CN110616484A - Method for preparing piezoelectric PVDF (polyvinylidene fluoride) coated carbon fiber by electrostatic spinning technology - Google Patents
Method for preparing piezoelectric PVDF (polyvinylidene fluoride) coated carbon fiber by electrostatic spinning technology Download PDFInfo
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- 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
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- 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
- D01D5/0061—Electro-spinning characterised by the electro-spinning apparatus
- D01D5/0092—Electro-spinning characterised by the electro-spinning apparatus characterised by the electrical field, e.g. combined with a magnetic fields, using biased or alternating fields
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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
- D01F6/02—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolymers obtained by reactions only involving carbon-to-carbon unsaturated bonds
- D01F6/08—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolymers obtained by reactions only involving carbon-to-carbon unsaturated bonds from polymers of halogenated hydrocarbons
- D01F6/12—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolymers obtained by reactions only involving carbon-to-carbon unsaturated bonds from polymers of halogenated hydrocarbons from polymers of fluorinated hydrocarbons
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- D—TEXTILES; PAPER
- D02—YARNS; MECHANICAL FINISHING OF YARNS OR ROPES; WARPING OR BEAMING
- D02G—CRIMPING OR CURLING FIBRES, FILAMENTS, THREADS, OR YARNS; YARNS OR THREADS
- D02G3/00—Yarns or threads, e.g. fancy yarns; Processes or apparatus for the production thereof, not otherwise provided for
- D02G3/02—Yarns or threads characterised by the material or by the materials from which they are made
- D02G3/04—Blended or other yarns or threads containing components made from different materials
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- D—TEXTILES; PAPER
- D02—YARNS; MECHANICAL FINISHING OF YARNS OR ROPES; WARPING OR BEAMING
- D02G—CRIMPING OR CURLING FIBRES, FILAMENTS, THREADS, OR YARNS; YARNS OR THREADS
- D02G3/00—Yarns or threads, e.g. fancy yarns; Processes or apparatus for the production thereof, not otherwise provided for
- D02G3/22—Yarns or threads characterised by constructional features, e.g. blending, filament/fibre
- D02G3/36—Cored or coated yarns or threads
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- D—TEXTILES; PAPER
- D02—YARNS; MECHANICAL FINISHING OF YARNS OR ROPES; WARPING OR BEAMING
- D02G—CRIMPING OR CURLING FIBRES, FILAMENTS, THREADS, OR YARNS; YARNS OR THREADS
- D02G3/00—Yarns or threads, e.g. fancy yarns; Processes or apparatus for the production thereof, not otherwise provided for
- D02G3/44—Yarns or threads characterised by the purpose for which they are designed
- D02G3/441—Yarns or threads with antistatic, conductive or radiation-shielding properties
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- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Mechanical Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Dispersion Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Spinning Methods And Devices For Manufacturing Artificial Fibers (AREA)
- Yarns And Mechanical Finishing Of Yarns Or Ropes (AREA)
- Artificial Filaments (AREA)
Abstract
The invention discloses a method for preparing piezoelectric PVDF (polyvinylidene fluoride) -coated carbon fibers by using an electrostatic spinning technology, which comprises the steps of firstly, mixing polyvinylidene fluoride (PVDF) and N, N-Dimethylformamide (DMF) to prepare a spinning solution; and then coating polyvinylidene fluoride (PVDF) on the surface of the carbon fiber by utilizing an electrostatic spinning technology to prepare the carbon fiber-PVDF piezoelectric core-spun yarn. The carbon fiber-PVDF piezoelectric core-spun yarn prepared by the electrostatic spinning technology can be more conveniently applied to piezoelectric fabrics.
Description
Technical Field
The invention relates to a method for preparing piezoelectric PVDF (polyvinylidene fluoride) coated carbon fibers by using an electrostatic spinning technology, belonging to the field of flexible piezoelectric materials.
Background
The piezoelectric fiber is a functional material which can mutually convert mechanical energy and electric energy, and the piezoelectric material is a material which generates corresponding change of induced charge due to the change of static pressure. Most of the currently studied piezoelectric materials are film-shaped or block-shaped, and piezoelectric fibers are more and more widely used as a special piezoelectric material form. Polyvinylidene fluoride (PVDF) is a piezoelectric material, has a strong piezoelectric effect, and is a polymer which is researched in piezoelectric polymer materials at present and has the system and the most extensive application. Compared with the prior common high polymer (such as quartz and piezoelectric ceramics), the high polymer has the advantages of small acoustic impedance, wide frequency response, small dielectric constant, strong impact resistance, convenient processing into any shape and the like.
With the continuous development of scientific technology, the technology for preparing PVDF piezoelectric film by traditional method is mature, and electrostatic spinning technology has the advantages of simple operation, low cost and the like, so that the PVDF piezoelectric film is spun by electrostatic spinning which is a widely advocated means at present. The yarn with piezoelectric property is prepared by the electrostatic spinning technology and can be more conveniently applied to the fabric, so the invention provides the method for preparing the piezoelectric PVDF-coated carbon fiber by the electrostatic spinning technology. The carbon fiber is a novel high-strength and high-modulus fiber material with the carbon content of more than 95 percent, has good electric conductivity, and can be used as core yarn to prepare the core-spun yarn by combining the electrostatic spinning technology and the piezoelectric PVDF.
Disclosure of Invention
The invention can lead out the piezoelectric signal generated by PVDF by utilizing the good conductivity of the carbon fiber, and meanwhile, the electrostatic spinning technology has the advantages of simple equipment, low cost and simple operation. Based on the above conditions, the invention provides a method for preparing piezoelectric PVDF-coated carbon fibers by using an electrostatic spinning technology, which specifically comprises the following steps:
1) cleaning a reaction vessel and magnetons with deionized water, drying, mixing polyvinylidene fluoride (PVDF) serving as a spinning solution solute and N, N-Dimethylformamide (DMF) serving as a solvent in the reaction vessel, adding the magnetons into the mixed solution to seal the mixed solution, slowly heating the sealed reaction vessel in a water bath kettle, stirring by using a magneton stirring device, and then standing and cooling to obtain a spinning solution;
2) extracting the spinning solution obtained in the step 1) by using an injector, fixing the injector in an injection pump, adjusting electrostatic spinning parameters, connecting a spinning nozzle with a high-voltage positive electrode and a high-voltage negative electrode respectively, accelerating the solution at the top point of a Taylor cone of the spinning nozzle under the action of an electric field force, and finally overcoming surface tension through enough electric field force to spray a trickle, wherein the trickle forms a fiber mesh at a horn mouth. Meanwhile, after the carbon fiber passes through the bell mouth, the carbon fiber is pulled out from the PVDF fiber net by the winding roller, so that the piezoelectric PVDF is uniformly coated on the carbon fiber through the rotary bell mouth and finally collected by the winding roller, and the core-spun yarn which takes the carbon fiber as the core yarn and is coated by the piezoelectric PVDF is obtained;
3) putting the core-spun yarn prepared in the step 2) into an oven for drying, and finally obtaining the carbon fiber-PVDF piezoelectric core-spun yarn.
Furthermore, the temperature of the water bath is 60-80 ℃, the magneton stirring time is 4-5 h, and the concentration of PVDF in the spinning solution is 8-12%.
Further, the electrospinning parameters were as follows: the extrusion speed of the spinning solution is 0.3 ml/h-0.7 ml/h, the spinning distance is 6 cm-10 cm, the distance of double needles is 10 cm-15 cm, the spinning voltage is 4 KV-5 KV, the rotating speed of a winding roller is 0.02 mm/s-0.2 mm/s, the rotating speed of a bell mouth is 300 rpm-800 rpm, the ambient temperature of electrostatic spinning is 20 +/-2 ℃, and the relative humidity is 60 +/-5%.
Furthermore, the drying temperature is 80-100 ℃, and the drying time is 2-5 h.
The invention relates to a method for preparing piezoelectric PVDF (polyvinylidene fluoride) coated carbon fibers by using an electrostatic spinning technology, which has the following beneficial effects:
(1) the method adopts the electrostatic spinning technology, has simple equipment, low cost and simple operation, and the electrostatic spinning process has the polarization function, thereby saving the subsequent polarization step.
(2) The carbon fiber has good mechanical property and conductivity, can fully exert the mechanical property when being used as the core yarn, and can derive the piezoelectric signal generated by the PVDF.
(3) Compared with the PVDF piezoelectric film prepared by the electrostatic spinning technology at present, the carbon fiber-PVDF piezoelectric yarn prepared by the electrostatic spinning technology can be more conveniently applied to weaving of piezoelectric fabrics.
Drawings
FIG. 1 is a schematic view of an apparatus for manufacturing a carbon fiber-PVDF piezoelectric core-spun yarn.
Fig. 2 is a surface SEM image of a carbon fiber-PVDF piezoelectric core spun yarn shown in example 3.
Figure 3 is a cross-sectional SEM image of a carbon fiber-PVDF piezoelectric core spun yarn shown in example 3,
fig. 4 is a graph of the piezoelectric voltage test results of a carbon fiber-PVDF piezoelectric core spun yarn shown in example 3.
In the drawings, the reference numerals denote the following components:
1. carbon fiber, 2, bell mouth, 3, injection needle, 4, fiber mesh, 5, core-spun yarn, 6, winding roller, 7, PVDF, 8 and carbon fiber.
Detailed Description
In order to make the technical solution of the present invention more apparent, the present invention will be described in further detail with reference to the following examples.
Example one
1) Washing a reaction container and magnetons with deionized water, drying, weighing 0.8 g of polyvinylidene fluoride (PVDF) and 9.2 g of N, N-Dimethylformamide (DMF), mixing, adding the magnetons into the mixed solution, sealing the mixed solution, slowly heating the sealed reaction container in a water bath kettle, heating to 70 ℃, stirring by using a magneton stirring device for 5 hours, and then standing and cooling to room temperature to obtain a spinning solution;
2) extracting the spinning solution obtained in the step 1) by using an injector, taking carbon fibers as core yarns, and preparing the carbon fiber-PVDF piezoelectric core-spun yarns by using an electrostatic spinning method, wherein the extrusion speed of the spinning solution is 0.5ml/h, the spinning distance is 8cm, the distance between two needle heads is 12cm, the spinning voltage is 4.5KV, the rotating speed of a winding roller is 0.05mm/s, the rotating speed of a bell mouth is 500rpm, the ambient temperature of electrostatic spinning is 20 +/-2 ℃, and the relative humidity is 60 +/-5%;
3) and (3) putting the carbon fiber-PVDF piezoelectric core-spun yarn prepared in the step 2) into an oven for drying at the drying temperature of 80 ℃ for 3h to finally obtain the carbon fiber-PVDF piezoelectric core-spun yarn.
Example two
1) Washing a reaction container and magnetons with deionized water, drying, weighing 0.8 g of polyvinylidene fluoride (PVDF) and 9.2 g of N, N-Dimethylformamide (DMF), mixing, adding the magnetons into the mixed solution, sealing the mixed solution, slowly heating the sealed reaction container in a water bath kettle, heating to 70 ℃, stirring by using a magneton stirring device for 5 hours, and then standing and cooling to room temperature to obtain a spinning solution;
2) extracting the spinning solution obtained in the step 1) by using an injector, taking carbon fibers as core yarns, and preparing the carbon fiber-PVDF piezoelectric core-spun yarns by using an electrostatic spinning method, wherein the extrusion speed of the spinning solution is 0.5ml/h, the spinning distance is 8cm, the distance between two needle heads is 12cm, the spinning voltage is 4.5KV, the rotating speed of a winding roller is 0.2mm/s, the rotating speed of a bell mouth is 500rpm, the ambient temperature of electrostatic spinning is 20 +/-2 ℃, and the relative humidity is 60 +/-5%;
3) and (3) putting the carbon fiber-PVDF piezoelectric core-spun yarn prepared in the step 2) into an oven for drying at the drying temperature of 80 ℃ for 3h to finally obtain the carbon fiber-PVDF piezoelectric core-spun yarn.
EXAMPLE III
1) Washing a reaction container and magnetons with deionized water, drying, weighing 1 g of polyvinylidene fluoride (PVDF) and 9 g of N, N-Dimethylformamide (DMF), mixing, adding the magnetons into the mixed solution, sealing the mixed solution, placing the sealed reaction container in a water bath kettle, slowly heating to 70 ℃, stirring by using a magneton stirring device for 5 hours, and then standing and cooling to room temperature to obtain a spinning solution;
2) extracting the spinning solution obtained in the step 1) by using an injector, taking carbon fibers as core yarns, and preparing the carbon fiber-PVDF piezoelectric core-spun yarns by using an electrostatic spinning method, wherein the extrusion speed of the spinning solution is 0.5ml/h, the spinning distance is 8cm, the distance between two needle heads is 12cm, the spinning voltage is 4.5KV, the rotating speed of a winding roller is 0.05mm/s, the rotating speed of a bell mouth is 500rpm, the ambient temperature of electrostatic spinning is 20 +/-2 ℃, and the relative humidity is 60 +/-5%;
3) and (3) putting the carbon fiber-PVDF piezoelectric core-spun yarn prepared in the step 2) into an oven for drying at the drying temperature of 80 ℃ for 3h to finally obtain the carbon fiber-PVDF piezoelectric core-spun yarn.
Example four
1) Washing a reaction container and magnetons with deionized water, drying, weighing 1 g of polyvinylidene fluoride (PVDF) and 9 g of N, N-Dimethylformamide (DMF), mixing, adding the magnetons into the mixed solution, sealing the mixed solution, placing the sealed reaction container in a water bath kettle, slowly heating to 70 ℃, stirring by using a magneton stirring device for 5 hours, and then standing and cooling to room temperature to obtain a spinning solution;
2) extracting the spinning solution obtained in the step 1) by using an injector, taking carbon fibers as core yarns, and preparing the carbon fiber-PVDF piezoelectric core-spun yarns by using an electrostatic spinning method, wherein the extrusion speed of the spinning solution is 0.5ml/h, the spinning distance is 8cm, the distance between two needle heads is 12cm, the spinning voltage is 4.5KV, the rotating speed of a winding roller is 0.2mm/s, the rotating speed of a bell mouth is 500rpm, the ambient temperature of electrostatic spinning is 20 +/-2 ℃, and the relative humidity is 60 +/-5%;
3) and (3) putting the carbon fiber-PVDF piezoelectric core-spun yarn prepared in the step 2) into an oven for drying at the drying temperature of 80 ℃ for 3h to finally obtain the carbon fiber-PVDF piezoelectric core-spun yarn.
EXAMPLE five
1) Washing a reaction container and magnetons with deionized water, drying, weighing 1.2 g of polyvinylidene fluoride (PVDF) and 8.8 g of N, N-Dimethylformamide (DMF), mixing, adding the magnetons into the mixed solution, sealing the mixed solution, slowly heating the sealed reaction container in a water bath kettle, heating to 70 ℃, stirring by using a magneton stirring device for 5 hours, and then standing and cooling to room temperature to obtain a spinning solution;
2) extracting the spinning solution obtained in the step 1) by using an injector, taking carbon fibers as core yarns, and preparing the carbon fiber-PVDF piezoelectric core-spun yarns by using an electrostatic spinning method, wherein the extrusion speed of the spinning solution is 0.5ml/h, the spinning distance is 8cm, the distance between two needle heads is 12cm, the spinning voltage is 4.5KV, the rotating speed of a winding roller is 0.05mm/s, the rotating speed of a bell mouth is 500rpm, the ambient temperature of electrostatic spinning is 20 +/-2 ℃, and the relative humidity is 60 +/-5%;
3) and (3) putting the carbon fiber-PVDF piezoelectric core-spun yarn prepared in the step 2) into an oven for drying at the drying temperature of 80 ℃ for 3h to finally obtain the carbon fiber-PVDF piezoelectric core-spun yarn.
EXAMPLE six
1) Washing a reaction container and magnetons with deionized water, drying, weighing 1.2 g of polyvinylidene fluoride (PVDF) and 8.8 g of N, N-Dimethylformamide (DMF), mixing, adding the magnetons into the mixed solution, sealing the mixed solution, slowly heating the sealed reaction container in a water bath kettle, heating to 70 ℃, stirring by using a magneton stirring device for 5 hours, and then standing and cooling to room temperature to obtain a spinning solution;
2) extracting the spinning solution obtained in the step 1) by using an injector, taking carbon fibers as core yarns, and preparing the carbon fiber-PVDF piezoelectric core-spun yarns by using an electrostatic spinning method, wherein the extrusion speed of the spinning solution is 0.5ml/h, the spinning distance is 8cm, the distance between two needle heads is 12cm, the spinning voltage is 4.5KV, the rotating speed of a winding roller is 0.2mm/s, the rotating speed of a bell mouth is 500rpm, the ambient temperature of electrostatic spinning is 20 +/-2 ℃, and the relative humidity is 60 +/-5%;
3) and (3) putting the carbon fiber-PVDF piezoelectric core-spun yarn prepared in the step 2) into an oven for drying at the drying temperature of 80 ℃ for 3h to finally obtain the carbon fiber-PVDF piezoelectric core-spun yarn.
TABLE 1 Performance test results for first to sixth core spun yarns of examples
Examples | Core spun yarn piezoelectric range | Performance of core spun yarn |
Example one | -6.5v-6.5v | The PVDF has moderate cladding and better evenness |
Example two | -4.5v-4.5v | The PVDF has thin coating and moderate yarn evenness |
EXAMPLE III | -10v-10v | The PVDF has thicker cladding and better evenness of yarn |
Example four | -7v-7v | The PVDF has thin coating and moderate yarn evenness |
EXAMPLE five | -8.5v-8.5v | The PVDF has thick coating and moderate evenness |
EXAMPLE six | -6v-6v | The PVDF has moderate cladding and poor evenness of yarn |
The above description is only exemplary of the present invention and should not be taken as limiting, and all equivalent modifications, equivalents, and improvements made within the spirit of the present invention should be included in the scope of the present invention.
Claims (4)
1. A method for preparing piezoelectric PVDF (polyvinylidene fluoride) coated carbon fibers by using an electrostatic spinning technology sequentially comprises the following steps:
1) cleaning a reaction vessel and magnetons with deionized water, drying, mixing polyvinylidene fluoride (PVDF) serving as a spinning solution solute and N, N-Dimethylformamide (DMF) serving as a solvent in the reaction vessel, adding the magnetons into the mixed solution to seal the mixed solution, slowly heating the sealed reaction vessel in a water bath kettle, stirring by using a magneton stirring device, and then standing and cooling to obtain a spinning solution;
2) extracting the spinning solution obtained in the step 1) by using an injector, fixing the injector in an injection pump, adjusting electrostatic spinning parameters, connecting a spinning nozzle with a high-voltage positive electrode and a high-voltage negative electrode respectively, accelerating the solution at the top point of a Taylor cone of the spinning nozzle under the action of an electric field force, and finally overcoming surface tension through enough electric field force to spray a trickle, wherein the trickle forms a fiber net at a horn mouth. Meanwhile, after the carbon fiber passes through the bell mouth, the carbon fiber is pulled out from the PVDF fiber net by the winding roller, so that the piezoelectric PVDF is uniformly coated on the carbon fiber through the rotary bell mouth and finally collected by the winding roller, and the core-spun yarn which takes the carbon fiber as the core yarn and is coated by the piezoelectric PVDF is obtained;
3) putting the core-spun yarn prepared in the step 2) into an oven for drying, and finally obtaining the carbon fiber-PVDF piezoelectric core-spun yarn.
2. The method for preparing the piezoelectric PVDF-coated carbon fiber by the electrostatic spinning technology as claimed in claim 1, wherein the temperature of the water bath kettle is 60-80 ℃, the stirring time of the magnetons is 4-5 h, and the concentration of PVDF in the spinning solution is 8-12%.
3. The method for preparing piezoelectric PVDF-coated carbon fiber by electrospinning technique according to claim 1, wherein the electrospinning parameters are as follows: the extrusion speed of the spinning solution is 0.3 ml/h-0.7 ml/h, the spinning distance is 6 cm-10 cm, the distance of double needles is 10 cm-15 cm, the spinning voltage is 4 KV-5 KV, the rotating speed of a winding roller is 0.02 mm/s-0.2 mm/s, the rotating speed of a bell mouth is 300 rpm-800 rpm, the ambient temperature of electrostatic spinning is 20 +/-2 ℃, and the relative humidity is 60 +/-5%.
4. The method for preparing the piezoelectric PVDF-coated carbon fiber by the electrospinning technology according to claim 1, wherein the drying temperature is 80-100 ℃, and the drying time is 2-5 h.
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CN112223879A (en) * | 2020-08-19 | 2021-01-15 | 西安工程大学 | Preparation method of piezoelectric PVDF (polyvinylidene fluoride) fiber membrane reinforced composite material capable of self diagnosis |
CN112226867A (en) * | 2020-08-19 | 2021-01-15 | 西安工程大学 | Method for preparing super-soft piezoelectric PVDF yarn |
CN112736188A (en) * | 2020-12-21 | 2021-04-30 | 西安交通大学 | Electric auxiliary preparation device and method for piezoelectric functional fiber |
CN113831687A (en) * | 2021-09-26 | 2021-12-24 | 西安工程大学 | Preparation method of piezoelectric yarn reinforced resin matrix composite material |
CN114075707A (en) * | 2021-10-26 | 2022-02-22 | 西安理工大学 | Preparation method of flexible wet-spun piezoelectric-conductive core-spun yarn |
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CN113831687B (en) * | 2021-09-26 | 2023-07-21 | 西安工程大学 | Preparation method of piezoelectric yarn reinforced resin matrix composite material |
CN114075707A (en) * | 2021-10-26 | 2022-02-22 | 西安理工大学 | Preparation method of flexible wet-spun piezoelectric-conductive core-spun yarn |
CN115302807A (en) * | 2022-09-06 | 2022-11-08 | 西安工程大学 | Preparation method of epoxy reversible resin-based three-dimensional braided hybrid structure composite material |
CN115948834A (en) * | 2022-12-27 | 2023-04-11 | 江苏臻圈科技有限公司 | High-sensitivity intelligent sensing yarn with imitated caterpillar structure and preparation method |
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