CN115850779A - Preparation method of polyvinylidene fluoride ferroelectric film with micro-nano array structure, product and application thereof - Google Patents
Preparation method of polyvinylidene fluoride ferroelectric film with micro-nano array structure, product and application thereof Download PDFInfo
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- CN115850779A CN115850779A CN202211539689.6A CN202211539689A CN115850779A CN 115850779 A CN115850779 A CN 115850779A CN 202211539689 A CN202211539689 A CN 202211539689A CN 115850779 A CN115850779 A CN 115850779A
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- 239000002033 PVDF binder Substances 0.000 title claims abstract description 44
- 229920002981 polyvinylidene fluoride Polymers 0.000 title claims abstract description 44
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- 230000005684 electric field Effects 0.000 claims abstract description 41
- 229920000131 polyvinylidene Polymers 0.000 claims abstract description 37
- XLOFNXVVMRAGLZ-UHFFFAOYSA-N 1,1-difluoroethene;1,1,2-trifluoroethene Chemical group FC(F)=C.FC=C(F)F XLOFNXVVMRAGLZ-UHFFFAOYSA-N 0.000 claims abstract description 35
- 238000000034 method Methods 0.000 claims abstract description 18
- 239000000758 substrate Substances 0.000 claims abstract description 18
- 239000000843 powder Substances 0.000 claims abstract description 16
- 238000010438 heat treatment Methods 0.000 claims abstract description 14
- 238000001035 drying Methods 0.000 claims abstract description 8
- 239000003960 organic solvent Substances 0.000 claims abstract description 7
- 238000003756 stirring Methods 0.000 claims abstract description 7
- 229920005601 base polymer Polymers 0.000 claims abstract description 6
- 239000010408 film Substances 0.000 claims description 49
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 33
- 239000010409 thin film Substances 0.000 claims description 14
- 238000003860 storage Methods 0.000 claims description 4
- 229920000642 polymer Polymers 0.000 claims description 3
- 229920005569 poly(vinylidene fluoride-co-hexafluoropropylene) Polymers 0.000 claims description 2
- 230000000052 comparative effect Effects 0.000 description 9
- 239000002086 nanomaterial Substances 0.000 description 9
- 230000001276 controlling effect Effects 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 238000010894 electron beam technology Methods 0.000 description 3
- 230000001105 regulatory effect Effects 0.000 description 3
- 230000003287 optical effect Effects 0.000 description 2
- 238000000059 patterning Methods 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- 238000001338 self-assembly Methods 0.000 description 2
- 229920001486 SU-8 photoresist Polymers 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000000609 electron-beam lithography Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 238000010884 ion-beam technique Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000004377 microelectronic Methods 0.000 description 1
- 230000010287 polarization Effects 0.000 description 1
- 238000004528 spin coating Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000002344 surface layer Substances 0.000 description 1
- 238000000233 ultraviolet lithography Methods 0.000 description 1
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Abstract
The invention discloses a preparation method of a poly (vinylidene fluoride-trifluoroethylene) ferroelectric film with a micro-nano array structure, which comprises the following steps: (1) Dissolving polyvinylidene fluoride base polymer powder in an organic solvent, and stirring until the polyvinylidene fluoride base polymer powder is completely dissolved to obtain a uniform transparent solution; (2) Dripping the uniform transparent solution obtained in the step (1) on a conductive substrate, drying, and removing the organic solvent to obtain a transparent polyvinylidene fluoride-based film; (3) And (3) applying an electric field on the needle point while carrying out heat treatment on the polyvinylidene fluoride base film obtained in the step (2) to enable the polyvinylidene fluoride base film to break down air to form a corona electric field, and applying the electric field on conductive grids with different patterns to regulate redistribution of the corona electric field to prepare the polyvinylidene fluoride base ferroelectric film with the micro-nano array structure. The preparation method provided by the invention has the advantages of simple process, controllable process, low cost and strong practicability, and the prepared poly (vinylidene fluoride-trifluoroethylene) has a clear micro-nano array structure.
Description
Technical Field
The invention belongs to the technical field of micro-nano manufacturing, and particularly relates to a preparation method of a polyvinylidene fluoride base ferroelectric film with a micro-nano array structure, a product and application thereof.
Background
With the rapid development of society, ferroelectric materials have more and more important applications in the technical fields of energy conversion and collection, microelectronics, biosensing, ferroelectric storage and the like. Poly (vinylidene fluoride-trifluoroethylene) (P (VDF-TrFE)) as a classical high-molecular ferroelectric material has good ferroelectric performance, and has the characteristics of good flexibility, stable chemical property, easiness in processing, easiness in integration and the like. Based on the excellent properties of the P (VDF-TrFE) ferroelectric film, the P (VDF-TrFE) ferroelectric film has great application value and advantages in the aspects of energy collection, biosensing, information storage and the like.
Aiming at the application fields of different P (VDF-TrFE) ferroelectric films, different micro-nano array structures are required to be adopted. In addition, many novel techniques for preparing micro-nano structures are developed to meet the development requirements of small size, high density and high performance of ferroelectric devices. Such as electron beam lithography, ultraviolet lithography, focused ion beam, and self-assembly. For example, chinese patent publication No. CN111646428a discloses a method for constructing a 3D micro/nano structure, which comprises the following steps: fixing a material source on a substrate, and vacuumizing; (2) Focusing the focus of the electron beam at the position of 0-100nm of the surface of the material source in the step (1) to form an interface local area containing the focus of the electron beam and surface layer atoms; (3) And controlling the focus of the electron beam to move point by point according to the designed 3D micro/nano structure, and realizing the construction of the 3D micro/nano structure. For example, a method for preparing a self-assembled three-dimensional micro-nano structure is disclosed in a Chinese patent with publication number CN111694219A, and belongs to the technical field of self-assembly. The method comprises the following steps: surface pretreatment; spin-coating SU-8 photoresist; pre-baking; aligning and exposing; postbaking; developing; secondary glue homogenizing; pre-baking; carrying out secondary exposure; postbaking; carrying out secondary development; and transferring and self-assembling to obtain the self-assembled three-dimensional micro-nano structure.
However, the application of the above process techniques is significantly limited either by high costs or by uncontrolled processes. Therefore, the development of a micro-nano structure preparation technology with low cost and simple process has very important value and significance.
Disclosure of Invention
The invention aims to provide a preparation method of a polyvinylidene fluoride-based ferroelectric film with a micro-nano array structure, and the preparation method provided by the invention has the advantages of simple process and low cost.
The invention provides the following technical scheme:
a preparation method of a polyvinylidene fluoride-based ferroelectric film with a micro-nano array structure is characterized by comprising the following steps:
(1) Dissolving polyvinylidene fluoride base polymer powder in an organic solvent, and stirring until the polyvinylidene fluoride base polymer powder is completely dissolved to obtain a uniform transparent solution;
(2) Dripping the uniform transparent solution obtained in the step (1) on a conductive substrate, drying, and removing the organic solvent to obtain a transparent polyvinylidene fluoride-based film;
(3) And (3) applying an electric field on the needle point while carrying out heat treatment on the polyvinylidene fluoride base film obtained in the step (2) to enable the polyvinylidene fluoride base film to break down air to form a corona electric field, and applying the electric field on conductive grids with different patterns to regulate redistribution of the corona electric field to prepare the polyvinylidene fluoride base ferroelectric film with the micro-nano array structure.
According to the preparation method provided by the invention, a corona electric field is introduced in the heat treatment process and a conductive grid is combined, so that the micro patterning of the polyvinylidene fluoride base ferroelectric film is realized.
Preferably, in step (1), the organic solvent is N, N-dimethylformamide; in the step (2), drying is carried out for 6h at 80 ℃; in the step (3), an electric field is applied to the conductive grids with different patterns to regulate the redistribution of the corona electric field, and the non-uniform corona electric field causes the polyvinylidene fluoride-based polymer to generate non-uniform flow and deformation, so that the patterning of the film is driven.
Preferably, in step (1), 0.8 to 1.2g of polyvinylidene fluoride-based polymer powder is dissolved in 10mL of N, N-dimethylformamide.
Preferably, in the step (3), the heat treatment temperature of the polyvinylidene fluoride-based film is 160-200 ℃, and the heat treatment time is 0.5-1 h.
Preferably, in the step (3), the distance between the needle point and the conductive substrate during the heat treatment is 10-20 mm, the electric field intensity applied to the needle point is 5-10 kV/cm, the distance between the conductive mesh and the conductive substrate is 2-10 mm, and the electric field intensity applied to the conductive mesh is 5-15 kV/cm.
The polyvinylidene fluoride base ferroelectric film is a poly (vinylidene fluoride-trifluoroethylene) ferroelectric film, a polyvinylidene fluoride-trifluoroethylene-chlorofluoroethylene ferroelectric film and a polyvinylidene fluoride-hexafluoropropylene ferroelectric film.
The invention also provides the polyvinylidene fluoride base ferroelectric film with the micro-nano array structure prepared by the preparation method.
Due to the special microstructure on the surface and the improved ferroelectric property, the invention also provides the polyvinylidene fluoride base ferroelectric film with the micro-nano array structure, which has very important application in the preparation of products in the fields of energy collection, biosensing, ferroelectric storage and the like.
The preparation method provided by the invention regulates and controls the redistribution of the corona electric field by applying the conductive mesh with certain electric field intensity, so that uneven electric field force is generated on the polyvinylidene fluoride base film to induce and form a specific micro-nano structure; and the polyvinylidene fluoride base ferroelectric film with different micro-nano structures can be obtained by changing the pattern of the conductive mesh.
The preparation method provided by the invention has the advantages of simple process, controllable process, low cost and strong practicability, and the prepared polyvinylidene fluoride-based ferroelectric film has a clear micro-nano array structure.
Drawings
FIG. 1 is a schematic view of an apparatus for preparing a poly (vinylidene fluoride-trifluoroethylene) ferroelectric thin film in examples 1 to 3;
FIG. 2 is a conductive grid used in examples 1-3;
FIG. 3 is an optical photograph of a poly (vinylidene fluoride-trifluoroethylene) ferroelectric thin film prepared in example 3;
fig. 4 is an SEM image of the poly (vinylidene fluoride-trifluoroethylene) ferroelectric thin films prepared in comparative example 1 and example 3:
FIG. 5 is an XRD pattern of the poly (vinylidene fluoride-trifluoroethylene) ferroelectric thin films prepared in comparative example 1 and example 3;
fig. 6 is a hysteresis chart of the poly (vinylidene fluoride-trifluoroethylene) ferroelectric thin films prepared in comparative example 1 and example 3.
Detailed Description
The technical scheme of the invention is further explained by combining specific examples.
Example 1
(1) Dissolving 0.8g of poly (vinylidene fluoride-trifluoroethylene) powder in 10mL of N, N-dimethylformamide, and continuously stirring for 6 hours at room temperature until the poly (vinylidene fluoride-trifluoroethylene) powder is completely dissolved to obtain a uniform and transparent solution;
(2) Dripping the uniform transparent solution obtained in the step (1) on a conductive substrate, drying at 80 ℃ for 6h, and removing N, N-dimethylformamide in the solution to obtain a transparent poly (vinylidene fluoride-trifluoroethylene) film;
(3) Carrying out heat treatment on the poly (vinylidene fluoride-trifluoroethylene) film obtained in the step (2) at 160 ℃ for 0.5h, and simultaneously applying an electric field with the electric field intensity of 6kV/cm to a needle point 18mm away from the conductive substrate to break down air to form a corona electric field; and applying an electric field with the electric field intensity of 7.5kV/cm on a conductive grid 5mm away from the conductive substrate, regulating and controlling the redistribution of the corona electric field, and preparing the poly (vinylidene fluoride-trifluoroethylene) ferroelectric film with the micro-nano array structure.
Example 2
(1) Dissolving 1.2g of poly (vinylidene fluoride-trifluoroethylene) powder in 10mL of N, N-dimethylformamide, and continuously stirring for 6 hours at room temperature until the poly (vinylidene fluoride-trifluoroethylene) powder is completely dissolved to obtain a uniform and transparent solution;
(2) Dripping the uniform transparent solution obtained in the step (1) on a conductive substrate, drying at 80 ℃ for 6h, and removing N, N-dimethylformamide in the solution to obtain a transparent poly (vinylidene fluoride-trifluoroethylene) film;
(3) Carrying out heat treatment on the poly (vinylidene fluoride-trifluoroethylene) film obtained in the step (2) at 200 ℃ for 1h, and applying an electric field with the electric field intensity of 7kV/cm to a needle point 18mm away from the conductive substrate to enable the film to break down air to form a corona electric field; and applying an electric field with the electric field intensity of 8.75kV/cm on a conductive grid 5mm away from the conductive substrate, regulating and controlling the redistribution of the corona electric field, and preparing the poly (vinylidene fluoride-trifluoroethylene) ferroelectric film with the micro-nano array structure.
Example 3
(1) Dissolving 1g of poly (vinylidene fluoride-trifluoroethylene) powder in 10mL of N, N-dimethylformamide, and continuously stirring for 6 hours at room temperature until the poly (vinylidene fluoride-trifluoroethylene) powder is completely dissolved to obtain a uniform and transparent solution;
(2) Dripping the uniform transparent solution obtained in the step (1) on a conductive substrate, drying at 80 ℃ for 6h, and removing N, N-dimethylformamide in the solution to obtain a transparent poly (vinylidene fluoride-trifluoroethylene) film;
(3) Carrying out heat treatment on the poly (vinylidene fluoride-trifluoroethylene) film obtained in the step (2) at 180 ℃ for 1h, and simultaneously applying an electric field with the electric field intensity of 8kV/cm to a needle point 18mm away from the conductive substrate to break down air to form a corona electric field; and applying an electric field with the electric field intensity of 10kV/cm on a conductive grid 5mm away from the conductive substrate, regulating and controlling the redistribution of the corona electric field, and preparing the poly (vinylidene fluoride-trifluoroethylene) ferroelectric film with the micro-nano array structure.
Comparative example 1
(1) Dissolving 1g of poly (vinylidene fluoride-trifluoroethylene) powder in 10mL of N, N-dimethylformamide, and continuously stirring for 6 hours at room temperature until the poly (vinylidene fluoride-trifluoroethylene) powder is completely dissolved to obtain a uniform and transparent solution;
(2) Dripping the uniform transparent solution obtained in the step (1) on a conductive substrate, drying at 80 ℃ for 6h, and removing N, N-dimethylformamide in the solution to obtain a transparent poly (vinylidene fluoride-trifluoroethylene) film;
(3) And (3) carrying out heat treatment on the poly (vinylidene fluoride-trifluoroethylene) film obtained in the step (2) for 1h at the temperature of 180 ℃.
As shown in fig. 1, a poly (vinylidene fluoride-trifluoroethylene) ferroelectric thin film having a micro-nano array structure was prepared by the apparatus of fig. 1 in the above examples 1 to 3.
The conductive grids used in examples 1-3 above are shown in figure 2.
FIG. 3 is an optical photograph of the poly (vinylidene fluoride-trifluoroethylene) ferroelectric thin film prepared in example 3, wherein the size of the surface structure is similar to that of the mesh of the conductive mesh.
Fig. 4 is an SEM image of the poly (vinylidene fluoride-trifluoroethylene) ferroelectric thin films prepared in comparative example 1 and example 3, and it can be seen from fig. 4 that the poly (vinylidene fluoride-trifluoroethylene) ferroelectric thin film prepared in example 3 forms smaller-sized and more platelets on the surface than that of comparative example 1.
Fig. 5 is XRD of the poly (vinylidene fluoride-trifluoroethylene) ferroelectric thin films prepared in comparative example 1 and example 3, and it can be found that the phase structure thereof is not changed by the preparation method.
Fig. 6 is hysteresis curves of the poly (vinylidene fluoride-trifluoroethylene) ferroelectric thin films prepared in comparative example 1 and example 3, and it can be found that the remanent polarization is significantly increased and the coercive field strength is significantly reduced in example 3 compared with comparative example 1.
Claims (8)
1. A preparation method of a polyvinylidene fluoride-based ferroelectric film with a micro-nano array structure is characterized by comprising the following steps:
(1) Dissolving polyvinylidene fluoride base polymer powder in an organic solvent, and stirring until the polyvinylidene fluoride base polymer powder is completely dissolved to obtain a uniform transparent solution;
(2) Dripping the uniform transparent solution obtained in the step (1) on a conductive substrate, drying, and removing the organic solvent to obtain a transparent polyvinylidene fluoride-based film;
(3) And (3) applying an electric field on the needle point while carrying out heat treatment on the polyvinylidene fluoride base film obtained in the step (2) to enable the polyvinylidene fluoride base film to break down air to form a corona electric field, and applying the electric field on conductive grids with different patterns to regulate redistribution of the corona electric field to prepare the polyvinylidene fluoride base ferroelectric film with the micro-nano array structure.
2. A method for preparing a polyvinylidene fluoride ferroelectric thin film with a micro-nano array structure according to claim 1, wherein in step (1), 0.8-1.2 g of polyvinylidene fluoride based polymer powder is dissolved in 10ml of n, n-dimethylformamide.
3. The preparation method of a polyvinylidene fluoride ferroelectric thin film with a micro-nano array structure according to claim 1, characterized in that in step (3), the temperature condition of the polyvinylidene fluoride thin film heat treatment is 160-200 ℃, and the treatment time of the heat treatment is 0.5-1 h.
4. The preparation method of a polyvinylidene fluoride-based ferroelectric film with a micro-nano array structure according to claim 1, wherein in the step (3), the distance between the needle point and the conductive substrate in the heat treatment process is 10-20 mm.
5. The method for preparing a polyvinylidene fluoride ferroelectric film with a micro-nano array structure according to claim 1, wherein in step (3), the electric field intensity applied to the needle point is 5-10 kV/cm, the distance between the conductive mesh and the conductive substrate is 2-10 mm, and the electric field intensity applied to the conductive mesh is 5-15 kV/cm.
6. The method for preparing a polyvinylidene fluoride ferroelectric film with a micro-nano array structure according to claim 1, wherein the polyvinylidene fluoride ferroelectric film is a poly (vinylidene fluoride-trifluoroethylene) ferroelectric film, a polyvinylidene fluoride-trifluoroethylene-chlorofluoroethylene ferroelectric film, a polyvinylidene fluoride-hexafluoropropylene ferroelectric film.
7. A polyvinylidene fluoride-based ferroelectric film with a micro-nano array structure prepared by the preparation method of any one of claims 1 to 6.
8. Application of the polyvinylidene fluoride-based ferroelectric film with the micro-nano array structure in preparation of products for energy collection, biosensing or ferroelectric storage according to claim 7.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1937274A (en) * | 2005-09-23 | 2007-03-28 | 清华大学 | Ferroelectric domain array structure, and its preparing method and ferroelectric film having same |
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| US20220069198A1 (en) * | 2020-09-01 | 2022-03-03 | Korea Advanced Institute Of Science And Technology | Method of preparing shape-reconfigurable micropatterned polymer haptic material using electric field technique |
| CN115043374A (en) * | 2022-05-18 | 2022-09-13 | 南昌大学 | Method for preparing micro-nano composite structure by droplet forming method based on electric field effect |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1937274A (en) * | 2005-09-23 | 2007-03-28 | 清华大学 | Ferroelectric domain array structure, and its preparing method and ferroelectric film having same |
| CN101880430A (en) * | 2010-06-22 | 2010-11-10 | 浙江大学 | Machining method for conductive polymer micro-nano linear array |
| US20170310087A1 (en) * | 2016-04-20 | 2017-10-26 | Areesys Technologies, Inc. | Controlled Thin-Film Ferroelectric Polymer Corona Polarizing System and Process |
| US20220069198A1 (en) * | 2020-09-01 | 2022-03-03 | Korea Advanced Institute Of Science And Technology | Method of preparing shape-reconfigurable micropatterned polymer haptic material using electric field technique |
| CN115043374A (en) * | 2022-05-18 | 2022-09-13 | 南昌大学 | Method for preparing micro-nano composite structure by droplet forming method based on electric field effect |
Non-Patent Citations (1)
| Title |
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