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Method for preparing high-oriented gamma phase polyvinylidene fluoride PVDF thin film

A technology of polyvinylidene fluoride and vinylidene fluoride is applied in the field of preparing high-orientation γ-phase polyvinylidene fluoride PVDF film, which can solve the problems of lack of γ-crystal phase, high price, low crystallinity and melting point, etc.

Inactive Publication Date: 2013-05-22
SHAANXI UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] However, the γ crystal phase needs a small degree of undercooling to be obtained. Through melting high-temperature crystallization or high-temperature annealing methods, even at a small degree of undercooling due to the low nucleation and growth rates, a large amount of γ cannot be obtained. crystalline phase, and α crystalline phase also exists in large quantities; the method of successfully preparing γ-type PVDF nanoarray whiskers by anodized alumina template solution infiltration method, due to high technical requirements, high price, and little use value; and adding a small amount The gamma thin films obtained by nucleating agents such as KBr have low crystallinity and melting point
There are also some methods of preparing gamma thin films such as micro-imprinting technology, which also have the disadvantages of the above methods.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] A method for preparing highly oriented γ-phase polyvinylidene fluoride PVDF film, comprising the following steps:

[0016] 1) First, heat the polyvinylidene fluoride PVDF solution-cast film to 200°C for 10 minutes to eliminate the heat history, and then rapidly cool the polyvinylidene fluoride PVDF film to 170°C at a rate of 50°C / min;

[0017] 2) Utilize a polymethylsiloxane plate to apply 10 5 Pa pressure applies shear stress to the melt at a shear rate of 1.5m / s, and after standing at 170°C for 96 hours, the γ-phase PVDF film can be obtained, and the crystallization process of the melt in the shear stress field is observed under a polarizing microscope and the crystal structure after crystallization;

[0018] 3) Analyze the crystal structure and morphology of the columnar crystals after crystallization by infrared spectrum FTIR, scanning electron microscope SEM, transmission electron microscope TEM, differential scanning calorimeter DSC and other characterization met...

Embodiment 2

[0021] A method for preparing highly oriented γ-phase polyvinylidene fluoride PVDF film, comprising the following steps:

[0022] 1) First, heat the polyvinylidene fluoride PVDF solution-cast film to 205 °C for 10 minutes to eliminate the heat history, and then rapidly cool the polyvinylidene fluoride PVDF film to 165 °C at a rate of 50 °C / min;

[0023] 2) Utilize a polymethylsiloxane plate to apply 10 5 Pa pressure applies shear stress to the melt at a shear rate of 2.0m / s, and after standing at 165°C for 72 hours, the γ-phase PVDF film can be obtained, and the crystallization process of the melt in the shear stress field is observed under a polarizing microscope and the crystal structure after crystallization;

[0024] 3) Analyze the crystal structure and morphology of PVDF columnar crystals by means of FTIR infrared spectroscopy, scanning electron microscope SEM, transmission electron microscope TEM, and differential scanning calorimeter DSC to verify the crystal form of c...

Embodiment 3

[0027] A method for preparing highly oriented γ-phase polyvinylidene fluoride PVDF film, comprising the following steps:

[0028] 1) First, heat the polyvinylidene fluoride PVDF solution-cast film to 195°C for 10 minutes to eliminate the heat history, and then rapidly cool the polyvinylidene fluoride PVDF film to 160°C at a rate of 50°C / min;

[0029] 2) Utilize a polymethylsiloxane plate to apply 10 5 Pa pressure applies shear stress to the melt at a shear rate of 0.6m / s, and the α-phase PVDF film can be obtained after standing at 160°C for 48 hours. After 2 days of crystallization, continue annealing at 160°C for 120h to obtain α The γ-phase thin film after phase transition, observe the crystallization process of the melt in the shear stress field and the crystal structure after crystallization under a polarizing microscope;

[0030] 3) Analyze the crystal structure and morphology of the columnar crystals after crystallization by infrared spectrum FTIR, scanning electron mic...

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PUM

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Abstract

The invention relates to a method for preparing a high-oriented gamma phase polyvinylidene fluoride PVDF thin film. The method comprises the following steps of: 1) first, casting a thin film for PVDF liquor to heat, insulate and eliminate thermal history, and quickly cooling the PVDF thin film at 50 DEG C / min to 160-170 DEG C; and 2) applying pressure to melt by a polymethylsiloxane plate to apply a shear stress, standing at 160-170 DEG C, wherein the crystallizing form at 160-163 DEG C is converted to alpha crystallizing form, and conversion from alpha crystallizing form to gamma crystallizing form occurs at 168-170 DEG C; the crystallizing crystal nucleus is alpha crystal nucleus at 164-167 DEG C, and the crystallizing form at 168-170 DEG C is gamma crystallizing form. A polarizing microscope, a scanning electron microscope and an infrared spectrometer represent crystallization of the melt in a shear stress field and a crystal structure after crystallization, so that the method is simple in process, and simple, convenient and accessible, and the problem that pure gamma phase PVDF thin film cannot be obtained by isothermal crystallization is solved. The gamma phase PVDF thin film which is high in purity, high in orientation and excellent in thermodynamic property can be prepared.

Description

technical field [0001] The invention belongs to the technical field of polyvinylidene fluoride PVDF film preparation, and in particular relates to a method for preparing highly oriented γ-phase polyvinylidene fluoride PVDF film. Background technique [0002] Polyvinylidene fluoride PVDF combines the characteristics of general-purpose resins and fluororesins. In addition to good high temperature resistance, chemical corrosion resistance, oxidation resistance, radiation resistance, and weather resistance, it also has piezoelectricity, dielectricity, Special properties such as pyroelectricity are currently the second largest products in the output of fluorine-containing plastic films. [0003] The diverse performance of PVDF is closely related to its complex and variable crystal structure (α, β, γ, δ, and ε are equal), and various crystal forms can be transformed into each other under certain conditions. However, people generally pay attention to the three crystal forms of α, ...

Claims

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Application Information

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IPC IPC(8): C08J5/18C08L27/16
Inventor 王海军赵庭山王学川冯会平李文举
Owner SHAANXI UNIV OF SCI & TECH
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