PVDF can be prepared, and the preparation of the fiber membrane is completed;
s7: the piezoelectric strain constant of the fiber membrane was calculated: based on the composite piezoelectric material fiber membrane prepared in S6, a 1 x 2cm piece is cut 2 The piezoelectric constant D33 of the fiber membrane is measured by selecting 5 points on the fiber membrane, and then the piezoelectric strain constant of the fiber membrane can be obtained by averaging the five values.
Preferably, the raw material barium titanate has a particle size range of 0.1-1 μm, and needs to be subjected to surface modification treatment by a silane coupling agent KH 570.
Preferably, the powder average particle size of the raw material polyvinylidene fluoride (PVDF) is 38 μm.
Compared with the prior art, the invention has the following beneficial effects:
in the invention, although the flexibility of the conventional PVDF film material is good, the processing type is excellent, but the piezoelectric constant is smaller, and the temperature characteristic and the aging characteristic have problems.
Drawings
FIG. 1 is a SEM picture of a scanning electron microscope according to a first embodiment of the invention;
FIG. 2 is a SEM picture of a scanning electron microscope in accordance with a second embodiment of the invention;
FIG. 3 is an SEM image of a scanning electron microscope in the third embodiment of the invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The invention relates to a method for preparing a composite piezoelectric material based on an electrostatic spinning process, which comprises the following steps:
s1: preparation of materials: the composite material comprises PVDF, barium titanate, graphene, ethanol, deionized water, KH570, barium titanate particles, dimethylformamide, acetone and graphene oxide, wherein the reference of PVDF is 100%, the content of barium titanate is 5-20%, the content of graphene is 0.05-0.20%, the content of ethanol is 10ml, the content of deionized water is 190ml, the content of KH570 is 0.2g, the content of barium titanate particles is 2g, the content of methyl formamide is 6g, the content of acetone is 4g, the content of graphene oxide is 0.0005-0.0020 g, the particle size of raw material barium titanate is 0.1-1 mu m, the surface of the raw material barium titanate is required to be modified by a silane coupling agent KH570, and the average particle size of powder of raw material polyvinylidene fluoride (PVDF) is 38 mu m;
s2: preparation of modified barium titanate particles: respectively adding 10ml of ethanol, 190ml of deionized water and 0.2g of KH570 into a beaker, adjusting the pH value of the solution to 10 by using ammonia water, mechanically stirring for 10min, then adding 2g of barium titanate particles, ultrasonically oscillating, mechanically stirring for 1 hour respectively, centrifuging, and drying at 120 ℃ to obtain KH570 modified barium titanate particles;
s4: preparation of solvent for electrostatic spinning: the solvent for electrostatic spinning is a Dimethylformamide (DMF) -acetone system, 6g of DMF (DMF) and 4g of acetone are weighed and stirred and mixed uniformly to obtain the solvent for spinning;
s5: preparation of spinning solution: weighing 1g of PVDF powder, 0.05-0.20 g of KH570 modified barium titanate particles prepared in S2, 0.0005-0.0020 g of graphene oxide and 10g of solvent for electrostatic spinning prepared in S4, mixing, sealing, heating in an oil bath at 50 ℃, and stirring for 2 hours to obtain a spinning solution;
s6: preparing the material by an electrostatic spinning process: defining parameters of electrostatic spinning equipment, wherein the spinning voltage is 10-16 kV; the spinning speed is 0.5-2 ml/h; the spinning distance is 9-15 cm; the inner diameter of the needle is 0.50-0.80 mm, the temperature in the spinning process is 20 ℃, and the ambient humidity is 30% -50%, so that the composite piezoelectric material containing nano barium titanate, graphene oxide and PVDF can be prepared, and the preparation of the fiber membrane is completed;
s7: the piezoelectric strain constant of the fiber membrane was calculated: based on the composite piezoelectric material fiber membrane prepared in S6, a 1 x 2cm2 fiber membrane is cut, 5 points are selected on the fiber membrane, the piezoelectric constant D33 of the fiber membrane is measured, and then the piezoelectric strain constant of the fiber membrane can be obtained by averaging the five values.
The first embodiment is as follows:
s1: weighing 1g of PVDF powder, 0.05g of KH570 modified barium titanate particles, 0.0020g of graphene oxide and 10g of solvent for spinning, mixing, sealing, heating in an oil bath at 50 ℃, and stirring for 2 hours to obtain a spinning solution;
s2: the material is prepared by using an electrostatic spinning device, and the related specific process parameters are as follows: the spinning voltage is 14 kV; the spinning speed is 0.5 ml/h; the spinning distance is 12 cm; the inner diameter of the needle is 0.68mm, the temperature in the spinning process is 20 ℃, and the environmental humidity is 50%, so that the composite piezoelectric material containing nano barium titanate, graphene oxide and PVDF is prepared;
s3: based on the fiber film prepared in S2, the piezoelectric performance of the fiber film is measured by using a quasi-static instrument D33 of model YE2730A, namely, a piece of fiber film of 1 multiplied by 2cm2 is cut, 5 points are selected on the fiber film, the piezoelectric constant D33 of the fiber film is measured, and then the piezoelectric strain constant of the fiber film is obtained by averaging the five values. The piezoelectric strain constant of the fiber membrane of this example was found to be 29pC/N, and FIG. 1 is SEM image of the first example.
The second embodiment is as follows:
s1: weighing 1g of PVDF powder, 0.05g of KH570 modified barium titanate particles, 0.0010g of graphene oxide and 10g of solvent for spinning, mixing, sealing, heating in an oil bath at 50 ℃, and stirring for 2 hours to obtain a spinning solution;
s2: the material is prepared by using an electrostatic spinning device, and the related specific process parameters are as follows: the spinning voltage is 16 kV; the spinning speed is 1.2 ml/h; the spinning distance is 15 cm; the inner diameter of the needle is 0.80mm, the temperature in the spinning process is 20 ℃, and the environmental humidity is 40%, so that the composite piezoelectric material containing the nano barium titanate, the graphene oxide and the PVDF is prepared.
S3: based on the fiber membrane prepared in S2, the piezoelectric performance of the fiber membrane is measured by using a quasi-static instrument D33 of model YE2730A, namely, a piece of 1 multiplied by 2cm is cut 2 The piezoelectric constant D33 of the fiber membrane is measured by selecting 5 points on the fiber membrane, and then the piezoelectric strain constant of the fiber membrane is obtained by averaging the five values. The piezoelectric strain constant of the fiber membrane of this example was found to be 31pC/N, and FIG. 2 is SEM image.
The third concrete embodiment:
s1: weighing 1g of PVDF powder, 0.20g of KH570 modified barium titanate particles, 0.0005g of graphene oxide and 10g of solvent for spinning, mixing, sealing, heating in an oil bath at 50 ℃, and stirring for 2 hours to obtain a spinning solution;
s2: the material is prepared by using an electrostatic spinning device, and the related specific process parameters are as follows: the spinning voltage is 10 kV; the spinning speed is 2 ml/h; the spinning distance is 9 cm; the inner diameter of the needle is 0.50mm, the temperature in the spinning process is 20 ℃, and the environmental humidity is 30%, so that the composite piezoelectric material containing nano barium titanate, graphene oxide and PVDF is prepared;
s3: based on the fiber membrane prepared in S2, the piezoelectric performance of the fiber membrane is measured by using a quasi-static instrument D33 of model YE2730A, namely, a piece of 1 multiplied by 2cm is cut 2 The piezoelectric constant D33 of the fiber membrane is measured by selecting 5 points on the fiber membrane, and then the piezoelectric strain constant of the fiber membrane is obtained by averaging the five values. The piezoelectric strain constant of the fiber membrane of this example was found to be 32pC/N, and FIG. 3 is SEM image of the third example.
In the invention, although the flexibility of the conventional PVDF film material is good, the processing type is excellent, but the piezoelectric constant is smaller, and the temperature characteristic and the aging characteristic have problems.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (3)
1. A method for preparing a composite piezoelectric material based on an electrostatic spinning process is characterized by comprising the following steps: the method comprises the following operation steps:
s1: preparation of materials: the composite material comprises PVDF, barium titanate, graphene, ethanol, deionized water, KH570, barium titanate particles, dimethylformamide, acetone and graphene oxide, wherein the PVDF accounts for 100 percent, the barium titanate accounts for 5-20 percent, the graphene accounts for 0.05-0.20 percent, the ethanol accounts for 10ml, the deionized water accounts for 190ml, the KH570 accounts for 0.2g, the barium titanate particles accounts for 2g, the methyl formamide accounts for 6g, the acetone accounts for 4g, and the graphene oxide accounts for 0.0005-0.0020 g;
s2: preparation of modified barium titanate particles: respectively adding 10ml of ethanol, 190ml of deionized water and 0.2g of KH570 into a beaker, adjusting the pH value of the solution to 10 by using ammonia water, mechanically stirring for 10min, then adding 2g of barium titanate particles, ultrasonically oscillating, mechanically stirring for 1 hour respectively, centrifuging, and drying at 120 ℃ to obtain KH570 modified barium titanate particles;
s4: preparation of solvent for electrostatic spinning: the solvent for electrostatic spinning is a Dimethylformamide (DMF) -acetone system, 6g of DMF (DMF) and 4g of acetone are weighed and stirred and mixed uniformly to obtain the solvent for spinning;
s5: preparation of spinning solution: weighing 1g of PVDF powder, 0.05-0.20 g of KH570 modified barium titanate particles prepared in S2, 0.0005-0.0020 g of graphene oxide and 10g of solvent for electrostatic spinning prepared in S4, mixing, sealing, heating in an oil bath at 50 ℃, and stirring for 2 hours to obtain a spinning solution;
s6: preparing the material by an electrostatic spinning process: limiting parameters of electrostatic spinning equipment, wherein the spinning voltage is 10-16 kV; the spinning speed is 0.5-2 ml/h; the spinning distance is 9-15 cm; the inner diameter of the needle is 0.50-0.80 mm, the temperature in the spinning process is 20 ℃, and the ambient humidity is 30% -50%, so that the composite piezoelectric material containing nano barium titanate, graphene oxide and PVDF can be prepared, and the preparation of the fiber membrane is completed;
s7: the piezoelectric strain constant of the fiber membrane was calculated: based on the composite piezoelectric material fiber film prepared in S6, a 1 × 2cm2 fiber film is cut, 5 points are selected on the fiber film, the piezoelectric constant D33 of the fiber film is measured, and then the piezoelectric strain constant of the fiber film can be obtained by averaging the five values.
2. The method for preparing the composite piezoelectric material based on the electrospinning process according to claim 1, wherein the method comprises the following steps: the raw material barium titanate has a particle size range of 0.1-1 mu m and needs to be subjected to modification treatment by a silane coupling agent KH 570.
3. The method for preparing the composite piezoelectric material based on the electrospinning process according to claim 1, wherein the method comprises the following steps: the powder average particle size of the raw material polyvinylidene fluoride (PVDF) was 38 μm.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108505213A (en) * | 2018-05-14 | 2018-09-07 | 广东石油化工学院 | A kind of preparation method of amino graphene/polyunsymfluorethylepiezoelectric piezoelectric nanometer electrospinning film |
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