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Preparation method of MgCl2-doped annular gamma-phase polyvinylidene-fluoride-base composite film

The technology of polyvinylidene fluoride and vinylidene fluoride is applied in the field of preparation of γ-phase polyvinylidene fluoride-based composite films, which can solve the problems of decreasing and shortening the service life of γ-phase polyvinylidene fluoride film materials, and achieves low-cost and easy-to-obtain raw materials. Excellent electrical properties, easy to operate

Active Publication Date: 2016-10-12
SHAANXI UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] In order to overcome above-mentioned deficiencies in the prior art, the object of the present invention is to provide a kind of MgCl 2 The preparation method of the doped annular gamma-phase polyvinylidene fluoride-based composite membrane can quickly obtain high-content and special-morphology gamma-type polyvinylidene fluoride, which reduces the need for long-term high-temperature cultivation to prepare gamma-phase polyvinylidene fluoride membrane materials. The technical disadvantage of reduced service life; it has the characteristics of simple and easy operation, cheap and easy-to-obtain raw materials, short production cycle, easy processing, and strong operability.

Method used

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  • Preparation method of MgCl2-doped annular gamma-phase polyvinylidene-fluoride-base composite film
  • Preparation method of MgCl2-doped annular gamma-phase polyvinylidene-fluoride-base composite film
  • Preparation method of MgCl2-doped annular gamma-phase polyvinylidene-fluoride-base composite film

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Embodiment 1

[0015] 1) MgCl 2 Use a mortar to grind the powder into particles with an average particle size of 0.5 μm, weigh polyvinylidene fluoride pellets with a mass average molecular weight of 107,000, and prepare a 5% polyvinylidene fluoride with N,N dimethylformamide (DMF) as a solvent. Polyvinylidene fluoride / MgCl with different mass ratios 2 Blending solution, the blending ratio is 100:0;

[0016] 2) Use the spin coating method on a hot stage at 80°C to make the blended solution in step 1) into a blended film with a thickness of 0.5 μm, and cut the blended film into a film with a size of 10 mm×10 mm×0.5 μm, It is sandwiched between two transparent glass plates with a size of 15mm×15mm×1mm to make a blended film with a sandwich structure;

[0017] 3) Melt the blended film prepared in step 2) on a constant temperature hot stage at 200°C for 5 minutes to eliminate the heat history, cool down to 150°C at a rate of 50°C / min for isothermal crystallization for 8 hours, and apply a press...

Embodiment 2

[0020] 1) MgCl 2 Use a mortar to grind the powder into particles with an average particle size of 0.5 μm, weigh polyvinylidene fluoride pellets with a mass average molecular weight of 107,000, and prepare a 5% polyvinylidene fluoride with N,N dimethylformamide (DMF) as a solvent. Polyvinylidene fluoride / MgCl with different mass ratios 2 Blending solution, the blending ratio is 99:1;

[0021] 2) Use the spin coating method on a hot stage at 80°C to make the blended solution in step 1) into a blended film with a thickness of 0.5 μm, and cut the blended film into a film with a size of 10 mm×10 mm×0.5 μm, It is sandwiched between two transparent glass plates with a size of 15mm×15mm×1mm to form a sandwich structure;

[0022] 3) Melt the blended film prepared in 2) on a constant temperature hot stage at 210°C for 5 minutes to eliminate the heat history, cool down to 155°C at a rate of 50°C / min for isothermal crystallization for 6 hours, and apply a pressure of 5 MPa to blend The...

Embodiment 3

[0025] 1) MgCl 2 Use a mortar to grind the powder into particles with an average particle size of 0.5 μm, weigh polyvinylidene fluoride pellets with a mass average molecular weight of 107,000, and prepare a 5% polyvinylidene fluoride with N,N dimethylformamide (DMF) as a solvent. Polyvinylidene fluoride / MgCl with different mass ratios 2 Blending solution, the blending ratio is 95:5;

[0026] 2) Use the spin coating method on a hot stage at 80°C to make the blended solution in step 1) into a blended film with a thickness of 0.5 μm, and cut the blended film into a film with a size of 10 mm×10 mm×0.5 μm, It is sandwiched between two transparent glass plates with a size of 15mm×15mm×1mm to form a sandwich structure;

[0027] 3) Melt the blended film prepared in 2) on a constant temperature hot stage at 220°C for 5 minutes to eliminate the heat history, then cool down to 160°C at a rate of 50°C / min for isothermal crystallization for 4 hours, and apply a pressure of 5 MPa to a tot...

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Abstract

The invention relates to a preparation method of an MgCl2-doped annular gamma-phase polyvinylidene-fluoride-base composite film. The preparation method comprises the following steps: 1) preparing a polyvinylidene fluoride / MgCl2 blend solution by using N,N-dimethylformamide (DMF) as a solvent; 2) preparing blend solutions with different mass percents into films on a hot stage, sandwiching each film between two transparent glass plates to prepare a sandwich structure; 3) eliminating the heat history of the blend films with different mass percents in the step 2), carrying out cooling and isothermal crystallization, and applying until the blend films completely crystallize; and 4) characterizing the gamma crystal form and gamma crystal form topographic characteristics of the blend films by using an infrared spectroscopy, a Raman spectroscopy, a differential scanning calorimeter, a polarized light microscope, a scanning electron microscope and other means. The method has the advantages of simple main technique and short preparation period, is convenient to operate, and can prepare the gamma-polyvinylidene-fluoride-base composite film with large size and special annular shape; and the gamma-polyvinylidene fluoride has the unique electric properties different from alpha-polyvinylidene fluoride.

Description

technical field [0001] The invention belongs to the technical field of preparation of gamma-phase polyvinylidene fluoride-based composite films, and in particular relates to a method for preparing an annular gamma-phase polyvinylidene fluoride-based composite film doped with MgCl2. Background technique [0002] The functionalization of polymer thin film materials has always been the development trend of thin film materials, among which polymer materials with special properties have been continuously developed in terms of further modification and improvement of their properties. [0003] As a flexible piezoelectric material, polyvinylidene fluoride has the characteristics of small size, chemical corrosion resistance, weather resistance, high dielectric strength, and long service life. Polyvinylidene fluoride with a variety of crystal forms The reported crystal forms mainly include α, β and γ three crystal forms. Among them, the β and γ phase crystal forms of polyvinylidene fl...

Claims

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Application Information

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IPC IPC(8): C08L27/16C08K9/00C08K3/16
CPCC08J5/18C08J2327/16C08K3/16C08K9/00C08K2003/166C08K2201/003C08L2203/16C08L2203/20C08L27/16
Inventor 王海军王帅毅高治进李镇伟阮潇潇
Owner SHAANXI UNIV OF SCI & TECH
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